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1.
采用三元胺及二元胺混配方法进行[Co(N)5Cl]2+配合物的合成,分离出分别由三元胺配体和二胺配体构成的2个钴胺配合物。晶体结构测定表明由三元胺配体构成的钴胺配合物中,三元胺为N-(2-Aminoethyl)-1,3-propanediamine(记为2,3-tri),但并未以六胺形式配位[Co(N)6]3+,而以六胺五配位形式形成[Co(N)6Cl]2+,这  相似文献   

2.
郭鸿旭  王庆华  陈晨  梁敏  陈铃 《中国化学》2008,26(4):640-644
水热合成并通过红外、热重、单晶X-射线衍射表征了一个新颖镍配位阳离子修饰的还原型钼磷酸盐,Ni[Mo6O12(OH)3(PO4)(HPO4)3]2][Ni(H2O)2][Ni(H2O)(bipy)2]4·5H2O。单晶X-射线衍射研究表明,两个{Mo6P4}簇单元通过一个镍离子连接形成一个Ni[Mo6P4]2二聚结构单元,其进一步和其他的镍配位阳离子连接成钼磷酸盐一维链状结构。在H2O2存在下的液-固体系中,使用该化合物催化氧化苯甲醛的探针反应结果表明,该化合物具有较高的催化氧化活性。  相似文献   

3.
Two novel organic amine templated lanthanide sulfates, layer (H3DETA)[Nd(H2O)(SO4)3] (I) and chain-like (H3DETA)[Ho(H2O)2(SO4)3] (II), are hydrothermally synthesized by using diethylenetriamine (DETA) as template, and are structurally characterized by ICP, elemental analysis, X-ray single-crystal diffraction, X-ray powder diffraction, IR, and TG. Compound I is monoclinic with space group P21 and data of unit cell: a = 6.6518(13), b = 10.373(2), c = 11.091(2) ?, β = 93.61(3)°, V = 763.7(3) ?3, ρ c = 2.421 g/cm3, μ(MoK α) = 3.885 mm−1, Z = 2, R 1 = 0.0194 for 3312 reflections with F o > 2σ(F o). The Nd ions are nine-coordinated by one oxygen atom of coordinated water and eight oxygen atoms of sulfates. Compound I displays the layer structure constructed by linking Nd ions with three-linkage SO4 tetrahedra as the bridge (affording one coordinated vertex and coordinated edge). Compound II crystallizes in the monoclinic space group P21/c with unit cell data: a = 6.594(13) ?, b = 14.783(3) ?, c = 16.599(3) ?, β = 93.47(3)°, V = 1614.2(6) ?3, ρ c = 2.454 g/cm3, μ(MoK α) = 5.37 mm−1, Z = 4, R 1 = 0.0259 for 1815 reflections with F o > 2σ(F o). The Ho ions are eight-coordinated by two oxygen atoms of coordinated water and six oxygen atoms of sulfates. The straight chain-like structure of II is attained by alternatively arranging HoO8 polyhedra and two-linkage SO4 tetrahedra (affording two coordinated vertices). The TG results indicate that the two compounds experience three weight losses and lead to distinct residues: Nd2O3 for I and HoO(SO4)0.5 for II.  相似文献   

4.
New mixed-ligand coordination compounds[Cd(DMSO)5(NCS)][Cr(NH3)2(NCS)4] · 3DMSO (I) and [Mn(DMSO)4(H2O)2][Cr(NH3)2(NCS)4]2 · 6DMSO · 2H2O (II) have been synthesized and studied by IR spectroscopy and X-ray diffraction analysis. The crystals of compound I are monoclinic, a = 14.5275(7), b = 23.1692(11), c = 14.6969(6) ?, β = 97.057(2)°, V = 4909.4(4) ?3, space group P21/c, Z = 4, ρcalcd = 1.507 g/cm3, R = 0.0556. The crystals of compound II are triclinic, a = 11.7784(3), b = 12.1760(3), c = 13.1922(2) ?, α = 85.5420(10)°, β = 87.9000(10)°, γ = 70.3680(10)°, V = 1776.46(7) ?3, space group P , Z = 1, ρcalcd = 1.444 g/cm3, R = 0.0350. Original Russian Text ? E.A. Gerasimova, T.V. Utkina, E.V. Peresypkina, A.V. Virovets, T.G. Cherkasova, 2009, published in Zhurnal Neorganicheskoi Khimii, 2009, Vol. 54, No. 5, pp. 751–755.  相似文献   

