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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.
Cs4[IrO4], a New Iridate with Planar Anion [IrO4]4? For the first time we obtained black single crystals of Cs4[IrO4] by heating intimate mixtures of CsO0.52 and IrO2 (molar ratio Cs : Ir = 4.30 : 1.00; “Ag-bomb”, 740°C/86 d). Cs4[IrO4] crystallizes monocline, C 2/m, with a = 1031.66(8) pm, b = 671.61(4) pm, c = 660.44(6) pm, b? = 108.118(7)° and Z = 2 in the K4[IrO4]-type. The structure has been determined by four-circle-diffractometer data (PW 1100 from Phillips, Ag? Kα , graphite) with 841 I0(hkl) with I ≥ 3s?(F) (from 947 I0(hkl) out of 3529 measured reflexes). 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
3.
Novel meander with Co3+ und Au3+: Na4[AuCoO5] = Na8 1∞ [(O2/2 (CoO)O2AuO2/2)2] By “reaction with the wall” we obtained for the first time transparent brown single crystals of Na4[AuCoO5] while heating intimate mixtures of Co3O4, Na2O2, and K2O2 (Co: Na: K = 1.00:4.91:2.20; 650°C/44d) in a sealed gold-tube: monoclinic, P21/m, with a = 555.69(4) pm, b = 1042.11 (8) pm, c = 555.69(4) pm, β = 117.387(5)°, Z = 2. Characteristic features of Na4[AuCoO5] are meandric chains [(O2/2 (CoO)O2AuO2/2)2]. The structure has been determined by four-circle diffractometer data (Siemens AED 2; Mo? Kα , graphite, 881 I0(hkl), R = 0.0366, Rw = 0.0316), parameters as given in the text. The Madelung Part of Lattice Energy, MAPLE, Effective Coordination Numbers, these via Mean Fictive Ionic Radii, and Charge-distribution, CHARDI, are calculated and discussed. 相似文献
4.
A New Oxoiridate(V): KLi6[IrO6] Hitherto unknown Kli6[IrO6] has been prepared by completely pulverized mixtures of K4[IrO4] and Li2O (closed silver cylinder, 30 d, 750°C). The deep dark red single crystals are trigonal-rhombohedral, space group R3 m, a = 819.61(8) pm, c = 709.96(11) pm, Z = 3. It is a “stuffed” variant of the α-Li6[UO6]-type; four-circle diffractometer data (PW 1100), R = 1.44% and Rw = 1.41% for 220 I0(h kl), MoKα. The Madelung Part of Lattice Energy, MAPLE, and Effective Coordination Numbers, ECoN, the latter derived from mean Fictive Ionic Radii, MEFIR, are calculated and discussed. 相似文献
5.
New Tetrapnictidotitanates(IV): Na3M3[TiX4] with M ? Na/Sr, Na/Eu and X ? P, As The four novel tetrapnictidotitanates(IV) Na4Sr2TiP4, Na4Sr2TiAs4, Na4.3Eu1.7TiP4 and Na4.3Eu1.7TiAs4 were prepared from the binary pnictides NaX, M3X, M′X (X ? P, As and M′ ? Sr, Eu) and elementary titanium in tantalum ampoules. The air and moisture sensitive transition metal compounds form dark red hexagonal crystals. They are semiconductors with Eg = 1.8eV (Sr) and Eg = 1.3eV (Eu), respectively. The compounds are isotypic with Na6ZnO4 (space group P63mc (no. 186); hP22; Z = 2; Na4Sr2TiP4; a = 936.8(1) pm, c = 740.5(1) pm; Na4Sr2TiAs4: a = 958.2(1) pm, c = 757.1(1) pm; Na4.3Eu1.7TiP4: a = 929.9(2) pm, c = 732.0(2) pm; Na4.3Eu1.7TiAs4: a = 953.9(1) pm, c = 749.5(1) pm). Main structural units are polar oriented [TiP4]8? and [TiAs4]8? tetrahedral anions with d (Ti? P) = 240.2(3) pm and d (Ti? As) = 248.6(3) pm. 相似文献
6.
