[2‐(Isopropylthio)benzoato‐O,S]phenyl(triphenylphosphine)palladium(II) tetrahydrofuran solvate

In the title compound, [Pd(C₆H₅)(C₁₀H₁₁O₂S)(C₁₈H₁₅P)]·C₄H₈O, an iso­propyl­thio­benzoate ligand is coordinated in a bidentate fashion to the central Pd atom through the O and S atoms. The square‐planar geometry of the Pd atom is completed by a phenyl ligand and a tri­phenyl­phosphine group but is distorted by the bidentate ligand, which forms a six‐membered chelate ring. This ring deviates strongly from planarity, which is illustrated by the plane through the phenyl portion of the chelate ring forming a dihedral angle of 62.3 (1)° with the coordination plane.     

Structure of tetra[β‐(1,2,4‐triazole‐l‐yl) propiophenone] dichloro nickel(II) solvate hexahydrate complex: [NiCl2(C2H2N3CH2CH2‐COPh)4]·6H2O

The mononuclear complex, [NiCl₂ (trzCH₂CH₂COPh)₄]·6H₂O (trz =1,2,4‐triazole), was synthesized and its structure was determined by single crystal X‐ray determination. It crystallizes in the monoclinic system, space group P2₁/c, with lattice parameters: a = 0.80391(2) nm, b = 1.08215(2) tun, c = 2.90133(2) nm, β = 94.792 (1)° and Z = 2. Each nickel atom is coordinated by four N atoms of triazole from four β‐(1,2,4‐triazole‐1‐yl)propiophenone ligands and two chloride anions in trans arrangement with octahedral coordination geometry. In addition to the coordinating nickel complex, there are six uncoordinated water molecules. The Ni‐Cl distance is 0.24865(8) nm and the Ni‐N distances are in the range of 0.2072(2) to 0.2099(2) nm, respectively. In the solid state, the title compound forms three dimensional network structure through hydrogen bonds. The intermolecular hydrogen bonds connect the [NiCl₂(C₂H₂N₃CH₂CH₂COPh)₄] and H₂O moieties. The deep green crystals were also examined by elemental analysis, FT‐IR and UV spectra, which are in agreement with the structural data.     

Bis­[2‐(pyrazol‐3‐yl)­phenolato‐κ2N2,O]copper(II) dimethanol solvate

The title compound, [Cu(C₉H₇N₂O)₂]·2CH₃OH, contains a crystallographically centrosymmetric near‐regular square planar Cu^II centre with trans‐disposed chelating ligands. The complex mol­ecules associate into a one‐dimensional polymeric chain via hydrogen bonding to the solvent mol­ecules.     

(Acetonitrile){2,6‐bis[1‐(2,4,6‐trimethylphenylimino)ethyl]pyridine}dichloridoruthenium(II) dichloromethane solvate

In the title compound, [RuCl₂(C₂H₃N)(C₂₇H₃₁N₃)]·CH₂Cl₂, the Ru^II ion is six‐coordinated in a distorted octahedral arrangement, with the two Cl atoms located in the apical positions, and the pyridine (py) N atom, the two imino N atoms and the acetonitrile N atom located in the basal plane. The two equatorial Ru—N_imino distances are almost equal (mean 2.087 Å) and are substantially longer than the equatorial Ru—N_py bond [1.921 (4) Å]. It is observed that the N_imino—M—N_py angle for the five‐membered chelate rings of pyridine‐2,6‐diimine complexes is inversely related to the magnitude of the M—N_py bond. The title structure is stabilized by intra‐ and intermolecular C—H...Cl hydrogen bonds, as well as by van der Waals interactions.     

Bis[N‐(2‐hydroxy­ethyl)‐β‐alaninato]copper(II)

The Cu^II ion in the title complex, [Cu(C₅H₁₀NO₃)₂] or [Cu(He‐ala)₂] [He‐ala = N‐(2‐hydroxy­ethyl)‐β‐alaninate], resides at the inversion centre of a square bipyramid comprised of two facially arranged tridentate He‐ala ligands. Each He‐ala ligand binds to a Cu^II ion by forming one six‐membered β‐alaninate chelate ring in a twist conformation and one five‐membered ethanol­amine ring in an envelope conformation, with Cu—N = 2.017 (2) Å, Cu—O_COO = 1.968 (1) Å and Cu—O_OH = 2.473 (2) Å. The [Cu(He‐ala)₂] mol­ecules are involved in a network of O—H⋯O and N—H⋯O hydrogen bonds, forming layers parallel to the (10) plane. The layers are connected into a three‐dimensional structure by van der Waals inter­actions, so that the mol­ecular centres form pseudo‐face‐centered close packing.     

