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1.
Synthesis and Structure of Cs11[(WN2,5O1,5)2](N3)2, a Cesium Oxo Nitrido Monotungstate(VI) Azide Cs11[(WN2,5O1,5)2](N3)2 results from the reaction of a mixture of CsNH2, W and WO3 at 620 °C in autoclaves. It crystallizes monoclinic in the space group C2/m with the lattice parameters a = 12.421(4) Å, b = 11.568(6) Å, c = 10.516(4) Å, β = 118.71(3)° and Z = 4. The crystal structure is built up by isolated tetrahedra [WX4] with X = N, O, which are connected by cesium cations. Between the cesium ions lie azide ions separated from the anions [WX4]. The tungsten atoms and azide ions together build up the motif of a distorted arrangement of the CsCl structure type. 相似文献
2.
Potassium Oxo Nitrido Mono Cyclo Tungstate(VI), K10[(WN2.5O0.5)4] with Rings of Four Corner‐Sharing Tetrahedra (WX2X2/2)4 with X = N, O Reactions of mixtures of potassium amide, tungsten powder and tungsten(VI) oxide in autoclaves at 650 °C lead to yellow potassium oxo nitrido mono cyclo tungstate (VI), K10[(WN2.5O0.5)4], which crystallizes isotypic to Ba10[(TiN3)4]. After the reaction is finished, crystals are embedded in a matrix of potassium metal. They were isolated by washing out the metal with liquid ammonia. X‐ray investigations showed that K10[(WN2.5O0.5)4] crystallizes in the space group P1 with lattice parameters a = 6.569(5) Å, b = 9.437(2) Å, c = 9.559(3) Å, α = 106.20(2)°, β = 101.93(5)°, γ = 108.20(3)° and Z = 1. The crystal structure contains rings of four corner‐sharing tetrahedra (WX2X2/2)4 with X = N, O which are packed along the a‐axis forming the motif of a hexagonal rod packing of columns. Potassium ions are located mainly between these columns but also within them. 相似文献
3.
Transparent yellow crystals of Ba4[WN4]Cl2 were grown at 850°C by the reaction of Ba(NH2)2 with W in a KCl melt under flowing nitrogen. The compound crystallizes monoclinic in P21/m and Z = 2 with the cell parameters a = 8.447(4) Å, b = 6.143(2) Å, c = 10.727(6) Å and β = 99.04(4)°. The crystal structure contains isolated anions [WN4]6? and Cl?. It is the first nitridotungstate(VI) chloride reported so far. 相似文献
4.
Alkali Metal Nitrido Tecto Metallates(VI) with Networks of Six‐membered Rings of Corner‐sharing Tetrahedra [(MNN3/2)6] with M = Mo, W of the Unexpected Composition A9+x[M6N15] with A = Rb, Cs and 0 < x < 1 Reactions of metal powders of Mo and W respectively with amides and azides of Rb and Cs lead to the compounds Rb9+x[W6N15] and Cs9+x[M6N15] with M = Mo, W and 0 < x < 1. The reactions are carried out at 650 °C in autoclaves for salt melts and are finished within 5 d. Crystals of the compounds are embedded in a matrix of the corresponding alkali metal. These metals result from the thermal decomposition of the amides and azides used in high molar ratios. The metals are washed out by liquid ammonia. Besides microcrystalline material of the above mentioned compounds single crystals suitable in size for x‐ray structure determinations were isolated. The compounds crystallize in the space group R3c (No. 167) with Z = 6 and the following lattice constants: Rb9+x[W6N15]: a = 12.743(7) Å, c = 27.794(8) Å, c/a = 2.181 Cs9+x[Mo6N15]: a = 13.104(5) Å, c = 28.430(9) Å, c/a = 2.170 Cs9+x[W6N15]: a = 13.136(5) Å, c = 28.472(6) Å, c/a = 2.167 The metal centres of tetrahedra [MNN3/2] are condensated to cyclohexane analogue six‐membered rings in chair‐form via nitrogen atoms and axial ones connect them to a three‐dimensional network. Nine – as to the formula unit – of the alkali metal atoms are located in vacancies of the anionic partial structure. The residual atoms with 0 < x < 1 centre the six‐membered rings and are coordinated planar hexagonal by N neighbours. 相似文献
5.
