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1.
《Journal of Coordination Chemistry》2012,65(18):2896-2904
A new organic-inorganic hybrid compound constructed from Keggin-type polyanion clusters and transition metal complexes, [Co(2,2′-bipy)3]1.5[SiWVWVI 11O40Co(2,2′-bipy)2(H2O)] ·?0.5H2O (1), has been hydrothermally prepared and characterized by elemental analysis, IR, UV–Vis, TG-DTA and single crystal X-ray diffraction. Compound 1 crystallized in the monoclinic system, space group C2/c, a =?46.995(15), b =?14.487(5), c =?26.205(9)Å, β =?90.000(0)°, V =?17841(10)Å3, Z =?4. Compound 1 contains a [SiWVWVI 11O40Co(2,2′-bipy)2(H2O)]3? polyoxoanion in which [Co(2,2′-bipy)2(H2O)]2+ is covalently bonded to the α-Keggin-type heteropolyanion [SiWVWVI 11O40]5? via a terminal oxygen. 相似文献
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A novel complex [Zn(FcCOO)2(2,2′-bipy)(H2O)]2·H2O (Fc = (η5-C5H5)Fe(η5-C5H4), 2,2′-bipy = 2,2′-bipyridine) has been synthesized and characterized by elemental analysis, IR and X-ray diffraction. It crystallizes in monoclinic system, space group P21/c with a = 6.8187(4), b = 21.7155(13), c = 19.7411(12) (A), α = 90, β = 97.7420(10), γ = 90°, C64H58Fe4Zn2N4O11, Mr = 1413.28, V = 2896.4(3) (A)3, Dc = 1.620 g/cm3, Z = 2, F(000) = 1444, μ(MoKα) = 1.857 mm-1, R = 0.0523 and wR = 0.0982 for 3219 observed reflections (I > 2σ(I)). Structural analysis shows that the zinc atom is coordinated with three oxygen atoms from two ferrocenemonocarboxylates and one water molecule together with two nitrogen atoms from 2,2′-bipyridine, giving a distorted square-pyramidal coordination geometry. The complex molecules are linked to form an infinite one-dimensional chain by both intermolecular hydrogen bonds and π-π stacking interactions of the bipyridine rings. 相似文献
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《Journal of Coordination Chemistry》2012,65(12):1317-1325
Two Zn(II) complexes, [Zn(Fura)2(2,2′-bpy)(H2O)] (1) and [Zn(µ-dnbc)2] (2), have been synthesized and characterized by X-ray diffraction and IR spectra. 1 is a quaternary Zn(II) complex with ZnN2O3 configuration distorted square pyramid geometry; 2 is a Zn(II) coordination polymer with 1D double-helical chains bridged by 3,5-dinitrobenzoic acid. 相似文献
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Two novel zeotype crystals, K4[Cr3O(H2O)3(OOCH)6]2[P2W18O62]·9.5H2O(1) and K4 [Cr3O(H2O)3·X-ray single crystal diffraction. Crystal data: C12H43O103.5K4Cr6P2W18(1), hexagonal P6(3)/m, a=1.5895(2)nm, b=1.5895(2) nm, c=2.1620(4) nm, α=90°, β=90°, γ =120°, V=4.7305(13) nm3, Z=2,R1 =0. 0726, wR2=0. 1542; C6H57O98K4Cr3CoP2W17(2), hexagonal P6(3)/mmc, a=1. 61328 (3) nm, b=1.61328(3) nm, c=2. 06613 (9) nm, α=90°,β=90°, γ=120°, V=4. 6570(2) nm3, Z=2, R1=0. 0377,wR2 =0.1070. These crystals were characterized using elemental analysis, IR, TG-DTA, and XRD. It was found that the polyoxometalate anions maintained Wells-Dawson structure for crystal 1 and lacunary Wells-Dawson structure for crystal 2. Thermal analysis showed that crystal 1 lost the water of crystallization at 132 ℃, whereas crystal 2 lost the water of crystallization at 100 ℃. Crystal 1 could reversibly desorb and adsorb water molecules and its crystal structure could be restored after re-adsorbing the water molecules. It was also found from the XRD patterns that the void size of crystal 2 is smaller compared with that of crystal 1, which is attributed to the higher anion charges. 相似文献
