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1.
A μ1,1,3 formic bridging Ni2 complex [Ni3(HCOO)6·H2O]]n 1 has been synthesi-zed under hydrothermal conditions. The single-crystal X-ray diffraction analysis shows that 1 exhibits a 3D open microporous tube formed by covalent and coordination bonds. Complex 1 crystallizes in the monoclinic system, space group P21/c with a = 11.1487(13), b = 9.7763(11), c =17.9685(17) A, β= 126.948(6)°, C6H6Ni3O13, Mr = 462.02, V = 1565.2(3) A3 Z = 4, Dc= 1.961 g/cm3, μ = 3.630 mm-1, F(000) = 917.7, Rint = 0.0234, the final R = 0.0234 and wR = 0.0734 for 3469 observed reflections (Ⅰ>2σ(Ⅰ)).  相似文献   

2.
Nickel(Ⅱ) complexes Ni(L1)2(1) and Ni(L2)2·CH3CN·H2O(2)(L1Cl = 2-(3-benzyl-2,3-dihydroimidazlo-1-yl)-N-(pyridin-2-yl)acetamide, chloride salt, L2Cl = 2-(3-naphthalene-2-ylmethyl)-2,3-dihydro-imidazlo-1-yl)-N-phenylacetamide, chloride salt) with amide-functionalized imidazolium NHC ligand were synthesized and determined by single-crystal X-ray diffraction. Complex 1 crystallizes in the monoclinic system, space group P21/c with a = 9.2561(19), b = 15.138(3), c = 20.750(4) , β = 90.216(3)°, V = 2907.3(10) 3 and Z = 4. Complex 2 crystallizes in the orthorhombic system, space group Pbca with a = 15.5469(16), b = 15.3521(15), c = 31.177(3) , V = 7441.2(13) 3 and Z = 8. They are stable in the air and formed via intermolecular weak interactions, including C–H···π contacts and C–H···O hydrogen bonds. Complex 1 was applied in Suzuki coupling reaction through the investigation of reaction conditions under the optimal choice conditions: 80 ℃, K3PO4, 3% mol catalysts, 6% mol PPh3 and toluene as solvent system could afford 96% yield in 5 h.  相似文献   

3.
A new polyoxomolybdate complex HNa7[Mo36O112(H2O)16]·47H2O 1 has been prepared in the beaker solution and characterized by single-crystal X-ray diffraction and elemental analyses. Crystal data: H127Mo36Na7O175, Mr = 6542.79, monoclinic, C2/c, a = 40.891(6), b = 17.900(3), c = 25.580(4) , β = 125.673(2)°, V = 15210(4) 3, Z = 4, Dc = 2.857 g/cm3, F(000) = 12464, μ = 3.013 mm-1, R = 0.0633 and wR = 0.1654 (I > 2σ(I)). With the bridging sodium cations, the [Mo36O112(H2O)16]8- units in compound 1 are linked to form a one-dimensional structure, on the basis of which a three-dimensional architecture is further constructed via other sodium cations and complicated hydrogen bonds.  相似文献   

4.
Reactions of NiCl2·6H2O with dmpzm and formic or acetic acid at PH = 7 pro- duced the two title compounds, [Ni(dmpzm)2(HCO2)]Cl·2H2O 1 and [Ni(dmpzm)2(OAc)]Cl·3H2O 2 (dmpzm = 1,1'-methylenebis(3,5-dimethyl-1H-pyrazole)). 1 and 2 were characterized by elemental analysis, IR spectra, and thermogravimetric analysis. 1 crystallizes in the orthorhombic system, space group Pcca with a = 18.700(2), b = 8.6843(9), c = 18.098(2) , V = 2939.1(5) 3, Z = 4, Dc = 1.319 g/cm3, T = 193 K, C23H37ClN8NiO4, Mr = 583.75, F(000) = 1232, μ(MoKα) = 0.792 cm-1, S = 1.079, R = 0.0772 and wR = 0.1958 for 2265 observed reflections with I > 2σ(I). 2 crystallizes in the orthorhombic system, space group Pcca with a = 17.011(3), b = 18.630(4), c = 19.300(4) , V = 6117(2) 3, Z = 8, Dc = 1.337 g/cm3, T = 193(2) K, C24H41ClN8NiO5, Mr = 615.79, F(000) = 2608, μ(MoKα) = 0.768 cm-1, S = 1.059, R = 0.0518 and wR = 0.1109 for 5124 observed reflections with I > 2σ(I). The Ni atoms in 1 or 2 are chelated by two dmpzm ligands and one formate or acetate anion, forming slightly distorted octahedral geometries. In the crystals of 1 or 2, intermolecular hydrogen bonding interactions result in the formation of 2D hydrogen-bonded frameworks.  相似文献   

