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1.
D. M. Tsymbarenko E. A. Bukhtoyarova I. E. Korsakov S. I. Troyanov 《Russian Journal of Coordination Chemistry》2011,37(11):825-831
A method for the synthesis of potassium pivalates (trimethylacetates) from potassium tert-butoxide and pivalic acid was proposed. The complexes of the formulas [K(H2O)(Piv)]∞(I) and [K2(Phen)(H2O)2(Piv)2]∞ (II) (Piv denotes the pivalate anion and Phen denotes 1,10-phenanthroline) were obtained and characterized by elemental analysis
and IR and 1H NMR spectroscopy. The crystal structures of complexes I and II were determined using X-ray diffraction. Crystal structure I has a layered motif with two nonequivalent K atoms (C.N.s 5 + 2 and 6). The coordination of phenanthroline in II gives rise to a ribbon motif, the structure containing three nonequivalent K atoms (C.N.s 6, 6 + 1, and 8). 相似文献
2.
E. A. Kiseleva S. I. Troyanov Yu. M. Korenev 《Russian Journal of Coordination Chemistry》2007,33(2):85-89
Single crystals of Mg pivalate hydrate, Mg(H2O)6(Piv)2 · 3H2O (HPiv = (CH3)3CCOOH) are synthesized and their structure is determined by X-ray diffraction method. The crystals are rhombic: a = 10.917(2) Å, b = 12.625(2) Å, c = 31.394(8) Å, Z = 8, space group Pbca, R 1 = 0.0525. The Mg atom has octahedral surrounding of the O atoms of water molecules (Mg-O 2.044–2.137 Å). The cationic chains of [Mg(H2O)6] ∞ 2+ lie in the voids of doubled network anionic layers of [(H2O)3(Piv)2] ∞∞ 2? . Inside the layer, the pivalate anions alternate with water molecules in the xy plane, being bonded to them by hydrogen bonds. The cationic chains and the anionic layers are united into layered packs by hydrogen bonds between coordinated water molecules and pivalate anions and between coordinated and crystal hydrate water molecules. 相似文献
3.
S. P. Khranenko E. A. Shusharina S. A. Gromilov S. V. Korenev 《Journal of Structural Chemistry》2011,52(3):544-549
Crystal structures of two modifications of a binuclear Pd2(μ-ac)2(acac)2 complex are studied at 150 K and 297 K (ac = acetate; acac = acetylacetonate). It is demonstrated that in both cases, the packing of the complexes can be considered as pseudohexagonal, the molecules forming infinite chains by interactions between chelate rings with the shortest contacts Pd...C γ ~ 3.3 Å. 相似文献
4.
A complex of Erbium perchloric acid coordinated with l-aspartic acid and imidazole, Er2(Asp)2(Im)8(ClO4)6·10H2O was synthesized for the first time. It was characterized by IR and elements analysis. The heat capacity and thermodynamic
properties of the complex were studied with an adiabatic calorimeter (AC) from 80 to 390 K and differential scanning calorimetry
(DSC) from 100 to 300 K. Glass transition and phase transition were discovered at 220.45 and 246.15 K, respectively. The glass
transition was interpreted as a freezing-in phenomenon of the reorientational motion of ClO4− ions and the phase transition was attributed to the orientational order/disorder process of ClO4− ions. The thermodynamic functions [H
T
− H
298.15] and [S
T
− S
298.15] were derived in the temperature range from 80 to 390 K with temperature interval of 5 K. Thermal decomposition behavior
of the complex in nitrogen atmosphere was studied by thermogravimetric (TG) analysis and differential scanning calorimetry
(DSC). 相似文献
5.
