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1.
The new lithium nitridotantalate(V), Li4[TaN3], was prepared by reaction of Li15[CrN4]2N with the wall of a welded Ta ampoule in the presence of metallic Li at 1470 K. Li4[TaN3] forms colourless single crystals (platelets, space group Ibca, No. 73, a = 491.85(4) pm, b = 973.59(6) pm, c = 1415.0(1) pm, Z = 8, R1 = 0.0288). The crystal structure is described as Li2O superstructure with ordered occupation of the tetrahedral sites by Li and Ta. The resulting arrangement leads to infinite chains [TaN2N2/24—] running along [100].  相似文献   

2.
New Alkali Oxoarsenates(V): NaLi2[AsO4] — A New Type of Formula [1] . By heating of well ground mixtures of the binary oxides As2O3, Na2O, and Li2O2, molar ratio As:Na:Li = 1.0:1.0:2.0, in a well closed Ni tube (650°C, 21 d) colourless single crystals of NaLi2[AsO4] were obtained for the first time. The new orthoarsenate(V) crystallizes orthorhombic (space group P mn21-C, No. 31) with Z = 2. The structure determination showed that it is isostructural to βII-Li3[VO4] and that means the Li3[PO4]-type. The lattice constants a = 702.9(2) pm, b = 520.5(1) pm, c = 505.4(2) pm were taken from Guinier-Simon powder data. The structure was determined by four-circle diffractometer data [Philips PW 1 100, AgKα , 679 independent out of 2 373 Io(hkl), R = 3.03%, Rw = 2.29%; parameter see text]. The Madelung Part of Lattice Energy, MAPLE, and Effective Coordination Numbers, ECoN, these calculated via Mean Fictive Ionic Radii, MEFIR, are calculated and discussed.  相似文献   

3.
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   

4.
The formation of ternary nitridometalates from the elements in the case of the systems Li—Cr, V, Mn—N leads to compounds which contain the transition metals in the highest (VV, CrVI) or a comparably high (MnV) oxidation state. In the corresponding calcium and strontium systems, the transition metals show a lower oxidation state (VIII, CrIII, MnIII). Transition metals with intermediate oxidation states (CrV, MnIV) are present in the quaternary (mixed cation) compounds Li4Sr2[CrN6], Li6Ca2[MnN6], and Li6Sr2[MnN6] (R3¯(#148), a = 585.9(3) pm, c = 1908.6(4) pm, Z = 3), as well as in the solid solution series Li6(Ca1—xSrx)2[MnN6].  相似文献   

5.
The New Orthotitanate CsNa3[TiO4] Colourless, square stonelike single crystals of CsNa3[TiO4] [1], isostructural with CsNa3[PbO4] [2], are obtained by heating a well grounded mixture of the binary oxides CsO0,56, NaO0,52 and TiO2 (Cs : Na : Ti = 1,1:3,1:1,0) in Nitubes (9d, 400°C). The structure determination by using four-circle diffactometer data (Siemens AED2, 5541 Io(hkl), MoK) leads to the residual-values R = 8.8% and Rw = 4.7%. Lattice constants (triclinic, Cmca, P1 , Z = 4, four-circle diffactometer data, MoK: a = 1161.2(6) pm, b = 854.9(3) pm, c = 651.1(3) pm, α = 100.52(2)°, β = 108.84(3)°, γ = 91.61(3)°; additional data see text). The Madelung Part of Lattice Energy (MAPLE), Effective Coordination Numbers (ECoN), Mean Fictive Ionic Radii (MEFIR) and the Charge Distribution in Solids (CHARDI) are calculated and discussed.  相似文献   

6.
On the Crystal Structure of Ba2ZnO3 Single crystals of Ba2ZnO3 were prepared by solid state reaction. It crystallizes monoclinic: space group C ? C12/c1; a = 5.833; b = 11.376; c = 12.585 Å; β = 93.63°; Z = 8. The crystal structure is characterised by [ZnO3] chains along [100]. They are connected by Ba2+ in seven fold oxygen coordination.  相似文献   

