The structure of bis(trimethylammonium) undecachlorotriantimonate(III) [(CH3)3NH]2Sb3Cl11 containing a novel antimony(III) anion

The structure of [(CH₃)₃NH]₂Sb₃Cl₁₁ (space group P2₁/n; a = 10.374(2), b = 23.723(5), c = 11.884(2) Å, = 113.46(3)°; V = 2682.9(9) ų) consists of a structurally novel [Sb₃Cl^2– ₁₁] anion and two crystallographically nonequivalent trimethylammonium cations. The anion is composed of three deformed octahedra in the asymmetric part of the unit cell. The octahedra are connected with each other by edges and corners forming a characteristic polyanionic layer. Trimethylammonium cations, one ordered and one disordered, are connected to the inorganic sublattice by N—H···Cl hydrogen bonds.     

Synthesis and structure of tetrakis(2,6-dichlorophenoxide) bis(THF) uranium(IV)

The reaction of UCl₄ with KO-2,6-Cl₂C₆H₃ in tetrahydrofuran results in the preparation of the title compound. The six-coordinate complex possesses pseudo-octahedral geometry about uranium, with U-O(phenoxide) bond lengths in the range 2.161(11) to 2.178(10) Å and U-O(THF) bond lengths of 2.467(10) and 2.475(11) Å. This complex crystallizes in the monoclinic space group P2₁/n (a = 11.169(2), b = 11.588(2), c = 35.119(5) Å, = 92.11(1)°, V = 4542.2(13) ų, and Z = 4).     

Crystal structure of the hemitoluene solvate of racemiccis-bis(bipyridyl)chloro(tri-n-propylphosphine)ruthenium(II) perchlorate,a species with disordered PPr3 and toluene moieties

The complexcis-[Ru(bpy)₂(PPr₃)Cl⁺][ClO ₄ ^– ] · 0.5 (toluene) crystallizes as a racemate in the monoclinic space group P2₁/n. Both the PPr₃ ligand and the toluene of crystallization are subject to disorder. Ruthenium—ligand distances are: Ru–PPr₃=2.348(2) Å, Ru–Cl=2.426(2) Å and Ru–N(bpy)=2.035(6)–2.112(5) Å.     

Structure of (Z)-1-p-methoxyphenyltelluro-1,4-diphenyl but-1-en-3-yne

C₂₃H₁₈TeO,M _r=437.97, ,a=9.940(2),b=13.664(3),c=7.895(2) Å, =80.60(1), =69.71(2), =75.95(1)°,V=972.0(4) ų,Z=2,R=0.041 for 2668 observed reflections. The Te–C bond distances are 2.109(5)Å and the C–Te–C angle is 96.0(2)°. The phenyl rings are planar to within experimental accuracy, making dihedral angles of 64.6(2), 65.3(2) and 31.1(3)°.     

Crystal structure of di(N-benzyl piperidinium) pentachloroantimonate(III) dihydrate

The salt di(N-benzyl piperidinium) pentachloroantimonate(III) dihydrate crystallizes in the orthorhombic system with space group Cmc2₁, the unit cell dimensions are: a = 29.383(1), b = 10.509(2), c = 9.941(1) Å, with Z = 8. The structure shows a layer arrangement perpendicular to the a axis: planes of SbCl₆ octahedra alternate with planes of [C₁₂H₁₇N]⁺ cations. The SbCl₆ octahedra are connected through a O(W)–HCl hydrogen bonds and a chlorine bridge, so that infinite unidimensional chains of composition [SbCl₅(H₂O)₂]^2n– _n are formed in the structure along the c direction. These chains are connected to [C₁₂H₁₇N]⁺ entities by N–HCl and N–HO(W) hydrogen bonds, forming a three-dimensional network. It was found that lengths of Sb–Cl bonds may differ from each other. The differences shown as a distortion of the SbCl₆ octahedra were attributed to the Sb(III) lone electron pair stereoactivity.     

3-D polymeric structure formed by hydrogen bonds of copper (II) complex

A new copper complex trans-Dichlorobis[4-methoxypyridine]copper(II) (1) was synthesized and its crystal structure determined by X-ray diffraction. The close Cu···Cl contacts between the molecular units form bi-bridged dimers. The Copper(II) ion completes its 4 + 2 coordination via interaction with the Cu···Cl close contact. The complex has a polymeric structure of infinite one-dimensional (1D) bi-bridged chains, consisting of six-coordinate copper(II) units. C–H···C l intermolecular interaction connect the 1D-chains in the structure of 1 which form to 3D structure. The π ··· π interactions between the aromatic rings are also observed in the hydrogen bonded assembly of 1.     

