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1.
Reaction of Diorganogallium(indium) Fluorides. The Crystal Structure of Mes2InF Mes2GaF ( 1 ) reacts with t-BuNH2 at 20°C to the amine adduct [Mes2Ga(F)(t-BuNH2)] ( 2 ). Treatment of 1 with H2S gives after a redox reaction γ-S8-Sulfur (Muthmanns' Sulfur) ( 3 ) as the only isolated product. When i-Pr2InF ( 4 ) is reacted with [SnCl2(dioxane)] in toluene at 70°C one yields after workup [i-PrInCl2(dioxane)] ( 5 ), which is formed after ligand exchange and reaction with dioxane. 2 and 5 were investigated by NMR-, IR- and MS-techniques. In addition, 2 · 2,5 THF, 3, 5 and Mes2InF were characterized by an X-ray structure determination. According to that 2 · 2,5 THF contains dimeres, associated by hydrogen brigdes, while 5 possesses a polymeric structure with bridging dioxane molecules. 3 forms eightmembered rings with C 2-symmetry. Me2InF is a trimer in the solid state with an In3F3-backbone. 相似文献
2.
Synthesis and Characterization of Organodilithium Phosphides. The Crystal Structure of [Li(THF)(TMEDA)P(H)Mes] t-BuPH2 and MesPH2 can be reacted with two equivalents n-BuLi at R. T. in Et2O/n-hexane to yield the corresponding organodilithium phosphides t-BuPLi2 ( 1 ) and MesPLi2 ( 2 ). 1 and 2 can be isolated solvent-free as bright orange-yellow solids. 1 and 2 were characterized by NMR, IR, and RE spectra. When MesPH2 is treated with one equivalent of n-BuLi, MesP(H)Li is crystallizing as [Li(THF)(TMEDA)P(H)Mes] ( 3 ) from THF/TMEDA/n-pentane in the space group P21/n with a = 893.41(6), b = 1 734.7(1), c = 1 391.1(1) pm and β = 90.613(6)°. 相似文献
3.
Crystal structure of AgIIF[AgIIIF4] For the first time dark brown single crystals of mixedvalent AgF[AgF4] were isolated under solvothermal conditions out of anhydrous HF/F2. The compound crystallizes in a new type of structure, triclinic with a = 499.9(2) pm, b = 1108.7(5) pm, c = 735.7(3) pm, α = 90.05(3)°, β = 106.54(4)°, γ = 90.18(4)°, spcgr. P1¯ — Ci1 (No. 2) and Z = 4. 相似文献
4.
Mesityltrifluoro Gallates. The Crystal Structures of Cs[MesGaF3] and K[MesInBr3] Mes3Ga reacts with GaBr3 in the ratio 1:2 in a commutation reaction to MesGaBr2 ( 1 ). 1 can be reacted with KF and CsF in MeCN to K[MesGaF3] ( 2 ) and Cs[MesGaF3] ( 3 ), respectively. K[MesInBr3] ( 4 ) was isolated when MesInBr2 was treated with KF in MeCN. The use of 15-crown-5 was leading to [K(15-crown-5)2][Mes2InBr2] ( 5 ) in a substituent exchange reaction. 1-5 were characterized by NMR-, IR- and MS-techniques. The solid state structures of 3 and 4 could be established by X-ray structure determinations. According to these determinations, a layer-type arrangement of the molecules is both structures in common. In the center of the layers, ionic interactions were formed, while the separation of the layers is caused by the bulky mesityl substituents. 相似文献
5.
Synthesis and Crystal Structure of [Cr(NH3)6][Cr(NH3)2F4][BF4]2 The action of ammonium fluoride on a mixture of boron and chromium in a sealed Monel ampoule at 300 °C yields single crystals of [Cr(NH3)6][Cr(NH3)2F4][BF4]2. The crystal structure (tetragonal, P4/mbm, Z = 2, a = 1056.0(1), c = 781.7(1) pm; R1 = 0.0414; wR2 = 0.1087 for 411 reflections with I0 > 2σ(I)) contains [Cr(NH3)6]3+ and [Cr(NH3)2F4]– octahedra and twice as many [BF4]– tetrahedra that are arranged in a quadrupled super‐structure of the CsCl‐type of structure. 相似文献
6.