Poly[[hexaaquabis[μ4‐2‐hydroxy‐5‐(4‐sulfonatophenyldiazenyl)benzoato]dibarium(II)] 4,4′‐bipyridine solvate]

The title compound, {[Ba₂(C₁₃H₈N₂O₆S)₂(H₂O)₆]·C₁₀H₈N₂}_n, possesses a novel two‐dimensional porous coordination network, in which each Ba^II ion is nine‐coordinated by three carboxylate O atoms, two sulfonate O atoms and four water molecules in an irregular coordination environment. Hydrogen‐bond interactions between coordinated water molecules and sulfonate/hydroxyl groups hold the network layers together and produce a three‐dimensional supramolecular architecture.     

(E)‐3‐(Benzo[b]thiophen‐2‐yl)‐2‐(3,4,5‐trimethoxyphenyl)acrylonitrile and (Z)‐3‐(benzo[b]thiophen‐2‐yl)‐2‐(3,4‐dimethoxyphenyl)acrylonitrile

The title compounds, C₂₀H₁₇NO₃S, (I), and C₁₉H₁₅NO₂S, (II), were prepared by the reaction of benzo[b]thiophene‐2‐carbaldehyde with (3,4,5‐trimethoxyphenyl)acetonitrile and (3,4‐dimethoxyphenyl)acetonitrile, respectively, in the presence of methanolic potassium hydroxide. In (I), the C=C bond linking the benzo[b]thiophene and the 3,4,5‐trimethoxyphenyl units has E geometry, with dihedral angles between the plane of the bridging unit and the planes of the two adjacent ring systems of 5.2 (3) and 13.1 (2)°, respectively. However, in (II), the C=C bond has Z geometry, with dihedral angles between the plane of the bridging unit and the planes of the adjacent benzo[b]thiophene and 3,4‐dimethoxyphenyl units of 4.84 (17) and 76.09 (7)°, respectively. There are no significant intermolecular hydrogen‐bonding interactions in the packing of (I) and (II). The packing is essentially stabilized via van der Waals forces.     

Methanol[1‐(methoxymethanimidoyl)‐2‐(pyridin‐2‐ylmethyl)guanidine]bis(perchlorato)copper(II)

The title complex, [Cu(ClO₄)₂(C₉H₁₃N₅O)(CH₃OH)], was synthesized from a methanolysis reaction of N‐(methylpyridin‐2‐yl)cyanoguanidine (L³) and copper(II) perchlorate hexahydrate in a 1:1 molar ratio. The Cu^II ion is six‐coordinated by an N₃O₃ donor set which confers a highly distorted and asymmetric octahedral geometry. Three N‐donor atoms from the chelating 1‐(methoxymethanimidoyl)‐2‐(pyridin‐2‐ylmethyl)guanidine (L^3m) ligand and one O atom from the methanol molecule define the equatorial plane, with two perchlorate O atoms in the apical sites, one of which has a long Cu—O bond of 2.9074 (19) Å. The dihedral angle between the five‐ and six‐membered chelate rings is 8.21 (8)°. Two molecules are associated into a dimeric unit by intermolecular N—H...O(perchlorate) hydrogen bonds. Additionally, the weakly coordinated perchlorate anions also link adjacent [Cu(ClO₄)₂(L^3m)(CH₃OH)] dimers by hydrogen‐bonding interactions, resulting in a two‐dimensional layer in the (100) plane. Further C—H...O hydrogen bonds link the two‐dimensional layers along [100] to generate a three‐dimensional network.     

