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1.
On Quaternary Oxoplumbates(IV). On the Knowledge of Rb2Li14[Pb3O14] and Cs2Li14[Pb3O14] For the first time, Rb2Li14[Pb3O14] and Cs2Li14[Pb3O14] have been prepared by heating of mixtures of Li2O, β-?PbO2”? and Rb2PbO3, Cs2PbO3 respectively with Li:Pb:A = 14:3:2, (A = Rb, Cs). [Ag-cylinders, sealed under vacuum in Duran-glass ampoule, 590 and 550°C, 40 d, powder (650°C, 200 d, single crystals of Rb2Li14[Pb3O14])]. Rb2Li14[Pb3O14] is nearly colourless with ivory nuance, Cs2Li14[Pb3O14] is pale yellow. According to powder and single crystal investigations, both are isotypic with K2Li14[Pb3O14]. Structure refinement of Rb2Li14[Pb3O14]: 1015 symmetry independent reflexions, four-circle-diffraktometer PW 1100 (Fa. Philips), ω-scan, MoKα, R = 5.73%, RW = 5.33%, absorption not considered, space group Immm with a = 1284.71(9), b = 793.90(4), c = 727,35(5) pm, dx-ray = 4.99 g · cm?3, dpyc = 5.01 g · cm?3, Z = 2. Cs2Li14[Pb3O14]: a = 1295.28(12), b = 796.69(8), c = 732.44(7) pm, dx-ray = 5.31 g · cm?3, dpyc = 5.28 g · cm?3, Z = 2. The Madelung Part of Lattice Energy, MAPLE, Effective Coordination Numbers, ECoN, these via Mean Effective Ionic Radii, MEFIR, are calculated.  相似文献   

2.
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 d = 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   

3.
Rb2PbO3 [single crystals, 244 (hkl)] crystallises orthorhombic [D? Pmcn] with a = 10.8, b = 7.49, c = 5.98 Å [Z = 4, dpyk = 5.69, d = 5.80 g · cm?3], Rb in 8(d) Pb in 4 (c), OI in 4 (c). The parameters are shown in table 2. The MADELUNG Part of Lattice Energy of Rb2RBO3 and structurally related models are calculated and discussed in detail. Characteristic for the structure are ldimensional chains consisting of alternatingly directed pseudo-tetragonal pyramids, ∞1[PbO1O4/2], connected via common basis edges.  相似文献   

4.
“Fragmentation” and “Aggregation” on Lead Oxides. On the Oligooxoplumbate(IV) K2Li6[Pb2O8] For the first time, the dinuclear Oxoplumbate(IV) K2Li6[Pb2O8] has been prepared as transparent colourless single crystals by heating mixtures of K2PbO3, Li2O, and “PbO2” with K:Li:Pb = 1:3:1 e. g. [Ag-cylinders, sealed under vacuum in Supremax-glass ampoule, 660°C, 120 d]. The structure determination verifies the space group P1 with a = 6.9720(9), b = 5.9252(6), c = 5.9312(7) Å, α = 88.05(1)°, β = 107.94(1)°, γ = 107.30(1)°; dx = 4.95 g · cm?3, dpyk = 4.91 g · cm?3; Z = 1, [2107 symmetry independent hkl, fourcircle-diffractometer Philips PW 1100, ω—2Θ—scan, MoKα, R = 5.07%, Rw = 4.59%, absorption not considered]. The structure is characterized by the group [Pb2O8] — two edge connected (equatorial/apical) trigonal bipyramids — that is observed for the first time. Several ways of synthesis are given. The Madelung Part of Lattice Energy, MAPLE, Effective Coordination Numbers, ECoN, these via Mean Effective Ionic Radii, MEFIR, are calculated.  相似文献   

5.
On the Constitution of ‘KPbO2’ Transparent, orangered single crystals of K2Pb2O4 have been obtained by heating mixtures of K2O2 and PbO (K:Pb = 1:1) [Ag-cylinders, 560°C, 40 d, after cooling (15°C/h)]. The space group is P1 , a = 1295.94(9), b = 753.35(7), c = 697.12(8) pm, α = 118.00(1)°, β = 106.15(1)°, γ = 93.44(1)°, Z = 4, dx = 6.573 und dpyk = 6.54 g · cm3. The structure is characterized by rutilanalogous chains of edge-connected [PbO6] octahedra along [001] according to [PbO4/2O2/1] = PbO4. On both sides of such a chain there are respectively three O2?, which belong to two octahedra, alternating capped with Pb2+ or not capped, corresponding to [PbO4]Pb2[PbO4]□2… = Pb2O4. Those capped chains are held together by K(1)…K(4), each of them with C.N. 6. The order of the chains corresponds to the motive of a closest packing. 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   

