共查询到20条相似文献,搜索用时 31 毫秒
1.
Some Reactions with [Mo6Cl8]Cl4 The reaction of [Mo6Cl8]Cl4 with different chemical agents has been investigated: The methoxylation depends on the CH3O? concentration in CH3OH. The reaction with HF leads to a partial fluorinated [Mo6Cl8] product. With NH4F (NH4)2[Mo6Cl8]F6 in formed, the hydrolysis of which leads to [Mo6Cl8]F3(OH) · 2.5 H2O. This compound can be decomposed thermically into [Mo6Cl8]O2. [Mo6Br8]F62? on hydrolysis leads to [Mo6Br8]F3(OH) · 5 H2O. With CsF Cs2[Mo6Cl8]F6 is formed, which by hydrolysis is transformed into [Mo6Cl8]F3(OH) · 2.5 H2O and possibly to [Mo6Cl8]F4 · xH2O(?). In reaction of [Mo6Cl8]Cl4 with H2SO4 one gets [Mo6Cl8](SO4)2. Salts e. g. [(C6H5)4As]2[Mo6Cl8](OC6F5)6 and adducts e. g. [Mo6Cl8](OC6F5)4 · 2 HMPA are prepared. The compounds have been characterized by X-ray powder-diagramms and by IR-spectra. 相似文献
2.
《Journal of Coordination Chemistry》2012,65(17):3122-3132
The Keggin-type cesium salt of transition metal-substituted phosphomolybdates, Cs5[PCo(H2O)Mo11O39]?·?6H2O (1) and Cs5[PMn(H2O)Mo11O39]?·?6H2O (2), were synthesized from commercially available H3PMo12O40. The compounds were characterized by thermal, structural, and spectroscopic techniques. X-ray structural analysis reveals that, in these isostructural disordered compounds, the transition metal (Co/Mn) and Mo atoms are distributed over 12 positions. The presence of Co/Mn atoms was confirmed by powder XRD, FT-IR, DR-UV-Vis, ESR, and 31P NMR studies. 相似文献
3.
A. Müller E. Krickemeyer S. Dillinger H. Bgge W. Plass A. Proust L. Dloczik C. Menke J. Meyer R. Rohlfing 《无机化学与普通化学杂志》1994,620(4):599-619
The compounds (NMe4)5[As2Mo8V4AsO40] · 3 H2O 2a , (NH4)21[H3Mo57V6(NO)6O183(H2O)18] · 65 H2O 3a , (NH2Me2)18(NH4)6[Mo57V6(NO)6O183(H2O)18] · 14 H2O 3b and (NH4)12[Mo36(NO)4O108(H2O)16] · 33 H2O 4a ( 3a and 4a were not correctly reported in the literature regarding to their composition, structures and the oxidation states of the metal centres) which contain large isolated anionic species, have been prepared (among them 3a, 3b , and 4a in rather high yield) and characterized by complete crystal structure analysis as well as IR/Raman, UV/VIS/NIR, ESR spectroscopy and magnetic susceptibility measurements, redox titrations, bond valence sum calculations, elemental analyses and thermogravimetric studies. Perspectives for polyoxometalate chemistry referring to the synthesis of “extremely” large nanoscaled species are discussed, together with the occurrence of a large transferable {Mo17} building block in the compounds 3a, 3b and 4a which also exists in the corresponding iron compound Na3(NH4)12[H15Mo57Fe6(NO)6O183(H2O)18] · 76 H2O 7a . 相似文献
4.
