Crystal structures and supra­molecular inter­actions of prism[6]arene-based host–guest systems with dihalohexa­nes

An investigation is reported of the crystal structures, Hirshfeld surface analysis and supra­molecular inter­actions of pereth­oxy prism[6]arene:di­chloro­hexane and pereth­oxy prism[6]arene:di­iodo­hexane host–guest systems.

Synthesis and structural characterization of the dichloride complex formed by carb­oxy-functionalized Cu(di­aza­cyclam)²⁺ cation and its heterometallic coordination polymer with CdCl₂

The coordination polyhedra of the Cu^II ions in mol­ecular complex I and coordination polymer II represent tetra­gonally elongated trans-CuN₄Cl₂ and trans-CuN₄(H₂O)Cl octa­hedra, respectively, with the four N atoms of the macrocyclic ligand forming the equatorial plane and monodentate ligands occupying the axial positions. The coordination polyhedron of the Cd^II ion in II is a CdO₄Cl₂ distorted octa­hedron formed by two bidentately coordinated deprotonated carb­oxy­lic groups of different Cu^II macrocyclic cations and two chloride anions, one of which displays a bridging function.

Synthesis, crystal structure and Hirshfeld surface analysis of 1,1′-[oxybis(ethane-2,1-di­yl)]bis­(2-methyl­sulfanyl-1H-benzo[d]imidazole)

In the title compound, the terminal benzimidazole moieties are inclined to one another by about 68°. In the crystal, tetra­molecular strands are generated by C—H⋯N hydrogen bonds and C—H⋯π(ring) inter­actions and are linked by C—H⋯π(ring) and π-stacking inter­actions.

Synthesis and crystal structure of 3-(2-{3-[2-(2-oxooxazolidin-3-yl)eth­oxy]quinoxalin-2-yl­oxy}eth­yl)oxazolidin-2-one

In the title compound, one of the oxazolidine rings adopts a twisted conformation and the other is a shallow envelope. In the crystal, weak C—H⋯O hydrogen bonds and π–π stacking inter­actions help to consolidate a three-dimensional architecture.

Crystal structure and Hirshfeld surface analysis of (E)-2-cyano-N′-(3,4,5-tri­meth­oxy­benzyl­idene)acetohydrazide

In the title compound, the crystal packing features strong N—H⋯O hydrogen bonds, which form C(4) chain-motifs.

Reversible phase transition in 8,19-di­methyl-2,3,8,19-tetra­aza­penta­cyclo[13.7.0.0^4,12.0^6,10.0^17,21]docosa-1(15),2,4(12),5,10,16,21-hepta­ene-7,9,18,20-tetrone

The title compound undergoes a reversible phase transition upon cooling, during which the space group changes from P2₁/c to P1, which is accompanied by a discontinuous change in the unit-cell volume. In the low-temperature phase, twinning is observed, which vanishes upon reheating to room temperature.

Synthesis, crystal structure and Hirshfeld surface analysis of a coordination compound of cadmium nitrate with 2-amino­benzoxazole

The Cd^II atom in the title complex [Cd(NO₃)₂(2AB)₄] (2AB is 2-amino­benzaxole; C₇H₆N₂O) has a distorted octa­hedral coordination environment. In the crystal structure, several N—H⋯O inter­actions lead to the formation of layers parallel to (001).

Synthesis, crystal structure and Hirshfeld surface analysis of Fmoc-β-amino butyric acid and Fmoc carbamate

In the context of the development of synthetic routes that facilitate the incorporation of β-amino acids into peptide synthesis, the synthesis, crystal structure and Hirshfeld surface analysis are reported of fluorenyl­meth­oxy­carbonyl (Fmoc) protected β-amino butyric acid. The importance of pH control in the reaction employing Fmoc-N₃ is demonstrated with another β-amino acid analogue from which Fmoc carbamate was identified as the major product.

Phenyl palladium(II) iodide complexes isolated after Sonogashira coupling of iodo­benzenes with terminal alkynes

The structure of four bis(tri­phenyl­phosphine)phenyl­palladium(II) iodides isolated after completion of Sonogashira coupling reactions, in which the aryl iodide was used in slight excess, are reported.

Synthesis and structure of (E)-3,4,5-trihy­droxy-N′-(3,4,5-tri­meth­oxy­benzyl­idene)benzohydrazide monohydrate

In the structure of the title compound, C₁₇H₁₈N₂O₇·H₂O, relatively strong bifurcated and simple hydrogen-bond inter­actions are present, together with extended van der Waals inter­actions. A hydrogen-bond coordination analysis suggests that polymorphs of the title structure may exist.

Synthesis and structure of 1′,4′-di­phenyl-1a,1′,4′,4′′,5′′,9b-hexa­hydro-2′′H-di­spiro­[cyclopropa[l]phenanthrene-1,2′-[1,4]ep­oxy­naphthalene-3′,3′′-thio­phene]

The title compound was inadvertently prepared as a Diels–Alder adduct between 1,3-di­phenyl­isobenzo­furan and 3-(1a,9 b-di­hydro-1H-cyclo­propa[l]phenanthren-1-yl­idene)tetra­hydro­thio­phene. A combination of fused, bridged, and spiro­cyclic ring systems are all featured within a single mol­ecular structure of this highly crowded polycyclic compound.

Bis(μ-thio­semicarbazide-κ³N¹,S:S;κ³S:N¹,S)bis­[(di­methyl­formamide-κO)(thio­semicarbazide-κ²N¹,S)cadmium(II)] tetra­kis­(2,4,6-tri­nitro­phen­olate): synthesis, crystal structure and Hirshfeld surface analysis

The complete binuclear cation of the title complex salt is generated by a crystallographic center of symmetry and features bridging S atoms.