5.
A uranylcontaining compound [U(CO3)3(H2O)2]·2H2O has been synthesized under hydrothermal condition and characterized by X-ray single-crystal analysis. Crystal structural analysis indicates that this compound consists of three CO32- molecules, one U6+. The results reveal that the title compound presents a 3D frame work built up by O-H…O week hydrogen bonds interactions. The central uranium atom is eight-coordinated through three CO32- molecules and two H2O. The compound shows a coplanar hexagonal network structure, each hexagon containing a hexagonal hole with a water moleculet. CCDC: 737313.  相似文献   

6.
By the reaction of [Mo3S4(C2O4)3(H2O)3]2− with PdCl2 and NH4H2PO2 as a reducing agent, followed by the addition of PPh3, a new oxalate cuboidal cluster complex [Mo3(PdPPh3)S4(C2O4)3(H2O)3]2− is obtained. It was isolated and structurally characterized as K2[Mo3(PdPPh3)S4(C2O4)3(H2O)3]·0.5H2O. Original Russian Text Copyright ? 2008 by A. L. Gushchin, M. N. Sokolov, D. Yu. Naumov, and V. P. Fedin __________ Translated from Zhurnal Strukturnoi Khimii, Vol. 49, No. 4, pp. 775–778, May–June, 2008.  相似文献   

7.
该文报道了N,N′-(2-苯并咪唑基甲基)亚氨基甲基膦酸{bbimpH2,[(C7H5N2)CH2]2NCH2PO3H2}的2个镍化合物Ni2(bbimp)2(4,4′-bipy)(H2O)2·2H2O (1)和[Ni2(bbimp)2(H2O)2][Ni(bbimp)(H2O)2]2·4H2O (2)。化合物1是4,4′-联吡啶作为桥连配体的中性双核结构。化合物2含有1个中性的[Ni2(bbimp)2(H2O)2]双核分子与2个中性的[Ni(bbimp)(H2O)2]单核分子。双核分子单元中的2个Ni(Ⅱ)离子被2个膦酸氧桥连。在化合物2中,膦酸氧桥连的2个Ni(Ⅱ)离子之间存在铁磁性相互作用。  相似文献   

8.
A single crystal of [Pd(NH3)4]3[Ir(NO2)6]2·H2O double complex salt is studied by X-ray diffraction. Crystallographic characteristics are as follows: a = 21.0335(5) ?, b = 8.0592(2) ?, c = 21.3452(5) ?, β = 91.254(1)°, V = 3617.43(15) ?3, P21/c space group, Z = 4, d x = 2.714 g/cm3. Single-layer pseudohexagonal packing of complex anions is determined along the [−1 0 1] direction in the structure. Complex cations and crystallization water molecules are located between the mentioned layers.  相似文献   

9.
The title complex [Sm(o-MOBA)3(phen)·H2O]2·4H2O has been synthesized by the reaction of SmCl3·6H2O with o-methoxybenzoic acid and 1,10-phenanthroline in 1∶3∶1 molar ratio. The crystal structure was determined by X-ray single crystal diffraction. The crystal belongs to triclinic system, space group P1 with a=1.203(10) nm, b=1.293(10) nm, c=1.306(11) nm, α=64.50(10)°, β=81.93(10)°, γ=74.81(10)°. The molecular structure shows that the Sm3+ ion coordinates to nine atoms. The carboxylate groups are bonded to the samarium ion in three modes: monodentate, bidentate chelating, tridentate chelating-bridging. CCDC: 603740.  相似文献   

