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1.
A New Type of Structure in Oxoiridates with Square-planar Groups [IrO4]4?: K2Na2[IrO4], a Network [Na2IrO4] with Channels (With a Remark on Rb2Na2[IrO4]) For the first time magnificent dark red cuboid single crystals of K2Na2[IrO4] were prepared by annealing intimate mixtures of a) KO0.51, Na2O2, IrO2 and Ir-powder (molar proportions 3.02 : 1.40 : 1.00 : 1.00; Ag-bomb, 740°C, 54 d) and of b) KO0.51, Na2O and IrO2 (molar proportions K : Na : Ir = 2.20 : 2.20 : 1.00; Ag-bomb, 760°C, 57 d) respectively. The oxide crystallizes mP36, space group P21/c with a = 600.35(6) pm, b = 1111.2(1) pm, c = 933.0(1) pm and β = 113.14(1)°. Structure determination via four-circle diffractometer data (Siemens AED 2, Mo-Kα-Radiation) for all 2347 unique reflexions (merged from 9397 Io(hkl) gave R = 0.0357 and Rw = 0.0340. K2Na2[IrO4] crystallizes in a new type of structure. The oxide is antiferromagnetic as magnetic measurements showed (TN = 32 K, Θ = ?60.2 K (single crystals) and ?49.2 K (powder) respectively, μ = 3.06 μB (single crystals) and 2.93 μB (powder) respectively). Effective coordination numbers ECoN, mean fictive ionic radii MEFIR and the Madelung part lattice energy MAPLE as well as the charge distributions CHARDI and CHARDINO are calculated and discussed. 相似文献
2.
Pnictogenidostannates(IV) with Discrete Tetrahedral Anions: New Representatives (E1)4(E2)2[Sn(E15)4] (with E1 = Na, K; E2 = Ca, Sr, Ba; E15 = P, As, Sb, Bi) of the Na6[ZnO4] Type and the Superstructure Variant of K4Sr2[SnAs4] The silvery to dark metallic lustrous compounds (E1)4(E2)2[Sn(E15)4] (E1 = Na, K; E2 = Ca, Sr, Ba; E15 = P, As, Sb, Bi) were prepared from melts of stoichiometric mixtures of the elements. They crystallize in the Na6[ZnO4]‐type structure (hexagonal, space group: P63mc, Z = 2; Na4Ca2[SnP4]: a = 938.94(7), c = 710.09(8) pm; K4Sr2[SnAs4]: a = 1045.0(2), c = 767.0(1) pm; K4Ba2[SnP4]: a = 1029.1(6), c = 780.2(4) pm; K4Ba2[SnAs4]: a = 1051.3(1), c = 795.79(7) pm; K4Ba2[SnSb4]: a = 1116.9(2), c = 829.2(1) pm; K4Ba2[SnBi4]: a = 1139.5(2), c = 832.0(2) pm). The anionic partial structure consists of tetrahedra [Sn(E15)4]8– orientated all in the same direction along [001]. In the cationic partial structure one of the two cation positions is occupied statistically by alkali and alkaline earth metal atoms. Up to now only for K4Sr2[SnAs4] a second modification could be isolated, forming a superstructure type with three times the unit cell volume (hexagonal, space group: P63cm, Z = 6; a = 1801.3(2), c = 767.00(9) pm) and an ordered cationic partial structure. 相似文献
3.
Preparation, Structure, and Magnetic Properties of the Alkaline Earth Manganese Compounds AMnX with A = Mg, Ca, Sr, Ba and X = Si, Ge, Sn The new compounds MgMnGe, MgMnSn, CaMnSi, CaMnSn, and SrMnSn were prepared by reaction of the elements. They crystallize tetragonally with the anti-PbFCl type structure (space group P4/nmm). The lattice constants see ”︁Inhaltsübersicht”︁”︁. Using a Faraday balance, magnetic measurements in the range 4.2 to 800 K were performed with the new substances and with the already known compounds CaMnGe, SrMnGe, and BaMnGe. They indicate metamagnetic behaviour at low temperatures. At high temperatures twodimensional magnetic interactions between the manganese atoms seem to persist. The construction of an unexpensive heating device for the Faraday balance is described. 相似文献
4.
