共查询到20条相似文献,搜索用时 15 毫秒
1.
On the Crystal Structure of In3Mo11O17 and the Physical Properties of Oligomeric Oxomolybdates In3Mo11O17 is characterized by its molybdate framework Mo22O348? belonging to the general series Mo4n+2O6n+4x? (with n = 5). The phase grows in star-like aggregates and crystallizes within the orthorhombic system (a = 988.0(2) pm, b = 951.2(2) pm, c = 3 176.7(4) pm). There are oligomeric clusters built from five trans edge-sharing Mo6 octahedra, surrounded by O atoms over all empty edges according to the Aufbau principle Mo22OOO. In the remaining structural channel one finds an In68+ polycation which is geometrically equivalent with the one of In11Mo40O62. The Mo—O and Mo—Mo distances within the cluster are the same like in In11Mo40O62, too, but there are shorter inter cluster distances (306 pm) in In3Mo11O17. Disorder in the structure may be understood in terms of the presence of constitutional isomers. While the electrical resistivity of PbMo5O8 resembles the one of a strongly disturbed metal (with a local minimum around 120 K), the temperature characteristic of Tl0.8Sn0.6Mo7O11 is typical for a semiconductor. Oxomolybdates with even longer oligomers like In11Mo40O62 and In3Mo11O17 show metallic conductivity. This course corresponds with the sizes of the clusters and their electronic intercoupling which can be estimated from the specific lengths of the inter cluster distances. The effective magnetic moment grows with increasing cluster length from 0.97 μB (PbMo5O8) to 1.40 μB (In11Mo40O62) per cluster (exception: In3Mo11O12), and so does the contribution of the temperature-independent paramagnetism (from 890 to 2191 × 10?6$ \frac{{{\rm emu}}}{{{\rm mol}}} $ per cluster). Thus, a single condensed octahedron carries roughly 440 × 10?6$ \frac{{{\rm emu}}}{{{\rm mol}}} $ as a temperature-independent paramagnetism, similar to the M6X17 halide clusters. In11Mo40O62 shows an interesting change in the temperature dependence of its magnetic suszeptibility. 相似文献
2.
Synthesis and Crystal Structure of PbMo5O8; a reduced Oxomolybdate with Mo10O28 Double Octahedra The crystal structure of the new phase PbMo5O8 contains oligometric Mo clusters which consist of two edge-sharing Mo6 octahedra connected according to Mo10OOO. The compound is isotypic with LaMo5O8. Isolated, divalent Pb atoms are located in the “channels” of the monoclinic structure (a = 999.3(2) pm, b = 924.7(1) pm, c = 753.6(2) pm, β = 109.39(2)°, P21/a. Compared to the compound In 11Mo40O62 the Mo? O distances (average 206 pm) and the Mo? Mo distances within the octahedral units (average 275 pm) are slightly decreased by 1 and 4 pm, respectively. The very short Mo? Mo distances (278 pm) between the cluster units which are not observed in In11Mo40O62 (320 pm) are due to excess electrons in these inter-cluster bonds which would otherwise occupy antibonding cluster states. 相似文献
3.
4.
Meinhard Waburg Hanskarl Müller-Buschbaum 《Monatshefte für Chemie / Chemical Monthly》1984,115(1):15-20
Zn3Ta2O8 was prepared by high temperature solid state reaction (CO2-Lasertechnique). X-ray investigations of single crystals yield monoclinic symmetry (a=9.499;b=8.411;c=8.881 Å; =116.03°, space group C
2h
6
—C2/c). There is no relationship between Zn3Ta2O8 and Zn3Nb2O8. Zn3Ta2O8 shows a characteristic structure type with octahedral coordination of Ta5+ and tetrahedral coordination of Zn2+. 相似文献
5.
Caroline Rhr 《无机化学与普通化学杂志》1995,621(9):1496-1500
Novel Suboxide Clusters [O5Ba18] in the Crystal Structures of Ba21M2O5 (M = Si, Ge) The compounds Ba21M2O5 (M = Si, Ge) crystallize in the cubic system with space group Fd3m, lattice constants 2 038.3(10) pm (Si), 2 039.8(9) pm (Ge) resp. and Z = 8. The crystal structure contains isolated Si/Ge atoms coordinated by barium atoms in an icosahedral arrangement. The oxygen atoms are situated in the centers of barium octahedra, four of which share common faces with an additional central octahedron. The novel clusters [O5Ba18] in principal are related to those in the crystal structures of the binary Cs/Rb suboxides. 相似文献
6.
