The title complex [Cu2(bipy)2(Hpht)2Cl](Hpht) (bipy = 2,2?-bipyridine, H2pht = o-phthalic acid) has been synthesized in the NaOH aqueous solution of CuCl2, Gd(NO3)3, bipy and H2pht, and its crystal structure was det...The title complex [Cu2(bipy)2(Hpht)2Cl](Hpht) (bipy = 2,2?-bipyridine, H2pht = o-phthalic acid) has been synthesized in the NaOH aqueous solution of CuCl2, Gd(NO3)3, bipy and H2pht, and its crystal structure was determined by single-crystal X-ray diffraction method. It crys- tallizes in triclinic, space group P1, C44H31ClCu2N4O12, Mr = 970.26, a = 8.175(2), b = 16.254(4), c = 16.946(4) ?, α = 62.966(6), β = 84.833(8), γ = 84.348(8)°, V = 1993.4(8) ?3, Z = 2, Dc = 1.616 g/cm3, F(000) = 988 and μ = 1.207 mm-1. The final R = 0.0429 and wR = 0.0843 for 5682 observed reflections with I > 2σ(I). Each copper(II) atom displays a distorted square-pyramidal geometry with two nitrogen atoms of one chelate 2,2?-bipy molecule, two oxygen atoms from two different bridging carboxylate groups of Hpht- and one bridging chloride atom occupying the apical position. The two copper(II) atoms are connected by a μ2-Cl atom and two bridging Hpht- ligands in a syn-syn coordination mode to form an isolated dinuclear unit. The molecular structure is extended to a one-dimensional wavy chain through hydrogen bonds. The title complex exhibits blue fluorescent emission at 443 nm (λex = 372 nm) in the solid state at room temperature.展开更多
High diffraction quality crystals of cucurmosin, a type I ribosome inactivating protein isolated from the sarcocarp of Cucurbita moschata (pumpkin), have been grown under newly optimised conditions. With in-house rota...High diffraction quality crystals of cucurmosin, a type I ribosome inactivating protein isolated from the sarcocarp of Cucurbita moschata (pumpkin), have been grown under newly optimised conditions. With in-house rotating anode X-ray source, these crystals diffract to 1.65 ?resolution which is much higher than that of the previously reported crystals that diffracted only to 3 ?resolution. The crystals belong to space group P212121 with cell parameters a = 41.5, b = 58.4 and c = 99.3 . Molecular replacement studies indicate that the cucurmosin structure is homologous to trichosanthin. The initial structural model has been obtained and the model fitting/ refinement is in progress.展开更多
The heterotrinuclear cluster compound [MoW_2O_2 (O_2CC_2H_5 )_6-( H_2O)_3] ZnBr4·4H_2O was prepared by the redox reaction of Mo (CO)_6 with Na_2W_O4 in propionic anhydride. The crystal is monoclinic of space grou...The heterotrinuclear cluster compound [MoW_2O_2 (O_2CC_2H_5 )_6-( H_2O)_3] ZnBr4·4H_2O was prepared by the redox reaction of Mo (CO)_6 with Na_2W_O4 in propionic anhydride. The crystal is monoclinic of space group P2/c with a =16. 334(4) , b= 9. 657(5) , c=19. 889(9) ,β= 139. 79 (5)°,V= 2026 (2) ￣3 , Z=2 , D_c=2. 30 g/cm￣3 μ(MoKa) =106. 6 cm￣(-1) ,F(000)=1176 ,final R=0. 065 and R_ω=0. 072 for 1964 reflections with I≥3σ(I). In the structure of cation [MoW_2O_2 (O_2CC_2H_5 )_6 (H_2O)_3]￣(2+) molybdenum and tungsten atoms are statistically disordered. Three metal atoms form an equilateral triangle with the distance of M-M being 2. 735.展开更多
The hydro(solvo)thermal reactions of cobalt powder or its chloride with 2,5- pyridine dicarboxylic acid (H2PYDC) yielded two new complexes: [Co(II)2(PYDC)2(H2O)2- (H2O)4]n 1 and {Co(II)[NH2(CH3)2]2(PYDC)2}n 2. It is o...The hydro(solvo)thermal reactions of cobalt powder or its chloride with 2,5- pyridine dicarboxylic acid (H2PYDC) yielded two new complexes: [Co(II)2(PYDC)2(H2O)2- (H2O)4]n 1 and {Co(II)[NH2(CH3)2]2(PYDC)2}n 2. It is observed that the reactive solvents result in different connectivity modes of ligand and diverse dimensional extension of crystal structures. The correlation between structure and magnetic property will be discussed in this paper. Crystal data for 1: space group P1, a = 7.0419(17), b = 8.937(2), c = 9.6182(19) ?, α = 91.532(4), β = 99.869(10), γ = 107.889(11)o, V = 565.5(2) ?3, Z = 1, Dc = 1.845 g/cm3, μ = 1.56 mm-1, F(000) = 322 , R = 0.0505 and wR = 0.1580; and those for 2: space group C2/c, a = 14.9075(6), b = 8.2523(3), c = 16.9643(2) ?, β = 100.982(2)o, V = 2048.75(11) ?3, Z = 4, Dc = 1.560 g/cm3, μ = 0.892 mm-1, F(000) = 996, R = 0.0443 and wR = 0.1134.展开更多
The self-assembly of a flexible bipyridyl ligand 2,2?-bis(4-pyridylmethyle- neoxy)-1,1?-biphenylene (4,4?-bpp) with cobalt(II) center gave rise to a one-dimensional chain complex [Co(μ-4,4?-bpp)2(SCN)2?H2O]n 1 which ...The self-assembly of a flexible bipyridyl ligand 2,2?-bis(4-pyridylmethyle- neoxy)-1,1?-biphenylene (4,4?-bpp) with cobalt(II) center gave rise to a one-dimensional chain complex [Co(μ-4,4?-bpp)2(SCN)2?H2O]n 1 which has been characterized by single-crystal X-ray diffraction. The polymer crystallizes in monoclinic, space group C2/c with unit cell parameters: a = 13.1888(13), b = 24.230(2), c = 15.4218(17) ?, β = 93.291(6)o, V = 4920.1(8) ?3, Z = 4, C50H42CoN6O5S2, Mr = 929.95, Dc = 1.255 g/cm3, F(000) = 1932 and μ(MoKα) = 0.484 mm-1. The final R and wR are 0.0691 and 0.1670 for 3746 observed reflections with I > 2σ(I). 1 possesses an infinite 1-D polymeric chain structure consisting of the repeated basic square units Co2(μ-4,4?-bpp)2, where the Co(II) center acts as the joint of the square ring. The Co(II) center is coordinated in a slightly distorted octahedral geometry with four nitrogen atoms from four different 4,4?-bpp ligands in the equatorial plane and two trans thiocyanate ligands occupying the axial positions, preventing the formation of an extended framework.展开更多