Synthesis and Crystal Structure of [Fe(MeCN)6][Fe2OCl6] [Fe(MeCN)6][Fe2OCl6] ( 2 ) is obtained by passing dry air through a solution of FeCl2 in acetonitrile in almost quantitative yield. 2 crystallises in the trigonal space group R 3 [a = b = 12.121(1), c = 29.875(6) Å, Z = 6]. The oxygen atom in the Fe2OCl6 anion occupies the 3 position and causes therefore an Fe–O–Fe angle of 180°. The refinement in the triclinic space group P1 leads to a slightly bent arrangement of the Fe–O–Fe fragment. 相似文献
7.
Investigations on Electronically Conducting Oxide Systems. XIV. Solid Solutions and Conductivity in the System MgTiO3? Ti2O3 Solid solution formation and conductivity is reported for the system Mg1?xTiTiO3 (0 < x < 1). TiIII atoms are predominantly substituted in pairs for MgII and TiIV. In the range of low x values TiIII? TiIII bonds typical for Ti2O3 in the semiconducting state are very weakened because of the distances preserved in the host lattice of MgTiO3. Up to x = 0,5 EPR measurements at 77 K indicate magnetic “dimers” with S = 1 at a distance of 550 pm resulting from antiparallel spin orientation of the TiIII pairs and transfer of the magnetic interaction by super exchange to a next-neighboured TiIII pair. Electrical conductivity is caused by polaron hopping. The steep increase in the range of small TiIII concentration is interpreted by a screening field approximation. 相似文献
8.
Synthesis and Structure Investigations of Iodocuprates(I). XV Iodocuprate(I) with Solvated Cations: [Li(CH3CN)4] [Cu2I3] and [Mg{(CH3)2CO}6][Cu2I4] [Li(CH3CN)4][Cu2I3] 1 and [Mg((CH3)2CO)6][Cu2I4] 2 were prepared by reactions of CuI with LiI in acetonitrile and of CuI with MgI2 in acetone. 1 crystallizes orthorhombic, Pnma, a = 552.7(2), b = 1258.8(8), c = 2516(1) pm, z = 4. [Li(CH3CN)4]+ cations are located between rod packings of CuI4 tetrahedra double chains [(CuI2/2I2/4)2]? parallel to the axis. Short intermolecular anion/cation contacts were observed. The crystal structure of 2 (monoclinic, P21/n, a = 1840(2), b = 1059.2(2), c = 1879(2)pm, β = 112.94(4)°, z = 4) is built up by [Mg((CH3)2CO)6]2+ cations forming a simple hexagonal sphere packing. The binuclear anions [Cu2I4]2? occupy holes in the trigonal prismatic channels formed by the cations. 相似文献
9.
Synthesis and Crystal Structure of [Ba(18-Crown-6)(DMF)4][Cd(Se4)2] The title compound has been prepared by the reaction of a DMF-solution of lithium polyselenide with BaSe2 and cadmium acetate in the presence of 18-crown-6, forming black crystals. The compound was characterized by IR spectroscopy and by an X-ray structure determination. Space group P2/a, Z = 4, 5392 observed unique reflections, R = 0.048. Lattice dimensions at ?90°C: a = 2021.9(12); b = 1019.8(6); c= 2270.8(14)pm, ß = 106.98(4)°. The structure consists of [Ba(18-crown-6)(DMF)4]2+ ions, in which the barium ions are coordinated by the six oxygen atoms of the crown ether molecule and by four oxygen atoms of the DMF molecules, and of [Cd(Se4)2]2? ions. The cadmium atoms are coordinated by two tetraselenide ions in a chelating fashion. 相似文献
10.
