Crystal structures of two ytterbium(III) complexes comprising alkynylamidinate ligands

Two ytterbium(III) complexes comprising alkynylamidinate ligands, Cp₂Yb[(ⁱPr₂N)₂C—C≡C—c-C₃H₅] (1) and Yb[(CyN)₂C—C≡C—Ph]₃ (Cy = cyclo­hex­yl) (2) have been synthesized and structurally characterized. Both complexes are monomers without any coordinated solvent in the solid state.

An unprecedented binuclear cadmium di­thio­carbamate adduct: bis­[μ₂-N-(2-hy­droxy­eth­yl)-N-iso­propyl­carbamodi­thio­ato-κ³S:S,S′]bis­{[N-(2-hy­droxy­eth­yl)-N-iso­propyl­carbamodi­thio­ato-κ²S,S′](3-{(1E)-[(E)-2-(pyridin-3-yl­methyl­idene)hydrazin-1-yl­idene]meth­yl}pyridine-κN)cadmium]} dihydrate

A distorted octa­hedral NS₅ donor set is found in the binuclear title mol­ecule which features an unprecedented [Cd(di­thio­carbamate)₂]₂ core. Mol­ecules are connected into a three-dimensional architecture by O—H⋯O,N hydrogen bonding.

Crystal structure of 1-amino-2-oxo-2,5,6,7,8,9-hexa­hydro-1H-cyclo­hepta­[b]pyridine-3-carbo­nitrile

In the title compound the seven-membered ring adopts a conformation such that the three atoms not involved in the aromatic plane lie on the same side of that plane. One hydrazinic H atom forms an intra­molecular hydrogen bond to the O atom; the other forms a classical inter­molecular hydrogen bond N—H⋯O, which combines with a `weak' H_ar⋯O inter­action to build up double layers of mol­ecules parallel to the bc plane.

Crystal structure of hexa­aqua­nickel(II) bis­{5-bromo-7-[(2-hy­droxy­eth­yl)amino]-1-methyl-6-oxido­quinolin-1-ium-3-sulfonate} monohydrate

The packing of the title compound is built up by columns of π–π stacking quinoline derivatives running along the c axis, which are inter­connected by [Ni(H₂O)₆]²⁺ complex cations through hydrogen bonding.

Crystal structure of [tris­(4,4′-bi­pyridine)]­diium bis­(1,1,3,3-tetra­cyano-2-eth­oxy­propenide) trihydrate

In the title hydrated salt, which was obtained from the hydro­thermal reaction between between potassium 1,1,3,3-tetra­cyano-2-eth­oxy­propenide and 4,4′-bi­pyridine in the presence of iron(II) sulfate hepta­hydrate, the ionic components are linked into a three-dimensional network by C—H⋯N hydrogen bonds.

Crystal structure of methyl (E)-4-[2-(8-hy­droxy­quinolin-2-yl)vin­yl]benzoate

The title 8-hy­droxy­quinoline derivative has an E conformation about the C=C bond, and the quinoline ring system and the benzene ring are inclined to one another by 29.22 (7)°.

Crystal structure of TiBi₂

Black granular single crystals of monotitanium dibismuth, TiBi₂, were synthesized by slow cooling of a mixture of Bi and Ti from 693 K. The title compound is isostructural with CuMg₂ (ortho­rhom­bic Fddd symmetry). Ti atoms are in the square anti­prisms of Bi atoms. The network of one type of Bi atom spirals along the a-axis direction while honeycomb layers of the other type of Bi atom spreading inn the ab plane inter­lace one another.

Crystal structure of methyl 3′-benzamido-4′-(4-meth­oxy­phen­yl)-1′-methyl­spiro­[indeno­[1,2-b]quinoxaline-11,2′-pyrrolidine]-3′-carboxyl­ate

In the title compound, the mean plane through pyrrolidine ring is approximately orthogonal to the mean plane of the cyclo­pentane ring, making a dihedral angle of 88.78 (10)°. An intra­molecular N—H⋯N inter­action is observed. The crystal packing features C—H⋯O hydrogen bonds.