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A novel complex [Zn(FcCOO)2(2,2′-bipy)(H2O)]2·H2O (Fc = (η5-C5H5)Fe(η5-C5H4), 2,2′-bipy = 2,2′-bipyridine) has been synthesized and characterized by elemental analysis, IR and X-ray diffraction. It crystallizes in monoclinic system, space group P21/c with a = 6.8187(4), b = 21.7155(13), c = 19.7411(12) (A), α = 90, β = 97.7420(10), γ = 90°, C64H58Fe4Zn2N4O11, Mr = 1413.28, V = 2896.4(3) (A)3, Dc = 1.620 g/cm3, Z = 2, F(000) = 1444, μ(MoKα) = 1.857 mm-1, R = 0.0523 and wR = 0.0982 for 3219 observed reflections (I > 2σ(I)). Structural analysis shows that the zinc atom is coordinated with three oxygen atoms from two ferrocenemonocarboxylates and one water molecule together with two nitrogen atoms from 2,2′-bipyridine, giving a distorted square-pyramidal coordination geometry. The complex molecules are linked to form an infinite one-dimensional chain by both intermolecular hydrogen bonds and π-π stacking interactions of the bipyridine rings. 相似文献
7.
X. F. Wang Y. F. Wang J. Wang Zh. H. Zhang J. Gao B. Liu Y. Ch. Jiang X. D. Zhang 《Russian Journal of Coordination Chemistry》2008,34(8):555-563
The title complexes, K3[Cd(Dtpa)] (H5Dtpa = diethylenetriamine-N,N,N,N′,N′-pentaacetic acid, (I)), K2[Cd(H2O)4][Cd(Edta)(H2O)]2 · 2H2O (H4Edta = ethylenediamine-N,N,N′,N′-tetraacetic acid, (II)), and Na2[Cd(H2O)4][Cd(Edta)(H2O)]2 · 2H2O (III), were prepared, and their compositions and structures were determined by elemental analyses, IR spectra, and single-crystal X-ray diffraction techniques, respectively. In complex I, the Cd is seven-coordinated by one Dtpa ligand yielding a pseudo-monocapped trigonal prism conformation, and the complex crystallizes in the triclinic crystal system with the Pi space group. The crystal data are as follows: a = 8.7300(17), b = 9.1200(18), c = 15.110(3) Å, α = 95.52(3)°, β = 96.59(3)°, γ = 99.63(3)°, V = 1170.0(4) Å3, Z = 2, ρ = 1.754 g/cm3, μ = 1.519 mm?1, F(000) = 616, R = 0.0644 and wR = 0.1712 for 3842 observed reflections with I ≥ 2σ(I). For complex II, in the [Cd(Edta)(H2O)]2? complex anion the Cd2+ ion is seven-coordinated by one Edta ligand and one water molecule, yielding a pseudo-pentagonal bipyramid conformation. In the [Cd(H2O)4]2+ cation, the bridged Cd is six-coordinated, yielding an almost standard octahedral conformation. The complex crystallizes in the monoclinic system with P21/n space group. The crystal data are as follows: a = 9.098(3), b = 16.442(6), c = 12.023(4) Å, β = 91.053(6)°, V = 1798.3(12) Å3, Z = 2, ρ = 2.098 g/cm3, μ = 2.086 mm?1, F(000) =1124, R = 0.0406 and wR = 0.1152 for 3680 observed reflections with I ≥ 2σ(I). In complex III, the conformations of Cd2+ ions are similar to those of the potassium salt complex, and the complex also crystallizes in the monoclinic crystal system with the P21/n space group. The crystal data are as follows: a = 9.134(7), b = 16.500(13), c = 12.075(10) Å, β = 91.054(12)°, V = 1820(2) Å3, Z = 2, ρ = 2.015 g/cm3, μ = 1.856 mm?1, F(000) = 1092, R = 0.0363 and wR = 0.0879 for 3707 observed reflections with I ≥ 2σ(I). 相似文献
8.