10.
The reaction of indium thiocyanate with bipyridine (4,4-Bipy) and urotropine (Ur) gave [H2(4,4′-Bipy)][In(H2O)2(NCS)4]2 (I) and [HUr]2[In(H2O)(NCS)5] · 2H2O (II), which were identified using elemental analysis, IR spectra, and thermogravimetric analysis. The thermal decomposition of compound I and II ends at 650 and 640°C, respectively, and gives In2O3. X-Ray diffraction analysis of compound I showed that complex anions in the crystal form chains through O-H…S hydrogen bonds. The anion chains form a close packing of columns with bipyridine cations located in the voids. Original Russian Text ? S.P. Petrosyants, A.B. Ilyukhin, V.A. Ketsko, 2008, published in Zhurnal Neorganicheskoi Khimii, 2008, Vol. 53, No. 6, pp. 951–955.  相似文献   

11.
In this work, the title complexes, NH4[ErIII(Cydta)(H2O)2] · 4.5H2O (I) (H4Cydta = trans-1,2-cyclo-hexanediamine-N,N,N′,N′-tetraacetic acid) and (NH4)2[Er2III(Pdta)2(H2O)2] · 2H2O (II) (H4Pdta= propylene-diamine-N,N,N′,N′-tetraacetic acid), were prepared, respectively, and their composition and structures were determined by elemental analyses and single-crystal X-ray diffraction techniques. Complex I selects a mononu-clear structure with pseudosquare antiprismatic geometry crystallized in the triclinic crystal system with space group $ P\bar 1 $ P\bar 1 and the central Er3+ ion is eight-coordinated by the hexadentate Cydta ligand and two water molecules. The crystal data are as follows: a = 8.568(3), b = 10.024(3), c = 14.377(4) ?, α = 88.404(4)°, β = 75.411(4)°, γ = 88.332(4)°, V = 1194.2(6) ?3, Z = 1, ρ c = 1.793 g/cm3, μ = 3.586 mm−1, F(000) = 648, R = 0.0257, and wR = 0.0667 for 4169 observed reflections with I ≥ 2σ(I). Complex II is eight-coordinated as well, which selects a binuclear structure with two pseudosquare antiprismatic geometry and crystallizes in the monoclinic crystal system with space group P21/n. The central Er3+ ion is coordinated by two nitrogens and four oxygens from one hexadentate Pdta ligand. Besides, two oxygens come from one carboxylic group of the neighboring Pdta ligand and one water molecule, respectively. The crystal data are as follows: a = 12.7576(8), b = 9.3151(6), c = 14.3278(9) ?, β = 96.1380(10)°, V = 1692.93(19) ?3, Z = 4, ρ c = 2.054 g/cm3, μ = 5.015 mm−1, F(000) = 1028, R= 0.0228, and wR = 0.0534 for 2984 observed reflections with I ≥ 2σ(I).  相似文献   

12.
张全争 《无机化学学报》2008,24(7):1168-1171
At room temperature, a coordination polymer [Ni(btec)(H2O)4][Ni(imi)2(H2O)4]·2H2O was synthesized by reaction of NiCl2·6H2O, 1,2,4,5-benzenetetracarboxylic dianhydridc and imidazole in a water/THF solution. The structure was determined by X-ray diffraction crystal structure analysis. It crystallizes in triclinic P1 space group with the crystal cell parameters of a=0.67542 (2) nm, b=1.000 14 (1) nm, c=1.09088 (3) nm, α=74.140(2)°, β= 74.388(1)°, y=73.239(2)°, and V=0.664 09(3) nm3, Z=1. The crystal structure shows that Ni1 atom is coordinated by four water and two imidazole molecules, while Ni2 is coordinated by four water molecules and two carboxyl oxygen atoms. The 1,2,4,5-benzenetetracarboxylate ions bridge Ni2 coordination centers to form one-dimensional chain structure. Moreover, the chains are further linked together by hydrogen bonds to form a two-dimensional network. CCDC: 295873.  相似文献   