The Crystal Structure of Lithiummetaperiodate, LiIO4 For the first time single crystals of LiIO4 were obtained. According to the results of an X-ray structure determination (monoclinic, P21/n; a = 525.5(3), b = 851.1(4), c = 796.9(5) pm, β = 104.21(3)°; Z = 4; 2 148 diffractometer data, R = 0.024) the coordination by oxygen is tetrahedral for iodine and strongly distorted trigonal bipyramidal for lithium. Two lithium-oxygen-polyhedra are connected via a common edge. LiIO4 crystallises isostructural to LiAlH4. The structure is discussed and compared to those of other metaperiodates and tetrahydridoaluminates. 相似文献
11.
The Crystal Structure of CsTcO4 CsTcO4 crystallizes orthorhombic with a = 5.727, b = 5.921 and c = 14.34 Å. Z = 4, space group Pnma (Nr. 62, I.T.). The metal positions were refined by single crystal data, the oxygen positions first determined: the CsTcO4 structure is a slight distortion of the scheelite arrangement (parameters: see text). The MADELUNG Part of Lattice Energy, MAPLE, ?Mean Effective Ionic Radii”?, MEIR, and Effective Coordination Numbers, ECoN, are calculated and discussed. 相似文献
12.
M. Jansen 《无机化学与普通化学杂志》1975,417(1):35-40
The Crystal Structure of Na4CoO4 According to X-Ray investigations on single crystals, Na4CoO4 crystallizes triclinic (P1, a = 8.648, b = 5.702, c = 6.400 Å, α = 123.9°, β = 98.1°, γ = 99.2°). There are almost tetrahedral CoO4-groups; sodium is coordinated by four or five O2?. 相似文献
13.
Jonas Bresien Kirill Faust Prof. Dr. Axel Schulz Dr. Alexander Villinger 《Angewandte Chemie (International ed. in English)》2015,54(23):6926-6930
The reaction of [ClP(μ‐PMes*)]2 ( 1 ) with the Lewis acid GaCl3 yielded a hitherto unknown tetraphosphabicyclo[1.1.0]butan‐2‐ium salt, [Mes*P4(Cl)Mes*][GaCl4] ( 3 [GaCl4]), which incorporates a positively charged phosphonium center within its bicyclic P4 scaffold. The formation of the title compound was studied by means of low‐temperature NMR experiments. This led to the identification of an intermediate cyclotetraphosphenium cation, which was trapped by reaction with dimethylbutadiene (dmb). All of the compounds were fully characterized by experimental and computational methods. 相似文献
14.
Mesityl Oxo Molybdenum and Tungsten Compounds. I. Structure of LiMoO2Me2Mes(OEt2)2 LiMoO2Me2Mes(OEt2)2 2 is prepared by literature method [2] from MoO2Mes2 1 and LiMe. Its x-ray structure and NMR-spectral data are presented. 2 adopts a dimer structure in which two [MoO2Me2Mes]? anions are linked via two bridging [Li(OEt2)2]+ cations bonded to the oxo ligands. The resulting [‥OMoOLi‥]2 ring is planar. 相似文献
15.
Preparation and Crystal Structure of (CH3NH3)8[NdCl6][NdCl4(H20)2]2Cl3 (CH3NH3)8[NdCl6][NdCl4 (H2O)2]2Cl3 is for the first time prepared and investigated by X-ray, single crystal work. It crystallizes in the monoclinic system (space group C2/m, Z = 2) with a = 9.358(5), b = 17.424(9), c = 15.360(8) Å, β = 108.30(4)°. The structure contains besides isolated Cl? ions distorted [NdCl6]3? octahedra and [NdCl4(H2O)2]? chains. 相似文献
16.
Synthesis and Crystal Structure of [N(Hex)4] [Cu2(CN)3] [N(Hex)4][Cu2(CN)3] has been prepared by solvothermal reaction of CuCN with Tetra‐n‐hexylammoniumiodide in acetone. The crystal structure is built up by condensed (CuCN)6 and (CuCN)7 rings, forming a zeolith type cyanocuprate(I) framework [Cu2(CN)3—]. Space group R3; α = 44.482(6), c = 21.283(4) Å, V = 36471(9) Å3; Z = 9. 相似文献
17.