A one dimension solid and a two dimension solid consisting of polyoxoanions bridged by {CoO 3N 2} and {CoO 4} groups respectively have been synthesized by the hydrothermal method and structurally characterized by...A one dimension solid and a two dimension solid consisting of polyoxoanions bridged by {CoO 3N 2} and {CoO 4} groups respectively have been synthesized by the hydrothermal method and structurally characterized by X Ray crystallography. Each structure has the [(PO 4) 4Mo 6O 15 ] 12- cluster that is commonly observed in many molybdophosphates. In compound 1, [(PO 4) 4Mo 6O 15 ] 12- clusters are linked by {CoO 3N 2} groups to form a chain like structure, and the chains are hydrogen bonded into a network. Compound 2 is a layer structure with channnels constructed from [(PO 4) 4Mo 6O 15 ] 12- clusters and {CoO 4} groups, the organic molecules and the lattice water molecules are distributed disorderly in the interlamellar region and form strong hydrogen bonds with inorganic framework. The IR and the fluorescent spectra were investigated and discussed.展开更多
A hydrothermal reaction of copper acetate with ammonium molybdate, 4,4-bpy (4,4-bipyridine) and 1,10-phen (1,10-phenanthroline) led to the formation of brown crystals of [Cu2(1,10-phen)2(4,4-bpy)]2 [Mo8O26]4H2O 1. Si...A hydrothermal reaction of copper acetate with ammonium molybdate, 4,4-bpy (4,4-bipyridine) and 1,10-phen (1,10-phenanthroline) led to the formation of brown crystals of [Cu2(1,10-phen)2(4,4-bpy)]2 [Mo8O26]4H2O 1. Single-crystal X-ray analysis has revealed that 1 (C68H56N12O30Cu4Mo8) crystallizes in the triclinic system, space group P with a = 11.270(3), b = 13.113(6), c = 13.906(3) ? = 103.33(4), b = 98.54(2), g = 101.29(2)? V = 1920.1(1) ?3, Mr = 2542.93, Z = 1, Dc = 2.199 g/cm3, m = 2.435 mm-1, F(000) = 1240, the final R = 0.0445, wR = 0.1082 and S = 1.021 for 5052 observed reflections with I >2s(I). It consists of copper (Ⅰ) tetramer units and -[Mo8O26]4- anions, which are further attached into a three-dimensional framework through hydrogen bonding and - stacking interactions.展开更多
The Cr doped into TiO2(110) surface has been studied systematically by using periodic DFT/B3LYP method with slab model. It is found that doping Cr into perfect TiO2 (110) surface can reduce the value of band-gap from ...The Cr doped into TiO2(110) surface has been studied systematically by using periodic DFT/B3LYP method with slab model. It is found that doping Cr into perfect TiO2 (110) surface can reduce the value of band-gap from 3.13 to 1.16 eV, and then photocatalysis reaction may be achieved in visual light area. The results are in good agreement with the experiments.展开更多
The crystal structure of the title compound {[Mn(phen)2(OAc)(H2O)]ClO4}2H2O (phen = 1,10-phenanthroline) has been synthesized and determined by X-ray diffraction. The crystal is of triclinic, space group P?with a = 12...The crystal structure of the title compound {[Mn(phen)2(OAc)(H2O)]ClO4}2H2O (phen = 1,10-phenanthroline) has been synthesized and determined by X-ray diffraction. The crystal is of triclinic, space group P?with a = 12.7955(4), b = 15.0544(4), c = 16.2183(4) , ?= 64.479(1), b =67.526(1), g = 83.582(1), C52H40Cl2Mn2N8O15, Mr = 1197.70, V = 2600.1(1) ?, Dc = 1.530 g/cm3, F(000) = 1224, = 0.666 cm-1 and Z = 2. The final refinement gave R = 0.0691 and wR = 0.1821 for 6131 observed reflections with I > 2s(I). The cell of the complex contains two uniform mono-manganese molecules [Mn(phen)2(OAc)(H2O)]ClO4 and a solvate water molecule. Four nitrogen atoms from two chelating phenanthroline ligands and one oxygen atom from acetate ligate to the MnⅡ ion, forming a distorted octahedral geometry together with one coordinated water molecule. One ClO4- anion and one water molecule exist outside the cation [Mn(phen)2(OAc)- (H2O)]+ as a counter ion and solvate molecule, respectively.展开更多
The solvothermal reaction of H3dhpmc (H3dhpmc = 2, 4-dihydroxypyrimidine- 5-carboxylic acid), CuCl2稨2O and NaVO3 results in the formation of a discrete mononuclear Cu(Ⅱ) complex [Cu(H2dhpmc)2]?H2O. It crystallizes i...The solvothermal reaction of H3dhpmc (H3dhpmc = 2, 4-dihydroxypyrimidine- 5-carboxylic acid), CuCl2稨2O and NaVO3 results in the formation of a discrete mononuclear Cu(Ⅱ) complex [Cu(H2dhpmc)2]?H2O. It crystallizes in monoclinic system, space group P21/c with a = 5.0497(9), b = 10.0196(6), c = 13.715(2) ? b = 96.237(1)? V = 689.8(2) 3, Z = 2, Dc = 1.973 g/cm3, ?= 1.654 mm-1, F(000) = 414, R = 0.0736 and wR = 0.1351. Each Cu(Ⅱ) is coordinated to four oxygen atoms of two 2, 4-dihydroxypyrimidine-5-carboxylic acid ligands in the equatorial position and two oxygen atoms of two water molecules in the axial position to form an axially elongated octahedral geometry. The title complex is further linked into a three-dimensional structure through the weak interactions of hydrogen bonds between the oxygen atoms and the nitrogen atoms.展开更多
