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1.
Single crystals of Cs4[(UO2)2(C2O4)(SO4)2(NCS)2] · 4H2O (I) and (NH4)4[(UO2)2(C2O4)(SO4)2(NCS)2] · 6H2O (II) have been synthesized and studied by X-ray diffraction. The crystals of both compounds are orthorhombic with the space group Pbam, Z = 2, and unit cell parameters a = 12.0177(3) ?, b = 18.6182(5) ?, c = 6.7573(10) ?, R = 0.0376 (I); a = 11.6539(9) ?, b = 18.3791(13) ?, c = 6.7216(5) ?, R = 0.0179 (II). The main structural units of crystals I and II are [(UO2)2(C2O4)(SO4)2(NCS)2]4− chains belonging to the crystal-chemical group A2K02B22M21 (A = UO22+, K02 = C2O42−, B2 = SO42−, M1 = NCS) of the uranyl complexes. The uranium-containing chains are joined into a three-dimensional framework due to a system of electrostatic interactions with the cesium or ammonium ions in the structure of I. In the structure of II, this framework is additionally stabilized by hydrogen bonds involving the outer-sphere water molecules and ammonium ions. Original Russian Text ? I.V. Medrish, A.V. Virovets, E.V. Peresypkina, L.B. Serezhkina, 2008, published in Zhurnal Neorganicheskoi Khimii, 2008, Vol. 53, No. 7, pp. 1115–1120.  相似文献   

2.
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   

3.
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   

4.
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   

5.
在水乙醇混合溶剂中,首次得到了2-羰基丙酸水杨酰腙、1,10-菲啰啉与硝酸钆形成的配合物[Gd(C10H9N2O4)(C10H8N2O4)(H2O)3]2·phen·4H2O,并测试了其单晶结构。该配合物属三斜晶系,空间群为P-1。每个配合物分子中有两个九配位的钆的结构单元,每个钆离子与两个三齿配体2-羰基丙酸水杨酰腙(分别以负一价和负二价形式)和三个水分子配位。每个钆单元在空间呈扭曲的单帽四方反棱柱。同时还有一个游离的1,10-菲啰啉存在于晶格中,通过氢键与配位水作用。生物活性试验表明该配合物对三种病原菌有一定的抑菌活性。  相似文献   

6.
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   

7.
A modified method of synthesis of a phosphoryl podand, 1,5-bis[2-(dihydroxyphosphinyl)phenoxy]-3-oxapentane (L), has been developed. The IR spectra of this podand and its dehydrate (L [L · H2O] · H2O (I) have been studied, the structure of I has been determined by X-ray crystallography. The crystals are orthorhombic, a = 9.4006(19) ?, b = 25.494(5) ?, c = 8.4264(17) ?, V = 2019.5(7) ?3, Z = 4, space group Pna21, R = 0.0512 for 3016 reflections with I > 2σ(I). Compound I is a host-guest molecular complex. Phosphoryl podand L acts as a host molecule, and one of the water molecules (H2O(11)) is a guest. This molecule forms one donor and one acceptor intramolecular hydrogen bond with hydroxyl groups of two phosphoryl groups (O(8)H(4) and O(3)H(2)) and combines them into an 18-membered macrocyclic ring, acting as a kind of “lock.” The H2O(11) molecule forms a second donor intramolecular hydrogen bond with the O(5) ether atom. The neutral molecular complexes are linked by hydrogen bonds directly and through the second water molecule (H2O(10)) into chains running along the c axis.  相似文献   

8.
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   

9.
The formation of the thioammelinium cation in an aqueous solution in the presence of uranyl ions is demonstrated. Single crystal X-ray diffraction study of (C3N5H6S)2[UO2(C2O4)2(H2O)] · C2N4H4 was carried out and the geometric characteristics of thioammelinium were determined for the first time. The crystals are triclinc, space group , Z = 2, a = 8.5201(11) ?, b = 11.4027(14) ?, c = 14.329(2) ?, α = 103.182(5)°, β = 99.607(6)°, γ = 109.698(4)°, R = 0.0526. The main structural units in the crystal are mononuclear complex groups [UO2(C2O4)2(H2O)]2− corresponding to the crystal chemical group AB 2 01 M1 (A = UO 2 2+ , B01 = C2O 4 2− , M1 = H2O) of uranyl complexes. Uranium-containing mononuclear complexes are connected into a three-dimensional framework through electrostatic interactions and hydrogen bonds involving thioammelinium ions, water molecules, and cyanoguanidine. Original Russian Text ? L.B. Serezhkina, A.V. Virovets, E.V. Peresypkina, I.V. Medrish, 2007, published in Koordinatsionnaya Khimiya, 2007, Vol. 33, No. 5, pp. 380–385.  相似文献   