Bis[2‐(2‐hydroxyethyl)pyridinium] μ‐decavanadato‐bis[pentaaquamanganate(II)] tetrahydrate

The structure of the title compound, (C₇H₁₀NO)₂[Mn₂V₁₀O₂₈(H₂O)₁₀]·4H₂O or (C₅H₄NHCH₂CH₂OH)₂[{Mn(H₂O)₅}₂V₁₀O₂₈]·4H₂O, at 293 (2) K has triclinic (P) symmetry. The asymmetric unit consists of one half of a decavanadate anion of C_i symmetry, one [Mn(H₂O)₅]²⁺ group, one 2‐(2‐hydroxyethyl)pyridinium cation and two solvent water molecules. The decavanadate ion bridges between two [Mn(H₂O)₅]²⁺ groups, thus forming a dodecanuclear complex unit. Complex units are connected via a hydrogen‐bonding network, forming supramolecular layers lying in the (001) plane. Cations and solvent water molecules are located between these layers.     

Aqua(n‐hexyl)[3,3′‐(propane‐1,3‐diyldinitrilo)­bis­(butan‐2‐one) dioximato‐­κ4N]cobalt(III) perchlorate

The title compound, [Co(C₆H₁₃)(C₁₁H₁₉N₄O₂)(H₂O)]ClO₄, is in the general class of coenzyme B₁₂ models which contain a ClO₄ anion and a [Co(C₆H₁₃)(C₁₁H₁₉N₄O₂)(H₂O)]⁺ cation. In the cation, the Co atom has a distorted octahedral coordination, with the n‐hexyl and H₂O ligands in axial positions. The crystal data reveal some degree of flexibility in the Costa‐type system, which is similar to the coenzyme B₁₂.     

A new polymorphic form of bis(acetato‐κO)bis[2‐(pyridin‐2‐yl)ethanol‐κ2N,O]nickel(II)

A new polymorph of a mononuclear nickel(II) acetate complex with 2‐(pyridin‐2‐yl)ethanol ligands, [Ni(CH₃COO)₂(C₇H₉NO)₂], has been prepared and structurally characterized. Its molecular structure resembles the structures of two previously reported polymorphs in that the Ni^II atom is located on an inversion centre and is coordinated by pairs of acetate and 2‐(pyridin‐2‐yl)ethanol ligands. The acetate anions are coordinated in a monodentate manner, while the 2‐(pyridin‐2‐yl)ethanol ligands are coordinated in a bidentate chelating mode involving the endocyclic N atom and the hydroxy O atom of the ligand side chain. A strong bifurcated intramolecular hydrogen‐bond interaction was observed involving the hydroxy O atom as donor and both acetate O atoms as acceptors. No classical intermolecular hydrogen‐bond contacts were observed. However, the crystal packing is effected through π–π and C—H...π interactions, giving rise to a different packing arrangement. A brief comparison of the three polymorphic forms is presented.     

Bis[1,1′‐bis(diphenylphosphino)ferrocenium] hexadecachlorotetraantimony(III) ethanol solvate

In the title compound, [Fe(C₁₇H₁₄P)₂]₂[Sb₄Cl₁₆]·C₂H₆O, the Fe atoms lie on inversion centres and the pairs of cyclopentadienyl rings are consequently in a fully staggered conformation. The centrosymmetric anionic clusters formed by [Sb₄Cl₁₆]^4? are surrounded by the cations and are held together by weak C—H?Cl interactions. These formations stack along the a axis to form columns, and the columns are interconnected by another weak C—H?Cl interaction along the b axis.     

trans‐Bis[3‐(2‐fluorophenyl)‐1‐(4‐nitrophenyl)triazenido‐κN3]bis(pyridine‐κN)palladium(II)

In the title complex, [Pd(C₁₂H₈FN₄O₂)₂(C₅H₅N)₂] or trans‐[Pd(FC₆H₄N=N—NC₆H₄NO₂)(C₅H₅N)₂], the Pd atom lies on a centre of inversion in space group P. The coordination geometry about the Pd²⁺ ion is square planar, with two deprotonated 3‐(2‐fluoro­phenyl)‐1‐(4‐nitro­phenyl)­triazenide ions, FC₆H₄N=N—NC₆H₄NO₂^?, acting as monodentate ligands (two‐electron donors), while two neutral pyridine mol­ecules complete the metal coordination sphere. The whole triazenide ligand is not planar, with the largest interplanar angle being 16.8 (5)° between the phenyl ring of the 2‐­fluorophenyl group and the plane defined by the N=N—N moiety. The Pd—N(triazenide) and Pd—N(pyridine) distances are 2.021 (3) and 2.039 (3) Å, respectively.     

