共查询到20条相似文献,搜索用时 0 毫秒
1.
2.
3.
Preparation of Crystal Structure of K6[Al2O6] and Rb6[Al2O6] Colourless single crystals of K6[Al2O6] have been prepared from intimate mixtures of KAlO2 and K2O (550°C, 90 d). The structure determination from four-circle diffractometer data (MoKα , 742 Io(hkl), R = 2.2%, Rw = 2.1%) confirms the space group C2/m with Z = 2; a = 698.25 pm, b = 1 103.54 pm, c = 646.49 pm, β = 102.49°. Colourless single crystals of hitherto unknown Rb6[Al2O6] have been prepared from intimate mixtures of RbAlO2 and Rb2O (520°C, 120 d). The structure determination from four-circle diffractometer data (MoKα , 1 240 Io(hkl)) results in the residual values R = 7.2%, Rw = 4.9%; space group C2/m; a = 725.92 pm, b = 1 143.33 pm, c = 678.06 pm, β = 104.05°; Z = 2. K6[Al2O6] and Rb6[Al2O6] are isostructural with K6[Fe2O6]. A characteristic structure unit is the anion [Al2O6]6? consisting of two edge-sharing [AlO4] tetrahedra. Effective Coordination Numbers (ECoN), Mean Fictive Ionic Radii (MEFIR), the Madelung Part of Lattice Energy (MAPLE) and the Charge Distribution (CHARDI) are calculated and discussed. 相似文献
4.
K2Zn3O4 and Rb2Zn3O4, Oxozincates with Framework Structure For the first time single crystals of K2Zn3O4 were obtained by heating mixtures of the binary oxides (K: Zn = 2.2:3) in sealed Ag- or Pt-capsules at 800°C (5 w). Powder of this colourless and moisture-sensitive oxide was prepared analogously at 500°C. It crystallizes monoclinic, space group C2/c with a = 1482.7(2), b = 637.3(1), c = 571,9(1) pm, β = 102.79(1)°, Z = 4, dx = 4.265 g/cm3, dpyk = 4.00 g/cm3. The crystal structure was determined from four-circle diffractometer data (MoKα, 730 unique hkl) and refined to R = 5.9%, Rw = 6.4%. It shows a Zn3O4 framework which consists of SiS2-like chains [ZnO4/2] connected by puckered layers of [ZnO3/3]. The crystal structure can be derived from a cubic closet packing of O2? and K+. Effective Coordination Numbers and the Madelung Part of Lattice Energy (MAPLE) are calculated. Rb2Zn3O4 was prepared from the binary oxides at 400°C (colourless hygroscopic powder). According to powder data it crystallizes isostructural to K2Zn3O4 with a = 1523.5(4), b = 649.8(2), c = 574.0(2) pm, β = 101.43(3)°, Z = 4, dx = 5.141 g/cm3, dpyk = 5.20 g/cm3. 相似文献
5.
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
6.
Alkaline Molybdotellurates: Preparation and Crystal Structures of Rb6[TeMo6O24] · 10H2O and Rb6[TeMo6O24] · Te(OH)6 · 6H2O Single crystals of Rb6[TeMo6O24] · 10 H2O and Rb6[TeMo6O24] · Te(OH)6 · 6 H2O, respectively, were grown from aqueous solution. Rb6[TeMo6O24] · 10 H2O possesses the space group P1 . The lattice dimensions are a = 963.40(13), b = 972.56(12), c = 1 056.18(13) pm, α = 97.556(10), β = 113.445(9), γ = 102.075(10)°; Z = 1, 2 860 reflections, 215 parameters refined, Rg = 0.0257. The centrosymmetrical [TeMo6O24]6? anions are stacked parallel to [010]. Rb(2) is coordinated with one exception by water molecules only. Folded chains consisting of [TeMo6O24]6? anions and Rb(2) coordination polyhedra which are linked to pairs represent the prominent structural feature. Rb6[TeMo6O24] · Te(OH)6 · 6 H2O crystallizes monoclinically in the space group C2/c with a = 1 886.4(3), b = 1 000.9(1), c = 2 126.5(3) pm, and β = 115.90(1)°; Z = 4, 3 206 reflections, 240 parameters refined, Rg = 0.0333. It is isostructural in high extent with (NH4)6[TeMo6O24] · Te(OH)6 · 7 H2O. Hydrogen bonds between Te(OH)6 molecules and [TeMo6O24]6? anions establish infinite strands. The [TeMo6O24]6? anions gather around Te(OH)6 providing channel-like voids extending parallel to [001]. 相似文献
7.