13.
The title complex [Cu3(TFSSB)2·(H2O)4·4H2O]n (TFSSB=taurine 3-formylsalicylic schiff base) was synthesized by TFSSB and copper(Ⅱ) acetate monohydrate in ethanol solution and the crystal structure was determined by X-ray diffraction method. The crystal belongs to monoclinic system, space group P21 / n,with cell parameters: a=0.927 9(6) nm, b=1.173 0(2) nm, c=1.471(2) nm, β=106.96(2)°, and V=1.531(2) nm3, Z=2, Dc=1.890 g·cm-3, μ=2.291 mm-1, F(000)=882, R1=0.025 9, wR2=0.065 9. The Cu1 is five-coordinate, the Cu2 is four-coordinate. CCDC: 253298.  相似文献   

14.
The title complexes, K[Dy(Edta)(H2O)3] · 3.5 H2O (I) (H4Edta = ethylenediamine-N,N,N′,N′-tetraacetic acid), (NH4)3[Dy(Ttha)] · 5H2O (II) (H6Ttha = triethylenetetramine-N, N,N′,N″,N‴,N‴-hexaacetic acid), and NH4[Dy(Cydta)(H2O)2] · 4.5H2O (III) (H4Cydta = trans-1,2-cyclohexanediamine-N,N,N′,N′-tetraacetic acid), were prepared, and their compositions and structures were determined by elemental analyses and single-crystal X-ray diffraction techniques, respectively. In complex I, the Dy3+ ion is nine-coordinated by an Edta ligand and three water molecules, yielding a pseudo-monocapped square antiprismatic conformation, and the complex crystallizes in the orthorhombic crystal system with space group Fdd2. The crystal data are as follows: a = 19.751(7), b = 35.573(12), c = 12.227(4) ?, V = 8591(5) ?3, Z = 16, space group Fdd2 ρc = 1.877 g/cm3, μ = 3.742 mm−1, F(000) = 4800, R = 0.0259, and wR = 0.0616 for 3218 observed reflections with I ≥ 2σ(I). For complex II, the Dy3+ ion is nine-coordinated by a Ttha ligand, yielding a pseudo-monocapped square antiprismatic conformation, and the complex crystallizes in the monoclinic crystal system with space group P21/c. In addition, there is a free non-coordinate carboxyl group (-CH2COO) in the [Dy(Ttha)]3− complex anion. The crystal data are as follows: a = 10.353(3), b = 12.746(4), c = 23.141(7) ?, β = 91.005(5)°, V = 3053.2(15) ?3, Z = 4, space group P21/c ρc = 1.730 g/cm3, μ = 2.532 mm−1, F(000) = 1620, R = 0.0332 and wR = 0.0924 for 5390 observed reflections with I ≥ 2σ(I). For complex III, the Dy3+ ion is eight-coordinated by a ligand Cydta and two water molecules, yielding a distorted square antiprismatic conformation, and the complex crystallizes in the triclinic system with space group P . The crystal data are as follows: a = 8.604(3), b = 10.012(4), c = 14.369(6) ?, α = 88.330(6)°, β = 75.363(6)°, γ = 88.285(6)°, space group P V = 1196.9(8) ?3, Z = 2, ρc = 1.776 g/cm3, μ = 3.194 mm−1, F(000) = 644, R = 0.0445 and wR = 0.1041 for 3931 observed reflections with I ≥ 2σ(I). The article is published in the original.  相似文献   