7.
Ba[CoN]: A Low-Valency Nitridocobaltate with Angled Chains [CoN2/22?] Ba[CoN] is prepared by reaction of barium and cobalt (molar ratio Ba : Co = 1 : 2.5) in tantalum crucibles at 870°C with flowing nitrogen (1 atm) within a period of 96 h. After cooling down to room temperature (24°C/h) black single crystals of the ternary phase with a platy habit are obtained (orthorhombic, Pnma; a = 959.9(2) pm, b = 2 351.0(3) pm, c = 547.6(2) pm; Z = 20). The crystal structure of Ba[CoN] contains angled (planar) chains [CoN2/22?] which run along the [010]-direction (N? Co? N[°]: 178.5(5), 179.6(6), 180.0; Co? N? Co[°]: 82.9(6), 84.2(5), 177.1(8); Co? N[pm]: 174.6(12), 177.2(12), 181.9(13), 184.3(13), 187.1(12)). Nitrogen is in an octahedral coordination (N Ba4Co2) and is arranged in a distorted cubic close packing. Barium occupies one half of the tetrahedral holes (Ba? N[pm]: 274.8(16) ? 308.2(12)). The cis-positions of the Co-atoms at the nitrogen coordination-octahedra cause short Co? Co contacts within the chains [CoN2/22?]. Through this, Co2-units (Co? Co[pm]: 247.8(4); bridged by nitrogen) and linear Co3-groups (Co? Co [pm]: 245.5(2); Co? Co? Co[°]: 180.0; bridged by nitrogen) alternate along the chains. The crystal structure of Ba[CoN] is closely related to the Ba[NiN] type structure.  相似文献   

8.
Dibromomethylsulfoniumsalts — Preparation and Crystal Structure The salts CH3SBrA? (A? = SbCl, AsF) were prepared by various routes and characterized by their Ramanspectra. CH3SBrAsF crystallized in the monoclinic space group P21/c with a = 770,5(4) pm, b = 942,4(12) pm, c = 1329,3(14) pm, β = 100,28(6)°, Z = 4. Distances and bond angles in the cation are as expected.  相似文献   

9.
Synthesis and Structure of MII[AuF4]2 (MII ? Cd, Hg) Cd[AuF4]2 and the isotypic compound Hg[AuF4]2, both are yellow, crystallize tetragonal in the space-group P4/mcc-D (No. 124) with a = 575.0/575.6 pm, c = 1034.8/1042.3 pm and Z = 2. The single-crystals were obtained by solid-state reactions in goldtubes.  相似文献   

10.
Tetraammine Lithium Cations Stabilizing Phenylsubstituted Zintl-Anions: The Compound [Li(NH3)4]2[Sn2Ph4] Ruby-red, brittle single crystals of [Li(NH3)4]2[Sn2Ph4] were synthesized by the reaction of diphenyltin dichloride and metallic lithium in liquid ammonia at ?35°C. The structure was determined from X-ray singlecrystal diffractometer data: Space group, P1 , Z = 1, a = 9.462(2) Å, b = 9.727(2) Å, c = 11.232(2) Å, α = 66.22(3)°, β = 85.78(3)°, γ = 61.83(3)°, R1 (F ? 4σF) = 5.13%, wR2 (F02 ? 4σF) = 10.5%, N(F ? 4σF) = 779, N(Var.) = 163. The compound contains to Sb2Ph4 isosteric centres [Sn2Ph4]2? as anions which are connected to rods by lithium cations in distorted tetrahedral coordination by ammonia. These rods are arranged parallel to one another in the b,c-plane, but stacked along [100].  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, 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   