K6[Mn2O6] and K6[Fe2O6] - a Comparison K6[Mn2O6] has been prepared (dark-red single crystals). The structure (a = 8.886, b = 6.760, c = 11.394 Å, γ = 132.1°, space group P21, Z = 2, 1151 symmetry independent reflections hk0–hk9, R = 0.051) shows Al2Cl6-like anions [Mn2O6]6?. By unit-cell transformation to the monoclinic setting P21/a (a = 6.760, b = 11.394, c = 6.638 Å, β = 96,9°) the structural similarity to K6[Fe2O6] becomes evident. The Madelung Part of Lattice Energy, MAPLE, is calculated. 相似文献
8.
Roland Baier Erhard Seipp Rudolf Hoppe 《Monatshefte für Chemie / Chemical Monthly》1987,118(6-7):677-690
The crystal structure of K6[CdO4] and Rb2CdO2 has been determined from single crystal X-ray diffraction data and refined toR=0.058 (K6[CdO4]) andR=0.088 (Rb2CdO2). K6[CdO4] crystallizes hexagonal, space group P63mc with lattice constantsa=867.42 (6),c=665.5 (1) pm,c/a=0.767 andZ=2. It is isotypic with Na6[ZnO4]. Rb2CdO2 is orthorhombic, space group Pbcn witha=1045.0 (2),b=629.1 (1),c=618.3 (1) pm,Z=4, and crystallizes with the K2CdO2 structure type. The crystal structures can be deduced from the motif of a closest packed arrangement of O2– with hexagonal (K6[CdO4]) or cubic (Rb2CdO2) stacking. The tetrahedra occupied by Cd2+ are isolated (K6[CdO4]) or edge-shared (formation of infinite SiS2-like chains [CdO4/2]) (Rb2CdO2). The powder diffraction pattern of Rb6[CdO4] [a=906.6 (1),c=694.3 (1) pm] and Rb2Cd2O3 [a=642.6 (2),b=679.0 (1),c=667.9 (2) pm, =115.2 (1)] confirm isotypie with K6[CdO4] and K2Cd2O3 respectively.
Herrn Prof. Dr.Gutman zum 65. Geburtstag gewidmet. 相似文献
9.
New Nesozincates: K4[ZnO3], Rb7Na[ZnO3]2 For the first time A) K4[ZnO3] and B) Rb7Na[ZnO3]2 have been prepared (from the binary oxides). They represent the first oxozincates of the alkali metals in which the coordination number of Zn2+ is exclusively 3 (carbonate-like groups [ZnO3]). Both oxides crystallize triclinic, space group P1 with A): a = 1103.3(3), b = 881.3(3), c = 698.2(2) pm, α = 109.65(2)°, β = 89.56(2)°, γ = 102.41(3)° and Z = 4, and B): a = 1128.3(3), b = 974.5(3), c = 711,8(2) pm, α = 114.12(2)β, = = 88.46(3)°,γ = 106.48(2)° and Z = 4. Their crystal structures have been determined from single crystal data (four circle diffractometer) and refined to R = 10.1%, Rw = 7.8% (2905 unique I0(hkl)) and R = 19.5%, Rw = 17.3% (2269 unique I0(hkl)), respectively. The Madelung Part of Lattice Energy (MAPLE), Effective Coordination Numbers (ECoN) and Mean Fictive Ionic Radii (MEFIR) have been calculated. 相似文献
10.
Angela Mller 《无机化学与普通化学杂志》1997,623(11):1685-1692
Synthesis, Crystal Structures, and Absorption Spectra of the New “Cupriosilicates”: K6[CuSi2O8] and Rb4[CuSi2O7] K6[CuSi2O8] and Rb4[CuSi2O7] were obtained by annealing intimate mixtures of K2O and Rb2O, respectively, CuO and SiO2 in sealed Ag cylinders at 500°C as transparent greenish-blue single crystals. The structure solution (IPDS-data Mo Kα; K6[CuSi2O8]: 1292 F2(hkl), R1 = 0.059; wR2 = 0.103 and Rb4[CuSi2O7]: 763 F2(hkl), R1 = 0.049; wR2 = 0.114) confirms the space group P1 for both compounds. K6[CuSi2O8]: a = 619.4(2); b = 665.5(2); c = 753.0(2) pm; α = 83.66(3); β = 87.71(3); γ = 70.19(3)°; Z = 1. Rb4[CuSi2O7]: a = 631.9(9); b = 707.5(10); c = 715.2(6) pm; α = 114.2(1); β = 100.7(1); γ = 107.9(1)°; Z = 1. The Madelung Part of the Lattice Energy, MAPLE, Effective Coordination Numbers, ECoN, these calculated via Mean Effective Ionic Radii, MEFIR, are given. The absorption spectra of K6[CuSi2O8] and Rb4[CuSi2O7] are discussed in terms of the Angular Overlap Model, AOM. 相似文献
11.