Na4[PbO4] — Preparation of new Plumbates(IV) by Oxidizing Intermetallic Phases By oxidizing NaPb with Na2O2 (molar ratio Na2O2:NaPb = 2.04:1; Ag-tubes; 600°C/50d) we obtained for the first time small orange coloured single crystals of Na4[PbO4]: Na4[SiO4]-type [2], P? 1 (I.T. No. 2) with a = 898.5(3); b = 675.6(3); c = 592.2(2) pm; α = 124.75(1)°; β = 96.75(1)°; γ = 100.18(2)°; Z = 2; (four circle diffractometer data (MoK; 3 251 Io(hkl); R = 3.4%; Rw = 3.0%), parameters see text. Furthermore the Madelung part of lattice energy (MAPLE), effective coordination numbers (ECoN), mean fictive ionic radii (MEFIR) and the charge distribution (CHARDI) are being calculated. 相似文献
7.
The First Oxocobaltate(II) with Dinuclear Anion: Rb2Na4[Co2O5] and K2Na4[Co2O5] By heating of well ground mixtures of the binary oxides [A2O, Na2O, ?CoO”?, A:Na:Co = 1.00:2.00:1, (A = K, Rb); Ag-tube, 600°C, 14 d] we obtained Rb2Na4[Co2O5] and K2Na4[Co2O5] rough, transparent, red single crystals. We find a new type of structure with the anion [O2CoOCoO2]6?. Space group P42/mnm; a = 634.4 pm, c = 1030.3 pm, Z = 2 (A = K) a = 647.6 pm, c = 1021.1 pm, Z = 2 (A = Rb); four-circle diffractometer data; MoKα -radiation; 360 from 364 I0(hkl), R = 4.34%, Rw = 3.54% (A = K); 361 from 366 I0(hkl), R = 6.54%, Rw = 2.70% (A = Rb). The anion is planar, the CN of Co is 3. The Madelung Part of Lattice Energy, MAPLE, and Effective Coordination Numbers, ECoN, are calculated and discussed. 相似文献
8.
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
9.
The First Titanate with ?Stuffed Pyrgoms”?: RbNa3Li12[TiO4]4 = RbNa3Li8{Li[TiO4]}4 By heating a well grounded mixture of the binary oxides Rb2O, Na2O, Li2O, and TiO2 [Rb:Na:Li:Ti = 1.1:3.1:12.5:4.0; 780°C, 41 d] we obtained RbNa3Li8{Li[TiO4]}4 as colourless platelike crystals. This first titanate with ?stuffed pyrgoms”? is isostructural with RbNa3Li8{Li[SiO4]}4, CsKNa2Li8{Li[SiO4]}4 and CsKNaLi9{Li[SiO4]}4 [2]. The compound crystallizes tetragonal I4/m with a = 1 125.8(1) pm and c = 652.4(1) pm (Guinier-Simon-Data, Z = 2). The structure was determined by four-cyrcle-data (Siemens AED2, MoK) and leds to the residual values R = 3.7% and Rw = 3.1% (additional data see text). The Madelung Part of Lattice Energy (MAPLE), Effective Coordination Numbers (ECoN), Mean Fictive Ionic Raddii (MEFIR) and the Charge Distribution in Solids (CHARDI) are calculated and discussed. 相似文献
10.
On Oxoosmates(VII). Na5[OsO6] and Li5[OsO6] For the first time bluish black single crystals of Na5[OsO6] have been prepared. The structure was determined according to four-circle-diffractometer data. According to powder samples Li5[OsO6] is isotypic to Na5[OsO6]. Both are of the NaCl-type like Na5[ReO6] (space-group C2/m (No. 12, I.T.), Z = 2): Na5[OsO6]: a = 568.10(4), b = 975.00(6), c = 559.65(5) pm, β = 111.00° (1), 436 hkl, 4° ? Θ ? 30°, MoK, R = 2.7%, RW = 2.6%. Li5[OsO6]: a = 568.10(4), b =975.00(6), c = 559,65(5) pm, β = 111.00° (1). Effective Coordination Numbers, ECoN, and the Madelung Part of Lattice Energy, MAPLE, are calculated and discussed. 相似文献
11.
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
12.
The First Basic Oxoindate: Na26O3[InO4]4 For the first time Na26O3[InO4]4 was obtained by annealing intimate mixtures of Na2O, CdO and elemental In (molar ratio 3.5:1.0:2.0) in closed Ni-cylinders (30 days, 600°C) in form of yellow single crystals. The structure determination by four circle diffractometer data (MoKα, 921 out of 921 Io(hkl), R = 2.53, Rw = 2.18%) confirms the space group 143d (cubic) with a = 1 427.37 pm and Z = 4. All kation are surrounded by tetrahedron of O2?. In3+ is coordinated with O(1) and O(2) (without O(3)) only. There are ?isolated”? [InO4]-tetrahedra. The Madelung Part of Lattice Energy, MAPLE, the Mean Fictive Ionic Radii, MEFIR, Effective Coordination Numbers, ECoN, and Charge Distribution, CHARDI, are calculated. 相似文献
13.