Michael Ruck 《无机化学与普通化学杂志》2002,628(2):453-457
Ruby‐red crystals of Ag2Bi2S3Cl2 were synthesized from AgCl and Bi2S3 by cooling a melt from 770 K to room temperature. X‐ray diffraction on powders and single‐crystals revealed a triclinic crystal structure with special lattice constants (P &1macr; (No. 2), a = 1085.0(2), b = 717.2(1), c = 1137.6(1) pm, α = 89.80(1)?, β = 74.80(1)?, γ = 87.81(1)?). In the structure [BiIIIS3Cl4] polyhedra form 2[BiS3/2Cl4/4]‐ double‐layers by sharing common faces and edges. The silver(I) cations between the layers are coordinated either octahedrally by sulfide ions or tetrahedrally by sulfide and chloride ions. The deviations from the monoclinic space group P 1 21/c 1 are small and induce twinning along [010]. Further pseudosymmetry is based on the stacking of layer packages with the symmetry of the layer group P (2/c) 21/c 2/b. 相似文献
7.
Preparation, Characterization, and Crystal Structures of Tetraiodoferrates(III) The extremely air and moisture sensitive tetraiodoferrates MFeI4 with M = K, Rb and Cs have been synthesized by reaction of Fe, MI and I2 at 300°C in closed quartz ampoules. The essentially more stable alkylammonium tetraiodoferrates NR4FeI4 with R = H, C2H5, n-C3H7, n-C4H9 and n-C5H11 can be obtained by reaction of Fe, NR4I and I2 in nitromethane. The Raman and UV/Vis-spectra of the black compounds show the existence of tetrahedral [FeI4]? ions in the structures. The crystal structure of the monoclinic CsFeI4 (CsTlI4 type, spgr P21/c; a = 7.281(1) Å; b = 17.960(3) Å; c = 8.248(2) Å; β = 107.35(15)°) is built up by tetrahedral [FeI4]? ions and CsI11 polyhedra. The crystal structure of the orthorhombic (n-C5H11)4NFeI4 (spgr Pnna; a = 20.143(4) Å; b = 12.683(3) Å; c = 12.577(3) Å) contains tetrahedral [(n-C5H11)4N]+ ions and [FeI4]? ions, respectively. 相似文献
8.
Synthesis and Crystal Structure of Cu6Mo5O18 Single crystals of the hitherto unknown compound Cu6Mo5O18 were prepared and investigated by X-ray methods (a = 18.884(19), b = 6.273(7), c = 15.259(23) Å, β = 130.40(5)°, space group C–C2/c, Z = 4). The typical features of the structure are described and compared with the crystal chemistry of oxocuprates(I). Observed and calculated powder patterns show that the correct composition of the earlier described compound Cu6Mo4O15 is Cu6Mo5O18. 相似文献
9.
Crystal Structures of Hexachalcogeno‐Hypodiphosphates of Magnesium and Zinc Five chalcogeno‐hypodiphosphates were synthesized and investigated by single crystal X‐ray methods. Mg2P2S6 (C2/m; a = 6.085(1), b = 10.560(2), c = 6.835(1)Å, β = 106.97(3)°; Z = 2) crystallizes with the Fe2P2S6 type structure, whereas Mg2P2Se6 (a = 6.404(1), c = 20.194(4)Å) and Zn2P2Se6 (a = 6.290(3), c = 19.93(2)Å) build up the Fe2P2Se6 type (R3; Z = 3). The structures are characterized by closest packings of sulfur (selenium) with Mg2+ (Zn2+) ions and P2 pairs in half the octahedra — analogous to the CdCl2 and CdI2 type, respectively. In Mg2P2S6 half the Mg2+ ions can be substituted by Ag+ ions resulting in Ag2MgP2S6 (C2/n; a = 6.364(1), b = 10.975(2), c = 13.999(3)Å, β = 108.29(3)°; Z = 4). In this compound the Ag+ ions are disordered and located in the octahedra originally occupied by Mg2+ ions. In Mg2P2Se6 an analogous substitution by K+ ions leads to the compound K2MgP2Se6 (P21/n; a = 6.546(1), b = 12.724(3), c = 7.599(2)Å, β = 103.02(3)°; Z = 2) with K2FeP2S6 type structure. The structure is characterized by columns of alternating face‐sharing Se octahedra (centered by Mg) and trigonal antiprisms (centered by P2 pairs) along [100]. The columns are interconnected by inserted K+ ions. 相似文献
10.