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
12.
On TiF3 and Hexafluorotitanates(III): Cs2K[TiF6] and Rb2K[TiF6], with a remark on Rb3[TiF6] By “redox-reaction with the wall” according to A2B[CuF6] + Ti = A2B[TiF6] + Cu we obtained for the first time single crystals of the Hexafluorotitanates(III). The violett irregular single crystals of Cs2K[TiF6] (a = 9.115 Å) and Rb2K[TiF6] (a = 8.910 Å) crystalise in accordance with the single-crystal studies as supposed in spcgrp. O-Fm3m No. 225. Dark blue crystals of TiF3 crystalises in the VF3-Typ. Parameters see text. TiF3 (3.9–251.3 K) and Rb3[TiF6] (3.8–251.3 K) have been measured magnetically. The madelung part of lattice energy, MAPLE, and the effective coordination number, ECoN, via the mean fictive ionic radii, MEFIR, are calculated and discussed. 相似文献
13.
Preparation and Crystal Structures of the first Alkalimetall‐hexacarbonato‐oxotetraberyllates: K6[Be4O(CO3)6] · 7 H2O and K6[Be4O(CO3)6] K6[Be4O(CO3)6] · 7 H2O has been prepared by dissolving freshly precipitated Be(OH)2 in an aqueous KHCO3 solution. After enriching the title compound by extraction with ethanol the heptahydrate crystallizes from the organic phase (triklin, P1¯ (No. 2) with a = 951, 01(11), b = 958, 45(12), c = 1601, 7(2) pm, α = 79, 253(13)°, β = 78, 943(12)°, γ = 65, 119(12)°, VEZ = 1290, 6(3)·106 pm3, Z = 2). Thermal decomposition forms rhombohedral crystals of the anhydrous compound (trigonal‐rhombohedric, R3¯ (No. 148) with a = 1416, 42(6), c = 1704, 5(1) pm, VEZ = 2961, 4(3)·106 pm3, Z = 6). 相似文献
14.
New Metal Oxides with Doubles of Tetrahedra as Building Units: Rb6[Tl2O6] and Cs6[In2O6] We prepared the hitherto unknown Rb6[Tl2O6] and Cs6[In2O6] by heating mixtures of Tl2O3 and RbO0.60 (Rb:Tl = 3.5:1) as well as In2O3 and CsO0.53 (Cs:In = 3.5:1) as single crystals [closed Ag-cylinder, 650°C, 14 d]. The single crystals of Rb6[Tl2O6] are yellow, those of Cs6[In2O6] pale yellow, all transparent and rude. The new type of structure was elucidated by 4-circle-diffractometer (PW 1100) data. Rb6[Tl2O6]: P21/a; a = 1145,7(3), b = 713,3(1), c = 783,9(2) pm, β = 93,73° (2), Z = 2; Ag–Kα, 2100 out of 2531 I0(hkl), R = 9,6% and Rw = 8,9%. Cs6[In2O6]: P21/a; a = 1178,5(4), b = 730,7(2), c = 816,3(2) pm, β = 95,38° (3), Z = 2; Mo–Kα, 1584 out of 2032 I0(hkl), R = 9,25%, and Rw = 8,44%. The Madelung Part of Lattice Energy, MAPLE, is calculated and discussed. 相似文献
15.
Rubidium Hexaamidolanthanate and -neodymate, Rb3[La(NH2)6] and Rb3[Nd(NH2)6]; Compounds. Structurally Related to K3[Cr(OH)6] and K4CdCl6 Colourless Rb3[La(NH2)6] (a = 12.298(4) Å, c = 13.759(2) Å, N = 6, R3 c) and pale blue Rb3[Nd(NH2)6] (a = 12.199(6) Å, c = 13.626(4) Å, N = 6, R32) have been prepared by the reaction of the corresponding metals (Rb: La resp. Nd = 3:1) with NH3(P(NH3) = 4–4.5 kbar) at 300°C. Single crystal x-ray methods gave their structures. It is shown by space group relations that these compounds are structurally related to one another and to further ternary amides as well as to K3[Cr(OH)6] and K4CdCl6. 相似文献
16.
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
17.