5.
The title complex bis{1-{[(6-ethyl-2-pyridinyl)imino]methylenyl}-2-naphthalenolato-N,O}-nickel(Ⅱ)(C36H32N4O2Ni) has been synthesized by the reaction of 1-{[(6-ethyl-2-pyridinyl)imino]methylenyl}-2-naphthalenol with Ni(CH3COO)2·4H2O, and characterized by IR spectrum, elemental analysis and TG. The complicated space structure has been confirmed by single-crystal X-ray diffraction analysis. The crystal belongs to the monoclinic system, space group P21/c with a = 11.410(4), b = 14.382(4), c = 18.121(6) , β = 97.147(6)°, V = 2950.5(16) 3, C36H32N4O2Ni, Mr = 611.37, Z = 4, Dc = 1.376 g/cm3, μ = 0.698 mm-1, F(000) = 1280, the final R = 0.0519 and wR = 0.1493(Ⅰ 2δ(Ⅰ)). This title compound was used as precatalysts for the polymerisation of norbornene. When activated with MAO, the complex exhibited excellent catalytic activity up to 1.98 × 107 g of PNB(mol of Ni)-1 h-1 with high monomer conversion.  相似文献   

6.
Two new polyoxomolybdate compounds,namely CuII2(HL)3]2[Mo8O26]·(H2O)4(1) and [NiII(HL)3]2(Mo8O26)·(H2O)3(2)(HL = 3-(2-pyridyl)pyrazole),were designed and synthesized under hydrothermal conditions.X-ray diffraction analyses reveal that compound 1 consists of one β-Mo8O264-cluster and a Cu2 dimer which is built from two Cu(II) ions linked by three 3-(2-pyridyl)pyrazole ligands.Compound 2 is generated by two kinds of polyoxomolybdate clusters of α-[Mo8O26]4-and β-[Mo8O26]4-.In complexes 1 and 2,the multi-dimensional frameworks are con-structed with the help of hydrogen-bonding links between the terminaloxygen atoms of [Mo8O26]4-,water molecules,and 3-(2-pyridyl)pyrazole ligands.Crystal data of 1:C24H25Cu2Mo4N9O15,Mr = 1190.37,monoclinic,space group P21/c,a = 10.850(2),b = 18.510(4),c = 17.230(3) ,β = 100.57(3)°,V = 3401.6(12) 3,Z = 4,Dc = 2.324 g/cm3,F(000) = 2312,μ = 2.742 mm-1,R = 0.0302 and wR = 0.0775(Ⅰ 2σ(Ⅰ));Crystal data for 2:C48H48Mo8N18Ni2O29,Mr = 2225.98,monoclinic,space group P21/n,a = 20.799(2),b = 14.7970(13),c = 23.141(2) ,β = 91.6180(10)°,V = 7119.0(11) 3,Z = 4,Dc = 2.077 g/cm3,F(000) = 4344,μ = 1.968 mm-1,R = 0.0309 and wR = 0.0696(Ⅰ 2σ(Ⅰ)).  相似文献   

