Hydrothermal Syntheses and Crystal Structures of Two New Mixed-valence Vanadium Oxides [Ni(en)2(H2O)2][Ni(en)3]2[V16O38Cl] · 3(H2O) and (H3O)2V3O8

2010 ◽  
Vol 65 (12) ◽  
pp. 1451-1456 ◽  
Author(s):  
Xing Liu ◽  
Xian-Hong Yin ◽  
Feng Zhang
Keyword(s):  
Vanadium Oxide ◽  
Single Crystal ◽  
Interlayer Space ◽  
Mixed Valence ◽  
Vanadium Oxides ◽  
Cluster Anions ◽  
X Ray Diffraction ◽  
Reaction Conditions ◽  
X Ray ◽  
Molar Ratios

Two vanadium oxides [Ni(en)2(H2O)2][Ni(en)3]2[V16O38Cl] ・3(H2O) (1) (en = ethylenediamine) and (H3O)2 V3O8 (2) were hydrothermally synthesized and characterized by single-crystal X-ray diffraction. 1 consists of [Ni(en)2(H2O)2]2+ and [Ni(en)3]2+ cations, discrete [V16O38Cl]6− cluster anions and H2O molecules, while 2 consists of anionic mixed-valent V5+/V4+ vanadium oxide layers constructed from pairs of corner-sharing VVO4 tetrahedra and VIVO5 square pyramids, with H3O+ cations occupying the interlayer space. Both 1 and 2 were synthesized under the same reaction conditions but with different V/Ni molar ratios, which shows that the reactant stoichiometry of the system plays a key role in the formation of different structures in the products.

scholarly journals Synthesis, Crystal Structure and Magnetic Properties of Bixbyite-type Vanadium Oxide Nitrides

2009 ◽  
Vol 64 (3) ◽  
pp. 281-286 ◽  
Author(s):  
Suliman Nakhal ◽  
Wilfried Hermes ◽  
Thorsten Ressler ◽  
Rainer Pöttgen ◽  
Martin Lerch
Keyword(s):  
Crystal Structure ◽  
Vanadium Oxide ◽  
Magnetic Ordering ◽  
Vanadium Oxides ◽  
Detectable Amount ◽  
X Ray Diffraction ◽  
X Ray ◽  
Vanadium Sulfide ◽  
Structure Result ◽  
X Ray Absorption

Ammonolysis of vanadium sulfide leads to the formation of bixbyite-type vanadium oxide nitrides. Small amounts of nitrogen incorporated in the structure result in the stabilization of the bixbyite type not known for vanadium oxides. The crystal structure was investigated using X-ray diffraction and X-ray absorption spectroscopy. At temperatures above 550 °C the powders decompose to corundumtype V2O3 containing no detectable amount of nitrogen. Below 39 K magnetic ordering is observed.

Die neuen Oxobismutate(III) Cs6Bi4O9, K9Bi5O13 und A2Bi4O7 (A = Rb, Cs) / The New Oxobismutates(III) Cs6Bi4O9, K9Bi5O13 and A2Bi4O7 (A = Rb, Cs)

2002 ◽  
Vol 57 (10) ◽  
pp. 1090-1100
Author(s):  
Franziska Emmerling ◽  
Caroline Röhr
Keyword(s):  
Single Crystal ◽  
Crystal Structures ◽  
Alkali Metals ◽  
Mixed Valence ◽  
Three Dimensional ◽  
X Ray Diffraction ◽  
X Ray ◽  
Trigonal Bipyramidal ◽  
Mixed Valence Compound

AbstractThe title compounds were synthesized at a temperature of 700 °C via oxidation of elemental Bi with the hyperoxides AO2 or via reaction of the elemental alkali metals A with Bi2O3. Their crystal structures have been determined by single crystal x-ray diffraction. They are dominated by two possible surroundings of Bi by O, the ψ-trigonal-bipyramidal three (B) and the ψ-tetrahedral four (T) coordination. Cs6Bi4O9 (triclinic, spacegroup P1̄, a = 813.82(12), b = 991.60(14), c = 1213.83(18) pm, α = 103.658(2), β = 93.694(3), γ = 91.662(3)°, Z = 2) contains centrosymmetric chain segmentes [Bi8O18]12- with six three- (T) and two four-coordinated (B) Bi(III) centers. K9Bi5O13 (monoclinic, spacegroup P21/c, a = 1510.98(14), b = 567.59(5), c = 2685.6(2) pm, β = 111.190(2)°, Z = 4) is a mixed valence compound with isolated [BivO4]3- tetrahedra and chains [BiIII4O9]6- of two T and two B coordinated Bi. In the compounds A2Bi4O7 (A = Rb/Cs: monoclinic, C2/c, a = 2037.0(3) / 2130.6(12), b = 1285.5(2) / 1301.9(7), c = 1566.6(2) / 1605.6(9) pm, β = 94.783(3) / 95.725(9)°, Z = 8) ribbons [Bi4O6O2/2]2- are formed, which are condensed to form a three-dimensional framework.

