Xiao-Niu Fang

Synthesis, structure, photoluminescence and theoretical study of (MQ)(CdBr4) with MQ2+ generated In Situ (MQ2+ = N-Me-4,4′-bipyridinium)

A new compound (MQ)(CdBr4) (1; MQ2+ = N-Me-4,4′-bipyridinium), in which the MQ2+ was generated in situ, has been synthesized via hydrothermal reaction. The title compound features an isolated structure, based on discrete MQ2+ moieties and tetrahedral cadmium atoms terminally coordinated by four bromine atoms. The MQ2+ moieties and tetrabromo-cadmium dianions are linked via hydrogen bonds. Photoluminescent investigation reveals that the title compound displays a strong blue-light emission, which is attributed to a ligand-to-ligand charge-transfer (LLCT; from the HOMO of the bromine atoms to the LUMO+1 of the MQ2+ moieties) mechanism probed by molecular orbital (MO) calculations.

(E)-N′-(3-Chlorobenzylidene)isonicotinohydrazide

The molecule of the title compound, C13H9ClN3O, is roughly planar and displays a trans configuration with respect to the C=N double bond. The dihedral angle between the benzene and pyridine rings is 4.8 (3)degrees. The crystal structure is stabilized by intermolecular N-H center dot center dot center dot N hydrogen bonds.

Synthesis and structure of [Nd(C6NO2H5)3(H2O)2]2n· (3nHgCl4) · (4nH2O)

Abstract Hydrothermal reaction of NdCl3 · 6 H2O, HgCl2 and isonicotinic acid gave a bimetallic 4f-5d metal-isonicotinato complex [Nd(C6NO2H5)3(H2O)2]2n · (3nHgCl4) · (4nH2O) (1) and an X-ray crystal structure analysis reveals that it features a one-dimensional polycationic chain-like structure. The crystal belongs to the monoclinic, space group C2/c with a = 24.208(1), b = 20.842(1), c = 15.379(1) Å, β = 127.759(1)°, V = 6134.5(7) Å3, Z = 4, C36H46Cl12Hg3N6Nd2O20, Mr = 2198.44, Dc = 2.380 g/cm3, S = 0.986, μ(MoKα) = 9.738 mm–1, F(000) = 4112, R = 0.0384 and wR = 0.0848. The neodymium atom has a distorted square anti-prism geometry, coordinated by eight oxygen atoms. Each mercury atom is bound by four chlorine atoms to form a HgCl42– tetrahedron. The [Nd(C6NO2H5)3(H2O)2]2n6n+ species, HgCl42– anions and lattice water molecules are held together via hydrogen bonds to form a three-dimensional framework.

Synthesis and Crystal Structure of (Nd(C6NO2H5)3(H2O)2)nn(ZnCl4)·nCl·2.5nH2O with Novel Poly-Cationic Chain

The title complex, [Nd(C6NO2H5)3(H2O)2]nn[ZnCl4]·nCl·2.5nH2O (1), was obtained by hydrothermal reactions and structurally characterized by X-ray diffraction. The crystal structure analysis reveals that the title complex is characteristic of a novel polycationic [Nd(C6NO2H5)3(H2O)2]n3n+ one-dimensional chain-like structure.

{6,6′-Diethoxy-2,2′-[ethane-1,2-diylbis(nitrilomethylidyne)]diphenolato}trinitratosamarium(III)copper(II)

A heteronuclear Cu–Sm complex (systematic name: {6,60diethoxy-2,20-[ethane-1,2-diylbis(nitrilomethylidyne)]diphenolato-1 O,O 0 ,O,O 0 :2 O,N,N0,O 0 }trinitrato-1 O,O0-samarium(III)copper(II)), [CuSm(C20H22N2O4)(NO3)3], with the hexadentate Schiff base compartmental ligand N,N0-bis(3ethoxysalicylidene)ethylene-1,2-diamine, has been synthesized and structurally characterized. The Cu and Sm atoms are doubly bridged by two phenolate O atoms provided by the Schiff base ligand. The coordination of the Cu atom is square planar, formed by two imine N and two phenolate O atoms. The Sm atom has a decacoordination environment, formed by the phenolate O atoms, two ethoxy O atoms and two O atoms each from the three nitrates. No classical intermolecular hydrogen bonds are found. Some weak C—H O and O Cu interactions [O Cu = 3.167 (4) Å] generate a two-dimensional zigzag sheet.

(E)-N '-(3-Bromobenzylidene)isonicotinohydrazide

The title compound, C13H10BrN3O, is roughly planar and displays a trans configuration with respect to the C=N double bond. The dihedral angle between the benzene and pyridine rings is 4.2 (3)degrees. The crystal structure is stabilized by intermolecular N-H center dot center dot center dot N hydrogen bonds.