7.
YU  Zhao-Wen HE  Min-Hui ZHANG  Wu SUN  Peng 《结构化学》2010,29(9):1301-1308
A Schiff base ligand(H2CSF,C13H11NO4,1) derived from 3-carboxylsalicylaldehyde and furfurylamine,and its trinuclear complex [Ni3(CSF)2(CH3COO)2(DMF)2(H2O)2](2) were synthesized.Compound 1 was characterized by elemental analysis,1H NMR,IR,MS and X-ray diffraction analysis.The crystal of 1 belongs to the monoclinic system,space group P21/c with a = 8.472(2),b = 19.743(5),c = 7.2300(18) ,β = 110.278(4)°,V = 1134.4(5) 3,Z = 4,Mr = 245.23,Dc = 1.436 g·cm-3,μ = 0.108 mm-1,F(000) = 512,λ = 0.71073 ,the final R = 0.0440 and wR = 0.1199 for 1426 observed reflections(I 2σ(I)).In the crystal of 1,there exist intramolecular hydrogen bonds and weak intermolecular C-H···O hydrogen bonds.Compound 2 was characterized by elemental analysis,IR,TG and X-ray diffraction analysis.The crystal of 2 is of triclinic system,space group P1 with a = 10.1237(17),b = 10.4086(18),c = 10.4884(18) ,α = 82.528(2),β = 67.339(2),γ = 83.010(2)°,V = 1008.1(3) 3,Z = 1,Mr = 962.87,Dc = 1.586 g·cm-3,μ = 1.463 mm-1,F(000) = 498,λ = 0.71073 ,the final R = 0.0517 and wR = 0.0805 for 2065 observed reflections(I 2σ(I)).The geometry of the trinuclear molecule is centrosymmetric,in which every Ni(Ⅱ) ion is coordinated in a slightly distorted octahedron.The three Ni(Ⅱ) ions are arranged in a straight line.The two CSF2-ions act as NOO tridentate ligands with the phenolate and carboxylate oxygen as bridging atoms.The coordination atoms of CSF2-anions and water molecules are coordinated on the equatorial plane,while the two bridging acetate ions and two DMF are trans-coordinated on the apical sites.  相似文献   

8.
A new O,O'-bis(4-tert-butylphenyl)dithiophosphate complex Ni[SSP(OC6H4But- p)2]2 (1) was synthesized and characterized by elemental analysis, IR, 1H NMR, thermogravimetric analysis (TGA) and single-crystal X-ray diffraction. The crystal belongs to the monoclinic system, space group P21/c with a = 12.8440(3), b = 6.18686(12), c=26.3018(5) , β=92.6135(18)°, V = 2087.87(7) 3, Z = 2, Dc = 1.345 g/cm3, μ = 0.780 mm-1, the final R = 0.0316 and wR = 0.0748 (Ⅰ >2σ(Ⅰ)). A total of 4269 unique reflections were collected, of which 3621 with Ⅰ > 2σ(Ⅰ) were observed. The NiII atom lies on an inversion center and is chelated by two (p-ButC6H4O)2PSS-ligands in a [NiS4] square-planar geometry with Ni-S bonds of 2.2408(5) and 2.2444(5) , respectively. A stepwise 1D chain structure is constructed via intermolecular S…S and C-H…S interactions. According to our knowledge this is the first case that intermolecular S…S interaction is observed in mononuclear transition metal complex of O,O'-dialkyldithiophosphates.  相似文献   

9.
A new complex constructed from a unit with two As3O6 rings capping Anderson-type moieties,[Ni(en)2(H2O)2]2[(NiO6)Mo6O18(As3O3)2]·2H2O(1,en = ethylenediamine),has been hydrothermally synthesized and characterized by IR,single-crystal X-ray diffraction and thermogra-vimetric analysis.The compound crystallizes in triclinic,space group P1 with a = 9.1230(16),b = 11.8078(9),c = 12.2111(9) ,α = 114.5210(10),β = 98.0350(10),γ = 100.0320(10)o,Mr = 2029.80,C8H44As6Mo6N8Ni3O36,V = 1145.0(2) 3,Dc = 2.944 g/cm3,Z = 1,GOF = 0.997,μ = 7.203 mm-1,F(000) = 970,R = 0.0352 and wR = 0.1019.Compound 1 consists of an Anderson-type capped by a two-ring(As3O6) unit [(NiO6)Mo6O18(As3O3)2]4-,two six-coordinate [Ni(en)2(H2O)2]2+ cations and two water molecules.  相似文献   