Synthesis and crystal structure of calcium dizinc iron(III) tris­(orthophosphate), CaZn₂Fe(PO₄)₃

The orthophosphate CaZn₂Fe(PO₄)₃ crystallizes in the monoclinic system. The structure of this phosphate is built up from edge-sharing [ZnO₅] polyhedra linked together by FeO₆ octa­hedra and PO₄ tetra­hedra.

Crystal structure of aqua­tris­(isonicotinamide-κN)bis­(thio­cyanato-κN)cobalt(II) 2.5-hydrate

In the crystal structure of the title compound, the Co^II cations are coordinated by two terminal N-bonded thio­cyanate anions, three isonicotinamide ligands and one water mol­ecule into discrete octa­hedral complexes that are connected by classical and non-classical hydrogen bonding into a three-dimensional network.

Crystal structure of 4-[4-(eth­oxy­carbon­yl)piperazin-1-yl]benzoic acid

4-[4-(Eth­oxy­carbon­yl)piperazin-1-yl]benzoic acid (EPBA) is the product of a reaction between ethyl 1-piperazine­carboxyl­ate and 4-fluoro­benzoic acid. The conformation of the two independent mol­ecules (A and B) in the asymmetric unit is similar. The piperazine ring adopts a chair conformation in both mol­ecules. The dihedral angles formed by the four approximately planar C atoms of the piperazine ring and the benzene ring is 30.8 (5)° in mol­ecule A and 30.6 (5)% in mol­ecule B.

Crystal structures of two C,N-disubstituted acetamides: 2-(4-chloro­phen­yl)-N-(2-iodo­phen­yl)acetamide and 2-(4-chloro­phen­yl)-N-(pyrazin-2-yl)acetamide

A combination of N—H⋯O and C—H⋯O hydrogen bonds together with C—Cl⋯π(arene) and C—I⋯π(arene) inter­actions links the mol­ecules of 2-(4-chloro­phen­yl)-N-(2-iodo­phen­yl)acetamide into twofold inter­woven sheets, and the mol­ecules of 2-(4-chloro­phen­yl)-N-(pyrazin-2-yl)acetamide are linked into complex sheets built solely from hydrogen bonds.

Synthesis and crystal structure of tri­carbonyl­chlorido­{1-[(pyridin-2-yl­methyl­idene)amino]­adamantane}rhenium(I)

The compound [ReCl(pyAm)(CO)₃], where pyAm is 1-[(pyridin-2-yl­methyl­idene)amino]­adamantane, comprises an Re^I atom with an octa­hedral C₃ClN₂ coordination set.

Redetermination of metarossite, CaV⁵⁺₂O₆·2H₂O

The redetermination of metarossite, CaV⁵⁺₂O₆·2H₂O, based on modern single-crystal diffraction data confirms the previous study based on precession photographs, however, with the H atoms located and all atoms refined with anisotropic displacement parameters.

Two forms of (naphthalen-1-yl)boronic acid

Two polymorphs of the title compound, C₁₀H₉BO₂, were prepared by recystallization from different solvents at room temperature. Both forms demonstrate nearly identical mol­ecular structures with all naphthalene group atoms located in one plane and all boronic acid atoms in another. In each extended structure, mol­ecules form dimers, connected via two O—H⋯O hydrogen bonds. The dimers are connected by further O—H⋯O hydrogen bonds, forming layered networks. The resulting layers are practically identical in both forms but are shifted along the [010] axis in the two forms, resulting in a slightly more effective packing for the monoclinic structure compared to the ortho­rhom­bic form.

Crystal structure of di­methyl­formamidium bis­(tri­fluoro­methane­sulfon­yl)amide: an ionic liquid

The cation and anion of the title salt are linked by an O—H⋯N hydrogen bond and a C—H⋯O inter­action, resulting in a high viscosity and a crystallization temperature slightly lower than ambient temperature.