During the reaction of Na2[WO4] with YF3 purposed to yield fluoride‐derivatized yttrium oxotungstates(VI), colourless platelet‐shaped single crystals of Na3F[WO4] emerged as main product. The title compound crystallizes orthorhombically in the space group Pnma (a = 559.59(5), b = 751.02(7), c = 1285.98(9) pm) with four formula units per unit cell. Besides isolated ortho‐oxotungstate units [WO4]2? (d(W–O) = 176–178 pm) the crystal structure contains two crystallographically independent Na+ cations which are both octahedrally coordinated by four oxygen atoms and two fluoride anions. The F? anions are surrounded by six sodium cations (d(F–Na) = 224–242 pm) also in an octahedral fashion. These octahedra built up chains along [100] by sharing trans‐oriented faces according to , which are stacked according to a hexagonal closest rod‐packing. The cationic strands are surrounded, interconnected and charge‐balanced by isolated [WO4]2? tetrahedra with almost ideal shape and every O2? ligand is terminally coordinated by three Na+ cations. 相似文献
14.
On Quaternary Oxoplumbates(IV). On Rb3NaPbO4 For the first time, Rb3NaPbO4 has been prepared by annealing mixtures of Na2PbO3 and RbO0.84 with Rb:Na:Pb = 4:2:1 [nonhermetic Ag-cylinders, sealed under vacuum in Duran-glass ampoule, 480°C, 180 d (single crystals)]. The colourless crystals are of squatted shape. The structure determination [2943 symmetry independent hkl, four-circle-diffractometer PW 1100 (Fa. Philips), ω-2Θ-scan, AgKα, R = 8.64%, RW = 6.59%, absorption not considered] confirms the space group P21/c with a = 1101.79(26), b = 662.66(11), c = 1115.01(30) pm, β 112.027(21)°. The structure is characterized by isolated [PbO4]-tetrahedra and [Na2O6]-tetrahedra-doubletts, C.N. 5 and 7 for Rb+. The Madelung Part of Lattice Energy, MAPLE, Effective Coordination Numbers, ECoN, these via Mean Effective Ionic Radii, MEFIR, are calculated. 相似文献
15.
On Oxostannates(II). V. Na4[SnO3] – The First Oxostannate (II) with Island Structure The new oxid Na4SnO3 (yellow, transparant single crystals) has been prepared by heating of mixtures of: 1. NaO0.45 and SnO (Na:Sn2+ = 4.1:1; Ag-cylinders; 600–730°C, 7–66 d); 2. NaO0.45′ SnO2 and Sn±0 (Na:Sn4+:Sn±0 = 8.2:1:1; Ag-cylinders; 650–680°C, 2–66 d); 3. NaO0.45′ Na2SnO3 and Sn±0 (Na:Na2SnO3:Sn±0 = 6.1:1:1; Ag-cylinders; 650–670°C, 5 d). Na4SnO3:804 I0(hkl); four circle diffractometer PW 1100; ω-scan; MoKα; R = 5.14%; Rw = 4.64%; monoclin, Cc? C; a = 582.77(11), b = 1667.44(24), c = 589.42(10) pm, β = 110.187(13)°; dx = 3.20 g/cm3; dpyk = 3.19 g/cm3; Z = 4; parameter look for text. It is a NaCl-variant with systemathical blanks of the anion part and “isolated” groups of [SnO3]. \documentclass{article}\pagestyle{empty}\begin{document}$ {\rm N}\mathop {\rm a}\limits^{\rm 1} $\end{document} has the uncommon coordination number 2. The Effective Coordination Numbers, ECoN, the Mean Fictive Ionic Radii, MEFIR, and the Madelung Part of Lattice Energy, MAPLE, are calculated. The structure is described using ?Erweiterte Schlegeldiagramme”?. 相似文献
16.
On Na4(CrO4) Dark-green single crystals of Na4[CrO4] were obtained for the first time. (Na2O/Cr2O3; Na:Cr = 4:1 not exactly closed Ni-tube; 1000°C; 30 d). It is isostructural to Na4(CoO4); space group P1 , a = 859.7 pm, b = 569.8 pm, c = 640 pm, α = 124°C, β = 98.4°, γ = 98.9°, 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
17.