A. L. Gushchin K. A. Kovalenko M. N. Sokolov D. Yu. Naumov N. F. Zakharchuk C. Vicent V. P. Fedin 《Russian Chemical Bulletin》2007,56(9):1701-1706
The reactions of the [Mo3(μ3-Q)(μ2-Q)3(H2O)3(C2O4)3]2− complex (Q = S or Se) with CuX salts (X = Cl, Br, I, or SCN) in water produce the cuboidal heterometallic clusters [Mo3(CuX)(μ3-Q)4(H2O)3(C2O4)3]2−, which were isolated as the potassium and tetraphenylphosphonium salts. Two new compounds, K2[Mo3(CuI)(μ3-S)4(H2O)3(C2O4)3]·6H2O and (PPh4)2[Mo3(CuBr)(μ3-S)4(H2O)3(C2O4)3]·7H2O, were structurally characterized. All compounds were characterized by elemental analysis and IR spectroscopy. The K2[Mo3(CuI)(μ3-Se)4(H2O)3(C2O4)3] compound was characterized by the 77Se NMR spectrum; the (PPh4)2[Mo3(CuI)(μ3-S)4(H2O)3(C2O4)3], (PPh4)2[Mo3(CuI)(μ3-Se)4(H2O)3(C2O4)3] and K2[Mo3(CuSCN)(μ3-S)4(H2O)3(C2O4)3]·7H2O compounds, by electrospray mass spectra.
Dedicated to Academician G. A. Abakumov on the occasion of his 70th birthday.
Published in Russian in Izvestiya Akademii Nauk. Seriya Khimicheskaya, No. 9, pp. 1639–1644, September, 2007. 相似文献
5.
A. A. Ostroushko V. Yu. Korotaev M. O. Tonkushina V. A. Vazhenin M. Yu. Artemov S. Yu. Men’shikov I. B. Kutyashev 《Russian Journal of Inorganic Chemistry》2011,56(2):276-281
Molybdenum polyoxometallates with the buckyball structure, ((NH4)42[Mo72VIMo60VO372(H3CCOO)30(H2O)72] · 30H3CCOONH4 · 250H2O (I), (NH4)42[Mo72VIMo60VO372(ClCH2COO)30(H2O)72)] · 250H2O · 15ClCH2COONa (II), in particular, as parts of polymer-containing compositions were studied by EPR, NMR, IR, and Raman spectroscopy. The structural
and chemical aspects responsible for the formation of the observed spectra were considered. 相似文献
6.
M. M. Godneva D. L. Motov M. P. Rys’kina 《Russian Journal of Inorganic Chemistry》2011,56(9):1363-1369
The ZrO(NO3)2-H3PO4-CsF-H2O system was studied at 20°C along the section at a molar ratio of PO43−/Zr = 0.5 (which is of the greatest interest in the context of phase formation) at ZrO2 concentrations in the initial solutions of 2–14 wt % and molar ratios of CsF: Zr = 1−6. The following compounds were isolated
for the first time: crystalline fluorophosphates CsZrF2PO4 · H2O, amorphous oxofluorophosphate Cs2Zr3O2F4(PO4)2 · 3H2O, and amorphous oxofluorophosphate nitrate CsZr3O1.25F4(PO4)2(NO3)0.5 · 4.5H2O. The compound Cs3Zr3O1.5F6(PO4)2 · 3H2O was also isolated, which forms in a crystalline or glassy form, depending on conditions. The formation of the following
new compounds was established: Cs2Zr3O1.5F5(PO4)2 · 2H2O, Cs2Zr3F2(PO4)4 · 4.5H2O, and Zr3O4(PO4)1.33 · 6H2O, which crystallize only in a mixture with known phases. All the compounds were studied by X-ray powder diffraction, crystal-optical,
thermal, and IR spectroscopic analyses. 相似文献
7.
P. A. Abramov S. A. Adonin E. V. Peresypkina M. N. Sokolov V. P. Fedin 《Journal of Structural Chemistry》2010,51(4):731-736
Adducts of cucurbit[6]uril with Ca2+ and trinuclear cluster chloroaquacomplexes (H9O4)2(H7O3)2[(Ca(H2O)5)2(C36H36N24O12)]Cl8·0.67H2O (1) and [(Ca(H2O)5)2(C36H36N24O12)]× [Mo3O2S2Cl6(H2O)3]2·13H2O (2) are obtained and structurally characterized. The structures of both compounds contain polymeric [Ca(H2O)
n
]22 CB[6]∞ cations that form infinite columns; the space between them is filled with Cls- (1) and [Mo3O2S2Cl6(H2O)3]2s- (2). A new (H7O3)2(H5O2)× [Mo3S4Cl6.25Br0.25(H2O)2](C36H36N24O12)·CH2Cl2·6H2O complex (3) is also obtained and structurally characterized. 相似文献
8.