15.
The title complexes, K[SmIII(Edta)(H2O)3] · 2H2O(I)(H4Edta = ethylenediamine-N,N,N′,N′-tetraacetic acid) and K2[SmIII(Pdta)(H2O)2]2 · 4.5H2O (II) (H4Pdta = propylenediamine-N,N,N′,N′-tetraacetic acid), were prepared and their compositions and structures were determined by elemental analyses and single-crystal X-ray diffraction techniques, respectively. Complex I has a mononuclear structure, and the Sm3+ ion is nine-coordinated by an Edta ligand and three water molecules, yielding a pseudo-monocapped square antiprismatic conformation, and the complex crystallizes in the orthorhombic crystal system with space group Fdd2. The crystal data are as follows: a = 19.84(5), b = 35.58(9), c = 12.15(3) ?, V = 8580(38) ?3, Z = 16, ρ c = 1.925 g/cm3, μ = 3.010 mm−1, F(000) = 4976, R = 0.0252, and wR = 0.0560 for 3510 observed reflections with I ≥ 2σ(I). Complex II has a binuclear structure and the Sm3+ ion is ten-coordinated by a Pdta ligand, two oxygen atoms from a carboxylic group of adjacent Pdta ligand and two water molecules, yielding a distorted bicapped square antiprismatic prism. The complex crystallizes in the triclinic crystal system with space group P $ \bar 1 $ \bar 1 . The crystal data are as follows: a = 8.9523(15), b = 10.7106(15), c = 11.6900(19) ?, α = 80.613(5)°, β = 80.397(5)°, γ = 76.530(4)°, V = 1065.7(3) ?3, Z = 1, ρc = 1.970 g/cm3, μ = 2.532 mm−1, F(000) = 1620, R = 0.0332 and wR = 0.0924 for 5390 observed reflections with I ≥ 2σ(I).  相似文献   

16.
The title compound, [Zn(pytpy)2][NO3]2·2H2O (pytpy = 4′-(4-pyridyl)-2,2′: 6′,2″-terpyridine), has been synthesized by the reaction of Zn(NO3)2·6H2O with pytpy, and its crystal structure was determined by single-crystal X-ray diffraction. The crystal belongs to tetragonal space group P43 with a = 0.90873(8) nm, b = 0.90873(8) nm, c = 4.4741(6) nm, V = 3.6946(7) nm3, Z = 4, D c = 1.521 g/cm−3, μ = 0.736 mm−1, F(000) = 1744, R = 0.0871, wR = 0.1302 for 5553 observed reflections with I > 2σ(I). X-ray analysis has revealed that the ZnII ion is surrounded by six N atoms from two pytpy ligands leading to a distorted octahedral geometry. In the crystal structure there are numerous strong intermolecular and intramolecular H-bonds and π-π interactions.  相似文献   

17.
通过有限个过渡金属离子如Fe,Ni,Cr,Mn与O、OH、-O或-O2CR等桥联原子或基团键合形成的具有不同尺寸的环形轮状金属离子簇合物或分子簇合物是近年来的研究热点之一[1,2].它们不仅具有独特的结构,而且在催化、非线性光学、分子自组装等方面具有潜在的应用价值[3~5].特别是具有三角型结构的过渡金属-氧轮簇化合物由于可以作为单分子磁体的磁性交换和电子耦合的研究体系,引起了研究人员的极大地兴趣[6,7].研究表明,具有[M(μ3-O)(O2CR)6L3]0/+,(M=Fe3+或Mn3+,L为水或吡啶,R为烷基或芳香基团)结构的化合物具有反铁磁作用[8,9].  相似文献   

18.
[Mn2(CHZ)4(H2O)2](PA)4·10H2O的制备和分子结构研究   总被引:10,自引:0,他引:10  
本文论述了苦味酸(PA,三硝基苯酚)锰与碳酰肼(CHZ, NH2NHCONHNH2)反应制备目标配合物的方法及该配合物的晶体结构。该配合物的结构式为[O,O′-μ-Mn2(CHZ)4(H2O2)](PA)4·10H2O。晶体属三斜晶系,P1 空间群。晶体学参数为:a=0.8269(1) nm, b=1.2812(1) nm, c=1.5915(1) nm; α=109.58(1)°, β=95.19(1)°, γ=92.76(1)°, V=1.5765(2)nm3; Z=1, Dc=1.580 g·cm-3, μ(Mo Kα)=520 m-1。晶体结构经全矩阵最小二乘法修正,最终偏离因子R=0.0557。该化合物为具有中心对称的双核配合物,以两个碳酰肼分子中羰基氧为桥原子将两个锰离子结合起来,与锰离子形成配位键的原子是碳酰肼分子第一、五氮原子,羰基氧原子和水分子中的氧原子,锰离子的配位数为七。若味酸根作为外界离子以库伦力和氢键与内界离子结合成配合物分子。  相似文献   

