搜索结果：Acta crystallographica. Section E, Crystallographic communications

The asymmetric unit of the title hydrated complex salt, (C12H12NO2)[Sn(C10H6NO2)Cl4]·H2O, consists of one 2-(eth-oxy-carbon-yl)quinolinium cation, one tetra-chlorido-(quinolinium-2-carboxyl-ato)stannate(IV) anion and one water mol-ecule. The compound was obtained by reaction of quinaldic acid with tin(II) chloride dihydrate in ethanol. The SnIV atom is six-coordinated by four chloride ligands and by one N and one O atom from the quinolinium-2-carboxyl-ate ligand, forming a distorted octa-hedral coordination environment. In the mol-ecular structure, intra-molecular O-H⋯O and C-H⋯Cl hydrogen bonds are observed. In the crystal, N-H⋯O, C-H⋯O and C-H⋯Cl hydrogen bonds link the components into a three-dimensional network. In addition, Y-X⋯π (Sn-Cl⋯π) and π-π stacking inter-actions involving three aromatic rings are present, with centroid-centroid separations in the range 3.633 (2)-3.864 (2) Å.

The first uranium-curcuminoid coordination compound has been synthesized and structurally characterized. The title complex, [U(O)2(C25H23O8)2(CH3OH)]·C6H5CH3, crystallizes in the monoclinic space group C2/c. The neutral complex comprises a uran-yl(VI) unit ({O=U=O}2+) coordinated by two monoanionic bidentate 4,4'-di-acetyl-curcuminato ligands (C25H23O8) and one methanol co-ligand, resulting in a distorted penta-gonal-bipyramidal coordination geometry. The O atoms from the β-diketonate moieties and the methanol mol-ecule form the equatorial plane, while the uranyl O atoms occupy the axial positions. In the crystal, O-H⋯O hydrogen bonds generate R 2 2(26) ring motifs, forming zigzag chains along the a-axis direction. Additional weak C-H⋯O inter-actions further consolidate the crystal packing through inter-chain aggregation.

Etoxazole is an agricultural pesticide that degrades into potentially haza-rdous metabolites, necessitating a thorough understanding of their chemical properties for accurate environmental and health risk assessments. This study reports the synthesis and structural characterization of two precursors of an etoxazole metabolite designated 'R8': 1-(4-tert-butyl-2-eth-oxy-phen-yl)-2-hy-droxy-ethan-1-one, C14H20O3 (I), and 1-(4-tert-butyl-2-eth-oxy-phen-yl)ethan-1-one, C14H20O2 (II). Compound I crystallizes with the symmetry of space group Pnma, while II crystallizes as P21/m. In both structures, the mol-ecules lie on crystallographic mirror planes (Z' = 1/2) and exhibit a high degree of conformational similarity, differing primarily in the torsion angle of the tert-butyl group. The crystal packing in both structures is consolidated by weak C-H⋯π contacts that assemble the mol-ecules into columns parallel to the crystallographic b axes. Hirshfeld-surface analyses show that the inter-molecular inter-actions in both compounds are overwhelmingly dominated by contacts involving hydrogen atoms.