6.
The First Oxoplumdat(II) with Island Structure: K4[PbO3] For the first time K4PbO3 has been prepared as colourless powder and transparent single crystals, respectively. K4PbO3 crystalizes orthorhombic, space group Pbca-D, a = 6.543, b = 11.405, c = 18.709 Å, Z = 8. d = 3.99, dpyk = 3.98. For 1040 independent reflextions we find R = 9.6%. Parameters see text. There are isolated PbO3 groups, with symmetry approximately C3v, which are ordered in a very complicated manner and connected by K+ ions forming layers. The Madelung Part of the Lattice Energy, MAPLE, and Effectiv Coordination Numbers, ECoN, these by means of Mean Fiktive Ionic Radii, MEFIR, are calculated and discussed.  相似文献   

7.
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   

8.
On the Structure of Li8PbO6 For the first time single crystals of Li8PbO6 have been prepared by heating of mixtures of Na2PbO3 and Li2O [Ag-cylinders, 650°C, 150 d]. The structure [382 I0(hkl), four circle diffractometer PW 1100, ω/2Θ-scan, MoKα, R = 3.07%, Rw = 3.00%, space group R3 ; a = 555.09(4), c = 1564.13(17) pm, Dx = 4.28 g · cm?3, Dpyk = 4.24 g · cm?3, Z = 3] is characterized by the motive of a hexagonal-closed O2? packing. Half of the octahedral sites are occupied by Pb4+ and Li+ and half of the tetrahedral sites only by Li+. The Madelung Part of Lattice Energy, MAPLE, and the Effective Coordination Numbers, ECoN, these via Mean Fictive Ionic Radii, MEFIR, are calculated.  相似文献   

9.
On Oxopalladates of Alkali Metals According to X-ray data of single crystals there are: Na2PdO2 (yellow rod-shaped crystals) orthorhombic, a = 3.077, b = 10.359, c = 8.351 Å, Z = 4; dx = 4.60, dpyk = 4.63 g · cm?3. ?K2PdO3”? (black square prism) orthorhombic, a = 6.202, b = 9.219, c = 4× 11.372 = 45.48 Å, Z = 24, dx = 3.60, dpyk = 3.50 g · cm?3, and ?K6PdO4”? (orange square prism) orthorhombic (pseudotetragonal), a = b = 12.368, c = 13.593 Å, Z = 8, D24—P212121. ?Rb2PdO3”? (black) is isostructural (Guinier data) to ?K2PdO3”?, a = 7.354, b = 9.605, c = 11.586 Å, dx = 4.58, dpyk = 4.47 g · cm?3. Na2PdO3 exists in another reddish brown form, isostructural to Li2MnO3 (C2h6—C2/c), a = 5.374, b = 9.309, c = 10.789 Å, β = 99.5°, Z = 8, dx = 5.00, dpyk = 4.73 g · cm?3.  相似文献   

10.
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, d = 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   

11.
On Quaternary Oxotungstates (VI). Na6Li2[W2O10] — a Ditungstate For the first time, Na6Li2[W2O10] has been prepared by annealing mixtures of WO3, Na2O and Li2O with W:Na:Li = 1:3:1 [closed Pt-tube in quartz-glass ampoule, 840°C, 60 d (single crystals)]. The colourless crystals are of squatted shape. The structure determination [1813/I0(h kl), four-cycle diffractometer PW 1100 (Fa. Philips), ω-scan, AgKα, R = 8.32%, absorption not considered] confirms the space group P1 with a = 784.66(11), b = 602.53(7) c, = 563.81(11) pm α = 106.784(14)°, β = 114.548(14)°, γ = 91.082(13)°, Z = 2, dx = 4.92 g · cm?3, dpyk = 4.85 g · cm?3. The structure may be described as a distorted derivative of the NaCl-type. 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   