New Organometallic Indium Nitrogen Compounds. Synthesis and Crystal Structures of [{Cp(CO)3Mo}2InN(SiMe3)2] and [{Cp(CO)3Mo}In{N(SiMe3)2}2] The reaction of [{Cp(CO)3Mo}2InCl] with LiN · (SiMe3)2 leads to the formation of [{Cp(CO)3Mo}2InN · (SiMe3)2] ( 1 ). 1 is monomeric and it contains an indium atom which is coordinated in a trigonal planar manner by two {Cp(CO)3Mo} fragments and a N(SiMe3)2 group. The corresponding bis-amide [{Cp(CO)3Mo}In{N(SiMe3)2}2] ( 2 ) is prepared by the reaction of [{Cp(CO)3Mo}InCl2] with two equivalents of LiN(SiMe3)2. In analogy to 1, 2 is monomeric and it contains an indium atom in a trigonal planar coordination. 相似文献
11.
Hans-Carsten Mumm Hanskarl Müller-Buschbaum 《Monatshefte für Chemie / Chemical Monthly》1987,118(12):1357-1362
Single crystals of -TlSm(WO4)2 were examined by X-ray diffractometer technique (space group C
2h
6
-C2/c;a=10.770,b=10.597,c=7.597 Å, =130.09°,Z=4). The coordination of W6+, Sm3+ and Tl+ are discribed and discussed.-TlSm(WO4)2 is isotypic to -KY(WO4)2. 相似文献
12.
Synthesis and Crystal Structure of (C5H5)Mo(CO)3(AuPPh3) and [(C5H5)Mo(CO)2(AuPPh3)4]PF6 CpMo(CO)3(AuPPh3) is obtained by the reaction of Li[CpMo(CO)3] with Ph3PAuCl at ?95°C in CH2Cl2. It crystallizes in the monoclinic space group C2/c with a = 2625.1(7), b = 883.2(1), c = 2328.4(7) pm, β = 116.39(1)° und Z = 8. In the complex the AuPPh3 group is coordinated to the CpMo(CO)3 fragment with a Au? Mo bond of 271,0 pm. The Mo atom thus achieves a square pyramidal coordination with the center of the Cp ring in apical position. CpMo(CO)3(AuPPh3) reacts under uv irradiation with an excess of Ph3PAuN3 to afford the cluster cation [CpMo(CO)2(AuPPh3)4]+. It crystallizes as [CpMo(CO)2(AuPPh3)4]PF6 · 2 CH2Cl2 in the orthorhombic space group P212121 with a = 1553.9(1), b = 1793.8(2), c = 2809.8(7) pm und Z = 4. The five metal atoms form a trigonal bipyramidal cluster skeleton with the Mo atom in equatorial position. The Mo? Au distances range from 275.5 to 280.8 pm, and the Au? Au distances are between 281.2 and 285.6 pm. 相似文献
13.
Marion Grün Klaus Harms Rolf Meyer Zu Kcker Kurt Dehnicke Helmut Goesmann 《无机化学与普通化学杂志》1996,622(6):1091-1096
Crystal Structures of [TiF3(NPPh3)(HNPPh3)]2 and of HNPPh3 The phosphoraneiminato-phosphaneimine complex [TiF3(NPPh3)(HNPPh3)]2 was obtained by the reaction of TiF4 with Me3SiNPPh3 in boiling dichloromethane. It crystallizes from 1,2-dichloroethane as yellow crystals which include four molecules C2H4Cl2 per dimeric formula unit. Space group P21/n, Z = 2, structure solution with 7270 independent reflections, R = 0.060 for reflections with I > 2σ(I). Lattice dimensions at ?50°C: a = 1417.5, b = 1896.9, c = 1586.6 pm, β = 101.22°. The compound forms centrosymmetric dimeric molecules via μ2-F bridges with TiF distances of 194.6 and 223.3 pm, the longer one being in trans-position to the N atom of the (NPPh3)? ligand. Its TiN bond length of 177.7 pm corresponds with a double bond. The TiN bond length of the HNPPh3 donor molecule of 213.4 pm is typical for a donor acceptor bond. According to the crystal structure determination the phosphaneimine HNPPh3 forms monomeric molecules without intermolecular hydrogen bridges with a PN bond length of 152.4 pm. Space group P21/c, Z = 4, structure solution with 3229 independent reflections, R = 0.062 for reflections with I > 2σ(I). Lattice dimensions at ?70°C: a = 1460.4, b = 928.9, c = 1096.6 pm, β = 93.35°. 相似文献
14.