A new phase of dibarium copper disilicate, b-Ba2CuSi2O7, was obtained by the solid-state reaction. Crystal data: Mr = 506.4, tetragonal, P421m, a = 8.284(2), c = 5.313(3) ? V = 364.6(4) ?, Z = 2, Dc = 4.61 g/cm3, l(Mo...A new phase of dibarium copper disilicate, b-Ba2CuSi2O7, was obtained by the solid-state reaction. Crystal data: Mr = 506.4, tetragonal, P421m, a = 8.284(2), c = 5.313(3) ? V = 364.6(4) ?, Z = 2, Dc = 4.61 g/cm3, l(MoKa) = 0.71703 ? ?= 13.91 mm-1, F(000) = 450 and T = 293(2) K; the final R = 0.0343, wR = 0.0382 and S = 1.02 for 512 observed reflections (I > 3s(I)) refined by 34 variables. The compound was characterized by a layered structure composed of CuO4 tetrahedra and Si2O7 anions with the Ba cations filling the cavities between the layers. The building blocks of the present structure are similar to those in the a-Ba2CuSi2O7, but the linkage of CuO4 tetrahedra and Si2O7 anions is significantly different. In particular, the double-tetrahedral anions of Si2O76- form an orthogonal arrangement in the present structure, in contrast to the parallel arrangement reported in the a-Ba2CuSi2O7.展开更多
A new cluster {Mo3S4[NH2CH2CH(O)CH2NH2]3}(DTP)?(H2O)2?(DMF) (DTP = diethyldithiophosphate) has been synthesized via ligand substitution reaction of Mo3S4(DTP)4(H2O) with an alkaline ligand 1,3-diamino-2-propanol(DAPRO...A new cluster {Mo3S4[NH2CH2CH(O)CH2NH2]3}(DTP)?(H2O)2?(DMF) (DTP = diethyldithiophosphate) has been synthesized via ligand substitution reaction of Mo3S4(DTP)4(H2O) with an alkaline ligand 1,3-diamino-2-propanol(DAPROH) in a mixed organic solvent, and its crys- tal structure was determined with the following data: Mo3S6PC16H48O8N7, Mr = 977.76, triclinic, space group P1, Z = 2, a = 10.319(2), b = 12.843(3), c = 15.335(3) ?, α = 65.26(3), β = 82.18(3), γ = 70.67(3)o, V = 1741.7(6) ?3, Dc = 1.864 g/cm3, μ = 1.517 mm-1, F(000) = 988, the final R = 0.0794 and wR = 0.2111 for 6318 observed reflections (I>2σ(I)). The structure analysis indicates that all DTP ligands of Mo3S4(DTP)4(H2O) are replaced and each DAPRO molecule acts as a tri- dentate ligand chelating to each Mo atom of the Mo3S4 core. Different from the precursor, the clus- ter symmetry is elevated to C3. In addition, the UV-spectrum of the title compound was measured.展开更多
The assembly of 1,4-benzenedicarboxylic acid (H2bdc), 4,4?bipyridine (4,4?bipy), trimethyltin chloride and MnBr24H2O in hydrothermal conditions gave rise to a hydrogen-bonded three-dimensional complex {[Mn(4,4?bipy)4H...The assembly of 1,4-benzenedicarboxylic acid (H2bdc), 4,4?bipyridine (4,4?bipy), trimethyltin chloride and MnBr24H2O in hydrothermal conditions gave rise to a hydrogen-bonded three-dimensional complex {[Mn(4,4?bipy)4H2O](bdc)}n which has been characterized by single- crystal X-ray diffraction. The complex crystallizes in the monoclinic system, space group P2/n with a = 7.0001(2), b = 11.5540(3), c = 11.4192(1) ? = 101.754(2)? V = 904.21(4) 3, Z = 2, C18H20MnN2O8, Mr = 447.30, Dc = 1.643 g/cm3, F(000) = 462 and m(MoK? = 0.783 mm-1. The final R and wR are 0.0499 and 0.1301, respectively for 1335 observed reflections with I ≥ 2(I). The Mn (Ⅱ) is six-coordinated in a distorted octahedral geometry. 4,4?Bipyridine in a m-bridge mode links [Mn(H2O)4]2+ into a linear cation chain. bdc acts as a counter anion and links the linear chains into a three-dimensional structure through hydrogen bonds.展开更多
A two-dimensional hydrogen-bonded cadmium(II) compound [Cd(dapm)2- (CH3COO)2(H2O)2] (dapm = diaminodiphenylmethane) has been synthesized and characterized by single-crystal X-ray diffraction analysis. It crystallizes ...A two-dimensional hydrogen-bonded cadmium(II) compound [Cd(dapm)2- (CH3COO)2(H2O)2] (dapm = diaminodiphenylmethane) has been synthesized and characterized by single-crystal X-ray diffraction analysis. It crystallizes in monoclinic, space group C2/c with a = 27.572(3), b = 5.5064(5), c = 23.310(2) , = 124.785(1)o, C15H19Cdo.5ON2O3, Mr =331.52, V = 2906.6(5) ?, Z = 4, Dc = 1.515 g/cm3, F(000) = 1368 and = 0.801 mm-1. The final R = 0.0403 and wR = 0.1014 for 1795 observed reflections with I≥4(I). The centrosymmetric Cd(II) is six- coordinated in a distorted octahedral geometry, and the dapm in a trans mode acts as a monoden- tate ligand. The intermolecular hydrogen bonds among coordinated aqua molecules with coordi- nated acetate oxygen atoms and uncoordinated dapm nitrogen atoms form a two-dimensional supramolecular framework.展开更多