10.
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   

11.
The vanadium(V) complexes K[VO2(SeO4)(H2O)] and K[VO2(SeO4)(H2O)2] · H2O were synthesized using original procedures; their physicochemical properties were studied, and the crystal structure was determined on the basis of X-ray diffraction and neutron diffraction data. The structure of K[VO2(SeO4)(H2O)2] · H2O is composed of VO6 octahedra connected to form infinite chains by bridging SeO4 tetrahedra. Each VO6 tetrahedron has short terminal V-O bonds forming the bent dioxovanadium group VO2+ The unit cell parameters of K[VO2(SeO4)(H2O)2] · H2O are a = 6.4045(1) ?, b = 9.9721(2) ?, c = 6.6104(1) ?, β = 107.183(1)°, V = 403.34 ?3, Z = 2, monoclinic system, space group P21. The complex K[VO2(SeO4)(H2O)] forms a two-dimensional layered structure composed of highly distorted VO6 octahedra having two short terminal V-O bonds and SeO4 groups coordinated simultaneously by three vanadium atoms. This compound crystallizes in the monoclinic system (space group P21/c): a = 7.3783(1) ?, b = 10.5550(2) ?, c = 10.3460(2) ?, β = 131.625(1)°, V = 602.894(5) ?3, Z= 4. The vibrational spectra of the studied compounds are fully consistent with their structural features.  相似文献   

12.
Crystals of the tetranuclear complex [Fe4O2(H2O)10(C5H5NCOO)4](NO3)8 · 2H2O are obtained by the slow evaporation of an aqueous solution of iron(III) nitrate and isonicotinic acid. According to the X-ray diffraction data, four metal atoms lie in the same plane and together with two μ3-O oxygen atoms form the fragment [Fe43-O)2]10+. The [Fe4O2(H2O)10(C5H5NCOO)4]8+ cation has been obtained and structurally characterized for the first time.  相似文献   

13.
用非等温热重法研究了Eu(III)的化合物[Eu(C10H9N2O4)(C10H8N2O4)(H2O)3]2·phen·4H2O 的热分解及其动力学,并用Kissinger和Ozawa 方法计算了第一分解阶段的活化能.  相似文献   

14.
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   

15.
A new complex with the formula (NH4)4[Mo8O24(C3H2O2)2] · 4H2O (1) has been synthesized and characterized by single crystal X-ray diffraction and infrared spectrum. The complex is small yellow crystal and space group P 1 with a = 9.9869(18) ?, b = 10.030(19) ?, c = 10.366(19) ?, α = 91.68(3)°, β = 98.94(3)°, γ = 119.37(2)°, V = 887(3) ?3, and Z = 1. The complex contains two malonic acid ligands bonded to the γ-Mo8 264− ions which consist of eight MoO6 edge-sharing octahedral. In this crystal structure, the octamolybdate anion is mutually hydrogen bonded by ammonium ions and water molecules.  相似文献   