Crown Ether Complexes of Lead(II). The Crystal Structures of [PbCl(18-Krone-6)][SbCl6], [Pb(18-Krone-6)(CH3CN)3][SbCl6]2 und [Pb(15-Krone-5)2][SbCl6]2 . [PbCl(18-crown-6)][SbCl6] has been prepared in low yield besides [Pb(CH3)2(18-crown-6)][SbCl6]2 by the reaction of Pb(CH3)2Cl2 with antimony pentachloride in acetonitrile solution in the presence of 18-crown-6, forming pale-yellow crystals. The other two title compounds are formed as colourless crystals by the reaction of PbCl2 with antimony pentachloride in acetonitrile solutions in the presence of 18-crown-6 and 15-crown-5, respectively. The complexes were characterized by IR spectroscopy and by crystal structure determinations. [PbCl(18-crown-6)][SbCl6]: Space group P21/c, Z = 8, 5 003 observed unique reflections, R = 0.046. Lattice dimensions at - 80°C: a = 1 386.9; b = 1 642.7; c = 2 172.1 pm, β = 92.95°. The lead atom in the cation [PbCl(18-crown-6)]+ is surrounded in an almost hexagonal-planar construction by the six oxygen atoms of the crown ether and an axially oriented Cl atom. [Pb(18-crown-6)(CH3CN)3][SbCl6]2: Space group P1 , Z = 2, 6 128 observed unique reflections, R = 0.076. Lattice dimensions at - 70°C: a = 1 228.0; b = 1 422.9; c = 1 463.2 pm, α = 69.08°; β = 65.71°; γ = 64.51°. In the cation [Pb(18-crown-6)(CH3CN)3]2+ the lead atom is coordinated by the six oxygen atoms of the crown ether and by the three nitrogen atoms of the acetonitrile molecules. The structure determination is restricted by disorder. [Pb( 15-crown-5)2][SbCI6]2: Space group P63/m, Z = 6, 5 857 observed unique reflections, R = 0.059. Lattice dimensions at -70°C: a = b = 2 198.5; c = 1499.4 pm, α = β = 90°, γ = 120°. In the cation [Pb(l5-crown-5)2]2 the lead atom is sandwich-like coordinated by the ten oxygen atoms of the two crown ether molecules. The structure determination is restricted by disorder. 相似文献
18.
Synthesis and Crystal Structure of [Li(DME)2I] . LiI can be dissolved at 50°C in toluene/DME (2:1). At - 20°C [Li(DME)2I] ( 1 ) was isolated in 75% yield. 1 was characterized by NMR techniques as well as an X-Ray structure determination. 1 crystallizes in the space group C2/c with a = 1 356.9(2), b = 813.2(1), c = 1 259.1(2) pm, and β = 99.74(1)°. 相似文献
19.
On the Crystal Structure of Ca2PbO4 Single crystals of Ca2PbO4 were prepared by flux technique and investigated by X-ray methods. It crystallizes with orthorhombic symmetry, space group D-Pbam. (a = 5.832; b = 9.766; c = 3.375 Å, Z = 2.) Ca2PbO4 belongs to the Sr2PbO4 type. It shows Ca2+ in a seven fold and Pb4+ in octahedral coordination. 相似文献
20.
Ulrich Müller 《无机化学与普通化学杂志》1976,422(2):141-148
The Crystal Structure of Antimony Tetrachloride Cyanurate [SbCl4NCO]3 [SbCl4NCO]3 crystallizes in the hexagonal space group P63/m with two formula units per unit cell; the lattice parameters are a = 1167 and c = 995 pm. The crystal structure was solved with X-ray diffraction data by means of a Patterson and a Fourier Synthesis and was refined by the method of least-squares to a reliability index of R = 3.6% for the 863 observed reflexions. The structure consists of [SbCl4NCO]3 molecules having the point symmetry 6 . The molecule is a derivate of cyanuric acid in a way such that each Sb atom is bonded in chelate manner by one N and one O atom; together with 4 Cl atoms the antimony attains a distorted octahedral coordination. The packing density in the crystal is not optimal, there exist cavities. 相似文献