The title complex, [Cu(L)Cl2]n (L = 2,5-di-2-pyridyl-1,3,4-oxodiazole) 1, has been obtained from the reaction of 3,6-di-2-pyridyl-1,2,4,5-tetrazine (bptz) and CuCl2?H2O in a mixture solvent of CH3CN and CH2Cl2 (L is g...The title complex, [Cu(L)Cl2]n (L = 2,5-di-2-pyridyl-1,3,4-oxodiazole) 1, has been obtained from the reaction of 3,6-di-2-pyridyl-1,2,4,5-tetrazine (bptz) and CuCl2?H2O in a mixture solvent of CH3CN and CH2Cl2 (L is generated from the metal-assisted hydrolysis reaction of bptz) and structurally characterized. It crystallizes in space group C2/c of monoclinic system with cell parameters: a = 9.812(2), b = 12.679(3), c = 11.111(2) ? b = 103.92(3)? V = 1341.6(5) 3, Z = 4, Dc = 1.776 g/cm3, Mr = 358.66, F(000) = 716, ?= 2.024 mm1 and S = 1.004. The final R = 0.0346 and wR = 0.0938 for 1011 observed reflections with I > 2(I). The Cu(Ⅱ) ion is six-coordinated by four N atoms of two L ligands and two Cl ions in a distorted octahedral geometry. The ligand L acts as a bis-bidentate ligand to bridge the Cu(Ⅱ) ions, resulting in an infinite chain structure.展开更多
The new oxovanadium (V) complex, [PyH][VO2(L)] 1 (salicyladehyde 5-bromo salicyloylhydrazone is abbreviated as H2L; Hpy is protonated pyridine) was obtained from a refluxed solution of VOSO4 and H2L in acetonitrile-me...The new oxovanadium (V) complex, [PyH][VO2(L)] 1 (salicyladehyde 5-bromo salicyloylhydrazone is abbreviated as H2L; Hpy is protonated pyridine) was obtained from a refluxed solution of VOSO4 and H2L in acetonitrile-methanol-pyridine. Similarly, another new complex, [VO(L)(OCH3)] 2 was synthesized by refluxing VOSO4 and H2L in methanol-pyridine. Crystal data for 1: C19H15N3O5BrV, Mr= 496.2, monoclinic, P21/n, a = 7.1885(3), b = 9.2718(3), c = 28.803(1) A, β = 96.185(1)°, Z = 4 and V = 1908.6(1) A3; for 2: C15H12N2O5BrV, Mr= 431.1, monoclinic, P2,/n, a = 12.202(2), b = 8.045(2), c = 16.604(3) A, β = 101.29(3)°, Z = 4 and V = 1598.4(2) A3. The structures of 1 and 2 have been determined by X-ray analyses and reveal that the coordination environments of V atoms in both complexes are of square-based pyramid. Three of the four based donor atoms are from the tridentate 'ONO' donor ligand while the fourth is one terminal oxygen atom with the V(1) - O(3) distance 1.646(4) A for 1 and one -OCH3 group with the V(1)-O(3) distance 1.753(3) A for 2. The V(1)-O(4) terminals occupy the axial sites in both cases. The complexes are also characterized by IR and 1H NMR spectroscopies.展开更多
Two silver(I) complexes were prepared by the reaction of [Ag(C≡CPh)]n with NP3 [NP3 = N(CH2CH2PPh2)3] or with NP3 and [Cu(CH3CN)4]ClO4. Complex 1 [(Ag2Cl(NP3)2)(Ag5- (C≡CPh)6)] contains both NP3 and PhC≡C- ligand...Two silver(I) complexes were prepared by the reaction of [Ag(C≡CPh)]n with NP3 [NP3 = N(CH2CH2PPh2)3] or with NP3 and [Cu(CH3CN)4]ClO4. Complex 1 [(Ag2Cl(NP3)2)(Ag5- (C≡CPh)6)] contains both NP3 and PhC≡C- ligands. The complex cation is (Ag2Cl(NP3)2)+, in which two Ag(NP3)+ cations were bridged by a Cl- donor. The anion is (Ag5(C≡CPh)6)-, where five Ag+ ions are linked by six C≡CPh- to form a pentanuclear cluster. Complex 2 only contains NP3 ligand, where the silver center adopts a trigonal-bipyramidal geometry. Crystal data for 1: C133H116Ag7Cl3- N2P6, Mr = 2789.54, triclinic, space group P1, a = 13.0780(2), b = 15.3678(2), c = 31.2041(3) ?, α = 91.3928(7), β = 90.9328(8), γ = 96.0244(4)o, V = 6233.8(1) ?3, T = 293(2) K, Z = 2, Dc = 1.486 g/cm3, F(000) = 2796, μ = 1.266 mm-1, the final R = 0.0746 and wR = 0.1953 for 16475 observed reflections with I > 2σ(I). Crystal data for 2: C42H42AgClNO4P3, Mr = 861.00, trigonal, space group R3, a = 17.451(1), b = 17.451(1), c = 11.3985(7) ?, V = 3006.0(3) ?3, T = 293(2) K, Z = 3, Dc = 1.427 g/cm3, F(000) = 1326, μ = 0.731 mm-1, the final R = 0.0251 and wR = 0.0663 for 1499 observed reflections with I > 2σ(I).展开更多
Crystals of the low temperature phase b-Ba3Y(BO3)3 have been synthesized by the flux method. The structure of the title compound crystallizes in the hexagonal system, space group P63cm with the following parameters: a...Crystals of the low temperature phase b-Ba3Y(BO3)3 have been synthesized by the flux method. The structure of the title compound crystallizes in the hexagonal system, space group P63cm with the following parameters: a = 9.416(3), c = 17.536(8) ? V = 1346.6(8) ?, Ba3YB3O9, Mr = 677.36, Z = 6, Dc = 5.012 g/cm3, l(MoKa) = 0.71073 ? m = 19.409 mm-1, Flack parameter = 0.02(3), F(000) = 1764, R = 0.0714 and wR = 0.1696 for 1076 observed reflections with I > 2s(I). The compound contains two sets of YO6 octahedra, four sets of BaO9 polyhedra and three sets of BO3 planar triangles.展开更多
The high temperature phase a-Ba3Y(BO3)3 was synthesized by Czochralski method, and its crystal structure has been determined by single-crystal X-ray diffraction. It crystallizes in the trigonal system, space group 3R ...The high temperature phase a-Ba3Y(BO3)3 was synthesized by Czochralski method, and its crystal structure has been determined by single-crystal X-ray diffraction. It crystallizes in the trigonal system, space group 3R with a = 13.028(2), c = 9.4992(2) ? V = 1396.1(5) ?, Ba3YB3O9, Mr = 677.36, Z = 6, Dc = 4.834 g/cm3, l(MoKa) = 0.71073 ? m = 18.721 mm-1, F(000) = 1764, the final R = 0.0718 and wR = 0.1640 for 1199 observed reflections with I > 2s(I). In this structure two alternate nonequivalent Y atoms form one-dimensional chains bridged by the Ba atoms with BO3 triangles which link Y(1) and Y(2), respectively. The Ba atom is surrounded by nine O atoms belonging to six BO3 triangles.展开更多