16.
The complexes [UO2(C6H4NO2)2(C6H5NO2) (I) and [UO2SO4(C6H5NO2)(H2O)] · H2O (II) were synthesized and studied by X-ray diffraction analysis. Crystals I are monoclinic: a = 7.0081(3), b = 14.9624(7), c = 9.1837(5) ?, β = 96.594(2)°, Z = 2, space group P21/m. Crystals II are triclinic: a = 6.8097(6), b = 9.3837(8), c = 10.4556(10) ?, α = 85.279(3), β = 75.434(3), γ = 69.180(3)°, Z = 2, space group . The main structural unit of crystal I is a mononuclear fragment, which belongs to the crystal chemical group AB 2 01 M1 (A = UO 2 2+ , B01 are ions of pyridine-2-carboxylic (picolinic) acid, M1 are molecules of picolinic acid) of the uranyl complexes. The main structural unit of crystal II is a chain, which belongs to the crystal chemical group AT3M 2 1 (where T3-SO 4 2− , M1 are water and picolinic acid molecules) of the uranyl complexes. Picolinic acid in complexes I, II was found to have a zwitterion structure. Original Russian Text ? E.V. Grechishnikova, E.V. Peresypkina, A.V. Virovets, Yu.N. Mikhailov, L.B. Serezhkina, 2007, published in Koordinatsionnaya Khimiya, 2007, Vol. 33, No. 6, pp. 468–475.  相似文献   

17.
A novel binuclear praseodymium(III) complex with N-(2-propionyl)salicyloylhydrazone (C10H10N2O4, H3L) and p-hydroxybenzoic acid (C7H6O3, Phba) was prepared in a H2O-C2H5OH mixed solution, and the crystal structure of [Pr2(H2L)2(Phba)4(H2O)2] · 2H2O (I) was determined by X-ray single crystal diffractometry. Complex I crystallizes in the monoclinic system, space group P21/c, a = 1.1050(4), b = 1.9534(7), c = 1.2376(4) ?, β = 94.955(7)°, and Z = 4. In the structure each Pr3+ ion lies in a single capped square antiprism geometry coordinated by carboxyl O and acyl O atoms and azomethine N atom of one ligand (H2L form), which coordinates via the keto form, four carboxyl O atoms from two Phba, and O atoms of two water molecules. In each molecule, two tridentate ligands were coordinated by the H2L form, and each Pr3+ ion was chelated by the carboxyl group from Phba. The carboxyl groups of H2L and other two Phba were coordinated via μ2-bridging form and bidentate bridging form, respectively. Complex I and ligands Phba and H3L were also searched for biological activity against Valsa mali by the growth rate method. The result showed that the inhibitory rate of ligands Phba and H3L is better than complex I, especially Phba.  相似文献   

18.
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   

19.
利用温度跃升傅立叶变换红外原位分析技术在0.1MPa氩气的条件下,对斯蒂酚酸碳酰肼铅和斯蒂酚酸碳酰肼镉的快速热分解过程进行了研究。研究结果表明,斯蒂酚酸碳酰肼铅的主要热分解气体为NH3, H2O和 HONO,而斯蒂酚酸碳酰肼镉的主要热分解气体为CO 和 NO,因此斯蒂酚酸碳酰肼镉不满足作为环境友好起爆药的使用要求。这两种化合物在快速热分解过程中均产生金属异氰酸盐、金属碳酸盐和金属氧化物。利用Real程序计算其燃烧温度可得斯蒂酚酸碳酰肼铅的燃烧温度要高于斯蒂酚酸碳酰肼镉,对其燃烧产物进行计算,发现HNCO不在燃烧产物之列,NO的含量也比实验得出的浓度要小。  相似文献   

20.
The structures of the crystals of Ba4[trans(N)-Co(Ida)2]3[cis-(N)-Co(Ida)2]2(ClO4)3 · 19.46H2O · 2CH3OH (I) and Ba[trans-(N)-Co(Ida)2]2 · 7H2O (II) (H2Ida is iminodiacetic acid) were determin by X-ray diffraction. The crystals of I containing two geometric isomers of the complex anions [Co(Ida)2] were obtained by a slow cooling of a hot solution, which contained initially only the cis-isomer. One Ba atom in I interacts with the trans-complex and with two cis-complexes to give a three-dimensional framework in crystal I. The positive charge of the last framework is compensated by one more trans-complex and by the perchlorate ions, one of which acts as a bidentate ligand with respect to the Ba atom. The crystals of II are built of the chains with the alternating Ba atoms and the trans-(N)-[Co(Ida)2] anions. The other anions of the same structure are each “suspended” to the Ba atoms of the chain. Original Russian Text ? M. Zabel, A.I. Poznyak, V.I. Pawlowskii, 2008, published in Koordinatsionnaya Khimiya, 2008, Vol. 34, No. 11, pp. 831–836.  相似文献   

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