Cs5[Na{W4N10}] was prepared from a mixture of NaNH2, CsNH2 and tungsten powder (molar ration 1 : 10 : 4) at 700°C in autoclaves. After the reaction is finished the nitride is embedded in an alkali metal matrix. Dark red crystals were isolated by washing out the alkali metal with liquid ammonia at room temperature. The structure of Cs5[Na{W4N10}] was solved by X-ray single crystal data: I41 (No. 80), Z = 4, a = 13.926(3) Å, c = 8.723(3) Å, Z(F) ≥ 3σ(F) = 1535, Z(Variables) = 63, R/Rw = 0.040/0.052. The compound is highly sensitive against moisture giving oxotungstates and ammonia. It contains a framework of tetrahedra [WNN3/21.5?]. Sodium shares four terminal nitrogen ligands. Including sodium a distorted, β-cristobalite type arrangement [Na{W4N10}5?] results. It contains caesium in all interstices formed by twelve nitrogen ligands in so-called Friauf polyhedra. 相似文献
6.
Synthesis, Structure, and Vibrational Spectra of the Oxofluorotungstates(VI) Cs2[WO3F2] and Cs3[W2O4F7] Cs2[WO3F2] crystallizes from a melt with the same composition. The orthorhombic unit cell with a = 6.779(2), b = 7.668(1) and c = 11.626(3) Å, space group Pn21a, contains 4 formula units. The WO3F22? anion is polymer, W octahedrally coordinated according to the results of the X-ray crystal structure determination. Planar dioxodifluoro groups are linked into chains by oxygen atoms. The lengths of the W? O bonds are alternating. Cs3[W2O4F7] crystallizes trigonal, space group P3 m1, with a = 21.118(4) and c = 8.434(2) Å, Z = 9. The structure consists of two sets of crystallographically non equivalent dimeric anions with the formula [O2F3W? F? WO2F3]3?. Part of the ligand atoms are disordered. The vibrational spectra of both compounds show the presence of cis-dioxo groups of the terminal ligands. 相似文献
7.
Synthesis and Crystal Structure of a Cesium-tetraimidophosphate-diamide, Cs5[P(NH)4](NH2)2 = Cs3[P(NH)4] · 2 CsNH2 Well crystallized Cesium-tetraimidophosphate-diamide is obtained by the reaction of CsNH2 with P3N5 in autoclaves at 673 K within three days. X-ray single crystal investigations led to the following data
- Ccca, Z = 4, a = 8.192(5) Å, b = 20.472(5) Å,
- c = 8.252(3) Å
- Z(F) ≥3σ(F) = 916, Z(Var.) = 32, R/Rw=1 = 0.017/0.021
8.
Crystalline cesium nitratometalates(II), Cs2[M(NO3)4] (M = Mn ( I ), Co ( II ), Ni ( III ), and Zn ( IV )) were synthesized from M(NO3)2 · n H2O and CsNO3 by heating at 80–120 °C over 10–12 h. According to X-ray crystal structure analysis, the compounds are built from Cs+ cations and [M(NO3)4]2– anions. The latter differ by the type of metal coordination: a dodecahedron for Mn in I (CN = 8, rMn–O 2.24–2.37 Å), a seven coordination for Co in II (CN = 4 + 3, rCo–O 2.03–2.16 Å and 2.21–2.35 Å) and a tetrahedral distorted dodecahedron for Zn in IV (CN = 4 + 4, rZn–O 1.98–2.15 Å and 2.38–2.72 Å). Ni atom in III has a distorted octahedral NiO6 environment provided by two unidentate and two bidentate NO3 groups with Ni–O distances of 2.01–2.14 Å. The differences in metal coordination are discussed in terms of valence electron configurations, ionic radii, and the packing effects. 相似文献
9.