12.
From the study of the hypothetical series Pb[PbInc–2pSbc]O6+p (O ? p < 1; 0 ? c < 2), the existence of the cubic pyrochlore Pb2II[In0.5Sb1.5]O6.5 has been established. This compound was obtained as an orange yellow powder, S.G. Fd4 m (No. 227), Z = 8, a = 10.5892(1) Å, V = 1187.38(3) Å3, Dc = 8.48 M gm?3. For Pb in 16(c) positions, In and Sb (1:3) randomly distributed in 16(d), oxygen atoms in 48(f) and in a half of the 8(a) sites, and oxygen positional parameter x = 0.429 (origin at center, 3 m), R = 0.062. The apparent interatomic distances (Å) are determined: Pb? O = 2.612; (In, Sb)? O = 2.019.  相似文献   

13.
On the Oxidation of Intermetallic Phases: The Oxoplumbates(II) K6[Pb2O5] [1] and K4[PbO3] [2] Very pale yellow crystals of K6[Pb2O5] were obtained by heating a wellground mixture of LiPb und K2O2 (K2O2: LiPb = 2.5:1) in Ag-tubes (550°C; 40 d). The crystal structure, triclinic, space group P1 , a = 1 326.7(6); b = 758.8(4); c = 637.0(3) pm; α = 92.17(3)°; β = 94.41(3)°; γ = 112.85(4)°; Z = 2 was determined (four-circle diffractometer data, Mo? K, 3 270 Io(hkl), R = 8.0%, Rw = 3.5%, parameters see text). The pale yellow crystals of K4[PbO3] were received by heating KPb and K2O2 (K2O2: KPb = 3.3:2) in Ni-tubes (450°C; 17 d). The crystal structure (orthorhombic, space group Pbca with a = 658.2(1); b = 1 131.8(4); c = 1 872.2(6) pm; Z = 8) was refined (four-circle diffractometer data, Mo? K, 2 003 Io(hkl), R = 4.9%, Rw = 2.8%). The Madelung Part of Lattice Energy (MAPLE), Effective Coordination Numbers (ECoN), the Mean Fictive Ionic Radii (MEFIR) and the Charge Distribution (CHARDI) are being calculated for both oxides.  相似文献   

14.
The blue mixed-crystal title compound Na15[MoMoO462H14 (H2O)70]0.5[MoMoO457H14 · (H2O)68]0.5 · ca. 400 H2O ≡ Na15[ 1 a ]0.5[ 1 b ]0.5 · ca. 400 H2O 1 , which crystallizes in the triclinic space group P 1 (a = 30.785(2), b = 32.958(2), c = 47.318(3) Å, α = 90.53(1), β = 89.86(1), γ = 96.85(1)°, V = 47665(6) Å3, Z = 2, Dcalc = 2.149 g cm–3), precipitates within one day when an acidic (pH ≈ 1) aqueous solution of sodium molybdate (because of the extremely high solubility of the reaction product used in relatively high concentration) is reduced by sodium dithionite. 1 contains hitherto unknown pure molybdenum-oxide based, nanosized, ring-shaped, crystallographically independent cluster anions of the type {Mo154} 1 a and {Mo152} 1 b , the lacunary-type analogue of 1 a . Using the same reducing agent but in the presence of a reagent with a high affinity to the specific {Mo2}-type building unit (also a leaving group) of 1 a , such as formic acid, the compound Na22[MoMoO442H14(H2O)58] · ca. 250 H2O 2 (space group P 1, a = 24.724(1), b = 35.726(2), c = 44.608(3) Å, α = 93.25(1), β = 93.51(1), γ = 106.72(1)°, V = 37552(4) Å3, Z = 2, Dcalc = 2.401 g cm–3) is obtained in which the giant rings, having four missing {Mo2} units compared to 1 a , are linked to chains. Until now, similar chain-type compounds could only be obtained using a non-well-defined synthetic method.  相似文献   

15.
Synthesis and Crystal Structure of [N(Hex)4] [Cu2(CN)3] [N(Hex)4][Cu2(CN)3] has been prepared by solvothermal reaction of CuCN with Tetra‐n‐hexylammoniumiodide in acetone. The crystal structure is built up by condensed (CuCN)6 and (CuCN)7 rings, forming a zeolith type cyanocuprate(I) framework [Cu2(CN)3]. Space group R3; α = 44.482(6), c = 21.283(4) Å, V = 36471(9) Å3; Z = 9.  相似文献   