Crystal structure of [2-(diphenylphosphino)phenyliminoethyl]- ferrocene, Fe(C5H5)(C25H21NP)

C30H26FeNP, monoclinic, P21/n (no. 14), a = 10.750(2) Å, b = 9.077(2) Å, c = 24.489(5) Å, * = 90.85(3)°, V = 2389.3 Å, Z = 4, Rgt(F) = 0.042, wRref(F) = 0.113, T = 293 K. Source of material The raw material 2-(diphenylphosphino)aniline was prepared by a literature method [1], and acetylferrocene was commercially obtained. Acetylferrocene (1.14 g, 5.0 mmol), 5 Å molecular sieve (2.0 g) and 2-(diphenylphosphino)aniline (1.325 g, 5.0.mmol) were suspended in dried toluene (20 cm). The reaction mixtures were refluxed at stirring for 5 6 day. In order to control the progress of the condensation reaction the infrared spectra of the solutions were recorded. Daily addition of small quantities of the amine (0.2 g, 1 mmol) and molecular sieve (4 Å) was needed to force the displacement of the equilibria. This procedure was repeated for 5 6 day until the infrared spectra of the samples did not exhibit the band due to the asymmetrical stretching of the C=O group of the acetylferrocene [!(C=O) 1662 cm]. Then, the molecular sieves were removed by vacuum filtration and washed with ether until the liquid became colourless. The orange-red solution was concentrated on a rotary evaporator, and the oil formed was treated with methylene dichloride (10 cm). Slow evaporation of the solvent afforded the red crystal of the title compound (1.950 g, yield 81 %). Discussion Ferrocene and its derivatives have attracted much attention for their potential applications as molecular sensors, magnetic and optical materials, and in homogeneous catalysis. Several studies on the Schiff base containing-ferrocene have been reported recently [2-6]. The title molecule is in a trans configuration of the benzene ring and the cyclopentadienyl ring in respect to the N=C11 bond; the dihedral angle between the planes C6-C10 and N/C13-C18 is 45(1)°. In the ferrocen group, the Fe—C bond lengths are within the normal range [7]. The Fe1···Cg1 and Fe1···Cg2 distances are 1.629 Å and 1.634 Å, respectively, and the Cg1···Fe···Cg2 angle is 178.9°, where Cg1 and Cg2 are the centroids of the substituted and unsubstituted Cp rings, respectively. The two Cp rings are almost eclipsed, with a dihedral angle of 1.4° , and the largest torsion angle C2···Cg1···Cg2···C9 is 6.1°. In the triphenylphosphine group, the P atom adopts a slightly distorted pyramidal coordination. Z. Kristallogr. NCS 224 (2009) 649-650 / DOI 10.1524/ncrs.2009.0286 649

1-(2-Fluoro-benz-yl)-1-(2-fluoro-benz-yl-oxy)urea.

In the title hydroxyurea derivative, C15H14F2N2O2, the dihedral angle between the two benzene rings is 48.64 (19)°. The urea group forms dihedral angles of 48.1 (2) and 79.2 (2)° with the two benzene rings. In the crystal, inversion dimers linked by pairs of N—H⋯O hydrogen bonds occur, and further N—H⋯O links lead to chains of molecules.

catena-Poly[bis{μ-dihydrogen [(5-carboxypentylimino)dimethylene]diphosphonato-κ2O:O′}cadmium(II)]

The title compound, [Cd(C(8)H(18)NO(8)P(2))(2)](n), synthesized by hydrothermal methods, exhibits a layered structure in which the Cd(II) ion, occupying a centre of symmetry, is coordinated by six O atoms from four phosphonate ligands. The crosslinkage of CdO(6) octahedra by bridging phosphonate ligands results in a cadmium(II) phosphonate layer. Within the layer, there exists a 16-membered ring incorporating four -Cd-O-P-O- linkages. The uncoordinated carboxyl group of the ligand is oriented so that it penetrates the adjacent layer, taking part in hydrogen bonding to two uncoordinated phosphonate O atoms to form a CO(2)H/HO(2)P motif.

Hydrothermal Synthesis, Crystal Structure and Spectroscopic Investigations of [Y(C6NO2H5)3(H2O)2]n(1.5nZnCl4)•nH2O with Unprecedented Polycationic Chains

Abstract A new heterometallic 4 f -3 d complex [Y(C 6 NO 2 H 5 ) 3 (H 2 O) 2 ] n (1.5 n ZnCl 4 ). n H 2 O( 1 ), was synthesized via a hydrothermal reaction and structurally characterized. Complex 1 crystallized in the monoclinic system with space group P 2 1 / c : a =0.94847(9) nm, b =2.0947(2) nm, c =1.6001(2) nm, β=104.467(2)°, V -3.0781(5) nm 3 , M r =823.04, D c =1.776 g/cm 3 , S =1.009, μ(Mo K α)=3.603 mm −1 , F (000)=1632, R =0.0787, and wR =0.2273. Complex 1 , with four formula units in a cell, was characteristic of a one-dimensional polycationic chain-like structure. Photolumincscent investigation showed that the title complex displayed a strong emission in the blue region, which was attributed to the intraligand π-π * transition of the nicotinic ligands. Optical absorption spectrum of complex 1 revealed the presence of a wide optical bandgap of 4.17 eV.