Crystal structure of bis­[trans-di­chlorido­bis­(propane-1,3-di­amine-κ²N,N′)chromium(III)] dichromate from synchrotron data

In the title organic–inorganic salt, [CrCl₂(tn)₂]₂[Cr₂O₇] (tn is propane-1,3-di­amine), the Cr^III ions are coordinated by four N atoms from two tn ligands and two chloride ions in a trans geometry, displaying a distorted octa­hedral arrangement. The crystal packing is stabilized by N—H⋯Cl and N—H⋯O hydrogen bonds.

A two-dimensional Cd^II coordination polymer: poly[di­aqua­[μ₃-5,6-bis­(pyridin-2-yl)pyrazine-2,3-di­carboxyl­ato-κ⁵O²:O³:O³,N⁴,N⁵]cadmium]

The reaction of cadmium dichloride with the ligand 5,6-bis­(pyridin-2-yl)pyrazine-2,3-di­carb­oxy­lic acid leads to the formation of a two-dimensional coordination polymer.

Crystal structure of bis­(η²-ethyl­ene)(η⁵-penta­methyl­cyclo­penta­dien­yl)cobalt

In the title compound, the Co—C(olefin) bonds have an average length of 2.022 (2) Å, while the Co—C(penta­dien­yl) bonds average 2.103 (19) Å. The olefin C=C bonds are 1.410 (1) Å. In the crystal, mol­ecules are linked into chains by weak C—H⋯π inter­actions.

mer-Tri­chlorido­tris­(tetra­hydro­thio­phene-κS)iridium(III): preparation and comparison with other mer-tri­chlorido­tris­(tetra­hydro­thio­phene-κS)metal complexes

The crystal structure of mer-tri­chlorido­tris­(tetra­hydro­thio­phene-κS)iridium(III) is reported and compared with a different form of the complex previously reported. It is also compared with other mer-tri­chlorido­tris­(tetra­hydro­thio­phene-κS)metal(III) complexes of molybdenum, ruthenium and rhodium.

Crystal structure of 6-(p-tol­yl)benzo[b]naphtho[2,3-d]thio­phene and of an ortho­rhom­bic polymorph of 7-phenyl­anthra[2,3-b]benzo[d]thio­phene

The title compounds, 6-(p-tol­yl)benzo[b]naphtho­[2,3-d]thio­phene and 7-phenyl­anthra[2,3-b]benzo[d]thio­phene, are benzo­thio­phene derivatives in which the benzo­thio­phene moiety is fused with a naphthalene ring system in the former and with an anthracene ring system in the latter. In the former, the 4-methyl­benzene ring substituent makes a dihedral angle of 71.40 (9)° with the mean plane of the naphthalene ring system, while the phenyl ring substituent in the latter makes a dihedral angle of 67.08 (12)° with the mean plane of the anthracene ring system.

Crystal structure of BaMnB₂O₅ containing structurally isolated manganese oxide sheets

The structure of BaMnB₂O₅ is characterized by infinite sheets of B₂O₅ units and Mn₂O₈ dimers of edge-sharing MnO₅ square pyramids while Ba²⁺ cations inter­leave successive sheets.

Crystal structures of ethyl {2-[4-(4-iso­propyl­phen­yl)thia­zol-2-yl]phen­yl}carbamate and ethyl {2-[4-(3-nitro­phen­yl)thia­zol-2-yl]phen­yl}carbamate

Two new thia­zole derivatives – the structural analogs of the alkaloid Thio­sporine B – were studied by X-ray diffraction.

Synthesis and crystal structure of ((E)-{2-[(E)-(4-hy­droxynaphthalen-1-yl)methyl­idene]hydrazin-1-yl}(methyl­sulfan­yl)methyl­idene)azanium hydrogen sulfate monohydrate

In the title mol­ecular salt, C₁₃H₁₄N₃S⁺·HSO₄⁻·H₂O, the protonation of the azomethine N atom in sulfuric acid medium involves the formation of a bis­ulfate anion. The mol­ecular structure of the cation is obtained from the thiol tautomer of thio­semicarbazone wherein the naphthalene moiety and the conjugation of the bonds contribute to the planarity of the mol­ecular skeleton.