Synthesis of Novel 2-Alkoxy-5H-benzo[6,7]cyclohepta[1,2-b]pyridine-3-carbonitriles

2003 ◽  
Vol 58 (7) ◽  
pp. 698-703 ◽  
Author(s):  
Adel S. Girgis ◽  
I. S. Ahmed-Farag
Keyword(s):  
Single Crystal ◽  
X Ray Diffraction ◽  
Reaction Conditions ◽  
X Ray ◽  
Independent Synthesis

Reaction of 6-arylmethylene-6,7,8,9-tetrahydro-5H-benzocyclo-hepten-5-ones (1) with malononitrile in the appropriate alcohol in the presence of sodium afforded the corresponding 2-alkoxy-4-aryl- 6,7-dihydro-5H-benzo[6,7]cyclohepta[1,2-b]pyridine-3-carbonitriles (2) and not their isomeric forms 2-alkoxy-4-aryl-6,7-dihydro-5H-benzo[3,4]-cyclohepta[1,2-c]pyridine-1-carbonitriles (3). The proposed structure was confirmed via independent synthesis of (2) through the reaction of 6,7,8,9- tetrahydro-5-benzocycloheptenone (4) with the appropriate ylidenemalononitriles 5 under the same reaction conditions. Single crystal X-ray diffraction proves the structures of 2a,b.

scholarly journals Darstellung und Kristallstrukturen von (PH4P)4Sb8I28 und (Ph4P)Sb3I10(Ph = C6H5) / Synthesis and Crystal Structures of (PH4P)4Sb8I28 and (Ph4P)Sb3I10(Ph = C6H5)

1987 ◽  
Vol 42 (12) ◽  
pp. 1493-1499 ◽  
Author(s):  
Siegfried Pohl ◽  
Wolfgang Saak ◽  
Detlev Haase
Keyword(s):  
Single Crystal ◽  
Crystal Structures ◽  
Diffraction Data ◽  
Lone Pair ◽  
X Ray Diffraction ◽  
Triclinic Space Group ◽  
X Ray ◽  
Molar Ratios ◽  
Polymeric Chains ◽  
Bond Strengths

AbstractThe compounds (Pn4P)4Sb8I28 (1) and (Ph4P)Sb3I10 (2) were prepared by the reaction of SbI3 and Ph4PI in acetonitrile (molar ratios 2:1 and 3:1 respectively). The structures of 1 and 2 were determined from single crystal X-ray diffraction data.1 crystallizes in the triclinic space group P1̄ with a - 1321.7(5). b = 1346.7(5), c = 2201.8(8) pm, α = 104.18(2). β = 99.92(2), γ = 100.33(2)°; 2: monoclinic, C2/c, a = 2371.1(2), b = 745.0(1), c = 2495.1(2) pm, β = 100.75(1)°.Whereas 1 exhibits isolated Sb8I284- ions, the anions of 2 are built up of polymeric chains [Sb3I10- ]∞. In both compounds the distorted Sbl6 octahedra are linked by common edges. The Sb-I distances are in the range between 277.4 and 354.8 pm (1) and between 277.4 and 342.4 pm (2). The observed structures do not only depend on stoichiometry, the nature of the counter cations, and the possibility of oligomerisation but also on the wide variety of the Sb-I bond strengths and the different bridges formed by iodine.The lone pair of Sb(III) seems to be predominantly 5 s2.

Room temperature conversion of X0.3V2O5· nH2O phase into X2V6O16· nH2O phase Influence of the nature of the cation X+

2004 ◽  
Vol 848 ◽  
Author(s):  
Olivier Durupthy ◽  
Saïd Es-salhi ◽  
Nathalie Steunou ◽  
Thibaud Coradin ◽  
Jacques Livage
Keyword(s):  
Vanadium Oxide ◽  
Room Temperature ◽  
Interlayer Space ◽  
Water Molecules ◽  
X Ray Diffraction ◽  
X Ray ◽  
Oxide Phases ◽  
New Phase ◽  
Supernatant Solution ◽  
Scanning Electron