Thio- and Selenomercurates(II). K6[HgS4], K6[HgSe4], Rb6[HgS4] and Rb6[HgSe4] We prepared by annealing intimate mixture of pure samples of K2S, K2Se, Rb2S, and Rb2Se with HgS or HgSe [360–380°C, 7d, Duran-glass-seal with Argon] with hexagonal Na6ZnO4 isotypic new mercurates: K6[HgS4] [bright citronic yellow a = 9.985, c = 7.652 Å], K6[HgSe4] [light orange yellow a = 10.36, c = 7.883 Å], Rb6[HgS4] [bright yellow a = 10.34, c = 7.942 Å], Rb6[HgSe4] [orange-red a = 10.72, c = 8.192 Å]. The crystal structure of K6 Hgs4 is elucidated by using diffractometer data of single crystals: P63mc, C46v, it is R = 6.6% for 304 reflexes [h k o–h k 4, anisotropic refinement MoKα]; for position and parameters see text drö = 2.835, dpyk = 2.99 g · cm?3. The Madelung Part of Lattice Energy, MAPLE, and Effective Coordination Numbers, ECoN, are calculated and discussed. 相似文献
18.
A New Lithosilicate: Rb5LiNiSi2O8 = Rb5[LiNiSi2O8] Nearly colourless crystals of Rb5LiNiSi2O8 resulted by heating intimate mixtures of RbO0.6, LiO0.5, and SiO2 (Rb : Li : Si = 3 : 1.2 : 1) in tightly closed Ni-tubes. The crystal structure was determined (four-circle-diffractometer-data, 1 733 of 1 740 I0 (h kl), R = 6.9%, Rw = 5.5%, parameters see text). The new “Lithosilicate” crystallizes monoclinic (Space group C2/c) with a = 860.0(2), b = 1 026.2(2), c = 1 376.1(3) pm, β = 101.28(2)° (Guinier-Simon-powder-data), Z = 4. The structure is built up by chains [O2/2SiO2LiO2SiO2NiO2/22] where Si4+ resp. Li+ are coordinated tetrahedrally, Ni2+ however quadratic planar. The Madelung Part of Lattice Energy, MAPLE, and Effective Coordination Numbers, ECoN, these calculated via Mean Fictive Ionic Radii, MEFIR, are given. 相似文献
19.
New Oxoterbates(IV) with Lithium: On Rb2Li14[Tb3O14] and Li6Tb2O7 For the first time we prepared Rb2Li14[Tb3O14] as yellow single crystals from Li8TbO6 and Rb2O (Tb:Rb = 1:2) [Ag-cylinder, 500°C, 30 d, then Au-tube, 700°C, 27 d]. The structure refinement [652 I0 (h kl), four circle diffractometer Philips PW 1100, ω-scan, MoKα, R = 4.69%, Rw = 3.24%, absorption considered, Immm with a = 1 283.07(10), b = 790.87(7), c = 736.87(7)pm, Z = 2, dx = 4.30 g · cm?3] confirms that it is isotypic with K2Li14[Pb3O14]. Furthermore we got for the first time Li6Tb2O7 as a bright yellow compound from Li2O2 and “Tb4O7*” [(Li:Tb = 3.4:1), Au-ube, 750°C, 13 d (powder), 850°C 22 d (single crystals)] and by thermal decomposition of Rb2Li14[Tb3O14] (Au-tube, 850°C, 25 d). Powder and single crystal data [1 327 I0 (h kl), four circle diffractometer PW 1100, ω-scan, AgKα, R = 9.38%, Rw = 5.23%, absorption not considered, P21/a, a = 1 056.30(10), b = 613.50(4), c = 546.56(5) pm, β = 109.668(7)°, Z = 2, dx = 4.67 g · cm?3 dpyc = 4.53 g · cm?3] reveal a new type of structure that may be deduced by the NaCl-type of structure. The Madelung Part of Lattice Energy, MAPLE, Effective Coordination Numbers, ECoN, these via Mean Fictive Ionic Radii, MEFIR, are calculated and discussed. 相似文献
20.
On the Knowledge of Hexafluororhodates(III): Cs2K[RhF6], Rb2K[RhF6], K2Na[RhF6], Rb2Na[RhF6] and Tl2Na[RhF6]. New prepared are the compounds Cs2KRhF6 (a = 9.049 Å), Rb2NaRhF6 (a = 8.492 Å), Rb2KRhF6 (a = 8.876 Å), K2NaRhF6 (a = 8.362 Å) and Tl2NaRhF6 (a = 8.526 Å), all cubic Elpasoliths of pink colour. The Madelung-Part of lattice energy, MAPLE, is calculated and discussed. 相似文献