The synthesis and structural characterization of two new heterobimetallic 3d-4f complexes is reported, namely, bis-[dimethyl (phenyl-sulfon-yl)amido-phosphato]-μ-nitrato-(μ-6,6'-{(1E,1'E)-[propane-1,3-diylbis(aza-nylyl-idene)]bis-(methanylyl-idene)}bis-(2-meth-oxy-phenolato))cerium(III)copper(II), [CeCu(C19H20N2O4)(C8H11NO5PS)2(NO3)] or [Cu(Vanpen)Ce(μ-NO3)(L)2] (1), and [μ-dimethyl (phenyl-sulfon-yl)amido-phosphato][dimeth-yl(phenyl-sulfon-yl)amido-phosphato](nitrato)(μ-6,6'-{(1E,1'E)-[propane-1,3-diylbis(aza-nylyl-idene)]bis-(methanylyl-idene)}bis-(2-meth-oxy-phenolato))gadolinium(III)copper(II), [CuGd(C19H20N2O4)(C8H11NO5PS)2(NO3)] or [Cu(Vanpen)Gd(μ-L)(L)(NO3)] (2), obtained by combining the Schiff base (6,6'-{(1E,1'E)-[propane-1,3-diylbis(aza-nylyl-idene)]bis-(methanylyl-idene)}bis-(2-meth-oxy-phenol)) complex Cu(Vanpen) with the lanthanide(III) nitrates and sulfonyl-amido-phosphate (SAPh) ligand dimeth-yl(phenyl-sulfon-yl)amido-phosphate (L -). Single-crystal X-ray diffraction studies of Cu-Ce and Cu2+-Gd3+ complexes reveal that these species contain the Ln(L)2NO3 unit. The lanthanide centers adopt nine-coordinate, distorted muffin (Cs) geometries. The coordination modes of L - and NO3- ligands change depending on the lanthanide. In the Cu2+-Ce3+ complex the NO3 - group acts as a bridging ligand, whereas in the Cu2+-Gd3+ analogue the bridging function is assumed by SAPh, with NO3 - binding only in a chelating fashion. The presence of a nitrate group can be explained by steric hindrance that prevents coordination of three SAPh ligands around the lanthanide center. Qualitative X-ray fluorescence analysis confirmed the presence of two different metal ions within each heterometallic species.

In the title biotin-conjugated di-hydro-artemisinin (DHA) derivative, C25H38N2O7S, the mol-ecule retains the essential endoperoxide bridge and links the C-10 position of DHA to the penta-noate chain of biotin via an ester bond. In the solid state, the tetra-hydro-pyran ring of DHA adopts a chair conformation, the fused peroxide seven-membered ring exhibits a twist conformation, the imidazolidone ring of biotin shows an envelope conformation and the tetra-hydro-thio-phene ring adopts a twisted conformation. Supra-molecularly, adjacent mol-ecules are linked through a classical N-H⋯O double hydrogen-bonding motif between the urea groups of biotin, forming anti-parallel cyclic dimers. These strong dimers are further supported by weaker C-H⋯O inter-actions. The SQUEEZE [Spek (2015 ▸). Acta Cryst. C71, 9-18] routine in PLATON was used to remove electron density corresponding to disordered solvent mol-ecules. This structure determination provides a valuable blueprint for the rational design of hybrid anti-malarial and anti-cancer therapies based on DHA-biotin conjugates.

The title benzimidazole derivative, C26H18N6, which contains two benzimidazole units connected through an azo (N=N) linkage, was isolated as yellow needle-shaped crystals and characterized by single-crystal X-ray diffraction. The compound crystallizes in the monoclinic crystal system (space group: P21 /c) with one mol-ecule in the asymmetric unit. The dominant inter-actions in the crystal are parallel π-π contacts, giving rise to one-dimensional π-stacks along the a-axis direction, with a centroid-to-centroid separation of 3.899 (1) Å, a slippage distance of 1.81 Å, and a slip angle of 27.61°. Within these stacks, two short C-H⋯C contacts of 2.74 Å are observed between adjacent mol-ecules, which may reflect packing constraints. Along the bc plane, the structure comprises two-dimensional ribbons formed by anti-parallel chains. No short inter-planar contacts are observed between neighboring stacks.

In the title solvate, C6H6N2O·0.5C2H6O2, the asymmetric unit consists of one nicotinamide mol-ecule and half of an ethyl-ene glycol mol-ecule, which is completed by crystallographic inversion symmetry. The dihedral angle between the acetamide group and the pyridine ring is 21.9 (8)°. In the crystal, the components are linked by N-H⋯O and O-H⋯N hydrogen bonds into (102) sheets and weak offset π-π stacking is also observed. Hirshfeld surface analysis indicates that the most important contacts in the structure are H⋯H (42.9%), O⋯H/H⋯O (26.4%), C⋯H/H⋯C (10.6%) and N⋯H/H⋯N (9.2%).

