Ninghai Hu

A novel one-dimensional manganese phosphomolybdate with rectangular cavities: [H3N(CH2)4NH3](H3O)2{[Mn(phen)2]4[MnMov12O30(HPO4)6(H2PO4)2]}·4H2O

Abstract A novel manganese phosphomolybdate, [H3N(CH2)4NH3](H3O)2{[Mn(phen)2]4[MnMov12O30(HPO4)6(H2PO4)2]}·4H2O 1, has been hydrothermally synthesized and structurally characterized by single crystal X-ray diffraction. The crystal data: triclinic, P 1 , a=14.172(7) A, b=16.547(2) A, c=16.679(3) A, α=62.881(12)°, β=73.83(3)°, γ=88.81(3)°. X-ray crystallography shows that the [Mn(phen)2] fragments are covalently bonded to the [Mn(Mo6P4)2] dimers leading to a one-dimensional chain with rectangular cavities occupied by tetramethylene-diamine cations and water molecules.

Synthesis and molecular structure of the five-coordinate zirconium complex (CH3C5H4)2ZrCl(α-C10H7COO)

Abstract Bis(methylcyclopentadienyl)chloro(α-naphthoyloxy)zirconium, (CH3C5H4)2Zr Cl(α-C10H7COO), has been synthesized by the reaction between (MeCp)2ZrCL2 and equimolar sodium α-naphthoate in toluene at room temperature. The molecular structure of the title complex was determined by X-ray diffraction. The molecules have a five-Coordinate bent metallocene structure in which the α-naphthoxyligand is bidentate [ZrO, 2.317(2), 2.260(2) A]. The remaining distances are [ZrCl, 2.521(1) A; ZrC, 480-2, 565 A; ZrcentCH3C5H4 2.217 and 2.230 A].

An organic-inorganic vanadium oxide with one-dimensional ladder-type structure: hydrothermal synthesis, structure and characterization of [V4O10(o-phen)(2)]

A novel organic-inorganic hybrid vanadium oxide [V4O10(o-phen)(2)], involving all vanadium atoms present in +5 oxidation, has been hydrothermally synthesized and characterized by elemental analysis, IR, UV-vis, ESR, XPS spectra and TG-DTA thermal analysis. The single-crystal X-ray diffraction shows that the red-brown crystal is formed in the triclinic system, space group P (1) over bar, a = 9.782(2), b = 6.5124(14), c = 19.765(4) Angstrom, alpha = 89.94(2)degrees, beta = 100.66(2)degrees, gamma = 89.86(2)degrees. The title compound exhibits an infinite one-dimensional ladder-type tetravanadate skeleton with organonitrogen donors of o-phenanthroline ligands coordinated directly to the vanadium oxide framework.

Hydrothermal synthesis and crystal structure of a novel compound: [Ni(phen) 3 ] 2 [SiMo 10 V IV 2 O 40 (V IV O) 2 ]·2H 2 O

Abstract A novel compound [Ni(phen)3]2[SiMo10VIV2O40(VIVO)2]·2H2O has been hydrothermally synthesized and structurally characterized by single-crystal X-ray diffraction. The compound crystallizes in the triclinic system, space group P-1, a=12.378(4) A , b=14.148(5) A , c=14.316(2) A , α=105.91(2)°, β=95.31(2)°, γ=96.89(3)°, V=2373.0(12) A 3 , Z=1, (λ Mo Kα )=0.71073 A , R1(wR2)=0.0869(0.2174). Data were collected on a Siemens P4 four-circle diffractometer at 293 K in the range of 1.51

Hydrothermal synthesis, crystal structure and properties of [HPDA][H 2 PDA] 2 [As 2 III AsMo 8 V 4 O 40 ]·3H 2 O (PDA=propane diamine)

Abstract [NH 3 CH 2 CH 2 CH 2 NH 2 ][NH 3 CH 2 CH 2 CH 2 NH 3 ] 2 [As 2 III As V Mo 8 V 4 IV O 40 ]·3H 2 O was hydrothermally synthesized and structurally characterized by single crystal X-ray diffraction. Crystal data: monoclinic, C 2/ c , a=45.375(9) A , b=11.774(2) A , c=23.438(5) A , β =96.62(3)°. X-ray crystallographic study showed that the crystal structure was constructed by bicapped α-Keggin fragments [As 2 III As V Mo 8 V 4 IV O 40 ] 5− polyoxoanion. The title compound had a high catalytic activity for the oxidation of benzaldehyde to benzoic acid using H 2 O 2 as oxidant in a liquid–solid biphase system.

Synthesis, properties and molecular structure of five-coordinate N,N-dibenzyldithiocarbamate complexes of titanocene, zirconocene and hafnocene

The five complexes (RC5H4)2M(S2CNBz2)Cl (R = H, CH3; M = Ti, Zr, Hf; Bz = CH2C6H5) have been prepared by the reaction of (RC5H4)2MCl2 with anhydrous sodium salts of dibenzyldithiocarbamate in refluxing CH2Cl2. These complexes have been characterized by elemental analysis, IR and H-1 NMR. X-ray crystal structure determination of Cp2Zr(S2CNBZ2)Cl shows the molecule has a five-coordinate bent metallocene geometry in which the zirconium atom is attached to two eta-5-C5H5 groups, one bidentate dibenzyldithiocarbamate ligand and one chlorine [Zr-Cl, 2.549(1) angstrom; Zr-S, 2.734(1), 2.667(1); Cl-Zr-S, 137.6(1)-degrees and 73.3(1)-degrees; S-Zr-S, 64.3(1)-degrees]. The catalytic system Cp2Ti (S2CNBZ2)Cl-NaH exhibits high initial catalytic activity of hydrogenation of hexene-1 under mild conditions.

Aqueous synthesis and molecular structure of a seven-coordinate complex (η-CH3C5H4)Zr(S2CNBz2)3

Abstract The title complex is conveniently prepared by the reaction of (MeCp)2ZrCl2 (MeCp = η-methylcyclopentadienyl) with 3 equivalents of NaS2CNBz2 in the water phase containing acetylacetone. The crystal and molecular structure of (η-methylcyclopentadienyl)tri(N,N-dibenzylthiocarbamato)zirconium(IV) has been determined by X-ray diffraction. The crystal contains two different seven-coordinate molecules (A and B) which both have pentagonal bipyramidal geometry. The zirconium is attached to one η-methylcyclopentadienyl ligand occupying the axial position. One of the bidentate dithiocarbamate ligands spans the other axial position and one equatorial position; the other two bidentate dithiocarbamato ligands take the remaining equatorial positions (ZrC = 2.509–2.569 A; ZrS = 2.658–2.717 A).