Triethylamine reacts with aqueous zinc acetate and the product of its thermolysis in the presence of benzoic acid to yield
the complexes [Zn7(μ4-O)(μ-OOCMe)10][η-OC(Me)OHNEt3]2 (1) and [Zn2(μOOCPh)4][η-OC(Me)OHNEt3]2 (2), respectively. The reactions of 1 and 2 with 3,5-dimethylpyrazole at room temperature in benzene yield pyrazolate-bridged binuclear complexes Zn2(μdmpz)2(Hdmpz)2(OOCR)2 (R = Me (3), Ph (4)). The structures of complexes 1–4 have been determined by X-ray crystallography. 相似文献
6.
The reaction of the trinuclear oxo-centered mixed-valence complex [Mn3O(O2CPh)6(Py)2(H2O)] with 2,2′-bipyridyl (Bipy) and another potential tripodal ligand affords the title compound [Mn3(PhCO2)6(Bipy)2] · H2O in good yield. The X-ray crystallographic diffraction study reveals that three mangenese ions are arranged in a linear mode with Mncenter-Mnterminal and Mnterminal-Mnterminal diatances of 3.588 and 7.176 Å, respectively. Molar magnetic susceptibility of the compound gradually decreases from 12.23 (300 K) to 4.45 cm3 K mol?1 (2 K). Taking into account the structure of this compound, the data in the 2.0–300 K range were fit to the appropriate theoretical expression to give J = ?2.73 cm?1, ρ = 2.07%, N a = ?0.0004 cm3 mol?1, g = 1.992, and R 2 = 0.99996. The magnetization versus external magnetic field measurements at 2 K shows that the ground state is S T = 5/2. 相似文献
7.
Abstract
Three novel lanthanide-organic frameworks: [Ln2(pyba)3(μ3-OH)2(μ2-OH)(H2O)] n (Ln = Er (1), Y (2), Dy (3) Hpyba = 4-pyridin-4-yl-benzoic acid) have been hydrothermally synthesized and structurally characterized by single crystal X-ray diffraction. Structure analysis shows that each {Ln4(μ3-OH)4(μ2-OH)2} cluster units interconnect to form 1-D chains, which are further linked by π–π interactions to make a 3-D supramolecular network structure. Furthermore, the IR, PXRD and TGA of compounds 1–3 were also studied. 相似文献8.
L. B. Serezhkina E. V. Peresypkina A. V. Virovets I. V. Medrish D. V. Pushkin 《Russian Journal of Inorganic Chemistry》2009,54(10):1577-1580
Single crystals of Cs[(UO2)2(C2O4)2(OH)] · H2O were synthesized and structurally studied using X-ray diffraction. The compound crystallizes in monoclinic space group P21/m, Z = 2, with the unit cell parameters a = 5.5032(4) Å, b = 13.5577(8) Å, c = 9.5859(8) Å, β = 97.012(3)°, V = 709.86(9) Å3, R = 0.0444. The main building units of crystals are [(UO2)2(C2O4)2(OH)]? layers of the A2K 2 02 M2 (A = UO 2 2+ , K02 = C2O 4 2? , and M2 = OH?) crystal-chemical family. Uranium-containing layers are linked into a three-dimensional framework via electrostatic interactions with outer-sphere cations and hydrogen bonds with water molecules. 相似文献
9.
Ray L. Frost Sara J. Palmer Ross E. Pogson 《Journal of Thermal Analysis and Calorimetry》2012,107(3):905-909
Thermogravimetry combined with evolved gas mass spectrometry has been used to characterise the mineral crandallite CaAl3(PO4)2(OH)5·(H2O) and to ascertain the thermal stability of this ‘cave’ mineral. X-ray diffraction proves the presence of the mineral and
identifies the products of the thermal decomposition. The mineral crandallite is formed through the reaction of calcite with
bat guano. Thermal analysis shows that the mineral starts to decompose through dehydration at low temperatures at around 139 °C
and the dehydroxylation occurs over the temperature range 200–700 °C with loss of the OH units. The critical temperature for
OH loss is around 416 °C and above this temperature the mineral structure is altered. Some minor loss of carbonate impurity
occurs at 788 °C. This study shows the mineral is unstable above 139 °C. This temperature is well above the temperature in
the caves of 15 °C maximum. A chemical reaction for the synthesis of crandallite is offered and the mechanism for the thermal
decomposition is given. 相似文献
10.