ABSTRACTVarious cations (Li+, Na+, K+, NH4+, Cs+, Mg2+, Ca2+, Ba2+) were introduced during the formation of a V2O5. nH2O gel. Cation intercalated Xy V2O5. nH2O (y = 0.3 for X = Li+, Na+, K+, NH4+ or y = 0.15 for Mg2+, Ca2+, Ba2+) were first obtained at room temperature but some of them evolve upon ageing into a new phase: XV3O8. nH2O for X = Na+, K+, NH4+ and Cs+ or XV6O16. nH2O for X = Mg2+, Ca2+, Ba2+. All the vanadium oxide phases were characterized by X-ray diffraction (XRD), scanning electron microscopy (SEM) and infrared spectroscopy (IR); the supernatant solutions were analysed by 51V NMR spectroscopy. These vanadium oxide phases exhibit a layered structure with cations and water molecules intercalated within the interlayer space. The formation of the different phases depends mainly on the pH of the supernatant solution and on the nature of the cation.

scholarly journals Electron localization in a mixed-valence diniobium benzene complex

2015 ◽  
Vol 6 (2) ◽  
pp. 993-1003 ◽  
Author(s):  
Thomas L. Gianetti ◽  
Grégory Nocton ◽  
Stefan G. Minasian ◽  
Nikolas Kaltsoyannis ◽  
A. L. David Kilcoyne ◽  
...  
Keyword(s):  
Single Crystal ◽  
Unpaired Electron ◽  
Mixed Valence ◽  
Metal Center ◽  
Electron Localization ◽  
X Ray Diffraction ◽  
X Ray

One electron oxidation of a neutral diniobium benzene complex leads to a mixed-valence species. Single crystal X-ray diffraction, EPR, L3,2-edge XANES, and DFT indicate that the unpaired electron is localized on one metal center.

Sn94– Zintl Ions as Reactive Precursor for Neat Solids: Syntheses and Crystal Structures of Rb4[SnTe4], KxCs4–x[SnTe4], and KxCs10–x[Sn4Te12]

2009 ◽  
Vol 64 (11-12) ◽  
pp. 1319-1324 ◽  
Author(s):  
Jian-Qiang Wang ◽  
Viktor Hlukhyy ◽  
Thomas F. Fässler
Keyword(s):  
Single Crystal ◽  
Crystal Structures ◽  
X Ray Diffraction ◽  
Compound K ◽  
Reaction Conditions ◽  
Elemental Tellurium ◽  
X Ray ◽  
Zintl Ions ◽  
Tetrahedral Anion

The reactions of Zintl ions Sn94− formed in ethylenediamine solutions of K2Cs2Sn9 and Rb4Sn9 with elemental tellurium have been investigated. Addition of elemental tellurium to the filtrates of these solutions leads - depending on the reaction conditions - to four different products: Compounds K0.36(1)Cs3.64(1)[SnTe4] (1) and Rb4[SnTe4] (2) contain the tetrahedral anion [SnTe4]4−, and Cs4[Sn2Te7] (3) features the anion [Te2Sn(μ-Te)(μ-Te2)SnTe2]4−, whereas a novel Zintl anion [Sn4Te12]10− is present in compound K0.44(1)Cs9.56(1)[Sn4Te12] (4). Compounds 1, 2 and 4 have been structurally characterized by single-crystal X-ray diffraction

Luminescent Silver(I) and Copper(I) Systems Containing Pyridyl Phosphine Bridges

2009 ◽  
Vol 64 (11-12) ◽  
pp. 1525-1534 ◽  
Author(s):  
Olga Crespo ◽  
M. Concepción Gimeno ◽  
Antonio Laguna ◽  
Carmen Larraz
Keyword(s):  
Solid State ◽  
Single Crystal ◽  
Room Temperature ◽  
Silver Salt ◽  
Phosphine Ligands ◽  
X Ray Diffraction ◽  
X Ray ◽  
Molar Ratios ◽  
Pyridylphosphine Ligands

Luminescent silver(I) and copper(I) complexes containing pyridylphosphine ligands have been synthesized and structurally characterized by single crystal X-ray diffraction methods. The reaction of Ag(OTf) (OTf = trifluoromethanesulfonate) with 2-pyridyldiphenylphosphine in different molar ratios gives the species [Ag2(OTf)2(μ-PPh2py)2] (1), [Ag(PPh2py)2]OTf (2), [Ag(PPh2py)3]OTf (3), and [Ag2(PPh2py)3](OTf)2 (4) with several modes of coordination of the pyridylphosphine. The oxidation of the phosphine in compound 4 gave [Ag2(OTf)(μ-PPh2py)2(OPPh2py)]OTf (5) which has been structurally characterized. It shows two bridging phosphine ligands and one chelating OPPh2py ligand. The reactions of the silver salt with bis(2-pyridyl)phenylphosphine in different molar ratios affords the complex [Ag2(OTf)2(μ-PPhpy2)2] (6), while the corresponding reactions with [Cu(NCMe)4]PF6 lead to two different compounds, namely [Cu2(NCMe)2(μ-PPhpy2)2](PF6)2 (7) and [Cu2(PPhpy2)2(μ-PPhpy2)2](PF6)2 (8). All complexes exhibit luminescence in the solid state at room temperature and at 77 K