Synthesis and structural characterization of the dinuclear bis(glutarato)bis(urea)copper(II)complex, dihydrate

The complex [Cu(OOC-(CH₂)₃-COO)(O=C(NH₂)₂]₂·2H₂O has been synthesized and characterized by X-ray crystallography. It crystallizes in the triclinic system P-1 with a = 8.003(2) ?, b = 8.611(2) ?, c = 8.620(2) ?, α = 96.14(3)°, β = 116.66(2)°, γ = 105.66(4)° and V = 492.9(3) ?³. The structure consists of discrete centrosymmetric binuclear units and water molecules. The Cu(II) ions adopt a square-pyramidal coordination with four oxygen atoms of four bridging carboxylate and one carbonyl oxygen of the monodentate urea ligand. There is a very strong interaction between the two copper centers in binuclear entities (CuCu: 2.6266(15) ?).     

Synthesis and crystal structure of a cobalt(II) complex with tris(1-pyrazolylmethyl)amine

The synthesis of a cobalt(II) complex of tris(1-pyrazolylmethyl)amine (amtp) is reported. The complex [Co(amtp)Cl](BPh₄) crystallizes in the space group P-1, with a = 8.979(2), b = 19.329(3), c = 20.251(3) Å, = 93.321(2), = 93.685(3), = 98.930(2)°, and Z = 4. The Co(II) atom is nearly tetrahedrally coordinated by three pyrazole N-atoms and one Cl^–. The tertiary amine N-atom of amtp is only weakly coordinated to Co(II) atom at a Co—N(amine) distance of ca 2.40 Å.     

Crystal structure and spectroscopy of bis-[bis(2-benzimidazolyl)propane]copper(II) bis(triflate)monohydrate, a copper complex with a geometry intermediate between tetrahedral and square planar

The structure of a mononuclear copper(II) compound with the ligand bis(2-benzimidazolyl)propane (abbreviated as tbz) is reported. The compound [Cu(tbz)₂](CF₃SO₃)₂(H₂O) crystallizes in the triclinic space group P , with a = 12.363(6), b = 13.218(9), c = 15.365(8) Å, = 82.74(5), = 68.04(4), = 65.30(5), and Z = 2. The Cu(II) atom has a geometry intermediate between tetrahedral and square planar, consisting of four nitrogen atoms of two tbz ligands. The Cu—N—Cu angles are about 135°, while the dihedral angle between them amounts to 62° (0° for square planar and 90° for a tetrahedron). Ligand field bands are observed at 10.2 × 10³, 13.8 × 10³, and 20.3 × 10³ cm^–1, while the most characteristic infrared vibrations of the triflate anion are observed at 1273, 1260, 1238, 1221, 1171, and 1157 cm^–1.     

Synthesis and crystal structure of Pr(mpo)3(DMSO)2 (Hmpo = 2-mercaptopyridine N-oxide)

A novel rare earth metal complex of 2-mercaptopyridine N-oxide (Hmpo) was synthesized and characterized by single crystal X-ray diffraction, element analysis, and IR spectroscopy. The complex Pr(mpo)₃(DMSO)₂ (Hmpo = 2-mercaptopyridine N-oxide) (DMSO = dimethyl sulfoxide) (C₁₉H₂₄N₃O₅S₅Pr) crystallizes in the triclinic system, space group with lattice parameters a = 9.570(2), b = 9.902(2), c = 15.743(3) Å. = 89.00(3), = 85.54(3), = 62.97(3)°, D _c =1.694 gcm^–3, Mr = 675.62, Z = 2. The coordination number of praseodymium (III) is eight, and its coordination geometry is a somewhat distorted bicapped trigonal prism. Surrounding Pr atom, three five-membered ring planes (Py, O, N, C, S) make dihedral angle of 84.86(7), 75.10(6), and 11.06(9)° respectively. One DMSO molecule is disordered and situated along a twofold axis with half-occupancy (occupation factor, G=0.5).     