Barbara Schüpp Liane Schrder Helga Schulte Carsten Bhtz Norbert Mattern Hans‐Lothar Keller 《无机化学与普通化学杂志》2002,628(7):1708-1714
Hochtemperatur‐Cs2[PdCl4] — New Results on a “wellknown” Compound Two modifications of Cs2[PdCl4] have been characterized by X‐ray powder and single crystal diffraction, respectively. The crystal structures are described and the group‐subgroup‐relations between these structures are discussed. In addition to the tetragonal (P4/mmm (No. 123), a = 7.4158(8) Å, c = 4.6792(6) Å) and the orthorhombic (Cmcm (No. 63), a = 10.529(1) Å, b = 10.310(1) Å, c = 9.460(1) Å) modification DSC investigations and high‐temperature X‐ray diffraction experiments with synchrotron radiation show the existence of another modification or of yet unknown decomposition products. The phase transformation from the orthorhombic to the tetragonal polymorph is completely finished at 100 °C. The second effect is detected at 319 °C. 相似文献
10.
Crystal Structures and Vibrational Spectra of Tetrahalogenoacetylacetonatoosmates(IV), [OsX4(acac)]?, X ? Cl, Br, I By reaction of the hexahalogenoosmates(IV) with acetylacetone the tetrahalogenoacetylacetonatoosmates(IV) [OsX4(acac)]? (X = Cl, Br, I) are formed, which have been purified by chromatography and precipitated from aqueous solution as tetraphenylphosphonium (Ph4P) or cesium salts. X-ray structure determinations on single crystals have been performed of (Ph4P)[OsCl4(acac)] ( 1 ) (triclinic, space group P1 , a = 9.9661(6), b = 11.208(2), c = 13.4943(7) Å, α = 101.130(9), β = 91.948(6), γ = 96.348(8)°, Z = 2), (Ph4P)[OsBr4(acac)] ( 2 ) (monoclinic, space group P21/n, a = 9.0251(8), b = 12.423(2), c = 27.834(2) Å, β = 94.259(7)°, Z = 4) and (Ph4P)[OsI4(acac)] ( 3 ) (monoclinic, space group P21/c, a = 18.294(3), b = 10.664(2), c = 18.333(3) Å, β = 117.68(2)°, Z = 4). Due to the increasing trans influence in the series O < Cl < Br < I the Os? O. distances of O.? Cl? X′ axes are lengthened and the OsO. stretching vibrations are shifted to lower frequencies. The Os? X′ bond lenghts are shorter as compared with symmetrically coordinated X? Os? X axes. 相似文献
11.
News on K2[MnF6], Rb2[MnF6], and Cs2[MnF6] Cs2[MnF6] (a = 8.972 Å) and Rb2[MnF6] (a = 8.531 Å) as well as this with K2[MnF6] (a = 8.221 Å and hexagonal a = 5.722, c = 9.331 Å) form mixed crystals of the K2PtCl6 type of structure. Calculations of the Madelung Part of Lattice Energy, MAPLE, and Effective Coordination Numbers, ECoN, lead contrary to former assumptions to distances Mn? F of about 1.86 Å (CN 6). 相似文献
12.
New Oxogallates of Alkaline Metals: On K6[Ga2O6] and Rb6[Ga2O6] as well as Na3GaO3 and Cs6[Ga2O6] Due to powder and single crystal data K6[Ga2O6] a = 7.099; b = 11.116; c = 6.484 Å; ß = 101.66° and Rb6[Ga2O6] a = 7.393; b = 11.475; c = 6.798 Å; ß = 103.5° crystallize isotypic with K6[Fe2O6]; space group C2/m-C32h; As well has been prepared the hitherto unknown Na3GaO3 a = 11.48, b = 10.82, c = 6.13 Å, space-group Imcm or I2cm Z = 8; and Cs6[Ga2O6] a = 7.26, b = 12.1, c = 7.68 Å, ß = 105°, Z = 4, space-group P21/a. 相似文献
13.
