Crystal structure of 1-(1,3-benzo-thia-zol-2-yl)-3-(4-bromo-benzo-yl)thio-urea.

The chemical reaction of 4-bromo-benzoyl-chloride and 2-amino-thia-zole in the presence of potassium thio-cyanate yielded a white solid formulated as C15H10BrN3OS2, which consists of 4-bromo-benzamido and 2-benzo-thia-zolyl moieties connected by a thio-urea group. The 4-bromo-benzamido and 2-benzo-thia-zolyl moieties are in a trans conformtion (sometimes also called s-trans due to the single bond) with respect to the N-C bond. The dihedral angle between the mean planes of the 4-bromo-phenyl and the 2-benzo-thia-zolyl units is 10.45 (11)°. The thio-urea moiety, -C-NH-C(=S) -NH- fragment forms a dihedral angle of 8.64 (12)° with the 4-bromo-phenyl ring and is almost coplanar with the 2-benzo-thia-zolyl moiety, with a dihedral angle of 1.94 (11)°. The mol-ecular structure is stabilized by intra-molecular N-H⋯O hydrogen bonds, resulting in the formation of an S(6) ring. In the crystal, pairs of adjacent mol-ecules inter-act via inter-molecular hydrogen bonds of type C-H⋯N, C-H⋯S and N-H⋯S, resulting in mol-ecular layers parallel to the ac plane.

Crystal structures of two CuII compounds: catena-poly[[chlorido-copper(II)]-µ-N-[eth-oxy(pyridin-2-yl)methyl-idene]-N'-[oxido(pyridin-3-yl)methyl-idene]hydrazine-κ4 N,N',O:N''] and di-µ-chlorido-1:4κ2 Cl:Cl-2:3κ2 Cl:Cl-di-chlorido-2κCl,4κCl-bis[µ3-eth-oxy(pyridin-2-yl)methano-lato-1:2:3κ3 O:N,O:O;1:3:4κ3 O:O:N,O]bis-[µ2-eth-oxy(pyridin-2-yl)methano-lato-1:2κ3 N,O:O;3:4κ3 N,O:O]tetracopper(II).

Two CuII complexes [Cu(C14H13N4O2)Cl] n , I, and [Cu4(C8H10NO2)4Cl4] n , II, have been synthesized. In the structure of the mononuclear complex I, each ligand is coordinated to two metal centers. The basal plane around the CuII cation is formed by one chloride anion, one oxygen atom, one imino and one pyridine nitro-gen atom. The apical position of the distorted square-pyramidal geometry is occupied by a pyridine nitro-gen atom from a neighbouring unit, leading to infinite one-dimensional polymeric chains along the b-axis direction. Each chain is connected to adjacent chains by inter-molecular C-H⋯O and C-H⋯Cl inter-actions, leading to a three-dimensional network structure. The tetra-nuclear complex II lies about a crystallographic inversion centre and has one core in which two CuII metal centers are mutually inter-connected via two enolato oxygen atoms while the other two CuII cations are linked by a chloride anion and an enolato oxygen. An open-cube structure is generated in which the two open-cube units, with seven vertices each, share a side composed of two CuII ions bridged by two enolato oxygen atoms acting in a µ3-mode. The CuII atoms in each of the two CuO3NCl units are connected by one µ2-O and two µ3-O atoms from deprotonated hydroxyl groups and one chloride anion to the three other CuII centres. Each of the penta-coordinated CuII cations has a distorted NO3Cl square-pyramidal environment. The CuII atoms in each of the two CuO2NCl2 units are connected by µ2-O and µ3-O atoms from deprotonated alcohol hy-droxy groups and one chloride anion to two other CuII ions. Each of the penta-coordinated CuII cations has a distorted NO2Cl2 square-pyramidal environment. In the crystal, a series of intra-molecular C-H⋯O and C-H⋯Cl hydrogen bonds are observed in each tetra-nuclear monomeric unit, which is connected to four tetra-nuclear monomeric units by inter-molecular C-H⋯O hydrogen bonds, thus forming a planar two-dimensional structure in the (01) plane.