The title compound, {(H3O)4(NH4)4[Mo8O28]?2H2O}n 1, has been synthesized from the reaction of Zn(OAc)2 and (NH4)6Mo7O24?4H2O in aqueous solution at ambient tempe- rature, and its crystal structure was determined by ...The title compound, {(H3O)4(NH4)4[Mo8O28]?2H2O}n 1, has been synthesized from the reaction of Zn(OAc)2 and (NH4)6Mo7O24?4H2O in aqueous solution at ambient tempe- rature, and its crystal structure was determined by X-ray single-crystal analysis with the following crystallographic data: monoclinic system, space group P21/n, a = 9.5234(6), b = 11.3235(8), c = 14.8812(10) ?, β = 107.467(2)o, V = 1530.77(18) ?3, Z = 4, F(000) = 1336, μ = 3.293 mm-1 and Dc = 3.037 g/cm3. The final R = 0.0619 for 2691 observed reflections (I > 2σ(I)). X-ray crys- tal structure analysis showed that the novel one-dimensional chain compound is built up by basic {Mo8O28} units via single μ2-O, and such chains are further linked into a three-dimensional net- work by hydrogen bonds.展开更多
基金This work was supported by the National Natural Science Foundation of China (20001007 20131020)+1 种基金and Natural Science Foundation of Fujian Province (2003I031 A0420002)
文摘The title complex [Cu2(bipy)2(Hpht)2Cl](Hpht) (bipy = 2,2?-bipyridine, H2pht = o-phthalic acid) has been synthesized in the NaOH aqueous solution of CuCl2, Gd(NO3)3, bipy and H2pht, and its crystal structure was determined by single-crystal X-ray diffraction method. It crys- tallizes in triclinic, space group P1, C44H31ClCu2N4O12, Mr = 970.26, a = 8.175(2), b = 16.254(4), c = 16.946(4) ?, α = 62.966(6), β = 84.833(8), γ = 84.348(8)°, V = 1993.4(8) ?3, Z = 2, Dc = 1.616 g/cm3, F(000) = 988 and μ = 1.207 mm-1. The final R = 0.0429 and wR = 0.0843 for 5682 observed reflections with I > 2σ(I). Each copper(II) atom displays a distorted square-pyramidal geometry with two nitrogen atoms of one chelate 2,2?-bipy molecule, two oxygen atoms from two different bridging carboxylate groups of Hpht- and one bridging chloride atom occupying the apical position. The two copper(II) atoms are connected by a μ2-Cl atom and two bridging Hpht- ligands in a syn-syn coordination mode to form an isolated dinuclear unit. The molecular structure is extended to a one-dimensional wavy chain through hydrogen bonds. The title complex exhibits blue fluorescent emission at 443 nm (λex = 372 nm) in the solid state at room temperature.
基金Supported by the National Natural Science Foundation of China (39970872) NSF of Fujian province+1 种基金 and International Cooperation program of Fujian province to the State Key Laboratory of Structural Chemistry Fujian Institute of Research on the Struct
文摘High diffraction quality crystals of cucurmosin, a type I ribosome inactivating protein isolated from the sarcocarp of Cucurbita moschata (pumpkin), have been grown under newly optimised conditions. With in-house rotating anode X-ray source, these crystals diffract to 1.65 ?resolution which is much higher than that of the previously reported crystals that diffracted only to 3 ?resolution. The crystals belong to space group P212121 with cell parameters a = 41.5, b = 58.4 and c = 99.3 . Molecular replacement studies indicate that the cucurmosin structure is homologous to trichosanthin. The initial structural model has been obtained and the model fitting/ refinement is in progress.
文摘The heterotrinuclear cluster compound [MoW_2O_2 (O_2CC_2H_5 )_6-( H_2O)_3] ZnBr4·4H_2O was prepared by the redox reaction of Mo (CO)_6 with Na_2W_O4 in propionic anhydride. The crystal is monoclinic of space group P2/c with a =16. 334(4) , b= 9. 657(5) , c=19. 889(9) ,β= 139. 79 (5)°,V= 2026 (2) ￣3 , Z=2 , D_c=2. 30 g/cm￣3 μ(MoKa) =106. 6 cm￣(-1) ,F(000)=1176 ,final R=0. 065 and R_ω=0. 072 for 1964 reflections with I≥3σ(I). In the structure of cation [MoW_2O_2 (O_2CC_2H_5 )_6 (H_2O)_3]￣(2+) molybdenum and tungsten atoms are statistically disordered. Three metal atoms form an equilateral triangle with the distance of M-M being 2. 735.
基金Financially support by NNSFC (No. 20031020) NSF of Fujian Province and the Key Project from CAS
文摘The hydro(solvo)thermal reactions of cobalt powder or its chloride with 2,5- pyridine dicarboxylic acid (H2PYDC) yielded two new complexes: [Co(II)2(PYDC)2(H2O)2- (H2O)4]n 1 and {Co(II)[NH2(CH3)2]2(PYDC)2}n 2. It is observed that the reactive solvents result in different connectivity modes of ligand and diverse dimensional extension of crystal structures. The correlation between structure and magnetic property will be discussed in this paper. Crystal data for 1: space group P1, a = 7.0419(17), b = 8.937(2), c = 9.6182(19) ?, α = 91.532(4), β = 99.869(10), γ = 107.889(11)o, V = 565.5(2) ?3, Z = 1, Dc = 1.845 g/cm3, μ = 1.56 mm-1, F(000) = 322 , R = 0.0505 and wR = 0.1580; and those for 2: space group C2/c, a = 14.9075(6), b = 8.2523(3), c = 16.9643(2) ?, β = 100.982(2)o, V = 2048.75(11) ?3, Z = 4, Dc = 1.560 g/cm3, μ = 0.892 mm-1, F(000) = 996, R = 0.0443 and wR = 0.1134.