12.
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   

13.
New Oxoplumbates(II) A2PbO2 (A = K, Rb, Cs), with Binuclear Groups [OPbO2PbO] Unknown K2PbO2, Rb2PbO2 and Cs2PbO2 (yellowish powder, yellowish transparent single crystals, respectively) have been prepared, The compounds crystallize triclinic with a = 10.901 Å, b = 7.606 Å, c = 7.328 Å, α = 119.35°, β = 88.42°, γ =117,73°, (K2PbO2); a = 10.907 Å, b = 8.510 Å, c = 7.815 Å, α = 124.00°, β = 84.97°, γ = 120.68° (Rb2PbO2) and a = 11.644 Å, b = 8.905 Å, c = 8.040 Å, α = 123.32°, β = 85.70°, γ = 120.49° Z = 4, space group P1 -C/i1. For K2PbO2 we find R = 8.65% and Rw = 9.32% (2283 independent reflections). Parameters see text. There are isolated [Pb2O4]groups, which are connected in a complicated way by mutual K+ ions forming layers. The Madelung Part of the Lattice Energy, MAPLE, and Effective Coordination Numbers, ECoN, these by means of mean Fictive Ionic Radii, MEFIR, are calculated and discussed.  相似文献   

14.
Rb2TiO3, a New Oxotitanate with Coordination Number 4 Rb2TiO3 cristallizes according to single crystal datas [544 Okl? 4kl, Mo? Kα] orthorhombic, a = 6.015, b = 11.936, c = 13.366 Å, Z = 8, space group D? Cmca, d = 3.69, dpyk = 3.65 g cm?3; for occupied positions and atomic parameters see text. Surprisingly the coordination number of Ti to 0 turns out to be 4. The chains [TiO1/1O1/1O2/2] are placed along [100]. The Madelung part of lattice energy (MAPLE) of Rb2TiO3 is calculated and discussed. In order to display the characteristics of the structure, further MAPLE-calculations have been carried out. K2TiO3 belongs to the Cs2PbO3-Family of structure with C.N. 5 of Ti to 0. Cs2TiO3 and Rb2TiO3 are not isotypic.  相似文献   

15.
On Mixed-valent Oxoplumbates. On Rb2Pb4O7 = Rb2Pb Pb O7 For the first time, Rb2Pb4O7 has been prepared by annealing mixtures of Rb2O3 and PbO with Rb:Pb = 1:2 [Ag-cylinders, sealed under vacuum in Duran-glass ampoule, 450°C, 30 d (single crystals)]. The rubin red single crystals are of longish [001] shape. The structure determination [5162 symmetry independent hkl, four-circle-diffractometer CAD 4 (Fa. Enraf-Nonius), ω-2Θ—scan, AgKα, ψ-scan absorption correction, R = 7.54%, RW = 7.71%] confirms the space group P1 with a = 1036.00(10), b = 733.72(8), c = 663.54(10) pm, α = 90.049(12)°, β = 99.236(12)°, γ = 101.641(12)°, Z = 2, d = 7,58 g · cm?3, dpyk = 7,55 g · cm?3. The structure is characterized by a layer-lattice. The coordination number is three for Pb2+, six for Pb4+. The Madelung Part of Lattice Energy, MAPLE, Effective Coordination Numbers, ECoN, these via Mean Effective Ionic Radii, MEFIR, are calculated.  相似文献   

16.
A New Cobaltate with Isolated Anion Structure: Li6[CoO4] For the first time transparent, blue single crystals of Li6[CoO4] have been prepared (Li2O/Na2O/?CoO”? (Li:Na:Co = 1.3:1.3:1), Co-tube, 580°C, 22 d). Corresponding to Li6□CoO; it is an ordered variant of the Li2O-type of structure: P42/nmc; a = 653.6(1) pm, c = 465.4(1) pm; Z = 2; dx = 2.75 g cm?3, dpyk = 2.71 g cm?3 (4-circle-diffractometer-data (PW 1100), AgKα; 230 from 936 I0(hkl); R = 9.58%, RW = 5.25%). Parameters see text. The Madelung Part of Lattice Energy, MAPLE, and Effective Coordination Numbers, ECoN, these via Mean Fictive Ionic Radii, MEFIR, are calculated and discussed. The magnetic properties are measured in the temperature range of 14–297 K.  相似文献   