10.
何敏  李庆丰  谢婷  徐国敏  于杰  李伟 《结构化学》2010,29(4):582-586
A new binuclear complex [Ni2(2,2'-bpy)2(C8H3NO6)2(H2O)4] 1 (2,2'-bpy = 2,2'- bipyridine, C8H3NO6 = 4-nitrophthalate) has been synthesized by a hydrothermal reaction and characterized by X-ray single-crystal diffraction analysis. The complex crystallizes in triclinic, space group P1 with a = 7.206(2), b = 10.337(4), c = 12.480(4) , α = 89.887(11), β = 77.033(9), γ = 78.349(6)o, V = 886.3(5) 3, Z = 1, C36H30Ni2N6O16, Mr = 920.08, Dc = 1.724 g cm-3, F(000) = 472, μ = 1.152 mm-1, the final R = 0.0458 and wR = 0.1163 for 3372 observed reflections with I 2σ(Ⅰ). The two Ni(Ⅱ) ions are bridged by two 4-nitrophthalates both in a bis-monodentate mode. Magnetic measurements reveal that the intramolecular exchange couplings in the dimer are ferromagnetic with 2J/k = 2.32 K, D =-1.44 K and g = 2.18.  相似文献   

11.
Two new borate compounds,C4H10N2·B6O8(OH)2 1 and (NH3CH2CH2NH3)B5O8-(OH) 2,have been solvothermally synthesized and structurally characterized by single-crystal X-ray diffraction,IR,elemental analysis and thermal analysis. Compound 1 crystallizes in the monoclinic system,space group P21/c,with a=8.3318(17),b=6.2118(12),c=12.479(3) ,β=108.96(3)o,V=610.8(2) 3,Mr=313.02,Z=2,Dc=1.702 g/cm3,μ=0.150 mm-1,F(000)=320,R =0.0387 and wR =0.0924. Its layered structure is linked by infinite covalently coordinated neutral sheets with 3,20-membered window system,which are built up from alternative B6O8(OH)2 subunits donated by two piperzazine nitrogen donors. 2 crystallizes in monoclinic,space group Cc,with a=6.7207(13),b=11.481(2),c=12.564(3) ,β=95.25(3)o,V=965.4(3) 3,Mr=261.18,Z=4,Dc=1.797 g/cm3,μ= 0.164 mm-1,F(000)=536,R=0.0396 and wR=0.0752. Its oxoborate structure is generated from the sheets of 3,9-membered boron rings bonded diamine molecules through electrostatic and H-bonding interactions to form a two-dimensional layered network.  相似文献   

12.
A new organic-inorganic hybrid sandwich-type arsenotungstate[H2dap]2H2[Ni(dap)2] [Ni(dap)2(H2O)2][Ni4(H2O)2(B-α-AsVW9O34)2]·8H2O 1 (dap = 1,2-diaminopropane) has been synthesized by the reaction of Na6[AsIII2W21O69(H2O)]·nH2O, NiCl2·6H2O and dap under hydro- thermal conditions and structurally characterized by elemental analysis, IR spectroscopy, thermo- gravimetric analysis and single-crystal X-ray diffraction. 1 crystallizes in the monoclinic space group P21/n with a = 13.5133(19), b = 19.043(3), c = 17.647(2) , β = 102.585(2)°, V = 4432.0(11) 3, T = 296(2) K, Z = 2, μ = 25.350 mm–1, GOOF = 1.058, R = 0.0353 and wR = 0.0838. The molecular unit of 1 consists of two diprotonated [H2dap]2+ cations, two protons, one four-coordinate [Ni(dap)2]2+ cation, one six-coordinate [Ni(dap)2(H2O)2]2+ cation, one classic tetra-NiII substituted sandwich-type [Ni4(H2O)2(B-α-AsVW9O34)2]10– polyoxoanion and eight lattice water molecules. Furthermore, some reported different types of transition-metal substituted sandwich-type poly- oxoanions are summarized and compared.  相似文献   

13.
Proton-conductive crystalline metal-organic framework nickel(Ⅱ) benzenetricarboxylate Ni3(BTC)2·12H2O(MOF-Ni) was prepared by the reaction of nickel(Ⅱ) nitrate and 1,3,5-benzenetricarboxylic(BTC) acid in a mixed solvent of N,N-dimethylformamide(DMF)/C2H5OH/ H2O(1:1:1, ν/ν) at low temperature and short reaction time. It was characterized by thermogravimetric analyses(TG), FT-IR and N2 adsorption-desorption. Single-crystal X-ray diffraction analysis indicated that the complex belongs to monoclinic system, space group C2 with a = 17.407(6), b = 12.878(5), c = 6.542(2) , β = 112.07°, V = 1359.0(8)3, Dc = 1.971 g/cm3, μ = 2.166 mm-1 and Z = 2. Linear polarization resistance(LPR) analysis showed that the complex possesses semiconducting properties.  相似文献   