A new organic-inorganic hybrid polyoxometalate based on Dawson-like polyoxotungstate anion [SbW18O60]9-, formulated [Co(2,2'-bpy)3]2[Co(2,2'-bpy)2Cl][Co(2,2'-bpy)2]H2[SbW18O60]·4H2O (2,2'-bpy= 2,2(-bipyridine) has been synthesized from Sb2O3, Na2WO4, CoCl2, and 2,2'-bipyridine materials by hydrothermal method, and which was characterized by elemental analyses, IR, XPS, EPR, TG, and X-ray single crystal diffraction. Structure analysis shows that the polyoxoanion self-assembled under hydrothermal conditions consists of a Dawson-like polyoxotungstate cluster anion [SbW18O60]9- encapsulating a pyramidal {SbO3} group within the {W18} cluster cage. EPR spectra show that the high-spin octahedral CoⅡ and low-spin CoⅡ ions coexist in the title compound. Magnetic properties indicate that the compound is antiferromagnetic. 相似文献
9.
《中国科学B辑(英文版)》2007,(6)
A new organic-inorganic hybrid polyoxometalate based on Dawson-like polyoxotungstate anion [SbW18O60]9, formulated [Co(2,2′-bpy)3]2[Co(2,2′-bpy)2Cl][Co(2,2′-bpy)2]H2[SbW18O60]·4H2O (2,2′-bpy= 2,2′-bipyridine) has been synthesized from Sb2O3, Na2WO4, CoCl2, and 2,2′-bipyridine materials by hydrothermal method, and which was characterized by elemental analyses, IR, XPS, EPR, TG, and X-ray single crystal diffraction. Structure analysis shows that the polyoxoanion self-assembled under hydrothermal conditions consists of a Dawson-like polyoxotungstate cluster anion [SbW18O60]9 en- capsulating a pyramidal {SbO3} group within the {W18} cluster cage. EPR spectra show that the high-spin octahedral CoII and low-spin CoII ions coexist in the title compound. Magnetic properties in- dicate that the compound is antiferromagnetic. 相似文献
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通过水热合成技术,一个新颖的基于Zn配合物修饰的Keggin型钴钨酸的有机-无机杂化化合物:[Zn(2,2’-bipy)3]3{[Zn(2,2’-bipy)2(H2O)]2 [HCoW12O40] 2 }.H2O已经被合成,化合物通过红外光谱、热重分析和单晶X-射线衍射进行了表征。单晶X-射线衍射的结果显示标题化合物是由一个单支撑的{[Zn(2,2’-bipy)2(H2O)]2 [HCoW12O40] 2}6-多阴离子,三个[Zn(2,2’-bipy)3]2+阳离子和一个水分子构成。有趣的是[Zn(1)(2,2’-bipy)3]2+阳离子通过氢键连接在一起形成螺旋链。另外标题化合物在空气中是稳定的,并且在室温下显示了强的荧光。 相似文献
13.
Shen Zhen Zuo Jing-Lin Shi Fa-Nian Xu Yan Song You You Xiao-Zeng Raj S. Shanmuga Sundara Fun Hoong-Kun Zhou Zhong-Yuan Che Chi-Ming 《Transition Metal Chemistry》2001,26(3):345-350
Two bimetallic assemblies, K2[NiII(cyclam)]3[FeII(CN)6]2 · 12H2O (1) and [NiII(cyclam)]3[FeIII(CN)6]2 · 16H2O (2) (cyclam = 1,4,8,11-tetraazacyclotetradecane), were obtained by reaction of K4[Fe(CN)6] and [Ni(cyclam)](ClO4)2 in aqueous media at different temperatures. Their crystals were structurally determined and magnetic properties were studied. Both of the compounds have honeycomb-layered structures, which are formed by Fe6Ni6 units linked through the cyanide bridges. Structure (1) consists of polyanions containing NiII–NC–FeII linkages and K+ cations, while structure (2) is a two-dimensional neutral layer containing NiII–NC–FeIII linkages. The magnetic properties of (1) and (2) have been investigated in the 5–300 K range. Compound (1) exhibits a weak antiferromagnetic interaction with Weiss constant = –0.35 K; compound (2) shows ferromagnetic intralayer and antiferromagnetic interlayer interactions. 相似文献
14.