Crystal structure of N,N'-[(ethane-1,2-di-yl)bis-(aza-nediylcarbono-thio-yl)]bis-(benzamide).

The reaction of benzoyl chloride and ethyl-endi-amine in the presence of potassium thio-cyanate yielded a white solid, C18H18N4O2S2, which consists of two benzoyl-thio-ureido moieties connected by an ethyl-ene chain. The asymmetric unit consists of one half of the mol-ecule, the complete mol-ecule being generated by crystallographic inversion symmetry. Both thio-urea moieties are in a trans conformation. An intra-molecular N-H⋯O hydrogen bond occurs. In the crystal, C-H⋯S and C-H⋯O hydrogen bonds link the molecules, forming layers parallel to the ac plane.

A new co-crystal dinuclear/trinuclear ZnII-ZnII/ZnII-SmIII-ZnII complex with a salen-type Schiff base ligand.

In the penta-nuclear title complex, [SmZn2(C22H18N2O4)2(NCS)2(C3H7NO)2][Zn2(C22H18N2O4)(NCS)3]·C3H7NO·0.32H2O, namely bis-{µ2-6,6'-dimeth-oxy-2,2'-[phenyl-ene-1,2-diylbis(nitrilo-methanylyl-idene)]diphenolato}-1κ4 O,N,N',O':2κ3 O,O',O 6;2κ3 O,O',O 6:3κ4 O,N,N',O'-bis-(di-methyl-formamide-2κO)di-thiocyanato-1κN,3κN-2-samarium(III)-1,3-dizinc(II) {µ2-6,6'-dimeth-oxy-2,2'-[phenyl-ene-1,2-diylbis(nitrilo-methanylyl-idene)]diphenolato-1κ4 O,N,N',O':2κ2 O,O'}trithio-cyan-ato-1κN;2κ2 N,N-dizinc(II) di-methyl-formamide monosolvate 1.32-hydrate, a dinuclear unit and a trinuclear unit co-exist. One of the ZnII centers in the dinuclear unit as well as the two ZnII centers in the trinuclear unit are located in the inner N2O2 cavity of the ligand and are coordinated to the nitro-gen atom of one thio-cyanate moiety, giving rise to a square-pyramidal geometry. The second ZnII center in the dinuclear unit is coordinated to the two phenolate oxygen atoms of the ligand and to two thio-cyanate groups via the nitro-gen atom in a tetra-hedral geometry. The SmIII ion is eight-coordinated by four phenolate O atoms from the two ligand mol-ecules, two meth-oxy O atoms from the two ligand mol-ecules and two O atoms from the DFM solvent mol-ecule. In the dinuclear unit, the two meth-oxy oxygen atoms remain uncoordinated while in the trinuclear unit, for each ligand one meth-oxy oxygen is coordinated and the other one remains uncoordinated. In the crystal, the trinuclear cationic units and dinuclear anionic units are assembled into infinite layers. These layers are held together via electrostatic inter-actions, forming a three-dimensional structure. In the dinuclear unit, the C and S atoms of one of the thio-cyanate groups are disordered over two sets of sites in a 0.680 (4)(4):0.320 (4) ratio.

Crystal structure of aqua-chlorido-(nitrato-κ2O,O')[1-(pyridin-2-yl-κN)-2-(pyridin-2-yl-methyl-idene-κN)hydrazine-κN2]manganase(II).

