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1.
A DTA study of thermal decomposition of (NH4)2[Ru(NO)Cl5] in helium atmosphere has been carried out, a synthetic procedure for preparation of the trans-diammine complex mer-[Ru(NO)(NH3)2Cl3] (I) with yield ∼70% has been developed. On re-crystallization of I from aqueous solution a trans-aquanitroso complex [Ru(NO)(NH3)2Cl2(H2O)]Cl·H2O (II) has been isolated. The structures of the compounds have been determined by single crystal X-ray diffraction: space group Pbcn, a = 6.607(1) ? b = 11.255(2) ? c = 9.878(2) ? (I) and space group Ima2, a = 8.3032(3) ?, b = 8.0890(2) ?, c = 15.9192(5) ? II). Original Russian Text Copyright ? 2008 by M. A. Il’in, V. A. Emel’yanov, and I. A. Baidina __________ Translated from Zhurnal Strukturnoi Khimii, Vol. 49, No. 6, pp. 1128–1136, November–December, 2008.  相似文献   

2.
New complexes of transition metals with organotellurium halide ligands are reported. Iodination of [CpMn(CO)2]2(μ-Ph2Te2) leads to the Te-Te bond cleavage and formation of CpMn(CO)2(PhTeI). Oxidative addition of PhTeBr3 to Fe(CO)5 gives the monomeric complex (CO)3FeBr2(PhTeBr) which is isostructural with the recently reported (CO)3FeI2(PhTeI). Insertion of phenyltellurenyl iodide (PhTeI) into the Fe-I bond of CpFe(CO)2I forms CpFe(CO)2(TeI2Ph). Molecular structures of the reported complexes were determined by single-crystal X-ray diffraction analysis (XRD). A considerable shortening of metal-tellurium distances is observed.  相似文献   

3.
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   

4.
Diamagnetic Pd(II) complexes with the chiral ethylenediaminodioxime (H 2 L) and bis-α-thiooxime (H2L1), the derivatives of monoterpenoid (+)-3-carene, of the composition Pd2(H2L)Cl4(I), Pd2(H2L1)Cl4 (II), and the solvate Pd2(H2L1)Cl4·3DCl3 (III) were synthesized. The crystal structures of complex I and solvate III were determined from X-ray diffraction data. The structures consist of acentric binuclear molecules with the coordination cores PdN2Cl2 (in I) and PdNSCl2 (in III) in the form of the distorted squares. In complex I, each Pd atom coordinates two N atoms of the tetradentate bridge-cyclic ligand H2L and two Cl atoms; in compound III, one N and one S atom of the tetradentate bridge-cyclic ligand H2L1, and 2 Cl atoms. The CDCl3 molecules in compound III lie in the cavities formed by the molecules of complex II. In both structures, the PdCl2 fragments are in the trans-positions. The 1H NMR spectra indicate that the structures of complexes I, II in solutions are similar to the structures of compounds I, III in the solid state. Original Russian Text ? T.E. Kokina, L.I. Myachina, L.A. Glinskaya, A.V. Tkachev, R.F. Klevtsova, L.A. Sheludyakova, S.N. Bizyaev, A.M. Agafontsev, N.B. Gorshkov, S.V. Larionov, 2008, published in Koordinatsionnaya Khimiya, 2008, Vol. 34, No. 2, pp. 120–132.  相似文献   

5.
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   

6.
Crystals of [Ba(H2O)4][Co(Gly)2(NO2)2]2 · 1.43H2O (a=8.1917(6) , b=8.4440(4) , c=19.444(1) , =98.189(9)°, Z=2, space group P2/n) contain infinite strips of alternating axially symmetric [Ba(H2O)4]2+ fragments and two dinitro-bis(glycinato)cobaltate(III) ions. In addition to four oxygen atoms of water molecules, the nearest environment of Ba includes six oxygen atoms of the carboxyl groups of four anions, two of which are also coordinated by the cobalt atoms (Ba-O, 2.77–3.01 ). The nitrite ions do not interact with the Ba2+ ions.__________Translated from Koordinatsionnaya Khimiya, Vol. 31, No. 5, 2005, pp. 329–332.Original Russian Text Copyright © 2005 by Zabel, Poznyak, Pawlowski.  相似文献   