Luminita Patron Oana Carp I. Mindru G. Marinescu J. Hanss A. Reller 《Journal of Thermal Analysis and Calorimetry》2008,92(1):307-312
The thermal behaviour of four coordination compounds (NH4)6[Y3Fe5(C4O5H4)6(C4O5H3)6]·12H2O, (NH4)6[Y3Fe5(C6O7H10)6(C6O7H9)6]·8H2O, (NH4)6[Er3Fe5(C4O5H4)6(C4O5H3)6]·10H2O and (NH4)6[Er3Fe5(C4O6H4)6(C4O6H3)6]·22H2O has been studied to evaluate their suitability for garnet synthesis. The thermal decomposition and the phase composition
of the resulted decomposition compounds are influenced by the nature of metallic cations (yttrium-iron or erbium-iron) and
ligand anions (malate or gluconate). 相似文献
9.
Thermal studies on various oxalato complexes have been of immense interest as they yield finely divided, highly reactive oxides which are usually obtained at a much lower temperature than that required in the conventional method of preparation, i.e., heating a mixture of two or more constituents [1]. A survey of the literature reveals that the compounds having the general formula A2[Mo2O5(C2O4)2(H2O)2], where A = K+, NH+4[2] and A = Cs+ [3], have been prepared and their thermal decomposition is studied, but no such information is available regarding the preparation and characterisation of Na2[Mo2O5(C2O4)2(H2O)2] (SMO), which forms the subject of study of this paper. Sodium dimolybdate (Na2Mo2O7), the decomposition product of SMO, is obtained at 280°C, a temperature much lower than that required in the conventional method of preparation of heating a mixture of Na2MoO4 and MoO3 [4]. 相似文献
10.
Ali Saad Guillaume Rousseau Hani El Moll Olivier Oms Pierre Mialane Jérôme Marrot Loïc Parent Israel-Martyr Mbomekallé Rémi Dessapt Anne Dolbecq 《Journal of Cluster Science》2014,25(3):795-809
The synthesis of MoVI bisphosphonates (BPs) complexes in the presence of a heterometallic element has been studied. Two different BPs have been used, the alendronate ligand, [O3PC(C3H6NH3)(O)PO3]4? (Ale) and a new BP derivative with a pyridine ring linked to the amino group, [O3PC(C3H6NH2CH2C5H4N)(O)PO3]4? (AlePy). Three compounds have been isolated, a tetranuclear MoVI complex with CrIII ions, (NH4)5[(Mo2O6)2(O3PC(C3H6NH3)(O)PO3)2Cr]·11H2O (Mo4(Ale)2Cr), its MnIII analogue, (NH4)4.5Na0.5[(Mo2O6)2(O3PC(C3H6NH3)(O)PO3)2Mn]·9H2O (Mo4(Ale)2Mn), and a cocrystal of two polyoxomolybdates, (NH4)10Na3[(Mo2O6)2(O3PC(C3H6NH2CH2C5H4N)(O)PO3)2Cr]2[CrMo6(OH)6O18]·37H2O ([Mo4(AlePy)2Cr]2[CrMo6]). In this latter compound an Anderson-type POM [CrMo6(OH)6O18]3? is sandwiched between two tetranuclear MoVI complexes with AlePy ligands. The protonated triply bridging oxygen atoms bound to the central CrIII ion of the Anderson anion develop strong hydrogen bonding interactions with the oxygen atoms of the bisphosphonate complexes. The UV–Vis spectra confirm the coexistence in solution of both POMs. Cyclic voltammetry experiments have been performed, showing the reduction of the Mo centers. In strong contrast with the reported MoVI BP systems, the presence of trivalent cations in close proximity to the MoVI centers dramatically impact the potential solid-state photochromic properties of these compounds. 相似文献
11.