Crystals of the title compound, {[CdBr2(C6H8N2)(H2O)]·C6H8N2·0.5H2O} n (C6H8N2 = 2,3-di-methyl-pyrazine), were obtained accidentally by the reaction of cadmium bromide with 2,3-di-methyl-pyrazine in water. The asymmetric unit consists of one Cd cation, two bromide anions, one 2,3-di-methyl-pyrazine ligand, one non-coordinating 2,3-di-methyl-pyrazine mol-ecule, and one water mol-ecule in general positions as well as an additional water mol-ecule that is located on a twofold rotation axis. The cadmium cations are octa-hedrally coordinated by four bromide anions, one 2,3-di-methyl-pyrazine ligand and one water mol-ecule, and are linked by pairs of μ-1,1-bridging bromide anions into chains that propagate in the a-axis direction. These chains are further connected into layers by inter-molecular hydrogen bonding. The coordinated water ligand is hydrogen bonded to the 2,3-di-methyl-pyrazine, and the water solvate mol-ecule and the 2,3-di-methyl-pyrazine mol-ecules of crystallization are linked by O-H⋯N hydrogen bonding via the water solvate mol-ecules into chains along the c-axis direction. The water solvate mol-ecule therefore acts as donor for two O-H⋯N and as acceptor for two O-H⋯O hydrogen bonds.

The synthesis and characterization of a single-crystal of tetra-aqua-tri-nitratoerbium/neodymium(0.359/0.641) dihydrate, Er0.359Nd0.641(NO3)3(H2O)4·2H2O, is reported herein. X-ray diffraction highlighted a crystal with structural features, including a network of water mol-ecules and extensive hydrogen bonding between layers, that are isomorphous with other light lanthanide crystal structures. Single-crystal XRD and SEM-EDS indicated the substitutional behavior of a heavy lanthanide, Er, into the lattice site of a light lanthanide, Nd. The diadochic nature of the lanthanides within a nitrate-containing structure culminated in a 1:0.95 ratio of Er:Nd.

Tris(pyridin-2-yl)borates are an emerging class of scorpionate ligands. Distinguished by their robustness and nucleophilicity, they have promise as alternatives to tris-(pyrazol-yl)borates in coordination chemistry, materials ap-plications, and catalysis. In this article, bis-[phenyl-tris-(pyridin-2-yl)borato]cobalt(III) tetra-carbonyl-cobalt(-I) di-chloro-methane monosolvate, [Co(C21H17BN3)2][Co(CO)4]·CH2Cl2 or [Tpy2Co][Co(CO)4]·CH2Cl2, was prepared by the reaction of hy-dro-gen phenyl-tris-(pyridin-2-yl)borate (TpyH), tri-ethyl-amine, and Co(CO)4I. Single-crystal X-ray diffraction resulted in a homoleptic com-plex consisting of the diamagnetic [Tpy2Co]+ cation and the tetra-car-bonyl-cobaltate {[Co(CO)4]-} counter-ion. The unusual CoIII/Co-I mixed-valence com-position presumably results from disproportionation. [Tpy2Co][Co(CO)4] represents the first mixed-valence tris-(pyridin-2-yl)borate com-plex.

Single-crystals of the hydrated sodium potassium orthomolybdate phases Na3K(MoO4)2(H2O)9, tris-odium potassium bis-(orthomolybdate) nona-hydrate, and NaK(MoO4)(H2O), sodium potassium orthomolybdate monohydrate, were obtained as by-products in a flux growth experiment aiming on the synthesis of silicates from the quaternary system Na2O-K2O-CaO-SiO2. The asymmetric unit of Na3K(MoO4)2(H2O)9 (space group P63/m, Z = 2) comprises one Na+ atom and one water mol-ecule on a mirror plane, one K+ atom on a 6 axis, one Mo6+ cation and one O atom on a threefold rotation axis, and one O atom and one water mol-ecule in general sites. The crystal structure is built from isolated MoO4 tetra-hedra, which are linked by common corners to trimers containing three face-sharing Na(H2O)4O2 octa-hedra. Linkage between the heteropolyhedral groups is provided by potassium cations, which are coordinated by six water mol-ecules in form of trigonal prisms. The resulting layers are located at z = 1/4 and z = 3/4, respectively. Intra- and inter-layer hydrogen bonds between the water mol-ecules and the oxygen atoms of the MoO4 tetra-hedra consolidate the structure. The backbone of the crystal structure of NaK(MoO4)(H2O) (space group P212121, Z = 4) is made from chains of edge-sharing Na(H2O)2O4 octa-hedra running parallel [100], which are decorated by MoO4 tetra-hedra via corner sharing. Neighbouring heteropolyhedral chains are linked by additional potassium cations, which are coordinated by seven oxygen ligands and one water mol-ecule. Moreover, intra- and inter-chain hydrogen bonds exist.