14.
A novel trinuclear nickel(Ⅱ) complex [Ni3(bushz)2(Himdz)2(H2O)2]?2DMF (1, bushz=N-butylsalicylhydrazide, Himdz=imidazole, DMF=N,N-dimethyl-formamide) has been synthesized and characterized by X-ray single-crystal diffraction characterization. Complex 1 crystallizes in the monoclinic system, space group P21/c with a=7.706(7), b=14.882(6), c=18.639(6) , β=108.08(2)o, V=2032(1) 3, Dc=1.525 g/cm3, Mr=932.95, Z=2, F(000)=972, μ=1.442 mm-1, the final R=0.0359 and wR=0.0771. The three nickel(Ⅱ) atoms in 1 are arranged in a strictly linear structure and exhibit alternating square-planar and octahedral geometries. The complex is connected to form a supramolecule with an infinite three-dimensional network through intermolecular hydrogen bonds. The electrochemical studies reveal that redox of Ni3+/Ni2+ in the complex is a quasi-reversible process. The thermal stability of the title complex was also studied.  相似文献   

15.
A novel NiⅡ complex {[Ni(IBG)(μ-H2O)(H2O)2]·2H2O}n 1(H2IBG = isophthaloylbisglycine) has been synthesized and characterized by single-crystal X-ray diffraction,elemental analysis,IR spectra,and thermogravimetric analysis.It crystallizes in monoclinic,space group P2/c with a = 15.40(2),b = 6.960(10),c = 7.865(11) ,β = 90.32(3)o,V = 843(2) 3,Z = 2,C12H18NiN2O11,Mr = 424.99,Dc = 1.675 g/cm3,F(000) = 440,μ(MoKα) = 1.214 mm-1,the final R = 0.0514 and wR = 0.1247 for 1078 observed reflections with I 2σ(I).In the structure,each NiⅡcenter is situated in the center of a rather regular octahedron.Moreover,thermal stability has been studied and magnetic measurements show antiferromagnetic interactions for this complex.  相似文献   

16.
A new dinuclear copper complex, [Cu(C13H9N2O)Cl]2·(CH3CN)2 (C30H24Cl2Cu2N6O2), has been synthesized and characterized by X-ray structure determination. It crystallizes in the tricli- nic system, space group P1, with a = 7.6677(14), b = 9.2375(17), c = 11.227(2) , α = 81.338(3), β = 88.173(4), γ = 66.199(3)o, V = 718.9(2) 3, Z = 1, Mr = 698.53, F(000) = 354, Dc = 1.613 g/cm3, μ(MoKα) = 1.705 mm-1, the final R = 0.0645 and wR = 0.1364 for 2474 unique reflections with 1809 observed ones (I > 2σ(I)). In the title complex, each copper(II) atom is located at the center of a distorted tetrahedron consisting of four coordinate atoms (one nitrogen atom, two oxygen anions, and one chlorine atom). Two copper(II) atoms are bridged by two oxygen anions (O(1) and O(1a)) of two phenolates to form a Cu(II)–Cu(II) binuclear entity, and the distance between two copper(II) atoms is 3.0144(15) .  相似文献   

17.
The reaction of Co(OAc)2·4H2O with the Schiff base H2L in a methanol solution affords the red crystals of {[CoIIIL2]·[CoII(H2O)6]0.5·2.25H2O}4 1 (H2L = N-(2-hydroxyphenyl) sali-cylidenimine). The molecular and crystal structures were determined by single-crystal X-ray diffraction. The crystal is of monoclinic, space group P21/n, C104H114Co6N8O37, Mr = 2421.61, a = 10.625(3), b = 16.335(4), c = 15.265(4) , β = 102.990(4)o, V = 2581.6(11) 3, Z = 1, Dc = 1.558 g/cm3, μ = 1.034 mm-1, F(000) = 1252, R = 0.0414 and wR = 0.1167 for 5889 reflections. The Co(III) atom is six-coordinated by two nitrogen atoms and four oxygen atoms of two tridentate L ligands. The abundant hydrogen bonding interactions extend the complex into a one-dimensional supra-molecular framework. The uncoordinated water molecules act as space-fillers and consolidate the whole architecture through the hydrogen bonding interactions.  相似文献   