17.
The First Mixed-valent Oxoplumbate with Isolated Anions. On KNa7[PbIVO4][PbIIO3] For the first time KNa7Pb2O7 has been prepared by reaction of K and Na Oxides with ?PbO2”? rsp. PbOred [e. g.: KO0.48:NaO0.36:?PbO2”? = 1:7:2 (Ag-cylinders, reduced Ar-pressure, sealed in supremax-glas ampoules, 600°C, 14 d): redorange single crystals of plated shape]. The structure determination [3269 Io(hkl), four-circle diffractometer PW 1100 (Fa. Philips), ω-scan, MoKα, R = 9.52%, Rw = 7.67%, absorption not considered] proves the space group P21/c with a = 1758.48(10), b = 596.76(3), c = 1066.46(8) pm, β = 90.682(8)°, Z = 4, dx = 4.311, dpyk = 4.28 g/cm3. The structure is characterized by isolated [PbIVO4] (symmetry nearly Td) and [PbIIO3] groups (symmetry nearly C3v), the latter connected by cations to double-layers. 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   

18.
Oxides of a New Type of Formula: On the Knowledge of K3Ni2O4 and K3Pt2O4 K3Ni3O4, greyblack single crystals, obtained by heating K2O and NaNiO2 [K:Ni = 2:1, 500°C, 7d, Ag-cylinders], crystallizes orthorhombic with a = 6.044, b = 9.049, c = 10.567 Å, Z = 4, space group Cmcm (d = 3.43, dpyk = 3.32 g · cm?3). Due to four cycle diffractometer data (374 hkl, MoKα, R = 8.6percnt;) a new type of structure is found with wavebands of [NiO4/2] \documentclass{article}\pagestyle{empty}\begin{document}$ \mathop {\rm N}\limits^{\rm 1} $\end{document} exhibits the C.N. 6, \documentclass{article}\pagestyle{empty}\begin{document}$ \mathop {\rm N}\limits^{\rm 2} $\end{document} the C.N. 4. Effective Coordination Numbers, ECoN, calculated by means of Mean Fictive Ionic Radii, MEFIR, the Madelung Part of Lattice Energy, MAPLE and the magnetic properties are discussed. K3Pt2O4, black single crystals with metallic lustre, obtained by heating KOx (x = 1.55 or 1.88) and Pt (powder) [K:Pt = 4:1,1000°C, lh, 600°C, 2d, Pt-capsules] is isotypic to K3Ni2O4 (four cycle diffractometer data: 458 hkl, MoKα, R = 12percnt;). Cellparameters are a = 6.15, b = 9.27, c = 11.51 Å (single crystal data), d = 5.79 and dpyk = 5.77 g · cm?3.  相似文献   

19.
Quaternary Monoborates of Alkali Metals: Na4Li5[BO3]3 We prepared hitherto unknown Na4Li5[BO3]3 in the shape of monoclinic, colourless-transparent and prismatic single crystals [a = 1238.8(5) pm, b = 729.6(3) pm, c = 973.8(3) pm, β = 107,29(4)°, Z = 4, dx = 2,397 g/cm3, dpyk = 2,37 g/cm3]. The crystal structure was solved by four-circle-diffractometer [PW 1100, MoKα , R = 9,02%, Rw = 5,29%, 1221 I0(hkl)]I0(hkl)]. Na4Li5[BO3]3 is sensitive against atmospheric moisture; hydrolysis takes place within 60 minutes. Effective Coordination numbers, ECoN, these via Mean Fictive Ionic Radii, MEFIR, and the Madelung Part of Lattice Energy, MAPLE, are calculated and discussed.  相似文献   

20.
On oxocadmates: The crystal structure of K2CdO2 According to single crystal data [438 hk0 — hk4; Mo — Kα] K2CdO2 crystallizes orthorhombic, space group No. 60, Pbcn — D, with a = 10.089, b = 6.186, c = 6.152 Å, Z = 4; d = 3.85 g · cm?3, dpyk = 3.61 g · cm?3 (for parameters see text). Though the space group is different from that of K2ZnO2, the similarities of the two crystal structures are unmistakable. The Madelung part of lattice energy is calculated and discussed.  相似文献   

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