[C6N2H18]2[Mo5O15(HPO4)2]·H2O的水热合成与结构表征 总被引:6,自引:0,他引:6
通过水热法合成了一个新化合物[C6N2H18]2[Mo5O15(HPO4)2]·H2O,并通过IR光谱、ICP、元素分析、差热与热重分析和X射线单晶衍射分析等手段进行了表征.结果表明,晶体属三方晶系,P3(2)21空间群,a=1.1231(1)nm,c=2.2802(5)nm,V=2.4911(7)nm3,Dx=2.835Mg/m3,Z=6,最后的一致性因子R=0.0227,wR=0.0675.阴离子中Mo5O15构成一环状结构,2个HPO4一个连在环的下方,一个连在环的上方,形成类似于“飞碟”状的结构,阳离子为2个质子化的四甲基乙二胺. 相似文献
15.
Synthesis and Crystal Structure of the Calcium Copper Diarsenate CaCuAs2O7 Solid state reactions led to single crystals of CaCuAs2O7. X-ray investigations revealed monoclinic symmetry, space group C52h-P21/c, lattice constants a = 7.272(1); b = 8.946(2); c = 9.307(2) Å; β = 109.48(2)°; Z = 4. CaCuAs2O7 is characterized by 1∞[CaO6] chains, connected by As2O7 double tetrahedra and elongated square CuO5 pyramids. The hitherto unknown crystal structure shows relationships to CaCuP2O7 but not to CaCuV2O7. 相似文献
16.
Phosphoraneiminato Complexes of Iodine. Syntheses and Crystal Structures of Ph3PNIO2 and Ph3PNSiMe3 · I2 Ph3PNIO2 has been prepared as yellow crystals by the reaction of Ph3PNSiMe3 with I2O5 in boiling acetonitrile, whereas the molecular complex Ph3PNSiMe3 · I2 is formed as brown crystals by the reaction of Ph3PNSiMe3 with iodine in acetonitrile solution. Both complexes were characterized by crystal structure determinations. Ph3PNIO2: Space group P21/n, Z = 4, 2 858 observed unique reflections, R = 0.039. Lattice dimensions at 19°C: a = 972.8(2), b = 1 743.4(3), c = 1 073.7(2) pm, β = 115.46(3)°. The compound forms monomeric molecules with pyramidal geometry at the iodine atom. The bond angle PNI (126.9°) is unusually small; the PN bond length of 159.2 pm corresponds with a double bond. Ph3PNSiMe3 · I2: Space group P1 , Z = 2, 3 560 observed unique reflections, R = 0.033. Lattice dimensions at 19°C: a = 941.2(2), b = 1 041.7(2), c = 1 287.4(3) pm, α = 78.34(1)°, β = 72.00(2)°, γ = 86.08(2)°. The compound forms monomeric molecules, in which the I2 molecule and the nitrogen atom of the phosphoraneimine molecule realize a linear N? I? I axis with a bond length N? I of 243.2 pm. 相似文献
17.