On Thallium(I)-oxochloromolybdates: Synthesis and Crystal Structures of Tl[MoOCl4(NCCH3)], Tl[Mo2O2Cl7], and Tl2[Mo4O4Cl14] and the Structure of Tl2[MoCl6] Black crystals of Tl2[MoCl6] are formed in the reaction of TlCl with MoOCl3 in a sealed evacuated glass ampoule at 350 °C. The crystal structure analysis shows that Tl2[MoCl6] (cubic, Fm 3¯m, a = 986.35(7) pm) adopts the K2[PtCl6] structure with a Mo–Cl bond length of 236.6 pm. Tl[MoOCl4(NCCH3)] was obtained by the reaction of TlCl with MoOCl3 in acetonitrile in form of yellow, moisture sensitive crystals. The structure (orthorhombic, Cmcm, a = 746.0(1), b = 1463.8(3), c = 857.3(2) pm) is built of Tl+ cations and octahedral [MoOCl4(NCCH3)]– anions in which the acetonitrile ligand is bound in trans position to the oxygen. The reaction of TlCl and MoOCl3 in dichloromethane yields Tl[Mo2O2Cl7] and Tl2[Mo4O4Cl14] as green moisture sensitive crystals. The structure of Tl[Mo2O2Cl7] (orthorhombic, Pmmn, a = 694.3(1), b = 951.9(2), c = 904.7(1) pm) consists of Tl+ cations and dinuclear [Mo2O2Cl7]– anions, with two equidistant chlorine bridges of 248.2 and one longer chlorine bridge of 265.7 pm. The oxygen atoms are located in the trans positions of the longer chloro bridge. The structure of Tl2[Mo4O4Cl14] (triclinic, P1¯, a = 692.8(1), b = 919.6(1), c = 998.9(1) pm, α = 104.94(1)°, β = 90.31(1)°, γ = 108.14(1)°) is build of Tl+ cations and [Mo4O4Cl14]2– anions which form tetramers of distorted octahedral, edgesharing (MoOCl5) units with chlorine atoms in the bridging positions. The oxygen atoms are located in the trans positions of the longest chlorine bridges. 相似文献
5.
Harald Krautscheid 《无机化学与普通化学杂志》1995,621(12):2049-2054
Synthesis and Crystal Structures of (Ph4P)4[Bi8I28], (nBu4N)[Bi2I7], and (Et3PhN)2[Bi3I11] – Bismuth Iodo Complexes with Isolated and Polymeric Anions Solutions of BiI3 in methanol react with NaI and (nBu4N)(PF6) or (Et3NPh)(PF6) to form anionic bismuth iodo complexes (nBu4N)[Bi2I7] 1 and (Et3PhN)2[Bi3I11] 2 . In 1 Bi4I16 units, and in 2 Bi6I24 units are linked by common I-atoms to onedimensional infinite chains. Reaction of BiI3 with (Ph4P)(PF6) in methanol yields (Ph4P)4[Bi8I28] 3 . The anions of 1–3 consist of edge-sharing BiI6 octahedra. (nBu4N)[Bi2I7] 1 : Space group I2/m (No. 13), a = 1 082.3(5), b = 2 597.1(13), c = 1 206.1(6) pm, β = 93.17(2)°, V = 3 385(3) · 106 pm3; (Et3PhN)2[Bi3I11] 2 : Space group P1 (No. 2), a = 1 283.5(6), b = 1 345.9(7), c = 1 546.3(8) pm, α = 83.87(2), β = 74.24(2), γ = 68.26(2)°, V = 2 388(2) · 106 pm3; (Ph4P)4[Bi8I28] 3 : Space group P1 (No. 2), a = 1 329.3(4), b = 1 337.0(4), c = 2 193.1(5) pm, α = 104.20(2), β = 99.73(2), γ = 100.44(2)°, V = 3 622(2) · 106 pm3. 相似文献
6.