Different intermolecular interactions in azido[2‐(diphenylphosphino)benzaldehyde semicarbazonato‐κ2P,N1,O]nickel(II)

The title compound, [Ni(C₂₀H₁₇N₃OP)(N₃)], is the first complex with a semicarbazide‐based ligand having a P atom as one of the donors. The influence of the P atom on the deformation of the coordination geometry of the Ni^II ion is evident but less expressed than in the cases of complexes with analogous seleno‐ and thiosemicarbazide ligands. The torsion angles involving the two bonds formed by the P atom within the six‐membered chelate ring have the largest values [C—P—Ni—N = 24.3 (2)° and C—C—P—Ni = −24.2 (4)°], suggesting that the P atom considerably influences the conformation of the ring. Two types of N—H...N hydrogen bond connect the complex units into chains.     

Bis{2,6‐bis[3‐(2,4,6‐trimethylphenyl)pyrazol‐1‐yl‐κN2]pyridine‐κN}zinc(II) diperchlorate bis(nitromethane) solvate

The title compound, [Zn(C₂₉H₂₉N₅)₂](ClO₄)₂·2CH₃NO₂, contains a Zn^II ion showing only small deviations from local D_2d symmetry. The lower rhombicity exhibited by this complex compared with that of its Cu^II congener suggests that the highly rhombic stereochemistry exhibited by the latter is largely imposed by the stereoelectronic preferences of the Cu^II ion.     

Bis[1‐(2‐hydroxyethyl)‐4,10‐diazapyrazolo[4,3‐b]fluoren‐5(1H)‐one thiosemicarbazonato]zinc(II) dimethylformamide trisolvate monohydrate

In the title Schiff base complex, [Zn(C₁₅H₁₂N₇OS)₂]·3C₃H₇NO·H₂O, each Zn^II atom is six‐coordinated in a distorted octahedral environment by two ligands acting in a tridentate chelating mode through two N atoms and one S atom. The coordination mode of the ligand is nearly planar. There are three dimethylformamide molecules and one water molecule solvating the complex. The coordination behavior of the ligand is compared with that of related ligands in similar complexes.     

(Z)‐2‐(3‐Hydroxy‐4‐methoxybenzylidene)‐1‐azabicyclo[2.2.2]octan‐3‐one

Crystals of the title compound, C₁₅H₁₇NO₃, were obtained from a condensation reaction of 3‐hydroxy‐4‐methoxy­benz­aldehyde with 1‐aza­bi­cyclo­[2.2.2]­octan‐3‐one and subsequent crystallization of the product from methanol. The title compound, containing a double bond that connects the aza­bicyclic ring system to the 3‐hydroxy‐4‐methoxy­benzyl­idene group, was obtained with Z geometry.     

Bis{1‐[N‐(2‐methoxy­phenyl)imino­methyl]naphthalen‐2(1H)‐onato‐κ3O,N,O′}zinc(II) ethanol solvate

In the crystal structure of the title compound, [Zn(C₁₈H₁₄NO₂)₂]·C₂H₆O, the Zn atom displays a highly distorted octa­hedral coordination involving the O and N atoms of two mol­ecules of the Schiff base 1‐[N‐(2‐methoxy­phenyl)imino­methyl]naphthalen‐2(1H)‐one, which acts as an O,N,O′‐tridentate ligand. The ethanol mol­ecule is bound to the methoxy group of one ligand mol­ecule via a hydrogen bond.     

Bromidobis[2‐(pyridin‐2‐yl)methanol‐κ2N,O]copper(II) bromide monohydrate

The title compound, [CuBr(C₆H₇NO)₂]Br·H₂O, is an ionic mononuclear complex in which the [CuBr(C₆H₇NO)₂]⁺ cation possesses distorted square‐pyramidal geometry. The Cu^II centre is coordinated by two neutral 2‐(pyridin‐2‐yl)methanol (2‐pyMeOH) ligands and a terminal bromide ligand. The 2‐pyMeOH ligands are coordinated in a bidentate chelating manner through the pyridine N and hydroxy O atoms, forming a five‐membered chelate ring with the Cu^II centre. The planes of the pyridine rings are twisted by 58.71 (14)° with respect to each other. The charge is balanced by a noncoordinating bromide anion which, together with a solvent water molecule, links the components through hydrogen bonds into infinite chains propagating along the a axis. The mononuclear cations appear to associate in pairs through weak interactions between the metal atom of one cation and the halogen atom of an adjacent cation.