The title compound, [HgCl2(C12H15N3O2S)2], was synthesized by the reaction of (E)-2-[1-(benzo[d][1,3]dioxol-5-yl)ethyl-idene]-N-ethyl-hydrazine-1-carbo-thio-amide [common name: 3',4'-(methyl-enedi-oxy)aceto-phenone 4-ethyl-thio-semicarbazone] with mercury(II) chloride in a 2:1 molar ratio at ambient temperature, using ethanol as solvent. A white solid was isolated and colourless single crystals of the title compound for the SC-XRD analysis were obtained from a solution in (methane-sulfin-yl)methane (common name: dimethyl sulfoxide, DMSO) with a hexane overlay. The HgII metal center is fourfold coordinated in a distorted tetra-hedral geometry by two neutral thio-semicarbazone derivatives, acting as κS-donors, and two chlorido ligands. The complex mol-ecule exhibits a sequence of four intra-molecular hydrogen-bonded rings, formed by two inter-actions of the N-H⋯Cl type, with graph-set motifs of S(6) and showing a chelate-like coordination environment around the metal center, and two additional inter-actions of the N-H⋯N type with S(5) graph-set motifs. In the crystal, the mol-ecules are linked via N-H⋯Cl inter-molecular inter-actions along the c-axis, forming a hydrogen-bonded ribbon-like supra-molecular arrangement that resembles a zigzag pattern along the c-axis direction, and with the Cl atoms acting as bridges between intra- and inter-molecular hydrogen bonds. The Hirshfeld surface analysis suggests that the major contributions for the crystal cohesion are the H⋯H (40.4%), H⋯Cl/Cl⋯H (14.5%), H⋯C/C⋯H (11.3%), H⋯O/O⋯H (10.6%) and H⋯S/S⋯H (9.2%) inter-molecular contacts, with the surface being mapped over the d norm, shape-index and curvedness properties.

The title com-pound, hydro-nium 3,5-di-carb-oxy-benzene-sulfonate trihydrate, H3O+·C8H5O7S-·3H2O, crystallizes in the triclinic space group P with one mol-ecule in the asymmetric unit. The structure is the pseudopolymorph with an additional three water mol-ecules to known hydro-nium 3,5-dicarb-oxybenzene-sulfonate. The 3,5-dicarb-oxybenzene-sulfonate (SIP-) moiety is surrounded by nine mol-ecules, i.e. three SIP- anions, five water mol-ecules and one oxonium ion. The structure, containing a hy-dro-gen-bonded water cluster with eight mol-ecules, forms an R 8 6(16) ring motif through inter-molecular hy-dro-gen bonding.

The thia-zine ring in the title mol-ecule, C23H19NOS, exhibits a screw-boat conformation and is significantly folded along the S⋯N axis. In the extended structure, aided by C-H⋯π(ring) inter-actions, the mol-ecules pack in wave-like layers parallel to the bc plane. A Hirshfeld surface analysis of the crystal structure indicates that the most important contributions for the crystal packing are from H⋯H (50.3%) and H⋯C/C⋯H (35.9%) inter-actions. An evaluation of the electrostatic, dispersion and total energy frameworks in the crystal structure indicates that dispersion energy contribution dominates.