7.
The structure of the interaction products of (NH4)2[Ru(NO)Cl5] solution with ammonium acetate on heating is studied. The crystal structure of the [Ru(NO)(NH3)3(H2O)Cl][Ru(NO)(NH3)3(OH)Cl] × [Ru(NO)(NH3)Cl4]2Cl-2H2O compound (compound I) containing a previously unknown anion of the nitrosomonoammine series is determined: Cc space group; a = 33.530(7) ?, b = 8.202(2) ?, c = 11.844(2) ?; β= 101.54(3)°.  相似文献   

8.
采用周期性密度泛函理论研究了H2和O2在Pd(111),Pd(100)及Pd(110)表面上直接合成H2O2的反应机理,对反应的主要基元步骤进行了计算和分析.结果表明,Pd(111)表面对H2O2直接合成的催化选择性最好,表面原子密度较低的Pd(100)表面和Pd(110)表面上含有O-O键的表面物种解离严重,不利于H2O2的生成.H2O2的选择性与含有O-O键表面物种的O-O键能和表面物种的结合能有关.含有O-O键的表面物种在表面的结合能越大,越容易发生解离,不利于形成H2O2.  相似文献   

9.
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   

10.
The possibility of synthesizing heteronuclear compounds in the systems based on Fe(II), Fe(III), Al(III), SO42−, Cl-H2O-OH, and NH3 was studied. A mathematical model based on data on the potentiometric titration was developed. The elemental and phase composition and the structure of the compounds synthesized were determined by the XPA, DTA and NMR methods to optimize the conditions of the synthesis.  相似文献   

11.
The syntheses of the complex copper salt CuL2 · 2H2O (I) and the erbium nitrate complex Er(NO3)3 · 2HL · 2H2O (II) (HL is 2-[2′-(oxymethyldiphenylphosphinyl)phenyldiazenyl]-4-tert-butylphenol) have been described. Basic vibrational frequencies in the IR spectra of I and II have been interpreted. The crystal structure of I has been determined by X-ray crystallography: the crystals are monoclinic, a = 15.157(3) ?, b = 17.080(2) ?, c = 22.451(9) ?, β = 106.09(3)°, V = 5584(3) ?3, Z = 4, space group C2/c, R = 0.0546 (for 1152 reflections with I > 2σ(I)). The coordination polyhedron of the copper atom (symmetry C 2) can be described as a symmetrically elongated square bipyramid (4+2). The basic square of the Cu polyhedron is formed by the oxygen atom of the substituted phenol and one of the nitrogen atoms of the azo group of each of the two deprotonated ligands L (Cu-N, 1.969(6) ?; Cu-O, 1.899(5) ?). The angles between the opposite O and N atoms are 157.6°, and the other equatorial angles are in the range 90.6°–95.9°. The axial positions are occupied by the anisole O(2) and O(2A) atoms (Cu-O, 2.737(6) ?, the O(2)Cu(1)O(2A) angle, 132.3°). In the crystal of I, complex molecules and water molecules of crystallization are combined by a system of hydrogen bonds. IR spectra show that, in complex II, as distinct from compound I, the HL ligand is coordinated to the erbium atom through the phosphoryl oxygen atom. Original Russian Text ? A.Yu. Tsivadze, L.Kh. Minacheva, I.S. Ivanova, V.E. Baulin, E.N. Pyatova, V.S. Sergienko, 2008, published in Zhurnal Neorganicheskoi Khimii, 2008, Vol. 53, No. 4, pp. 601–607.  相似文献   

12.
Two modifications of the new uranyl oxalate hydroxide dihydrate [UO2)2(C2O4)(OH)2(H2O)2] (1 and 2) and one form of the new uranyl oxalate hydroxide trihydrate [(UO2)2(C2O4)(OH)2(H2O)2]·H2O (3) were synthesized by hydrothermal methods and their structures determined from single-crystal X-ray diffraction data. The crystal structures were refined by full-matrix least-squares methods to agreement indices R(wR)=0.0372(0.0842) and 0.0267(0.0671) calculated for 1096 and 1167 unique observed reflections (I>2σ(I)), for α (1) and β (2) forms, respectively and to R(wR)=0.0301(0.0737) calculated for 2471 unique observed reflections (I>2σ(I)), for 3. The α-form of the dihydrate is triclinic, space group , Z=1, a=6.097(2), b=5.548(2), , α=89.353(5), β=94.387(5), γ=97.646(5)°, , β-form is monoclinic, space group C2/c, Z=4, a=12.180(3), b=8.223(2), , β=95.817(4), . The trihydrate is monoclinic, space group P21/c, Z=4, a=5.5095(12), b=15.195(3), , β=93.927(3), . In the three structures, the coordination of uranium atom is a pentagonal bipyramid composed of dioxo UO22+ cation perpendicular to five equatorial oxygen atoms belonging to one bidentate oxalate ion, one water molecule and two hydroxyl ions in trans configuration in 2 and in cis configuration in 1 and 3. The UO7 polyhedra are linked through hydroxyl oxygen atoms to form different structural building units, dimers [U2O10] obtained by edge-sharing in 1, chains [UO6] and tetramers [U4O26] built by corner-sharing in 2 and 3, respectively. These units are further connected by oxalate entities that act as bis-bidentate to form one-dimensional chains in 1 and bi-dimensional network in 2 and 3. These chains or layers are connected in frameworks by hydrogen-bond arrays.  相似文献   