X. F. Wang X. Zh. Liu J. Wang Zh. H. Zhang W. Sun Y. M. Kong X. D. Zhang 《Russian Journal of Coordination Chemistry》2008,34(2):134-145
The three title complexes, NH4[HoIII(Edta)(H2O)3] · 1.5H2O (I) (H4Edta = ethylenedianine-N,N,N′,N′-tetraacetic acid), (NH4)4[Ho 2 III (Dtpa)2] · 9H2O (II) (H5Dtpa = diethylenetriamine-N,N,N′,N″,N″-entaacetic acid), and (NH4)3[HoIII(Ttha)] · 5H2O (III) (H6 Ttha = triethylenetetramine-N,N,N′,N″,N?,N?-hexaacetic acid), have been prepared and characterized by FT-IR, elemental analyses, and single-crystal X-ray diffraction technique. Complex I has a nine-coordinate mononuclear structure with distorted monocapped square antiprismatic conformation and its crystal structure belongs to orthorhombic system and Fdd2 space group. The crystal data are as follows: a = 19.343(9), b = 35.125(17), c = 12.364(6) Å, V = 8400(7) Å3, Z = 16, M = 552.26, ρcalcd = 1.747 g cm?3 μ = 3.828 mm?1, and F(000) = 4368. Complex II has a binuclear nine-coordinate pseudomonocapped square antiprismatic conformation and its crystal structure belongs to triclinic system and space P1 group. The crystal data are as follows: a = 9.7637(16), b = 9.9722(16), c = 12.945(2) Å, α= 85.853(2)°, β = 77. 140(2)°, γ = 77.140(2)°, V = 1198.4(3) Å3, Z = 1, M = 1340.80, ρcalcd = 1.858 g cm?3, μ = 3.380 mm?1, and F(000) = 674. As for complex III, it also has nine-coordinate mononuclear structure with distorted tricapped trigonal prism and its crystal structure belongs to monoclinic system andP21/c space group. The crystal data are as follows: a = 10.349(3), b = 12.760(4), c = 23.142(7) Å, β = 91.020(6)°, V = 3055.6(16) Å3, Z = 2, M = 797.55, ρcalcd = 1.734 g cm?3, μ = 2.674 mm?1, and F(000) = 1624. The results showed that although the ligands are different from one another in the shape and the numbers of coordination atoms, they all have nine-coordinate structures. However, one of them has binuclear structure and the other two have mononuclear structures because of the difference of the ligands. 相似文献
15.
Three new inorganic-organic composite polyoxotungstates [Cu(2,2'- bpy)2]5[α- PW11.5Cu0.5O40]·2H2O 1, [Co(2,2'-bp3)2(N3)2]4H3[α-PW12O40]·3H2O 2 and [Cu(2,2'-bpy)2(4,4'- bpy)]2[α-GeW12O40].4H2O 3 (2,2'-bpy = 2,2'-bipyridine, 4,4'-bpy = 4,4'-bipyridine) have been hydrothermally synthesized and structurally characterized. 1 crystallizes in the orthorhombie space group Pna21 with α = 27.847(3), b = 21.597(2), c = 20.1179(19) A, V = 12099(2) A3, Z = 4, GOF= 1.038, R = 0.0427 and wR = 0.1035; 2 belongs to the triclinic space group P1 with a= 12.31150(10), b = 16.1954(4), c = 19.36290(10) A, α = 99.366(11), β=105.168(8),γ = 111.836(8)°, V = 3309.98(9) A3, Z = 1, GOF = 1.024, R = 0.0739 and wR = 0.2216; and 3 crystallizes in the monoclinic space group P21/n with a = 12.858(4), b = 20.943(6), c = 15.598(5) A, β = 102.338(5)°, V = 4103(2) A3, Z = 2, GOF = 1.026, R = 0.0557 and wR = 0.1316. The common structural features of 1~3 are that their molecular structures all consist of a saturated a-Keggin polyoxoanion and several discrete metal-organic moieties. Intriguingly, 2 and 3 are composed of metal-organic coordination moieties with two mixed ligands. 相似文献
16.