Synthesis and crystal structures of four nickel(II) 1,5-naphthalenedisulfonate compounds

Four nickle(II) 1,5-naphthalenedisulfonate (1,5nds) complexes, namely [Ni(H₂O)₆] (1,5nds) (1), trans-[Ni(en)₂(H₂O)₂](1,5nds)·2H₂O (2), [Ni(tren)(H₂O)₂](1,5nds)·H₂O (3), and [Ni(dien)₂](1,5nds)·2H₂O (4), where en = ethylenediamine, tren = tris(2-aminoethyl)amine, and dien = diethylenetriamine, have been synthesized and structurally characterized. Compound 1 crystallizes in space group P2₁/c, with a = 13.200(2) Å, b = 6.6197(10) Å, c = 9.6001(14) Å, and = 92.005(3)° compound 2 crystallizes in space group C2/c, with a = 15.698(2) Å, b = 13.006(2) Å, c = 12.845(2) Å, and = 119.262(4) Å compound 3 crystallizes in space group P , with a = 8.8971(10) Å, b = 11.5440(13) Å, c = 11.9169(14) Å, = 77.254(2)°, = 74.079(2)°, and = 82.162(2)° compound 4 crystallizes in space group P2₁/c, with a = 10.3600(13) Å, b = 12.5650(16) Å, c = 9.9853(12) Å, and = 103.599(2)°. Compound 1 crystallizes in a typical inorganic–organic layered structure adopted by metal naphthalenesulfonate, while compounds 2–4 crystallize in a hybrid inorganic–organic pattern. Unlike their Cu²⁺ analogue, the sulfonate does not coordinate directly to Ni²⁺. The hydrogen bonds formed between sulfonate and water molecules are the predominant packing forces for all structures. The inherited inversion center of the 1,5nds anion is carried into the crystal structure and results in centrosymmetric crystallization of all compounds.     

EPR spectra of (L-aspartate)di(2-pyridyl)aminezinc(II) hydrate substitutionally copper(II) doped complex

The [(L-aspartate)di(2-pyridyl)aminezinc(II)]hydrate doped with traces of copper was prepared. Electron paramagnetic resonance spectra of the polycrystalline sample were recorded at room temperature by using the X-band of the EPR spectrometer. The observedg factors for the complex areg _‖=2.258 andg _⊥=2.066. TheA _‖ value is 165.10⁻⁴ cm⁻¹. The crystal and molecular structure of the complex are also reported. The complex crystallizes in the monoclinic system; space groupP2₁ witha=7.2053(11),b=10.447(2),c=10.812(2) Å, β=108.489(14)° andZ=2. The structure can be described in the crystal lattice as polymeric chains.     

EPR spectra of (L-aspartate)di(2-pyridyl)aminezinc(II) hydrate substitutionally copper(II) doped complex

The [(L-aspartate)di(2-pyridyl)aminezinc(II)]hydrate doped with traces of copper was prepared. Electron paramagnetic resonance spectra of the polycrystalline sample were recorded at room temperature by using the X-band of the EPR spectrometer. The observedg factors for the complex areg _‖=2.258 andg _⊥=2.066. TheA _‖ value is 165.10⁻⁴ cm⁻¹. The crystal and molecular structure of the complex are also reported. The complex crystallizes in the monoclinic system; space groupP2₁ witha=7.2053(11),b=10.447(2),c=10.812(2) Å, β=108.489(14)° andZ=2. The structure can be described in the crystal lattice as polymeric chains.     

Synthesis and crystal structure of a terephthalato-bridged copper(II) complex [Cu2(tpt)(bpy)2(H2O)4] [Cu2(tpt)3 (bpy)2(H2O)2]

A terephthalato-bridged copper(II) complex [Cu₂(tpt)(bpy)₂(H₂O)₄][Cu₂(tpt)₃(bpy)₂ (H₂O)₂] (1) (tpt = terephthalate, bpy =; 2,2'-bipyridine) was synthesized by the reaction of Cu(ClO₄)₂ 6H₂O and terephthalic acid in the presence of 2,2'-bipyridine in H₂O solution. Crystal structure of 1 was determined by X-ray diffraction analysis in the triclinic space group P , with a = 10.7327(10) Å, b = 11.1658(11) Å, c = 17.3768(16) Å, = 108.063(2), = 91.064(2), = 116.721(2), V = 1737.5(3) ų, and Z = 2. Both the anion and the countercation in 1 are copper(II) complexes linked by terephthalate bridges in the bis(monodentate) (syn–anti) mode. The anion and the countercation are also linked by two hydrogen bonds between coordinating water molecules and terephthalate ligand.     