There is a great deal of inter-est in the synthesis and structural features of a newly emerged class of salt-inclusion solids (SISs), which are made of a hybrid framework exhibiting integrated covalent (metal oxides) and ionic (metal halides) structural units. In general, we explored the conditions under which desired phase formation occurs and, for this study, we selected one of the com-pounds in the series of salt-templated phosphates and arsenates, A 2 M 3(X 2O7)2·(salt) [where A = K, Rb, Cs; M = Mn, Cu; X = P, As] commonly known as CU-2 materials, which crystallize in two different space groups (I4/mcm and P4/nbm) due to the variation of the structural units. In our attempt to incorporate mixed Rb+/Na+ cations along with Cl- anions into the negatively charged framework, Cu3(P2O7)2 2-, the title com-pound, Rb9Na2Cu6(P2O7)4Cl7, nona-rubidium disodium hexa-copper(II) tetra-kis-(pyrophosphate) hepta-chloride, has been synthesized by employing a high-tem-per-a-ture RbCl/NaCl eutectic flux and structurally characterized by single-crystal X-ray diffraction, revealing I4/mcm as the space group. In the title com-pound, the same negatively charged framework, Cu3(P2O7)2 2-, characteristic of the CU-2 materials, is retained, while the extended salt-like part of the structure, com-posed of mixed alkali metal chloride fragments, is different from the known CU-2 materials, and includes rarely seen corner-sharing {Na4Cl8} units.

The crystal structures of the flavonoid datiscetin [3,5,7-trihy-droxy-2-(2-hy-droxy-phen-yl)chromen-4-one], C15H10O6, and its monohydrate, C15H10O6·H2O, were determined by single-crystal X-ray diffraction analysis. The flavonoid was isolated from the ethyl acetate fraction of Datisca cannabina L. collected in Tashkent region, Uzbekistan. In both structures, the chromenone ring system and the phenyl ring form nearly the same dihedral angles (38.3 and 38.7° for the anhydrate and monohydrate, respectively). In addition, in both structures, the mol-ecules stack through π-π inter-actions along the shortest translation axis of the unit cell [3.7601 (1) and 3.9274 (5) Å, respectively], resulting in the formation of needle-shaped single crystals.

The asymmetric unit of the title compound, C15H15BrN2OSe, contains two crystallographically independent mol-ecules in which the cyclo-hexene and pyrrole rings are in boat and envelope conformations, respectively. In the crystal, C-H⋯O and N-H⋯Se hydrogen bonds link the mol-ecules into [100] chains, enclosing R 2 2(20), R 3 3(18) and R 4 4(4) ring motifs. C-H⋯π(ring) inter-actions help to consolidate the packing. Hirshfeld surface analysis revealed that the most important contributions to the crystal packing are from H⋯H, H⋯C/C⋯H, H⋯Br/Br⋯H and H⋯Se/Se⋯H inter-actions.

The title com-pound, C14H14N4OS, was crystallized at -20 °C by ether diffusion into an ethanol solution. The dihedral angle between the planes of the aromatic rings is 38.19 (19)° and the mol-ecular conformation is supported by two intra-molecular N-H⋯N hy-dro-gen bonds. In the extended structure, N-H⋯O hy-dro-gen bonds link the mol-ecules into [011] chains. Hirshfeld surface analysis shows that H⋯H (44%), C⋯H/H⋯C (25%) and S⋯H/H⋯S (11.4%) contacts contibute the largest amounts.

In the hydrated complex tetra-kis-(μ-2-carb-oxy-6-nitro-benzoato-κ2 O:O')bis-(μ-3-nitro-benzene-1,2-di-carboxyl-ato-κ2 O:O')tetra-kis-[(1,10-phenanthroline-κN:N')copper(II)] hexahydrate, [Cu4(C8H4NO6)4(C8H3NO6)2(C12H8N2)4]·6H2O, the CuII centres exhibit distorted coordination geometries defined by nitro-gen atoms from chelating 1,10-phenanthroline ligands and oxygen atoms from 3-nitro-phthalate anions. The centrosymmetric mol-ecular assembly is consolidated by bridging carboxyl-ate groups, while the crystal packing is governed by hydrogen bonding and π-π stacking inter-actions between aromatic rings. The scattering contribution of one disordered water mol-ecule contribution was treated using the SQUEEZE procedure.