Michael Ruck 《无机化学与普通化学杂志》1997,623(10):1583-1590
Bi4RuBr2 and Bi4RuI2: Two Varieties of a Column Structure with Face-Sharing [RuBi8/2] Square Antiprisms Reaction of the elements yields black, lustrous, air insensitive crystals of the subhalides Bi4RuI2 (tetragonal, I4/m, a = 1183.9(2) pm, c = 669.7(2) pm, V = 938.66 · 106 pm3) and Bi4RuBr2 (monoclinic, I112/m, a = 1211.9(2) pm, b = 1072.6(2) pm, c = 663.9(2) pm, γ = 91.63(1)°, V = 862.64 · 106 pm3). The structures of the homöotypic compounds contain [RuBi8/2] strands of face-sharing square antiprisms. Halogen atoms lie above the edges of alternate Bi4 squares. Thereby chemical bonding differs significantly within the two types of Bi4 squares. Though the Ru atoms on the central axis of the strand of antiprisms form pairs, extended Hückel calculations give no evidence of Ru? Ru bonds. 相似文献
18.
A New Perowskite with Deficiencies in the Oxygen Part: Ba4[Na2W2O11] For the first time colourless single crystals of Ba2NaWO5.5 were prepared by reaction of Na4WO5 [2] and ?BaO2”? [Ba:Na:W = 4:4:1, Ni-cylinder, 725°C, 35 d]. Single crystal data [432 of 505 I0 (hkl), Four-circle-diffractometer Siemens AED2, MoKα , R = 6.1%, Rw = 5,6%] verify the space group P mmm with a = 579.16(8), b = 580.85(8), c = 859.4(1) pm, Z = 1. The structure is based upon the CaTiO3-type of structure. Ba2+ take the place of Ca2+ meanwhile Ti4+ is substituted alternately by W6+ and Na+. Complete occupation of all lattice positions would lead to a deficite of positive charge. This is compensate by deficiencies in the oxygen part of the lattice. Related to [Na(1)1Na(2)1W(1)1W(2)1O(1)4O(2)2O(3)2O(4)3] these deficiencies are statistically distributed on O(4). Structural relations are deduced by Schlegel-Diagrams. The Madelung Part of Lattice Energie, MAPLE, Effektive Coordination Numbers, ECoN, these via Mean Fictive Ionic Radii, MEFIR, are calculated and discussed. 相似文献
19.
A New Nesoindate: KNa9In2O8 = KNa9[InO4]2 We prepared hitherto unknown KNa9[InO4]2 (colourless, transparent single crystals) from NaIn, Na2O2, and ?K2O2”? (molar ratio NaIn:Na2O2:?K2O2”? = 2:3.5:0.6, Ag-cylinder, 460°C, 6d). A new type of structure is found. The single crystal data are: Pnma, a = 1802.4(3), b = 729.5(2), c = 907.9(3) pm; Z = 4 [four-circle diffractometer PW 1100, MoKα; 1856 out of 1870 I0(hkl); R = 3.7% and Rw = 3.4%]. The Madelung Part of Lattice Energy, MAPLE, is calculated and discussed. 相似文献
20.
The Layer Structure of Tl[CuAsO4] and Tl[CuPO4] with Layers of Thallium(I) with Stereoactive Lone Pair Single crystals of Tl[CuAsO4] and Tl[CuPO4] were prepared by reaction of oxygen with Tl/Cu/As and Tl/Cu/P alloys, respectively. The new isotypic compounds crystallize in spacegroup C2/c with Z = 8 and lattice constants a = 684.70(7) pm, b = 712.64(5) pm, c = 1822.4(2) pm, β = 92.76(1)° for Tl[CuAsO4] and a = 671.57(8) pm, b = 697.09(6) pm, c = 1789.1(2) pm, β = 93.12(1)° for Tl[CuPO4]. Square planar [CuO4]-units are connected by common corners to form undulated [CuO3]2-chains running along [010]. Interconnection of the chains by arsenate or phosphate groups results in the formation of anionic cuprate-arsenate- and cuprate-phosphate-slabs, respectively. Along [001] these slabs are alternating with double layers of thallium(I) ions in which the stereochemical activity of the Tl+ lone pair is apparent from an hemispheric coordination of thallium by oxygen. The structure is related to that of the orthorhombic form of KCuPO4. 相似文献