Zh. V. Akhmerkina E. V. Peresypkina A. V. Virovets L. B. Serezhkina 《Russian Journal of Inorganic Chemistry》2008,53(9):1396-1400
Single crystals of Ba3[UO2(C2O4)2(NCS)]2 · 9H2O are synthesized and studied by X-ray diffraction. The crystals are orthorhombic, space group Fddd, Z = 16, and the unit cell parameters are a = 16.253(3) Å, b = 22.245(3) Å, c = 39.031(6) Å. The main crystal structural units are mononuclear complex groups [UO2(C2O4)2NCS]3? of the crystal-chemical family (AB 2 01 M1 (A = UO 2 2+ , B01 = C2O 4 2? , M1 = NCS?) of the uranyl complexes linked into a three-dimensional framework by electrostatic interactions and hydrogen bonds involving oxalate ions and water molecules. 相似文献
11.
The structure of tris-complexes Y(MDA)3, Y(HFA)3 and their dimeric forms of Y2(MDA)6 and Y2(HFA)6 (MDA = C3O2H3; HFA = C5O2F6H) are investigated by the non-empirical Hartree-Fock method and also taking into account the correlation of electrons in the context of density functional theory (DFT/B3LYP) using effective pseudopotentials to describe the atomic core and double-exponential valence basis sets supplemented with polarization functions. For the first time the structure of Y(HFA)3, Y2(MDA)6, and Y2(HFA)6 molecules has been studied in this work. The equilibrium configuration of Y(HFA)3 monomer is a structure with a coordination polyhedron of [YO6] that has the form of a distorted octahedron with planar chelate fragments and CF3 substituents in which the C-F bond screens the C-C bond in the chelate fragment. The barrier of the internal rotation of one CF3 group is ~3.0 kJ/mole (DFT/B3LYP). It is shown that rotations of CF3 groups in Y(HFA)3 molecule could be considered as mutually independent. The structures of C 1 and C 2 symmetry are the equilibrium configurations of Y2(MDA)6 and Y2(HFA)6 dimers respectively (DFT/B3LYP). The structure of the coordination polyhedron of [Y2O12] in C 1 and C 2 symmetry configurations can be represented as a combination of eight-and seven-coordinated polyhedra or two seven-coordinated polyhedra respectively. The energy stability of dimeric complexes is studied. According to DFT/B3LYP data, the dimerization energy equals ?80.8 kJ/mole and ?62.3 kJ/mole for Y2(MDA)6 and Y2(HFA)6 respectively. The force fields and frequencies of normal vibrations are calculated for the equilibrium configurations. The trends of changes in the vibrational spectra in Y(MDA)3→Y(HFA)3 and monomer→dimer transitions are discussed. The comparison with available experimental data is made. 相似文献
12.
G. B. Andreev M. Yu. Antipin N. A. Budantseva N. N. Krot 《Russian Journal of Coordination Chemistry》2005,31(11):800-803
A new neptunium(V) complex [(NpO2)2(CH3COO)2(H2O)] ? 2H2O was synthesized and its crystal structure was determined. The unit cell parameters are: a = 24.007(10) Å, b = 6.779(3) Å, c = 8.076(3) Å, space group Pnma, Z = 4, V = 1314.2(9) Å3, R = 0.049, wR(F2) = 0.105. The crystal structure of the compound is composed of neutral [(NpO2)2(CH3COO)2(H2O)] layers and molecules of the water of crystallization. Each of the crystallographically independent neptunoyl ions performs a bidentate function thus forming a composite system of cation-cation bonds. 相似文献
13.