18.
The title compound,[Zn2(H2C4BIm)(ox)2]·2H2O(1,H2C4BIm = 2,2'-(1,4-bu-tanediyl)bis(1H-benzimidazole),has been synthesized by the hydrothermal reaction of Zn(NO3)2·6H2O with H2C4BIm and Na2C2O4 in water solution.It crystallizes in the triclinic system,space group P1 with a = 9.445(9),b = 9.598(9),c = 14.962(14) ,α = 72.160(10),β = 79.905(12),γ = 83.680(11)°,Mr = 633.18,V = 1269(2) 3,Z = 2,Dc = 1.657 g/cm3,F(000) = 644,μ = 1.953 mm-1,the final R = 0.0671 and wR = 0.1689.X-ray crystal structure analysis revealed that 1 is a 3D network with(203)2(20)3 topology in which the ZnII atom can be considered as a 3-connected node and both ox2-and H2C4BIm serve as the linear linkers.  相似文献   

19.
王鸾  张纯喜  赵井泉 《结构化学》2014,33(10):1479-1487
A new ligand, 2-(2-hydroxyphenyl)-5,6-dichlorobenzimidazole, H2pbmCl2(1), and a novel MnIII complex, [MnIII(HpbmCl2)(pbmCl2)(DMF)2](2),(DMF = N,N-dimethylformamide), have been synthesized and characterized. The crystal of compound 1(C13H8Cl2N2O, Mr = 279.12) belongs to the monoclinic system, space group P21 with a = 3.770(5), b = 25.20(3), c = 5.865(7) , = 92.727(17)o, V = 556.6(12) 3, Z = 2, Dc = 1.665 g/cm3, S = 1.137, μ= 0.568 mm-1, F(000) = 284, the final R = 0.0876 and wR = 0.2334 for 1848 independent reflections. The molecule is planar due to the presence of a strong intramolecular hydrogen bond between O–H group of phenol and N atom of imidazole. H2pbmCl2(1) molecules are arranged into a one-dimensional linear chain through intermolecular hydrogen bonds(N–H···O and C–H···Cl). The crystal of complex 2(C32H27Cl4MnN6O4, Mr = 756.34) belongs to the monoclinic system, space group P21/c with a = 19.043(10), b = 10.808(5), c = 18.704(11), = 115.540(6)o, V = 3473(3) 3, Z = 4, Dc = 1.446 g/cm3, S = 1.3, μ = 0.733 mm-1, F(000) = 1544, the final R = 0.1219 and wR = 0.2681 for 7811 independent reflections. The Mn ion adopts a distorted octahedral geometry coordinated by two deprotonated H2pbmCl2 ligands and two DMF molecules. The [MnIII(HpbmCl2)(pbmCl2)(DMF)2] molecules are arranged into a three-dimensional structure through hydrogen bonds(N–H···N, C–H···N and C–H···Cl) and weak π···πinteractions. The activity measurements suggest that complex 2 is able to serve as a catalyst for H2O2 disproportionation reaction to form O2 in neutral water solution.  相似文献   

20.
Under hydrothermal conditions, 4-(4,5-dicarboxy-1H-imidazol-2-yl)pyridine 1-oxide (H3DCImPyO) reacted with ZnCl2 to give the 1D chain complex {[Zn(DCImPyO)·(H2O)2·]·H3O}n (1). Single-crystal X-ray determination shows that complex 1 crystallizes in the monoclinic system, space group P2 1 /c with a=9.488(2), b=13.247(3), c=12.959(4) , β=126.716(19)°, Z=4, V=1305.6(6) 3 , C10H11N3O8Zn, D c=1.865 g/cm3 , M r=366.61, λ(MoKa)=0.71073 , μ=1.930 mm -1 , F(000)=744, R=0.0472 and wR=0.1487. Fluorescent analysis showed an intense emission band at 422 nm when the exciting radiation was set at 378 nm. Dielectric constant of complex 1 was measured at different frequencies with temperature variation.  相似文献   

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