New Oxonium Bromochalcogenates(IV) — Synthesis, Structure, and Properties of [H3O][TeBr5] · 3 C4H8O2 and [H3O]2[SeBr6] Dark red crystals of the composition [H3O][TeBr5] · 3 C4H8O2 ( 1 ) were isolated from a saturated solution of TeBr4 in 1,4-dioxane containing a small amount of water. In this compound (space group P21/m, a = 8.922(4) Å, b = 13.204(7) Å, c = 9.853(5) Å, β = 91.82(4)° at 150 K) a square pyramidal [TeBr5]? anion has been isolated for the first time. The coordination sphere of the anion is completed to a distorted octahedron by weak interaction with a dioxane molecule of the cationic system. The [H3O]+ cations are connected to chains by dioxane molecules. At room temperature the compound is stable only in its mother liquor. Crystalline [H3O]2[SeBr6] ( 2 ) (space group Fm3m, a = 10.421(1) Å at 170 K) is a bromoselenous acid of high symmetry. The [H3O]+ ion is only weakly coordinated by Br atoms of the anion. The anions are isolated octahedral [SeBr6]2? units. The structure is isotypic to the K2[PtCl6] structure. Despite being a halogenochalcogen(IV) acid, 2 exhibits a remarkable thermal stability. Both oxonium compounds were characterized by single-crystal X-ray structure analyses. Vibrational spectra of 2 are reported. 相似文献
14.
Novel Halogenochalcogeno(IV) Acids: [H3O(Benzo‐18‐Crown‐6)]2[Te2Br10] and [H5O2(Dibenzo‐24‐Crown‐8)]2[Te2Br10] Systematic studies on halogenochalcogeno(IV) acids containing tellurium and bromine led to the new crystalline phases [H3O(Benzo‐18‐Crown‐6)]2[Te2Br10] ( 1 ) and [H5O2(Dibenzo‐24‐Crown‐8)]2[Te2Br10] ( 2 ). The [Te2Br10]2‐ anions consists of two edge‐sharing distorted TeBr6 octahedra, the oxonium cations are stabilized by crownether. ( 1 ) crystallizes in the monoclinic space group P21/n with a = 14.520(5) Å, b = 22.259(6) Å, c = 16.053(5) Å, β = 97.76(3)° and Z = 4, whereas ( 2 ) crystallizes in the triclinic space group with a = 11.005(4) Å, b = 12.103(5) Å, c = 14.951(6) Å, α = 71.61(3)°, β = 69.17(3)°, γ = 68.40(3)° and Z = 1. 相似文献
15.
Three Novel Selenoborato- closo -dodecaborates: Syntheses and Crystal Structures of Rb8[B12(BSe3)6], Rb4Hg2[B12(BSe3)6], and Cs4Hg2[B12(BSe3)6] The three selenoborates Rb8[B12(BSe3)6] (P1, a = 10.512(5) Å, b = 10.450(3) Å, c = 10.946(4) Å, α = 104.53(3)°, β = 91.16(3)°, γ = 109.11(3)°, Z = 1), Cs4Hg2[B12(BSe3)6] (P1, a = 9.860(2) Å, b = 10.740(2) Å, c = 11.078(2) Å, α = 99.94(3)°, β = 90.81(3)°, γ = 115.97(3)°, Z = 1), and Rb4Hg2[B12(BSe3)6] (P1, a = 9.593(2) Å, b = 10.458(2) Å, c = 11.131(2) Å, α = 99.25(3)°, β = 91.16(3)°, γ = 116.30(3)°, Z = 1) were prepared from the metal selenides, amorphous boron and selenium by solid state reactions at 700 °C. These new chalcogenoborates contain B12 icosahedra completely saturated with six trigonal-planar BSe3 entities functioning as bidentate ligands to form a persubstituted closo-dodecaborate anion. The two isotypic compounds Rb4Hg2[B12(BSe3)6] and Cs4Hg2[B12(BSe3)6] are the first selenoborate structures containing a transition metal which are characterized by single crystal diffraction. 相似文献
16.