16.
K3Au5Pb: Layers of [AuAu3/2] Gold Tetrahedra and [Pb2/2] Lead Chains Silver coloured, brittle single crystals of K3Au5Pb were synthesized by reaction of potassium azide with gold sponge and lead powder at T = 920 K. The structure of the compound (space group Imma, Z = 4, a = 5.646(1) Å, b = 19.500(4) Å, c = 8.412(1) Å) was determined from X-ray single-crystal diffractometry data. The gold lead partial structure consists of layers of [AuAu3/2] tetrahedra and [Pb2/2] zigzag chains with four-bonded lead atoms which are connected to a framework structure via Au–Pb contacts. The potassium atoms occupy channels within the gold lead partial structure.  相似文献   

17.
New Borates of the Alkali Metals: NaLi2[BO3] The hitherto unknown NaLi2[BO]3 is prepared in the shape of monoclinic, colourless-transparent and prismatic single crystals [a = 950.7(4) pm, b = 1 203.7(4) pm, c = 493.0(3) pm, β = 104.0(10)°, dx = 2.32 g/cm3, dpyk = 2.28 g/cm3]. The crystal structure has been solved by four-circle-diffractometer [PW 1100, MoK, R = 7.52%, Rw = 4.66%]. Effective Coordination Numbers, ECoN, these via Mean Fictive Ionic Radii, MEFIR, are calculated.  相似文献   

18.
Synthesis and Structure of Tetrafluoroaurates(III) MI[AuF4] with MI = Li, Rb Single crystal investigations on Rb[AuF4], light yellow, confirm the tetragonal unit cell (K[BrF4]-type) with a = 618.2(1) and c = 1191(1) pm, Z = 4, space group I 4/mcm-D (No. 140). Li[AuF4], light yellow too, crystallizes monoclinic with a = 485.32(7), b = 634.29(8), c = 1004.43(13) pm, β = 92.759(12), Z = 4; space group P 2/c-C (No. 13). The structure of Li[AuF4] is related to the Rb[AuF4]-type of structure.  相似文献   

19.
Reaction of A2CO3 (A = K, Rb) with Sn and Se in an H2O/CH3OH mixture at 115–130°C affords the isotypic selenidostannates(IV) A6Sn4Se11 _. xH2O (A = K, x = 8) 1 and 2 whose discrete [Sn4Se11]6– anions each contain two corner‐bridged ditetrahedral [Sn2Se6]4– species. Similar reaction conditions with A = Cs afford Cs2Sn2Se5 _. H2O ( 3a ) and Cs2Sn2Se5 ( 3b ) in which such [Sn2Se6]4– building blocks are connected through common Se atoms into infinite [Sn2Se52–] chains. The [Sn3Se72–] ribbons of (Et4N)2Sn3Se7 ( 4 ), formed by treating (Et4N)I with Sn and Se in methanol at 130°C, can be regarded as resulting from the condensation of [Sn2Se52–] chains with molecular [SnSe4]4– anions. The anions [Sn4Se11]6–, [Sn2Se52–], and [Sn3Se72–] represent the products of individual reaction steps on the potential condensation pathway of [Sn2Se6]4– to the lamellar selenidostannates(IV) [Sn4Se92–] or [Sn3Se72–].  相似文献   

20.
Synthesis and Crystal Structure of LiPdAlF6 and PdZrF6 . For the first time single crystals of the new compounds LiPdAlF6 and PdZrF6 have been obtained. LiPdAlF6 (blue) crystallizes trigonal, space group P3 1c—D (No. 163; LiCaAlF6-type [2]), in an ordered structure variant of the Li2[ZrF6]-structure [3], with a=497.21(9) pm, c=914.0(9) pm and Z=2. PdZrF6 (also blue) is isotypic with LiSbF6 [4] and crystallizes trigonal-rhomboedric with a=552,3(1) pm, c=1 447,5(4) pm, space group R 3 —C (No. 148) and Z=3.  相似文献   

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