Synthesis and Coordination Behaviour of a Phosphanyl(vinyl)ferrocene

2006 ◽  
Vol 71 (2) ◽  
pp. 215-236 ◽  
Author(s):  
Petr Štěpnička ◽  
Ivana Císařová
Keyword(s):  
Single Crystal ◽  
X Ray Diffraction ◽  
X Ray ◽  
Molar Ratios ◽  
Coordination Behaviour

Donor properties of 1-(diphenylphosphanyl)-1'-vinylferrocene (1) were investigated in a series of reactions with palladium(II), rhodium(I), and copper(I) compounds. In all complexes obtained, compound 1 coordinates exclusively as a monodentate phosphorus donor, giving trans-[PdCl2(1-κP)2] (3) with [PdCl2(cod)], [PdCl(LNC)(1-κP)] (4) with [{Pd(LNC)}2(μ-Cl)2], and trans-[RhCl(CO)(1-κP)2] (5) with [{Rh(CO)2}2(μ-Cl)2] (cod = cycloocta-1,5-diene, LNC = 2-[(dimethylamino)methyl-κN]phenyl-κC1). Copper(I) precursors CuI and [Cu(MeCN)4]PF6 reacted with 1 in a similar manner, yielding at appropriate molar ratios heterocubane [(μ3-I)4{Cu(1-κP)}4] (6) and the bis(phosphane) complex [Cu(MeCN)(1-κP)2]PF6 (7), respectively. The structures of 1-(diphenylthiophosphoryl)-1'-vinylferrocene (2), 3, 4·CHCl3, 6·C6H6, and 7 have been determined by single-crystal X-ray diffraction.

Mangan(II)-Komplexe mit dem vierzähnigen Stickstoffliganden C12H22N6(L): Synthese von [MnX2L] (X = Cl, Br, I, NCS), Kristallstrukturen von [MnCl2L] und [MnBr2L] / Manganese(II) Complexes with the Tetradentate Nitrogen Ligand C12H22N6(L): Synthesis of [MnX2L] (Χ = Cl, Br, I, NCS), Crystal Structures of [MnCl2L] and [MnBr2L]

1989 ◽  
Vol 44 (6) ◽  
pp. 632-636 ◽  
Author(s):  
Peter Stolz ◽  
Wolfgang Saak ◽  
Henry Strasdeit ◽  
Siegfried Pohl
Keyword(s):  
Single Crystal ◽  
Diffraction Data ◽  
Tetradentate Ligand ◽  
Distorted Tetrahedron ◽  
X Ray Diffraction ◽  
Orthorhombic Space Group ◽  
Reaction Conditions ◽  
X Ray ◽  
Nitrogen Ligand ◽  
Bond Lengths

[MnCl2(C12H22N6)] (1) and [MnBr2(C12H22N6)] (2) are obtained from the reaction of MnX2 (X = Cl, Br) with C12H22N6 in methanolic solution.In chloroform MnI2, OPPh3, and C12H22N6 react to give [MnI2(C12H22N6)] (3). With small variations of the reaction conditions [MnI2(C12H22N6)] · xCHCl3 (4) may be crystallized. The reaction of [Mn(NCS)2(OPPh3)4] with C12H22N6 in CHCl3 solution gives [Mn(NCS)2(C12H22N6)] · xCHCl3 (5). The structures of 1 and 2 were determined from single crystal X-ray diffraction data. The isotypic compounds crystallize in the orthorhombic space group Pbcn with Z = 4; 1: a = 1592.4(1), b = 785.0(1), c = 1270.7(1) pm; 2: a = 1590.0(1), b = 802.6(1), c = 1316.6(1) pm. C12H22N6 acts as a tetradentate ligand. The isolated complexes exhibit a twofold symmetry.Manganese(II) is in a six-coordinate environment, which can be described better as a distorted tetrahedron with two additional Mn-N bonds rather than as a distorted octahedron.The Mn-N bond lengths are 229.9(1) and 248.7(1) pm for 1 and 228.2(3) and 248.4(3) pm for 2. The Mn-Hal bond lengths are 239.2(1) (1) and 254.2(1) pm (2)

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