Crystal structure of chloro­methyl 2-[2-(2,6-di­chloro­phenyl­amino)­phen­yl]acetate

The previously unknown mol­ecular SCXRD structure and crystal-packing pattern of a diclofenac derivative were assessed in detail including intra- and inter­molecular inter­actions such as hydrogen bonds and halogen bonds. The validity of these inter­actions was further evaluated computationally using QM calculations.

Crystal structure and Hirshfeld-surface analysis of 1-(4-fluoro­phen­yl)-3,3-bis­(methyl­sulfan­yl)prop-2-en-1-one

The crystal structure and a Hirshfeld-surface analysis of the chalcone derivative 1-(4-fluoro­phen­yl)-3,3-bis­(methyl­sulfan­yl)prop-2-en-1-one are presented.

Some thio­ether-ketones and their related derivatives

Structures are reported for two thio­ether-ketones, and for some derived hydrazones, and instances of conformational enanti­omerism are delineated. Various types of hydrogen bonds, such as weak C—H⋯S and stronger N—H⋯N and N—H⋯S hydrogen bridges are noted, and inter­molecular cases examined via DFT calculations.

Ortho­rhom­bic cerium(III) carbonate hydroxide studied by synchrotron powder X-ray diffraction

A synchrotron powder X-ray diffraction study of commercially obtained ‘cerium(III) carbonate hydrate' indicates that multiple Ce-containing phases coexist, none of which are Ce₂(CO₃)₃. The majority phase is an ortho­rhom­bic phase of composition CeCO₃OH.

Bis[1,2-bis­(3,5-di­methyl­phen­yl)ethyl­ene-1,2-di­thiol­ato(1−)]nickel(II)

Square-planar bis­[1,2-bis­(3,5-di­methyl­phen­yl)ethyl­ene-1,2-di­thiol­ato(1–)]nickel(II) crystallizes on an inversion center in monoclinic P2₁/c in a packing arrangement defined by a dense network of inter­molecular methyl C—H→π_arene hydrogen bonds.

Syntheses and structures of 1-[2,2-di­chloro-1-hy­droxy-3-(4-methyl­phen­yl)-3-oxoprop­yl]urea and 1-[2,2-di­chloro-3-(4-fluoro­phen­yl)-1-hy­droxy-3-oxoprop­yl]urea

The title compounds, C₁₀H₉Cl₂FN₂O₃, (I), and C₁₁H₁₂Cl₂N₂O₃, (II), are α,α-dihalo-β-diketone urea derivatives, which contain 4-fluoro­phenyl and p-tolyl groups, respectively. The conformation about the C_O—C_Cl2—C_O—N_u (O = keto, Cl2 = di­chloro, u = urea) bond is anti in (I) and gauche in (II). In the crystals of both compounds, O—H⋯O hydrogen bonds generate inversion dimers and the dimers are linked into (100) layers by N—H⋯O hydrogen bonds.

Crystal structure and Hirshfeld surface analysis of di­methyl 3-methyl-8-{[4-(tri­fluoro­meth­yl)phen­yl]sulfon­yl}-7,8-di­hydro-4H-4,6a-ep­oxy­benzo[b]naphtho­[1,8-de]azepine-5,6-di­carboxyl­ate

In the crystal, mol­ecules are linked by C—H⋯O inter­actions and C—H⋯F inter­actions to form sheets parallel to the (002) plane. In addition, S—O⋯π and π–π inter­actions link mol­ecules along the a-axis direction. van der Waals inter­actions between mol­ecular sheets consolidate the packing.

Crystal engineering of a 1:1 5-fluoro­cytosine–4-hy­droxy­benzaldehyde cocrystal: insights from X-ray crystallography and Hirshfeld analysis

The cocrystal of 5-fluoro­cytosine and 4-hy­droxy­benzaldehyde (1/1), C₄H₄FN₃O·C₇H₆O₂, crystallizes in the monoclinic P2₁/c space group. The crystal structure features a robust supra­molecular network stabilized by N—H⋯O, N—H⋯N, O—H⋯O, C—H⋯O and C–H⋯F hydrogen bonds, forming diverse ring motifs including R₂²(8), R₄⁴(22), R₆⁶(32), and R₈⁸(34). Additional C—F⋯π inter­actions contribute to the crystal cohesion. Hirshfeld surface analysis reveals that O⋯H/H⋯O contacts dominate the inter­molecular inter­actions, emphasizing the key role of hydrogen bonding in the crystal packing.

Crystal structure, computational study, and Hirshfeld analysis of exo-1,2,3,5-tetra­phenyl-1a',9b'-di­hydro­spiro­[bi­cyclo­[3.1.0]hexane-6,1′-cyclo­propa[l]phenanthren]-2-en-4-one

The reaction of dibenzonorcarynyliden(e/oid) with phencyclone was recently reported to give a congested spiro­pentane with endo stereochemistry. Herein it is reported that, in sharp contrast, an analogous reaction using tetra­cyclone, instead of phencyclone, gives the highly crowded title spiro­pentane but with exo stereochemistry as determined by X-ray crystallography.

Crystal structure and characterization of a new chain-like polyrotaxane zinc(II) coordination polymer with mixed pyridine-2,6-di­carboxyl­ate and 1,4-bis­(1H-imidazol-1-ylmeth­yl)benzene ligands

The crystal structure of a new polyrotaxane Zn^II coordination polymer, {[Zn₂(2,6-PDC)₂(bix)₂]·9H₂O}_n, is comprised of dinuclear macrocyclic units and a zigzag chain-like structure extending parallel to [101].