Mehmet Somer Wilder Carrillo‐Cabrera Eva‐Maria Peters Karl Peters Martin Kaupp Hans Georg von Schnering 《无机化学与普通化学杂志》1999,625(1):37-42
Dark red crystals of [K‐(2,2,2)‐crypt)]2Sn5 precipitate after the reaction of (2,2,2)‐crypt with a solution of K1.33Sn in liquid ammonia at room temperature. The compound is sensitive to oxidation and hydrolysis. The sequence of Raman bands (104, 120, 133 and 180 cm–1) is characteristic for the trigonal bipyramidal closo‐[Sn5]2– cluster anion. The wave numbers correspond with the data from Hartree‐Fock calculations (114, 128, 142 and 187 cm–1). The compound crystallizes trigonally (a = 11.736 Å, c = 22.117 Å, Z = 2, space group P3c1 (No. 165); Pearson code hP262), isotypic with [Na‐(2,2,2)‐crypt)]2Pb5. The atoms of the cluster show strange anisotropic displacements, which are perfectly reducible to a helical rigid‐body motion around and along [001] (libration: ± 9.5°; translation ± 0.29 Å). The structure can be described as a hierarchical derivative of the initiator CaIn2 (P63/mmc, hP6), generated by an atom‐to‐aggregate replacement: [Ca][In]2 = [Sn5][K @ C36H72N4O12]2. Thus, the distribution of the [Sn5]2– Zintl anions is hexagonal primitive, and the cation complexes are located close to the centers of trigonal superprisms formed by Sn5 clusters. 相似文献
7.
The Adduct of BiCl3 and Mo6Cl12: [BiCl] Dumbbells in the Structure of [BiCl][Mo6Cl14] MoCl3 reacts under decomposition to MoCl2 and Cl2 with BiCl3 in a sealed evacuated glass ampoule at 550 °C to form light red crystals of [BiCl][Mo6Cl14]. The crystal structure determination (monoclinic, C 2/c, a = 1268.1(4) pm, b = 1304.6(3) pm, c = 2571.9(8) pm, β = 91.79(3)°, Z = 8) shows that the structure is built of [(Mo6Cl8)Cl6] units containing nearly regular octahedral Mo6 clusters. These units are arranged in the motiv of a cubic closest packing. The octahedral interstices contain [BiCl] dumbbells with a Bi–Cl bond length of 249 pm. The coordination sphere of the Bi atom is completed by six weaker Bi–Cl-contacts of 275 to 308 pm length to a distorted monocapped trigonal prism. Neglecting the secondary Bi–Cl bonds, the title compound can be formulated as [(BiCl)2+][(Mo6Cl14)2–]. 相似文献
8.
ChemInform is a weekly Abstracting Service, delivering concise information at a glance that was extracted from about 200 leading journals. To access a ChemInform Abstract of an article which was published elsewhere, please select a “Full Text” option. The original article is trackable via the “References” option. 相似文献
9.
[Na · Triglyme]2[S(BH3)4]: a Salt of the New Anion Tetrakis(borane)sulfate(2? ). Crystal Structure and Theoretical Investigation of the Structure Na[H3B-m?2-S(B2H5)] 1 is produced by the reaction between NaSH and THF · BH3, under dehydrogenation. 1 is also formed as the first 11B-NMR-spectroscopically detectable reaction product by the reaction between anhydrous Na2S and THF · BH3. Adducts of BH3 with the S2? ion are not detectable in THF. The anion [S(BH3)4]2? can however be obtained, by the addition of NaBH4 to 1 in diglyme or triglyme respectively: [Na — Triglyme]2[S(BH3)4] 2. 2 crystallizes in the monoclinic space group P21/n (Nr. 14). Structural data of 1 and 2 have been calculated by SCF methods. The anion of 2 may be viewed either as an adduct of B2H6 with S2?, or as a bridge substituted thia derivative of B2H7?; furthermore the anion of 2 is isoelectronic and isostructural with the SO ion. 相似文献