《Journal of Coordination Chemistry》2012,65(16):2563-2569
Two new supramolecular compounds [M(4,4′-bipy)2 (H2O)4] ·?(4,4′-bipy)2 ·?(3,5-daba)2 ·?8H2O (M=Zn(1) or Mn(2), 4,4′-bipy =?4,4′-bipyridine, 3,5-daba =?3,5-diaminobenzoic acid anion) were synthesized and characterized by elemental analysis and X-ray crystal diffraction. In [M(4,4′-bipy)2(H2O)4]2+, the M(II) is coordinated by two nitrogen atoms from two 4,4′-bipy molecules and four oxygen atoms from four waters to form an octahedral configuration. There exist uncoordinated 4,4′-bipy molecules, 3,5-diaminobenzolate counterions and water guests in the compounds. The 3D structures of the title supramolecular compounds are constructed by rich hydrogen bonds among [M(4,4′-bipy)2(H2O)4]2+, uncoordinated 4,4′-bipy molecules, water molecules and 3,5-daba, containing a diverting hexa-member water ring. 相似文献
17.
The crystals of the title compounds (H3O)(C3H5N2)[Mn(OH)6Mo6O18]·3.5H2O 1 and (H3O)3[Co(OH)6Mo6O18]·7H2O 2 have been prepared and structurally determined by X-ray single-crystal diffraction. Compound 1 crystallizes in monoclinic, space group C2/c with a = 21.5018(9), b = 10.9331(5), c = 11.8667(5)A,β = 95.3570(10)o, V = 2777.5(2)A3, Z = 4, Dc = 2.802 g/cm3, Mr = 1171.80,μ(MoKα) = 3.173 mm-1, F(000) = 223, the final R = 0.0458 and wR = 0.1041 for 2093 observed reflections (I>2σ(I)); Compound 2 crystallizes in monoclinic, space group P21/c with a = 11.4042(12), b = 10.9481(11), c = 11.6722(12)A, β= 99.948(2)o, V = 1435.4(3)A3, Z = 2, Dc = 2.794 g/cm3, Mr = 1207.80,μ(MoKα) = 3.223 mm-1, F(000) = 1160, the final R = 0.0544 and wR = 0.1066 for 1906 observed reflections (I > 2σ(I)). Both compounds 1 and 2 adopt the Anderson structure, in which the anion is of centrosymmetry and formed by six octahedral edge-sharing MoO6 units surrounding the central MO6 (M = Mn or Co) octahedron. 相似文献
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《Journal of Coordination Chemistry》2012,65(23):3810-3818
Two supramolecular compounds based on tungstoferrate [FeW12O40]5?, [FeII(2,2′-bipy)3]2[HFeW12O40] · 5H2O (1), and [Hpy]2[4,4′-H2bipy]6(H3O)[FeW12O40]3 · 11H2O (2) (py = pyridine, bipy = bipyridine) were synthesized hydrothermally and characterized structurally. The hydrogen bonds between polyoxoanions and water and the edge-to-face π–π interaction between [FeII(2,2′-bipy)3]2+ with a shortest C–C distance of 3.513 Å are the main forces to construct the 3-D architecture of 1. In 2, a 3-D supramolecular architecture is assembled by the tungstoferrate anions, protonated 4,4′-bipy cations, and water through hydrogen bonding. The variable-temperature magnetic susceptibilities indicate that 1 is paramagnetic with μ eff corresponding to one Fe(III) with spin-only contribution, showing that Fe in the coordination cations has a +II oxidation number and low spin state. 相似文献