I. V. Medrish E. V. Peresypkina A. V. Virovets L. B. Serezhkina 《Russian Journal of Coordination Chemistry》2008,34(8):629-634
The single crystals of Rb2[(UO2)2(C2O4)2(SeO4)] · 1.33H2O were synthesized and studied by X-ray diffraction. The crystals are monoclinic, space group P21/m, Z= 2, the unit cell parameters: a = 5.6537(8), b = 18.736(3), c = 9.4535(15) Å, β = 98.440(5)°, V = 990.6(3) Å3, R 1 = 0.0506. The main structural units of the crystal are infinite layers of [(UO2)2(C2O4)2(SeO4)]2?, corresponding to the crystal chemical group A2K 2 02 B2 (A = UO 2 2+ , K02 = C2O 4 2? , B2 = SeO 4 2? ) of uranyl complexes. The uranium-containing layers are united into a three-dimensional framework through the electrostatic interactions with the outer-sphere rubidium ions and the hydrogen bonding system involving the outer-sphere water molecules. 相似文献
14.
B. T. Usubaliev P. S. Abdurakhmanova M. K. Munshieva D. M. Ganbarov 《Russian Journal of Coordination Chemistry》2010,36(11):865-869
The clathrate [Zn(C6H5COO)2(H2O)2] · 2CH3COOH (I) was obtained for the first time from zinc(II) benzoate. The individuality, the unit cell parameters, and the number of “guest”
molecules in complex I were determined from X-ray diffraction and derivatographic data. Its crystal structure was solved. 相似文献
15.
N. A. Sanina S. M. Aldoshin T. N. Rudneva N. I. Golovina G. V. Shilov Yu. M. Shul’ga V. M. Martynenko N. S. Ovanesyan 《Russian Journal of Coordination Chemistry》2005,31(5):301-306
Binuclear iron nitrosyl complex Na2[Fe2(S2O3)2(NO)4] · 4H2O (I) was synthesized by the reaction of iron(II) sulfate with sodium thiosulfate in the flow of NO gas. According to X-ray diffraction data, the [Fe2(S2O3)2(NO)4]2– anion has binuclear centrosymmetric structure with Fe atoms bonded by the µ-S atoms of thiosulfate groups. The isomeric shift for complex I =0.168(1) mm/s and quadrupole splitting E
Q
=1.288 mm/s at T=80 K. When heated, complex I transforms to Na2[Fe2(S2O3)2(NO)4] (II), whose unit cell parameters found by X-ray diffraction method differ from those of complex I. The process of transformation of I to II was studied by calorimetric method. Complex I transforms to complex II without chemical decomposition, which was confirmed by IR and mass spectroscopy data.__________Translated from Koordinatsionnaya Khimiya, Vol. 31, No. 5, 2005, pp. 323–328.Original Russian Text Copyright © 2005 by Sanina, Aldoshin, Rudneva, Golovina, Shilov, Shulga, Martynenko, Ovanesyan. 相似文献
16.
S. E. Nefedov I. V. Pruss E. V. Perova G. L. Kamalov 《Russian Journal of Inorganic Chemistry》2009,54(11):1713-1729
We discovered that reactions of hydrous cobalt and zinc acetates with 3,5-dimethylpyrazole (Hdmpz) in boiling xylene or toluene
or upon the thermolysis of solid precursors (150°C) yield trinuclear pyrazolate-bridged complexes M3 (μ-dmpz)4(Hdmpz)2 (OOCMe)2(M = Zn or Co). Depending on the crystallization conditions, these complexes contain various solvating molecules (benzene,
toluene, or Hdmpz), which influences the character of intramolecular and intermolecular hydrogen bonding, as shown by X-ray
crystallography. 相似文献
17.
