A new layered mixed valence vanadium oxide, [CH 3NH 3] 2[(V ⅣO) 2(V ⅤO 4) 2], which contains interlamellar organic cations was prepared under hydrothermal conditions and its single crystal structure was determined. It crystallizes in a triclinic system with space group P 1, a =0 625 59(8) nm, b =0 639 84(9) nm, c =0 747 19(10) nm, α =78 718(2)°, β =80 099(2)°, γ =77 100(2). The compound contains mixed valence V 4+ /V 5+ vanadium oxide layers constructed from VO 4 tetrahedra, pairs of edge sharing VO 5 square pyramid and methylamine with protonated organic amines occupying the interlayer space.
A novel complex, (H 3O) 2[Ni(2,6-pydc) 2]·2H 2O was synthesized in an aqueous solution and characterized by means of single-crystal X-ray diffraction, elemental analyses and IR spectra. The X-ray structural analysis revealed that the novel compound forms three-dimensional(3D) networks by both π-π stacking and hydrogen-bonding interactions. The crystal data for the complex are a=13.853(3) nm, b=9.6892(19) nm, c=13.732(3) nm, α=90.00°, β=115.52(3)°, γ=90.00°, Z=3, R 1=0.0786, wR 2=0.1522.
The oxidation of Na4Fe(CN)6 complex by S2O8 2- anion was found to follow an outer-sphere electron transfer mechanism. We firstly carried out the reaction at pH=1. The specific rate constants of the reaction, kox, are (8.1± 0.07)×10-2 and (4.3±0.1)×10-2 mol-1?L?s-1 at μ=1.0 mol?L-1 NaClO4, T=298 K for pH=1 (0.1 mol?L-1 HClO4) and 8, respectively. The activation parameters, obtained by measuring the rate constants of oxidation 283—303 K, were ?H≠=(69.0±5.6) kJ?mol-1, ?S≠=(-0.34±0.041)×102 J?mol-1?K-1 at pH=1 and ?H≠= (41.3±5.5) kJ?mol-1, ?S≠=(-1.27±0.33)×102 J?mol-1?K-1 at pH=8, respectively. The cyclic voltammetry of Fe(CN)36 -/4- shows that the oxidation is a one-electron reversible redox process with E1/2 values of 0.55 and 0.46 V vs. normal hydrogen electrode at μ=1.0 mol?L-1 LiClO4, for pH=1 and pH=8 (Tris), respectively. The kinetic results were discussed on the basis of Marcus theory.
A novel compound, (HGly) 4[HPMo 12 O 40 ] 2·22H 2O, was synthesized and characterized by means of elemental analysis, IR and X ray diffraction. The compound crystallized in a monoclinic space group Cc with a =4 0060(0 8) nm, b =1 2527(0 3) nm, c =1 9930(0 4) nm, β =96 36(3)°, V =9 940(3) nm 3, Z =2, R 1=0 0576, wR 2 =0 1746. The anti tumor activity of this compound was tested in two human tumor cell lines in vitro .
The open-framework iron phosphate IIIII21.543FeFe(PO) was hydrothermally synthesized and characterized by elemental analysis, IR, EPR, XPS and single crystal X-ray diffraction analysis. The title compound crystallized in the triclinic, space group P1with a=0.64724(4) nm, b=0.79651(6) nm, c=0.94229(5) nm, =104.447(2)? =108.919(4)? =101.741(4)? V=0.42302(5) nm3, Z=1 and R1 (wR2)=0.0307 (0.0793). Crystal data were collected on a Rigaku R-AXIS RAPID IP diffractometer with Mo K?(=0.071073 nm) at 293(2) K in the range of 2.43埃迹?7.46? The structure of 1 consists of 19 non-hydrogen atoms including three and a half crystallographically in-dependent Fe and three P atoms. Fe(1) connects its symmetrical Fe(1A) through bridging oxygen forming a dimer and the dimers are connected by Fe(4) forming an infinite staircase-like chain. Fe(2) and Fe(3) connect the infinite chains into a layer with bridging oxygen. Layers are interconnected via Fe(4) forming the six-membered and eight-membered channel systems.
The title compound [(CH 3CH 2) 4N] 4H 3O{Na[(HMo 2O 5) 3(HPO 4)(H 2PO 4) 3] 2}·(H 2PO 4) 2·10H 2O was synthesized by hydrothermal method and its structure was determined with single crystal X ray analysis. The cluster anion of the title compound shows a P1 symmetry sandwich structure. The crystal is triclinic, space group P 1 with a =15.151 3(2) nm, b =15.851 7(10) nm, c =23\^025 1(10) nm, α = 89.00(1)° , β =80.09(3)°, γ = 74.30(2)°, V =5.241 90(8) nm 3, Z =2, D c=2.105 g/cm 3, F (000)=3 270, S =1.039, μ =1. 655 mm -1 .
Decavanadium oxide [Co 2Cl 8V 10 O 18 (H 2O)]Cl 2·6H 2O was synthesized hydrothermally with NH 4VO 3, Na 2MoO 4·2H 2O, H 3PO 4(85%), CoCl 2·6H 2O and hexamethylenetetraamine. The X ray diffraction analysis showed that [Co 2Cl 8V 10 O 18 (H 2O)]Cl 2·6H 2O crystallized in a monoclinic crystal system, the space group was C2/m with cell parameters a =1 6065(3) nm, b =2 2699(5) nm, c =1 3897(3) nm, β = 125.29(3)°, V =4 1363(14) nm 3, Z =2 and the final R =0 06, wR =0 1926. Its crystal structure is a 3 D open framework constructed by VO x polyhedra and CoCl 4 tetrahedra with channels along the crystallographic axes a, b, and c .
5-Fluorouracil salt(WBF) of 12-tungstoboric acid with Keggin structure was synthesized and its structure was characterized by IR, 1H NMR, 183 W NMR and elementary analysis. The MTT experimental results show that WBF has a stronger killing ability for liver cancer cells in vitro. The acute toxicity of WBF was carried out. The half toxicity dose LD_ 50 of WBF orally administrated to mice is 1 117.4 mg/kg. [WT5HZ]