(+)-trans-Chlorido­{2-[(R_p)-2-(methyl­sulfan­yl)ferro­cen­yl]-2,5,6,7-tetra­hydro­pyrrolo­[1,2-c]imidazol-3-yl­idene}bis­(tri­phenyl­phosphane-κP)palladium(II) hexa­fluorido­phosphate di­chloro­form disolvate

A solvated palladium(II) complex bearing a planar chiral ferrocenyl pyrrolo­imidazolyl­idene (NHC) ligand, synthesized by oxidative addition of a chloro­imidazolium salt to Pd(PPh₃)₄, features a pendant thio­ether group that is not involved in coordination to Pd.

Crystal structure of methyl 4-(4-hy­droxy­phen­yl)-6-methyl-2-oxo-1,2,3,4-tetra­hydro­pyrimidine-5-carboxyl­ate monohydrate

The title hydrate crystallizes with two formula units in the asymmetric unit (Z′ = 2). The organic mol­ecules form a dimer, linked by a pair of N—H⋯O hydrogen bonds. Further hydrogen bonding together with weak C—H⋯π and π–π inter­actions further consolidates the packing, generating a three-dimensional network.

Crystal structure of (E)-4-hy­droxy-N′-(3-meth­oxy­benzyl­idene)benzohydrazide

The mol­ecules of C₁₅H₁₄N₂O₃ are slightly twisted. N—H⋯O, O—H⋯N and O—H⋯O hydrogen bonds play an important role in the crystal packing, resulting in the formation of mol­ecular sheets parallel to the bc plane.

Crystal structures of N-[(4-phenyl­thia­zol-2-yl)carbamo­thio­yl]benzamide and N-{[4-(4-bromo­phen­yl)thia­zol-2-yl]carbamo­thio­yl}benzamide from synchrotron X-ray diffraction

The crystal structures of two new thio­urea derivatives – potential active pharmaceutical ingredients (APIs) – were studied by synchrotron X-ray diffraction.

Solvent inclusion in the crystal structure of bis­[(adamantan-1-yl)methanaminium chloride] 1,4-dioxane hemisolvate monohydrate explained using the computed crystal energy landscape

Energy computations on the title salt show a clear preference for solvated structures, which correlates with the most effective formation of hydrogen bonds.

Crystal structure of 1,3-bis­(3-tert-butyl-2-hy­droxy-5-methyl­benz­yl)-1,3-diazinan-5-ol monohydrate

The asymmetric unit comprises one 1,3-bis­(3-tert-butyl-2-hy­droxy-5-methyl­benz­yl)-1,3-diazinan-5-ol mol­ecule and one water mol­ecule. The two mol­ecular components are held together through an O—H⋯O hydrogen bond.

Crystal structure of 3-(2-hy­droxy­eth­yl)-2-methyl­sulfanyl-6-nitro-3H-benzimidazol-1-ium chloride monohydrate

The title hydrated salt, C₁₀H₁₂N₃O₃S⁺·Cl⁻·H₂O, forms centrosymmetric (20) dimers through inter­molecular C—H⋯O hydrogen bonds. These dimers are stacked via N—H⋯O and O—H⋯Cl hydrogen bonds involving the water mol­ecules and chloride anions. Offset π–π inter­actions are also present.

Azido­{1-[(2-di­ethyl­amino­ethyl­imino)meth­yl]naphthalato}copper(II). Erratum

Erratum to Acta Cryst. (2006), E62, m849–m850.

Azido­{1-[2-(di­methyl­amino)­ethyl­iminometh­yl]naphthalenolato}copper(II). Erratum

Erratum to Acta Cryst. (2006), E62, m983–m985.