基金This work was supported by the National Natural Science Foundation of China (No. 20231020)
文摘The self-assembly of a flexible bipyridyl ligand 2,2?-bis(4-pyridylmethyle- neoxy)-1,1?-biphenylene (4,4?-bpp) with cobalt(II) center gave rise to a one-dimensional chain complex [Co(μ-4,4?-bpp)2(SCN)2?H2O]n 1 which has been characterized by single-crystal X-ray diffraction. The polymer crystallizes in monoclinic, space group C2/c with unit cell parameters: a = 13.1888(13), b = 24.230(2), c = 15.4218(17) ?, β = 93.291(6)o, V = 4920.1(8) ?3, Z = 4, C50H42CoN6O5S2, Mr = 929.95, Dc = 1.255 g/cm3, F(000) = 1932 and μ(MoKα) = 0.484 mm-1. The final R and wR are 0.0691 and 0.1670 for 3746 observed reflections with I > 2σ(I). 1 possesses an infinite 1-D polymeric chain structure consisting of the repeated basic square units Co2(μ-4,4?-bpp)2, where the Co(II) center acts as the joint of the square ring. The Co(II) center is coordinated in a slightly distorted octahedral geometry with four nitrogen atoms from four different 4,4?-bpp ligands in the equatorial plane and two trans thiocyanate ligands occupying the axial positions, preventing the formation of an extended framework.
文摘A one dimension solid and a two dimension solid consisting of polyoxoanions bridged by {CoO 3N 2} and {CoO 4} groups respectively have been synthesized by the hydrothermal method and structurally characterized by X Ray crystallography. Each structure has the [(PO 4) 4Mo 6O 15 ] 12- cluster that is commonly observed in many molybdophosphates. In compound 1, [(PO 4) 4Mo 6O 15 ] 12- clusters are linked by {CoO 3N 2} groups to form a chain like structure, and the chains are hydrogen bonded into a network. Compound 2 is a layer structure with channnels constructed from [(PO 4) 4Mo 6O 15 ] 12- clusters and {CoO 4} groups, the organic molecules and the lattice water molecules are distributed disorderly in the interlamellar region and form strong hydrogen bonds with inorganic framework. The IR and the fluorescent spectra were investigated and discussed.
基金This work was supported by the National Natural Science Foundation of China (20073048) NSF of Fujian and the Chinese Academy of Sciences
文摘A hydrothermal reaction of copper acetate with ammonium molybdate, 4,4-bpy (4,4-bipyridine) and 1,10-phen (1,10-phenanthroline) led to the formation of brown crystals of [Cu2(1,10-phen)2(4,4-bpy)]2 [Mo8O26]4H2O 1. Single-crystal X-ray analysis has revealed that 1 (C68H56N12O30Cu4Mo8) crystallizes in the triclinic system, space group P with a = 11.270(3), b = 13.113(6), c = 13.906(3) ? = 103.33(4), b = 98.54(2), g = 101.29(2)? V = 1920.1(1) ?3, Mr = 2542.93, Z = 1, Dc = 2.199 g/cm3, m = 2.435 mm-1, F(000) = 1240, the final R = 0.0445, wR = 0.1082 and S = 1.021 for 5052 observed reflections with I >2s(I). It consists of copper (Ⅰ) tetramer units and -[Mo8O26]4- anions, which are further attached into a three-dimensional framework through hydrogen bonding and - stacking interactions.
基金This work was supported by the State Key Laboratory of Structural Chemistry, the National Natural Science Foundation of China (20273013), and the Education Foundation of Fujian Province (JA03007)
文摘The Cr doped into TiO2(110) surface has been studied systematically by using periodic DFT/B3LYP method with slab model. It is found that doping Cr into perfect TiO2 (110) surface can reduce the value of band-gap from 3.13 to 1.16 eV, and then photocatalysis reaction may be achieved in visual light area. The results are in good agreement with the experiments.
基金This work was supported by the State Key Basic Research and Development Plan (G1998010100) and NNSFC (No. 30170229 29973047 and 39970177)
文摘The crystal structure of the title compound {[Mn(phen)2(OAc)(H2O)]ClO4}2H2O (phen = 1,10-phenanthroline) has been synthesized and determined by X-ray diffraction. The crystal is of triclinic, space group P?with a = 12.7955(4), b = 15.0544(4), c = 16.2183(4) , ?= 64.479(1), b =67.526(1), g = 83.582(1), C52H40Cl2Mn2N8O15, Mr = 1197.70, V = 2600.1(1) ?, Dc = 1.530 g/cm3, F(000) = 1224, = 0.666 cm-1 and Z = 2. The final refinement gave R = 0.0691 and wR = 0.1821 for 6131 observed reflections with I > 2s(I). The cell of the complex contains two uniform mono-manganese molecules [Mn(phen)2(OAc)(H2O)]ClO4 and a solvate water molecule. Four nitrogen atoms from two chelating phenanthroline ligands and one oxygen atom from acetate ligate to the MnⅡ ion, forming a distorted octahedral geometry together with one coordinated water molecule. One ClO4- anion and one water molecule exist outside the cation [Mn(phen)2(OAc)- (H2O)]+ as a counter ion and solvate molecule, respectively.
基金This work was supported by the National Natural Science Foundation of China
文摘The solvothermal reaction of H3dhpmc (H3dhpmc = 2, 4-dihydroxypyrimidine- 5-carboxylic acid), CuCl2稨2O and NaVO3 results in the formation of a discrete mononuclear Cu(Ⅱ) complex [Cu(H2dhpmc)2]?H2O. It crystallizes in monoclinic system, space group P21/c with a = 5.0497(9), b = 10.0196(6), c = 13.715(2) ? b = 96.237(1)? V = 689.8(2) 3, Z = 2, Dc = 1.973 g/cm3, ?= 1.654 mm-1, F(000) = 414, R = 0.0736 and wR = 0.1351. Each Cu(Ⅱ) is coordinated to four oxygen atoms of two 2, 4-dihydroxypyrimidine-5-carboxylic acid ligands in the equatorial position and two oxygen atoms of two water molecules in the axial position to form an axially elongated octahedral geometry. The title complex is further linked into a three-dimensional structure through the weak interactions of hydrogen bonds between the oxygen atoms and the nitrogen atoms.