S. P. Goel G. R. Verma Sanjive Kumar M. P. Sharma 《Journal of Thermal Analysis and Calorimetry》1991,37(2):427-432
A new molybdenum(VI) complex Cs2(NH4)2[Mo3O8(C2O4)3] (CAMO) has been prepared and characterized by chemical analysis and IR spectral studies. Thermal decomposition studies have been made using TG, DTA and DTG techniques. The compound is anhydrous and stable up to 160°C. Thereafter it decomposes in three stages. The first and the second stages occur in the temperature ranges 160–220°C and 220–280°C to give the intermediate compounds having the tentative compositions Cs4(NH4)2[Mo6O16(C2O4)3(CO3)2] and Cs4[Mo6O16(C2O4)2(CO3)2] respectively, the later then decomposing to give the end product Cs2Mo3O10 at 370°C. The end product was characterized by chemical analysis, IR spectral and X-ray studies. 相似文献
12.
《Journal of Coordination Chemistry》2012,65(4):627-639
Two polyoxometalate-based inorganic metal-organic hybrid supramolecular complexes [Cu(2,2′-bpy)2]2[VIV 2MoV 5MoVI 7O38(PO4)] (1) (2,2′-bpy?=?2,2′-bipyridine) and [Cu(2,2′-bpy)2]2[MoVMoVI 11O36(PO4)]?·?3H2O (2), have been hydrothermally prepared and structurally characterized by single-crystal X-ray diffraction. Both complexes are constructed from polyoxoanions (the bivanadyl capped α-Keggin polymolybdate anion [VIV 2MoV 5MoVI 7O38(PO4)]4? for 1 and the reduced 12-molybdophosphate anion [MoVMoVI 11O36(PO4)]4? for 2) and copper(II) complex cations [Cu(2,2′-bpy)2]2+, forming two-dimensional (2D) layer network structures, in which the polyoxoanion and the complex fragment cation connect with each other through Cu?···?Opolyoxoanion short contact weak interactions, which mediate ferromagnetic interaction. 相似文献
13.
Ying Wang Lan Cui Zhang Zai Ming Zhu Na Li Ai Fang Deng Shu Yue Zheng 《Transition Metal Chemistry》2011,36(3):261-267
Four Strandberg-type phosphomolybdate-based Cu(II) complexes of 2,2′-biimidazole (C6H6N4, H2biim) and H2O molecules, namely [Cu(H2biim)2(H2O)][Cu(H2biim)2(HPO4)2(Mo5O15)]·2H2O (1), [{Cu(H2biim)(H2O)}2{μ-Cu(H2biim)(H2O)}(P2Mo5O23)]2·20H2O (2), [Cu(H2biim)2][{Cu(H2biim)(H2O)2}{Cu(H2biim)2}(HPO4)(PO4)(Mo5 O15)]2·20H2O (3), and [Cu(H2biim)2(H2O)][Cu(H2biim)2(HPO4)2(Mo5O15)]·6H2O (4) have been synthesized and characterized by physico-chemical and spectroscopic methods. Single-crystal X-ray diffraction
analysis reveals that compound 1 consists of a mono-supporting heteropolyoxoanion [Cu(H2biim)2(H2P2Mo5O23)]2−and an isolated [Cu(H2biim)2(H2O)]2+ cation. Compound 2 is composed of two tetra-supporting heteropolyoxoanions linked via two Cu(II) complex fragments. In compound 3, there exist two symmetrical bi-supported polyoxoanion clusters and an isolated [Cu(H2biim)2]2+ fragment lying in the center of the clusters. Compound 4 is also constructed from a [Cu(H2biim)2(H2P2Mo5O23)]2− polyoxoanion and a [Cu(H2biim)2(H2O)]2+ cation, but it has a different space group and packing interactions compared with compound 1. 相似文献
14.