13.
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   

14.
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   

15.
利用紫外-可见吸收光谱和核磁研究了[Ru(phen)2(H2bbim)](PF6)2配合物与Cl-,Br-,I-,NO3-,HSO4-,H2PO4-,OAc-和F-离子之间的作用。结果表明OAc-和F-可以使该配合物苯并联咪唑上的质子逐步脱去,相应的溶液颜色由黄色变为橙棕色,最后变为紫色。因此该配合物可以对阴离子实现目视识别。  相似文献   

16.
Two metal-organic coordination polymers [Cu(bpy)2(H2O)2](NO3)2·4.5C2H5OH (1) and [Cu2(bpy)(H2O)(L-pha) 2](NO3)2·H2O (2) (L-Hpha = L-phenylalanine, bpy = 4,4′-bipyridyl) are prepared by slow evaporation of an aqueous alcoholic solution of copper nitrate, L-phenylalanine, and 4,4′-bipyridyl. The structure and composition of the obtained compounds are determined by single crystal XRD. The framework of compound 1 is positively charged and forms two types of intersecting channels. Compound 2 is a homochiral metal-organic coordination polymer whose structure contains L-phenylalanine anions.  相似文献   

17.
The viscosity of dilute aqueous solutions of K3[AI(ox)3]·3H2O, K3[Fe(ox)3]·3H2O, K3[Co(ox)3]·3H2O, and K3[Cr(ox)3]·3H2O complexes, as well as K2(ox)·H2O, were measured between 15 and 35°C. Those of CoCl2, 6H2O, FeCl3, A12(SO4)3·18H2O, and CrCl3·6H2O were measured at 25°C. These data were analyzed by the Jones–Dole equation. The ionic B coefficients of the above complex anions were discussed in terms of ion–solvent interactions and the overall change in B associated with complex formation.  相似文献   

18.
Methods for the synthesis of trans-diammino complexes [RuNO(NH3)2(NO2)2(OH)] (I) and [RuNO(NH3)2(H2O)(NO3)2](NO3)·H2O (II) are suggested. The compounds were studied by IR spectroscopy and X-ray phase and X-ray structural analyses. Crystal data: space group P-1; a = 6.2328(2) ?, b = 11.0488(3) ?, c = 11.0981(4) ?, α = 71.942(1)°, β = 83.291(1)°, γ = 86.877(1)° (I); space group P21; a = 6.6290(2) ?, b = 13.4389(5) ?, c = 7.0180(2) ?, β 114.281(1)° (II). Complex II readily lost some part of crystal water on storage in open air. Original Russian Text Copyright ? 2009 by M. A. Il’in, E. V. Kabin, V. A. Emel’yanov, I. A. Baidina, and V. A. Vorob’yov __________ Translated from Zhurnal Strukturnoi Khimii, Vol. 50, No. 2, pp. 341–348, March–April, 2009.  相似文献   

19.
Ammonium hydrogen hexaaquacobaltate(III) isopolyvanadate [(NH4)2][Co(H2O)6] · H[V10O28] · 8H2O was synthesized and studied by X-ray diffraction, thermogravimetry, and IR and NMR spectroscopy. The crystals are triclinic, space group P [`1]\bar 1, a = 8.216(2), b = 9.965(2), c = 11.796(2) ?, α = 77.71(3)°, β = 71.11(3)°, γ = 86.11(3)°, V = 867.0(3) ?3, ρ(calcd.)= 2.501 g/cm3, Z = 1.  相似文献   

20.
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   

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