New Oxocuprates(I). On Cs3Cu5O4, Rb2KCu5O4, RbK2Cu5O4 and K3Cu5O4 Cs3Cu5O4 light yellow, powder as well as single crystals [a = 10.313(9), b = 7.630(1), c = 14.750(4) Å, β = 106.48(6)°], Rb2KCu5O4 [a = 9.724(2), b = 7.443(0), c = 14.246(2) Å, β = 106.78(8)°], RbK2Cu5O4 [a = 9.561(1), b = 7.411(0), c = 14.111(1) Å, β = 106.76(7)°] and K3Cu5O4 [a = 9.422(1), b = 7.364(1), c = 13.995(2) Å, β = 107.00(2)°] are new prepared. The colour of the powders becomes lighter according to the sequence showed above. K3Cu5O4 shows pale yellow. The Madelung Part of Lattice Energy, MAPLE, is calculated and discussed. 相似文献
17.
New Oxozineates of Alkali Metals: Rb2[ZnO2] and Cs2[ZnO2] Colorless single crystals of the hitherto unknown Rb2[ZnO2] (a = 9.558, b = 6.335, c = 15.91 Å, β = 118.6°, z = 8, dpyk = 4.11, drö = 4.21 g · cm?3) and Cs2[ZnO2] (a = 9.851, b = 6.619, c = 16.26 Å, β = 116.8°) have been prepared, which crystallize monoclinic, P21/c – D. (For parameters see text.) Unexpected there are “isolated” groups [Zn4O8]. Half of the Zn atoms exhibit the unusual coordination number 3 towards O2?. The Madelung Part of Lattice Energy, MAPLE, and the Effective Coordination Number, ECoN, the latter by means of Mean Fictive Ionic Radii, MEFIR, are calculated and discussed. 相似文献
18.
Brown crystals of [PPh4]2[Se2Br6] ( 1 ) and [PEtPh3]2[Se2Br6] ( 2 ) were obtained when selenium and bromine reacted in acetonitrile solution in the presence of tetraphenylphosphonium bromide and ethyltriphenylphosphonium bromide, respectively. The crystal structure of 2 has been determined by X‐ray methods and refined to R = 0.0420 for 4161 reflections. The crystals are monoclinic, space group P21/n with Z = 2 and a = 13.055(3) Å, b = 12.628(3) Å, c = 13.530(3) Å, β = 92.40(3)° (293(2) K). In the solid state structure of 2 the dinuclear hexabromo‐diselenate(II) anion is centrosymmetric and consists of two distorted almost square‐planar SeBr4 units sharing a common edge through two bridging Br atoms. The terminal SeII–Br bond distances are found to be 2.419(1) and 2.445(1) Å, the bridging μBr–SeII bond distances 2.901(1) and 2.802(1) Å. 相似文献
19.
L.F. Schneemeyer S.E. Spengler F.J. Di Salvo J.V. Waszczak C.E. Rice 《Journal of solid state chemistry》1984,55(2):158-164
A systematic investigation of crystal growth in the cesium molybdate/molybdenum trioxide system is described. A previously unknown blue cesium molybdenum bronze phase has been prepared as well as the known red bronze, Cs0.33MoO3, and high-quality crystals of the Magneli-phase compound, γ-Mo4O11. This new blue bronze, with empirical formula, Cs0.19MoO2.85, is monoclinic with cell constants, a = 19.198(4) Å, b = 5.519(2) Å, c = 12.213(2) Å, and β = 119.44(2)°. Measurements of the susceptibility and of the resistivity vs temperature are reported. As is the case for other alkali molybdenum bronzes, the product formed is determined by the molar ratio of alkali molybdate to molybdenum trioxide and the melt temperature. 相似文献
20.
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