《Journal of Coordination Chemistry》2012,65(20):3674-3683
Two new compounds, (H2en)3(H2enMe)4(H3O){CuI[MoV 6O12(OH)3(HPO4)(PO4)3]2}?·?6H2O (1) and (H2enMe)4{CuICuII[MoV 6O12(OH)3(PO4)(HPO4)2(H2PO4)]2}?·?3H2O (2), were hydrothermally synthesized and characterized by elemental analysis, IR, TGA, and single-crystal X-ray diffraction analysis. Crystallographic analysis reveals that 1 is constructed from cluster anions {CuI[MoV 6O12(OH)3(HPO4)(PO4)3]2}15?, protonated organic amines, and water molecules. Each cluster is bridged through hydrogen bonds to form a 3-D supermolecular structure. For 2, {CuI[MoV 6O12(OH)3(PO4)(HPO4)2(H2PO4)]2}11? are connected by CuII cations to form an infinite chain. The formation of 1 and 2 reveals that organoamines influence the structures of the crystals. 相似文献
15.
Silke Buth Klaus Harms Peter Knig Sigrid Wo
adlo Frank Weller Kurt Dehnicke 《无机化学与普通化学杂志》1993,619(5):853-858
Syntheses and Crystal Structures of the Nitridodiolato Osmates(VI) PPh4[OsNCl2(O2C2H4)] and PPh4[OsNCl2(O2C2Me4)] · 2 THF The title compounds were prepared by the reaction of PPh4[OsNCl4] with glycole and pinacole, respectively, in CH2Cl2 and THF, respectively, in the presence of triethylamine, forming orange-red single crystals. According to the crystal structure determinations the compounds have ionic structures. In the anions the nitrido ligand occupies the apical position of the distorted tetragonal pyramid, and the two chlorine atoms and the two oxygen atoms of the diolato ligands are in equatorial positions. PPh4[OsNCl2(O2C2H4)] : Space group P21/n, Z = 4, 3 331 observed unique reflections, R = 0.031. Lattice dimensions at 19°C: a = 1 750.3, b = 816.8, c = 1 816.5 pm, β = 95.16°. PPh4[OsNCl2(O2C2Me4)] · 2 THF : Space group P1 , Z = 2, 5 238 observed unique reflections, R = 0.051. Lattice dimensions at -80°C: a = 898.9, b = 1 405.1, c = 1 518.6 pm, α = 93.66°, β = 92.89°, γ = 92.51°. 相似文献
16.
Pedro Gili Pedro Núez Pedro Martín‐Zarza Pablo A. Lorenzo‐Luis 《Acta Crystallographica. Section C, Structural Chemistry》2000,56(10):e441-e442
The title compound, (C3H5N2)4[β‐Mo8O26], has been prepared from imidazole octamolybdate, (C3H5N2)4[(C3H4N2)2(γ‐Mo8O26)], which was described previously. The γ→β conversion is produced in the presence of Cu(NO3)2·3H2O and is reported for the first time in this work. The X‐ray structure analysis confirmed the presence of the [Mo8O26]4? anion. The structure consists of β‐Mo8O26 polyanions and imidazolium cations. These cations are linked to the terminal and bridging O atoms of the anion by hydrogen bonds. 相似文献
17.
《Journal of Inorganic and Nuclear Chemistry》1978,40(7):1365-1367
The salts of the new types M2[UO2F2(C2O4)], M4[UO2F2(C2O4)2] and M2[(UO2)2F4(C2O4)] (where M = potassium and rubidium) have been prepared by mixing saturated solutions of H[UO2F3]·H2O with alkali metal oxalate solutions in cold in different mole ratios. Molecular conductances of the salt solutions indicate that the ions are decomposed in dilute solution to a great extent. The complexes are also completely decomposed on passing their solutions through a column of cation exchange resin in hydrogen form. The IR spectra of the salts of [UO2F2(C2O4)]2− and [UO2F2(C2O4)2]4− indicate that oxalate is acting as a normal chelating agent, while the spectra of the salts of [(UO2)2F4(C2O4)]2− support that the ion contains bridged oxalate group. The lattice parameters of the three potassium salts have been reported. 相似文献
18.