The search for novel manganese(II) compounds having inter-esting magnetic properties, using 1-(pyridin-2-yl)-2-(pyridin-2-yl-methyl-idene)hydrazine (HL) as a tridendate ligand, led to the preparation of the title mononuclear material, [MnCl(NO3)(C11H10N4)(H2O)], and the determination of its structure by XRD. The asymmetric unit comprises a discrete mol-ecule in which the cation MnII is hepta-coordinated. The environment around the cation is an almost perfect penta-gonal bipyramid. The base is defined by the two N atoms of the pyridine rings, the N atom of the imino function of the ligand and the two O atoms of the chelating bidentate nitrate ligand. The apical positions are occupied by a Cl atom and a water mol-ecule. In the crystal, there are numerous hydrogen bonds of the types Ow-H⋯ONO2 and C-H⋯ONO2, which generate layers parallel to the bc plane in which the ligands in the axial positions point into the inter-layer space. These axial ligands give rise to hydrogen bonds of the types Ow-H⋯ONO2, Ow-H⋯Cl, N-H⋯Cl and C-H⋯Cl, leading to a three-dimensional framework. The chain bridging the two pyridine rings is disordered over two sets of sites in a 0.53 (2):0.47 (2) ratio.

Crystal structure of bis-(acetato-κ2O,O')di-aqua-[1-(pyridin-2-yl-methyl-idene-κN)-2-(pyridin-2-yl-κN)hydrazine-κN1]terbium(III) nitrate monohydrate.

In the title compound, [Tb(C2H3O2)2(C11H10N4)(H2O)2]NO3·H2O, the Tb3+ ion is nine-coordinated in a distorted tricapped trigonal-prismatic geometry by the three N atoms of the tridentate 1-(pyridin-2-yl-methyl-idene)-2-(pyridin-2-yl)hydrazine ligand, four carboxyl-ate O atoms of two chelating acetate groups and two O atoms of the coordinating water mol-ecules. The organic hydrazine ligand is disordered over two orientations with a refined occupancy ratio of 0.52 (3):0.48 (3). All bond lengths in the coordination environment of the Tb3+ ion are slightly larger than those observed in the isostructural Y3+ and Er3+ complexes. In the crystal, the complex cations are linked by pairs of O-H⋯O hydrogen bonds into dimers. These dimers, nitrate anions and non-coordinating water mol-ecules are joined by O-H⋯O and N-H⋯O hydrogen bonds into a three-dimensional structure.

Bis(benzohydrazide-κO,N')bis-(nitrato-κO)copper(II).

In the title compound, [Cu(NO(3))(2)(C(7)H(8)N(2)O)(2)], the Cu(II) atom is located on a centre of inversion, and is coordinated by two bidentate benzohydrazide ligands and two monodentate nitrate anions in an axially distorted octa-hedral geometry within an N(2)O(4) donor set. The crystal structure is stabilized by N-H⋯O and weak N-H⋯N hydrogen bonds.

1,2-Bis(N'-benzoyl-thio-ureido)benzene.

The title compound, C(22)H(18)N(4)O(2)S(2), was characterized by (1)H and (13)C NMR, solid-state IR spectroscopy and X-ray crystallographic techniques. The crystal structure determination reveals that the twisting modes of the two side arms are different [C-N-C-O and C-N-C-N torsion angles = -1.2 (3) and 1.1 (3)°, respectively, in one arm and 24.1 (3) and -5.1 (3)°, respectively, in the other]. The crystal structure involves N-H⋯O and N-H⋯S hydrogen bonds.

Bis(2-benzamido-benzimidazolato-κN,O)(N,N-dimethyl-formamide-κO)copper(II).

In the title compound, [Cu(C(14)H(10)N(3)O)(2)(C(3)H(7)NO)], the Cu(II) atom is five-coordinated by two N,O-bidentate 2-benzamido-benzimidazolate anions and one O-coordinated dimethyl-formamide (DMF) mol-ecule, resulting in a distorted square-based pyramidal CuN(2)O(3) geometry for the metal atom, with the DMF O atom at the apical site. In the crystal structure, inter-molecular N-H⋯N hydrogen bonds result in chains of mol-ecules propagating along [100].