基金the Innovative Project (No.IP01007) and Hundred-Talent Program (No. 990168) of the Chinese Academy of Sciences
文摘A new phase of dibarium copper disilicate, b-Ba2CuSi2O7, was obtained by the solid-state reaction. Crystal data: Mr = 506.4, tetragonal, P421m, a = 8.284(2), c = 5.313(3) ? V = 364.6(4) ?, Z = 2, Dc = 4.61 g/cm3, l(MoKa) = 0.71703 ? ?= 13.91 mm-1, F(000) = 450 and T = 293(2) K; the final R = 0.0343, wR = 0.0382 and S = 1.02 for 512 observed reflections (I > 3s(I)) refined by 34 variables. The compound was characterized by a layered structure composed of CuO4 tetrahedra and Si2O7 anions with the Ba cations filling the cavities between the layers. The building blocks of the present structure are similar to those in the a-Ba2CuSi2O7, but the linkage of CuO4 tetrahedra and Si2O7 anions is significantly different. In particular, the double-tetrahedral anions of Si2O76- form an orthogonal arrangement in the present structure, in contrast to the parallel arrangement reported in the a-Ba2CuSi2O7.
基金This work was supported by the State Key Basic Research and Development Plan of China (001CB108906)the NNSF of China (20173063) NSF of Fujian Province (E0020001)
文摘A new cluster {Mo3S4[NH2CH2CH(O)CH2NH2]3}(DTP)?(H2O)2?(DMF) (DTP = diethyldithiophosphate) has been synthesized via ligand substitution reaction of Mo3S4(DTP)4(H2O) with an alkaline ligand 1,3-diamino-2-propanol(DAPROH) in a mixed organic solvent, and its crys- tal structure was determined with the following data: Mo3S6PC16H48O8N7, Mr = 977.76, triclinic, space group P1, Z = 2, a = 10.319(2), b = 12.843(3), c = 15.335(3) ?, α = 65.26(3), β = 82.18(3), γ = 70.67(3)o, V = 1741.7(6) ?3, Dc = 1.864 g/cm3, μ = 1.517 mm-1, F(000) = 988, the final R = 0.0794 and wR = 0.2111 for 6318 observed reflections (I>2σ(I)). The structure analysis indicates that all DTP ligands of Mo3S4(DTP)4(H2O) are replaced and each DAPRO molecule acts as a tri- dentate ligand chelating to each Mo atom of the Mo3S4 core. Different from the precursor, the clus- ter symmetry is elevated to C3. In addition, the UV-spectrum of the title compound was measured.
基金supported by the National Natural Science Foundation of China (No. 29890210) and the Key Project of the Chinese Academy of Sciences (KJCX2-H3)
文摘The assembly of 1,4-benzenedicarboxylic acid (H2bdc), 4,4?bipyridine (4,4?bipy), trimethyltin chloride and MnBr24H2O in hydrothermal conditions gave rise to a hydrogen-bonded three-dimensional complex {[Mn(4,4?bipy)4H2O](bdc)}n which has been characterized by single- crystal X-ray diffraction. The complex crystallizes in the monoclinic system, space group P2/n with a = 7.0001(2), b = 11.5540(3), c = 11.4192(1) ? = 101.754(2)? V = 904.21(4) 3, Z = 2, C18H20MnN2O8, Mr = 447.30, Dc = 1.643 g/cm3, F(000) = 462 and m(MoK? = 0.783 mm-1. The final R and wR are 0.0499 and 0.1301, respectively for 1335 observed reflections with I ≥ 2(I). The Mn (Ⅱ) is six-coordinated in a distorted octahedral geometry. 4,4?Bipyridine in a m-bridge mode links [Mn(H2O)4]2+ into a linear cation chain. bdc acts as a counter anion and links the linear chains into a three-dimensional structure through hydrogen bonds.
文摘A two-dimensional hydrogen-bonded cadmium(II) compound [Cd(dapm)2- (CH3COO)2(H2O)2] (dapm = diaminodiphenylmethane) has been synthesized and characterized by single-crystal X-ray diffraction analysis. It crystallizes in monoclinic, space group C2/c with a = 27.572(3), b = 5.5064(5), c = 23.310(2) , = 124.785(1)o, C15H19Cdo.5ON2O3, Mr =331.52, V = 2906.6(5) ?, Z = 4, Dc = 1.515 g/cm3, F(000) = 1368 and = 0.801 mm-1. The final R = 0.0403 and wR = 0.1014 for 1795 observed reflections with I≥4(I). The centrosymmetric Cd(II) is six- coordinated in a distorted octahedral geometry, and the dapm in a trans mode acts as a monoden- tate ligand. The intermolecular hydrogen bonds among coordinated aqua molecules with coordi- nated acetate oxygen atoms and uncoordinated dapm nitrogen atoms form a two-dimensional supramolecular framework.
基金This work was supported by the National Natural Science Foundation of China (No.20001007 20131020) Natural Science Foundation of the Chinese Academy of Sciences (KJCX2-H3) and Fujian province (2000F006)
文摘The title complex, [Cu(L)Cl2]n (L = 2,5-di-2-pyridyl-1,3,4-oxodiazole) 1, has been obtained from the reaction of 3,6-di-2-pyridyl-1,2,4,5-tetrazine (bptz) and CuCl2?H2O in a mixture solvent of CH3CN and CH2Cl2 (L is generated from the metal-assisted hydrolysis reaction of bptz) and structurally characterized. It crystallizes in space group C2/c of monoclinic system with cell parameters: a = 9.812(2), b = 12.679(3), c = 11.111(2) ? b = 103.92(3)? V = 1341.6(5) 3, Z = 4, Dc = 1.776 g/cm3, Mr = 358.66, F(000) = 716, ?= 2.024 mm1 and S = 1.004. The final R = 0.0346 and wR = 0.0938 for 1011 observed reflections with I > 2(I). The Cu(Ⅱ) ion is six-coordinated by four N atoms of two L ligands and two Cl ions in a distorted octahedral geometry. The ligand L acts as a bis-bidentate ligand to bridge the Cu(Ⅱ) ions, resulting in an infinite chain structure.