《Polyhedron》1999,18(21):2781-2785
The compounds (NH4)6[Mo6V2O24(C2O4)2]·6H2O (I) and (NH4)4[H2Mo2V2O12(C2O4)2]·2H2O (II) have been prepared from molybdenum(VI) oxide and ammonium vanadate in aqueous solution through the addition of ammonium oxalate, and their structures determined by X-ray structure analysis. Whereas the molybdovanadate anion [Mo6V2O24(C2O4)2]6− found in (I) consists of six MoO6 and two VO6 edge-sharing octahedra of the γ-[Mo8O26]4− type structure, the tetranuclear anion [H2Mo2V2O12(C2O4)2]4− of (II) adopts the structure with a M4O16 core. Both complexes contain bidentate oxalato ligands bonded to the vanadium ions. In both crystal structures the molybdovanadate anions are mutually hydrogen bonded by ammonium ions and water molecules. 相似文献
19.
Michael Gorol Nadia C. Msch‐Zanetti Mathias Noltemeyer Herbert W. Roesky 《无机化学与普通化学杂志》2000,626(11):2318-2324
Reaction of [M(NH3)6]Cl3 (M = Co, Rh, Ir) and [Ir(NH3)5(OH2)]Cl3 with (NH4)2C2O4 · H2O in aqueous solution resulted in the isolation of [M(NH3)6]2(C2O4)3 · 4 H2O and [Ir(NH3)5(OH2)]2(C2O4)3 · 4 H2O, respectively. The complexes have been characterized by X‐ray crystallography, IR and UV/VIS spectroscopy. The isomorphous compounds crystallize in the orthorhombic space group Pnnm (No. 58). Four molecules of crystal water are involved in an extended three‐dimensional hydrogen bonding network. The librational modes of the lattice water around 600 cm–1 allow the characterization of [Ir(NH3)6]2(C2O4)3 · 4 H2O and [Ir(NH3)5(OH2)]2(C2O4)3 · 4 H2O, respectively, by IR spectroscopy. The band around 600 cm–1 shows a significant frequency shift in the IR spectra of the hexaammine and aquapentaammine complex of iridium(III) and, by that, a distinction is possible. 相似文献
20.
Molybdenum(II) Halide Clusters with six Alcoholate Ligands: (C18H36N2O6Na)2[Mo6Cl8(OCH3)6] · 6CH3OH and (C18H36N2O6Na)2[Mo6Cl8(OC6H5)6] . The reaction of Na2[Mo6Cl8(OCH3)6] and 2,2,2-crypt yields (C18H36N2O6Na)2[Mo6Cl8(OCH3)6] · 6 CH3OH ( 1 ), which is converted to (C18H36N2O6Na)2[Mo6Cl8(OC6H5)6] ( 2 ) by metathesis with phenol. According to single crystal structure determinations ( 1 : P3 1c, a=14.613(3) Å, c=21.036(8) Å; 2 : P3 1c, a=15.624(1) Å, c=19.671(2) Å) the compounds contain anionic clusters [Mo6Cl8i(ORa)6]2? ( 1 : d(Mo—Mo) 2.608(1) Å to 2.611(1) Å, d(Mo—Cl) 2.489(1) Å to 2.503(1) Å, d(Mo—O) 2.046(4) Å; 2 : d(Mo—Mo) 2.602(3) Å to 2.608(3) Å, d(Mo—Cl) 2.471(5) Å to 2.4992(5) Å, d(Mo—O) 2.091(14) Å). Electronic interactions of the halide cluster and the phenolate ligands in [Mo6Cl8(OC6H5)6]2? is investigated by means of UV/VIS spectroscopy and EHMO calculations. 相似文献