D. A. Bashirov N. A. Pushkarevsky A. V. Vitovets O. Fuhr S. N. Konchenko 《Russian Journal of Coordination Chemistry》2008,34(10):739-749
In the reaction of Na2Se with [Fe(CO)5] in isopropanol with subsequent acidification with HCl, which is used to synthesize [(μ-H)2Fe3(μ3-Se)(CO)9] (II), the cluster [(μ-H)2Fe5(μ3-Se)2(CO)14] (I) was detected. In assumption that compound I could serve as a suitable synthon for preparing the bulky heterometallic clusters, its reactions with the Rh-containing complexes were studied. The reaction of I with [Rh(CO)2Cp*] (Cp* is pentamethylcyclopentadienyl) was found to give a mixture of the products. The main reaction products were isolated and their structures were determined: [Fe2Rh(μ3-Se)2(CO)6Cp*], [Fe2Rh(μ3-Se)(μ3-CO)(CO)6Cp*], [FeRh2(μ3-Se)(μ-CO)(CO)3Cp 2 * ], [Fe2Rh2(μ4-Se)(μ-CO)4(CO)2Cp 2 * ]. Potassium hydride treatment of II with subsequent addition of [Cp*Rh(CH3CN)3](CF3SO3)2 leads to the well-known cluster complex [Fe3Rh(μ4-Se)(CO)9Cp*]. A set of the reaction products indicates that the {Fe5Se2} core cannot be used as one-piece “building block” in the synthesis of heterometallic clusters. 相似文献
18.
M. S. Tarasenko N. G. Naumov A. V. Virovets S. -J. Kim V. E. Fedorov 《Journal of Structural Chemistry》2008,49(6):1128-1131
The structure of the salt Cs[Gd(H2O)4Re6Te8(CN)6]·4H2O (space group P-1, a = 9.436(5) Å, b = 12.365(7) Å, c = 15.187(8)Å, α = 89.104(10)°, β = 86.996(10)°, γ = 82.304(9)°) has been established by single crystal XRD. The structure of the compound features layers involving Gd3+ cations bound to cluster anions [Re6Te8(CN)6]4? through cyanide groups. The interlayer space contains cesium cations and crystallization water molecules. 相似文献
19.
D. V. Korchagin E. I. Zhilyaeva G. V. Shilov N. S. Ovanesyan S. M. Aldoshin 《Russian Journal of Inorganic Chemistry》2009,54(2):226-231
Single crystals of the Na4[Na2Cr2(C2O4)6] · 10H2O complex were synthesized for the first time. The structure of the complex was determined by X-ray diffraction analysis. The compound crystallizes in the monoclinic crystal system with the unit cell parameters a = 17.290(4) Å, b = 12.521(3) Å, c = 15.149(3) Å, β = 100.45(3)°, Z = 4, space group Cc. Anionic layers [NaCr(C2O4)3] 2n 4n? can be distinguished in the crystal structure of the complex. The Na+ cations and water molecules, involved in the formation of a hydrogen bond network, are located between the anionic layers. 相似文献
20.
Kathleen H. Bakon Sara J. Palmer Ray L. Frost 《Journal of Thermal Analysis and Calorimetry》2010,100(1):125-131
The mineral reevesite and the cobalt substituted reevesite have been synthesised and studied by thermal analysis and X-ray diffraction. The d(003) spacings of the minerals ranged from 7.54 to 7.95 Å. The maximum d(003) value occurred at around Ni:Co 0.4:0.6. This maximum in interlayer distance is proposed to be due to a greater number of carbonate anions and water molecules intercalated into the structure. This increase in carbonate anion content is attributed to an increase in surface charge on the brucite like layers. The maximum temperature of the reevesite decomposition occurs for the unsubstituted reevesite at around 220 °C. The effect of cobalt substitution results in a decrease in thermal stability of the reevesites. Four thermal decomposition steps are observed and are attributed to dehydration, dehydroxylation and decarbonation, decomposition of the formed carbonate and oxygen loss at ~807 °C. A mechanism for the thermal decomposition of the reevesite and the cobalt substituted reevesite is proposed. 相似文献