基金The work was supported by the Chinese Academy of Sciences, the National Natural Science Foundation of China(20073048)the NSF of Fujian province for financial support
文摘The new oxovanadium (V) complex, [PyH][VO2(L)] 1 (salicyladehyde 5-bromo salicyloylhydrazone is abbreviated as H2L; Hpy is protonated pyridine) was obtained from a refluxed solution of VOSO4 and H2L in acetonitrile-methanol-pyridine. Similarly, another new complex, [VO(L)(OCH3)] 2 was synthesized by refluxing VOSO4 and H2L in methanol-pyridine. Crystal data for 1: C19H15N3O5BrV, Mr= 496.2, monoclinic, P21/n, a = 7.1885(3), b = 9.2718(3), c = 28.803(1) A, β = 96.185(1)°, Z = 4 and V = 1908.6(1) A3; for 2: C15H12N2O5BrV, Mr= 431.1, monoclinic, P2,/n, a = 12.202(2), b = 8.045(2), c = 16.604(3) A, β = 101.29(3)°, Z = 4 and V = 1598.4(2) A3. The structures of 1 and 2 have been determined by X-ray analyses and reveal that the coordination environments of V atoms in both complexes are of square-based pyramid. Three of the four based donor atoms are from the tridentate 'ONO' donor ligand while the fourth is one terminal oxygen atom with the V(1) - O(3) distance 1.646(4) A for 1 and one -OCH3 group with the V(1)-O(3) distance 1.753(3) A for 2. The V(1)-O(4) terminals occupy the axial sites in both cases. The complexes are also characterized by IR and 1H NMR spectroscopies.
基金This work was supported by the NSF of Fujian Province (E0310029) and the Innovation Fund of Fujian Province (2003J044)
文摘Two silver(I) complexes were prepared by the reaction of [Ag(C≡CPh)]n with NP3 [NP3 = N(CH2CH2PPh2)3] or with NP3 and [Cu(CH3CN)4]ClO4. Complex 1 [(Ag2Cl(NP3)2)(Ag5- (C≡CPh)6)] contains both NP3 and PhC≡C- ligands. The complex cation is (Ag2Cl(NP3)2)+, in which two Ag(NP3)+ cations were bridged by a Cl- donor. The anion is (Ag5(C≡CPh)6)-, where five Ag+ ions are linked by six C≡CPh- to form a pentanuclear cluster. Complex 2 only contains NP3 ligand, where the silver center adopts a trigonal-bipyramidal geometry. Crystal data for 1: C133H116Ag7Cl3- N2P6, Mr = 2789.54, triclinic, space group P1, a = 13.0780(2), b = 15.3678(2), c = 31.2041(3) ?, α = 91.3928(7), β = 90.9328(8), γ = 96.0244(4)o, V = 6233.8(1) ?3, T = 293(2) K, Z = 2, Dc = 1.486 g/cm3, F(000) = 2796, μ = 1.266 mm-1, the final R = 0.0746 and wR = 0.1953 for 16475 observed reflections with I > 2σ(I). Crystal data for 2: C42H42AgClNO4P3, Mr = 861.00, trigonal, space group R3, a = 17.451(1), b = 17.451(1), c = 11.3985(7) ?, V = 3006.0(3) ?3, T = 293(2) K, Z = 3, Dc = 1.427 g/cm3, F(000) = 1326, μ = 0.731 mm-1, the final R = 0.0251 and wR = 0.0663 for 1499 observed reflections with I > 2σ(I).
基金The project was supported by the Key Project of Science and Technology of Fujian province (2001H107) and the National Natural Science Foundation of China (N0. 50272066)
文摘Crystals of the low temperature phase b-Ba3Y(BO3)3 have been synthesized by the flux method. The structure of the title compound crystallizes in the hexagonal system, space group P63cm with the following parameters: a = 9.416(3), c = 17.536(8) ? V = 1346.6(8) ?, Ba3YB3O9, Mr = 677.36, Z = 6, Dc = 5.012 g/cm3, l(MoKa) = 0.71073 ? m = 19.409 mm-1, Flack parameter = 0.02(3), F(000) = 1764, R = 0.0714 and wR = 0.1696 for 1076 observed reflections with I > 2s(I). The compound contains two sets of YO6 octahedra, four sets of BaO9 polyhedra and three sets of BO3 planar triangles.
基金the Key Project of Science and Technology of Fujian province (2001H107) and National Natural Science Foundation of China (N0. 59972037)
文摘The high temperature phase a-Ba3Y(BO3)3 was synthesized by Czochralski method, and its crystal structure has been determined by single-crystal X-ray diffraction. It crystallizes in the trigonal system, space group 3R with a = 13.028(2), c = 9.4992(2) ? V = 1396.1(5) ?, Ba3YB3O9, Mr = 677.36, Z = 6, Dc = 4.834 g/cm3, l(MoKa) = 0.71073 ? m = 18.721 mm-1, F(000) = 1764, the final R = 0.0718 and wR = 0.1640 for 1199 observed reflections with I > 2s(I). In this structure two alternate nonequivalent Y atoms form one-dimensional chains bridged by the Ba atoms with BO3 triangles which link Y(1) and Y(2), respectively. The Ba atom is surrounded by nine O atoms belonging to six BO3 triangles.
基金This project was supported by the 973 program of the MOST (001CB108906) the National Natural Science Foundation of China (90206040+4 种基金20073048) the NSF of Fujian Province (2002F015 2002J006) the State Key Lab of Chemistry (030065) the Chinese Academy of Sciences
文摘The title compound, {(H3O)4(NH4)4[Mo8O28]?2H2O}n 1, has been synthesized from the reaction of Zn(OAc)2 and (NH4)6Mo7O24?4H2O in aqueous solution at ambient tempe- rature, and its crystal structure was determined by X-ray single-crystal analysis with the following crystallographic data: monoclinic system, space group P21/n, a = 9.5234(6), b = 11.3235(8), c = 14.8812(10) ?, β = 107.467(2)o, V = 1530.77(18) ?3, Z = 4, F(000) = 1336, μ = 3.293 mm-1 and Dc = 3.037 g/cm3. The final R = 0.0619 for 2691 observed reflections (I > 2σ(I)). X-ray crys- tal structure analysis showed that the novel one-dimensional chain compound is built up by basic {Mo8O28} units via single μ2-O, and such chains are further linked into a three-dimensional net- work by hydrogen bonds.