Crystal structure of [Cu2(II)(dmpa)2(p-Cl-C6H5COO)2] (Hdmpa = N,N-dimethyl-3-amino-1-propanol)

The copper complex, [Cu₂(II)(dmpa)₂(p-Cl-C₆H₅COO)₂], has been prepared and its structure determined using X-ray crystallography. The dimer is a di-₂-alkoxo complex which is a five-coordinate copper dimer with unsupported alkoxo bridges. The complex crystallizes in the triclinic space group P-1 with a = 11.384(2), b = 14.636(5), c = 9.609(2) Å, = 100.07(2), = 104.33(3), = 72.79(2)°, V = 1471.8(7) ų, and Z = 2. The structure is comprised of discrete binuclear clusters in which the metal atoms are bridged by two alkoxo oxygens of the dmpa^– ligands. The Cu-O and Cu-N distances are in good agreement with those found for other copper(II) aminoalcoholato complexes. The Cu···Cu distance is 2.9765(6) Å. In the crystal, every two dimeric coordination molecules are combined together by the recognition through intermolecular hydrogen-bonding interactions between the apical water molecule and the non-coordinated O atom from the p-chlorobenzoato ligand, forminga tetramer.     

A new phase of the complex trinitratotris (triphenylphosphineoxide)neodymium(III)

The crystal structure of the complex [Nd(NO₃)(OPPh₃)] (1) was obtained by single-crystal X-ray diffraction. The central neodymium(III) ion is nine coordinate arranged in a tricapped trigonal prism geometry. Crystallization of 1 occurs in the centrosymmetric monoclinic space group P2₁/c (No. 14) with a = 14.6496(9), b = 18.4506(11), c = 20.5491(11); = 102.925(3)°; and Z = 4.     

The crystal and molecular structure of ammonium-bis(malonato) oxovanadium(IV) dihydrate

The title compound, (NH₄)₂[VO(C₃H₂O₄)₂]·2H₂O, crystallizes in the monoclinic space group P2₁/n, with a=7.1889(7), b=19.254(2), c=9.879(2) Å, β=108.19(1)^o, and Z=4. The VO²⁺ cation is five-fold coordinated with two malonate anions acting as bidentate ligands and a water molecule. Infrared and Raman spectra are also reported to attain a wider insight into the compound characteristics.     

Self-assembly in transition metal complexes: structural characterization of a copper histamine nitrate [Cu(II)(him)2(NO3)2]

A new monomeric copper (II) complex with histamine (him), [Cu(II)(him)₂(No₃)₂], has been prepared by the reaction of Cu(NO₃)₂ with histaminium dichloride and its structure was determined by x-ray crystallography. The complex crystallizes in the triclinic system, space group with a = 5.7238(4), b = 8.7094(7), c = 9.2481(11) Å, = 69.693(8), = 73.242(7), = 71.050(7)°, V = 400.84(6) ų, and Z = 1. The structure consists of discrete [Cu(II)(him)₂(NO₃)₂] molecules in which the metal atom is centrosymmetrically coordinated by two histamine ligands forming an equatorial plane with Cu–N(imidazole ring) being 2.032(2) and Cu–N(NH₂ group) being 2.023(2) Å. Two O atoms from nitrate anions coordinate on the elongated axial positions with Cu–O being 2.549(2) Å. In the crystal structure, the molecules are organized by hydrogen bonds forming a two-dimensional network.     

Synthesis and characterization of inorganic‐organic ZnS(aminopropane)n composite materials

The main goal of our work was the synthesis and characterization of ZnS(aminopropane)_n hybrid inorganic‐organic layered materials. The basic material of our investigation was ZnS(1,3‐dap)_1/2, (where dap denotes diaminopropane). Its crystal structure has been solved by X‐ray powder diffraction methods. This layered compound was prepared using 1,3‐diaminepropane, zinc sulphate (ZnSO₄) and tioacetamide (CH₃CSNH₂). We have also tried to obtain and characterize other materials: ZnS(1‐ap) and ZnS(1,2‐dap), where ap denotes aminopropane. But in these last two cases diffraction patterns were of much poorer quality, which prevented a full structural survey; thus we cannot directly prove that hybrid lamellar materials were obtained. All compounds were studied using X‐ray diffraction, chemical analysis, UV‐vis spectroscopy and scanning electron microscopy. Additionally, using X‐ray diffraction as a function of temperature, we obtained information about structural changes of obtained composite materials under temperature treatment. (© 2011 WILEY‐VCH Verlag GmbH & Co. KGaA, Weinheim)     

Crystal structure of [WI2(CO)3{P(OMe)3}2]

[WI₂(CO)₃{P(OMe)₃}₂]crystallizes in the orthorhombic space group Pca2₁, with a = 26.924(5), b = 10.726(2), c = 14.136(3) Å, and Z = 8. There are two molecules in the asymmetric unit, the metal atoms in each case being seven-coordinate with a capped fac-(CO)₃ octahedral geometry. The molecular dimensions in the two molecules are nearly identical. The W–P distance to the capping atom 2.397 Å (average) is significantly shorter than the other W–P distance, 2.525 Å (average).