Dorothea Wolff von Gudenberg Hak-Chul Kang Werner Massa Kurt Dehnicke Ccilia Maichle-Mssmer Joachim Strhle 《无机化学与普通化学杂志》1994,620(10):1719-1724
Silanolato Complexes of Titanium and Zirconium. The Crystal Structures of Cp2TiCl(OSiPh3) and Cp2ZrCl(OSiPh3) The title compounds have been prepared by the reaction of Cp2MCl2 (M = Ti, Zr) with triphenylsilanole in diethylether in the presence of piperidine. They form only sparingly moisture sensitive orange (Ti) or colourless (Zr) crystal needles, which were characterized by X-ray crystallography. Cp2TiCl(OSiPh3): Space group P21/n, Z = 4, structure solution with 3961 observed unique reflections, R = 0.057. Lattice dimensions at 20°C: a = 1029.6, b = 1719.3, c = 1388.9 pm, β = 100.69°. The compound forms monomeric molecules with bond lengths TiO of 184.2 pm, SiO of 161.5 pm, and a TiOSi bonding angle of 164.5°. Cp2ZrCl(OSiPh3): Space group P3 , Z = 18, structure solution with 2799 observed unique reflections, R = 0.047. Lattice dimensions at ?20°C: a = b = 3518, c = 1058.3 pm. The structure consists of three symmetry-independent monomeric molecules, which differ only slightly. The bond lengths are (in average): ZrO 196.4 pm, SiO 162.1 pm, the ZrOSi bond angle is 173.7°. 相似文献
18.
Crystal Structure of the Monohydrates of Lithium Chloride and Lithium Bromide Using single crystal analysis and powder diffraction data the crystal structures of the monohydrates of lithium chloride and lithium bromide were solved. Both compounds crystallise isotypic in the space group Cmcm (LiCl·H2O: single crystal analysis; T = 100 K; a = 758, 35(2); b = 768, 07(2); c = 762, 35(2) pm; Z = 8; 1179 unique reflections; R1 = 0, 0196. LiBr·H2O: Rietveld‐refinement; T = 220 K; a = 806, 15(1); b = 799, 44(1) und c = 794, 61(1) pm; Z = 8; 157 unique reflections; Rp = 0, 0922; Rwp = 0, 0979; Rexp = 0, 0657). The structure derives from the perowskite structure according to the formula X(H2O)Li□2 (X = Cl, Br). The orientation of the water molecules is linked clearly to the distribution of the lithium cations and vice versa. The high level ionic conductivity in the cubic high temperature phase of LiBr·H2O is related to the initial rotation of the water molecules during the phase transformation. This motion favours the lithium ion hopping and the melting of the lithium substructure respectively. 相似文献
19.
The crystal structures of Mn5O8 and Cd2Mn3O8 are determined from single crystal and high resolution X-ray powder data. Both structures have very similar monoclinic unit cells, space group C–C2/m, and are isotypic: Hence, the true formula of Mn5O8 is MnMnO8. The crystal structure consists of pseudohexagonal MnIV sheets (bc) with similar oxygen sheets on either side, giving a distorted octahedral coordination to the MnIV. As every fourth MnIV is missing in these “main layers”, their composition becomes Mn3O8, and chains of coordination octahedra linked by common edges become distinct. Above and below the empty MnIV sites are either MnII or CdII completing the composition MnMnO8 or Cd2Mn3O8 respectively. Examples of similar “double layer” structures are given. 相似文献
20.
New Polynuclear Organotin(IV)–Nitrogen Compounds. Synthesis and Crystal Structures of [(PhSn)4(NPh)5Cl2] and [(MeSn)4(NHPh)4(NPh)4] The reaction of the organotin halides PhSnCl3 and MeSnCl3 with LiNHPh leads to the formation of two new nitrogen bridged organotin compounds, [(PhSn)4(NPh)5Cl2] ( 1 ) and [(MeSn)4(NHPh)4(NPh)4] ( 2 ). The crystal structures of 1 and 2 have been determined by low temperature X‐ray diffraction. 1 contains a bicyclic Sn4N5 framework, which consists of two six‐membered Sn3N3‐rings. All tin atoms are coordinated nearly tetrahedrally. Two tin atoms are bonded to a phenyl group and three nitrogen atoms, the other two tin atoms are coordinated by a phenyl group, two nitrogen atoms and a terminal chlorine atom. In 2 the tin atoms define the corners of a distorted square. Each edge of the square is bridged by a μ2‐NHPh and a μ2‐NPh group. The bridging NHPh and NPh groups are arranged at opposite sides of the Sn4 plane. The tin atoms are coordinated square pyramidally by 4 nitrogen atoms and a methyl group. 相似文献