19.
用直接法培养了配合物[Co(H2O)6]·(Hnip)2·(H2nip)2·(DMA)2·(H2O)8(DMA=CH3NHCH3)的晶体并用X射线单晶衍射,元素分析和傅里叶变换红外光谱进行了表征。该晶体属于三斜晶系,P-1空间群,晶胞参数为a=0.7012(1)nm, b=1.1378(2) nm, c=1.6612(3) nm, α=84.92(3)º, β=85.19(3)º,γ=85.91(3)º。晶胞体积V=1.3128(5) nm3, Z=1, 理论密度Dc=1.573 g/cm3. 最终R因子[I>2σ(I)]为: R1=0.0279,wR2=0.0765; 所有衍射点的R因子为: R1=0.0327, wR2=0.0806.衍射结果表明,在晶体结构中两个Hnip分子,两个H2nip分子,两个DMA分子和八个水分子通过氢键和π-π堆积作用连接到每个Co配位八面体中心上。对配合物进行了DSC和TG-DTG热分析,根据热分析结果推测得到配合物的热分解机理,并且用Kissinger,Ozawa,积分法和微分法确定了最可能的动力学模型函数。  相似文献   

20.
The NH4[EuIII(Cydta)(H2O)2]·4.5H2O (I) (H4Cydta = trans-1,2-cyclohexanediamine-N,N,N′,N′-tetraacetic acid) and K2[Eu2III(pdta)2(H2O)2]·6H2O (II) (H4pdta = propylenediamine-N,N,N′,N′-tetraacetic acid) complexes are prepared by heat-refluxing and acidity-adjusting methods respectively, and their composition and structures are determined by elemental analyses and single crystal X-ray diffraction techniques. The complex I has a mononuclear structure, crystallizes in the triclinic crystal system with the P[`1]P\bar 1 space group; the central EuIII ion is eight-coordinated by a hexadentate Cydta ligand and two water molecules. The crystal data are as follows: a = 8.653(4) ?, b = 10.041(4) ?, c = 14.405(6) ?, α = 88.469(6)°, β = 74.892(6)°, γ = 88.256(7)°, V = 1207.5(9) ?3, Z = 1, D c = 1.731 g/cm3, μ = 2.669 mm−1, F(000) = 638, R = 0.0257, and wR = 0.0667 for 3807 observed reflections with I ≥ 2σ(I). The EuN2O6 part in the [EuIII(Cydta)(H2O)2] complex anion forms a pseudo-square antiprismatic polyhedron. The complex II is eight-coordinate as well; it is a binuclear structure that crystallizes in the monoclinic crystal system with the C 2/c space group; half of the central EuIII ion is coordinated by two nitrogen atoms from one hexadentate pdta ligand and six oxygen atoms from the same pdta ligand, one water molecule and carboxylic group from the neighboring pdta ligand respectively. The crystal data are as follows: a = 19.866(3) ?, b = 9.1017(12) ?, c = 21.010(3) ?, β = 104.972(2)°, V = 3670.1(9) ?3, Z = 8, D c = 2.046 g/cm3, μ = 3.710 mm−1, F(000) = 2240, R = 0.0213 and wR = 0.0460 for 4183 observed reflections with I ≥ 2σ(I). Otherwise, the two EuN2O6 parts in the [Eu2III(pdta)2(H2O)2]2− complex anion form a pseudo-square antiprismatic polyhedron.  相似文献   

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