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1.
The first isocyanide ligated hexanuclear zirconium halide cluster is reported. The unoxidized [(Zr6Be)Cl12(CNXyl)6] (CNXyl = 2,6-dimethylphenyl isocyanide) was obtained from the solid state precursor K3Zr6Cl15Be by dissolution in CH3CN in the presence of CNXyl. The CNXyl ligands occupy all the axial positions on the cluster. The compound was recrystallized from CH2Cl2 and Et2O. [(Zr6Be)Cl12(CNXyl)6].2CH2Cl2 crystallizes in the space group
(#2) with a = 12.092(5) Å, b=12.728(5) Å, c = 14.102(8) Å, = 104.98(4)°, =107.11°, = 100.94°, V = 1919(2) Å3, Z = l, R = 11.3% and R
W
= 27.0%. For the bound isocyanide ligands, v
CN increases to 2140 cm–1. 相似文献
2.
Yue-Qing Zheng Ekaterina Jonas Jürgen Nuss Hans Georg von Schnering 《无机化学与普通化学杂志》1998,624(9):1400-1404
Octahedro-hexatungsten octadecachloride, W6Cl18, is soluble in dimethyl sulfoxide (DMSO). Brownish black crystals of W6Cl18(DMSO)4 are formed from the brown solution by evaporation of DMSO under dynamic vacuum. The compound crystallizes monoclinically in the space group P21/n (no. 14) with a = 10.420 Å, b = 9.271 Å, c = 20.828 Å, β = 91.10° and Z = 2. The crystal structure is formed by isolated cluster molecules [W6Cl]Cl of the hexameric tungsten trichloride and DMSO molecules. It is the first hierarchical variant of the tetragonal BaAl4 type of structure where all atoms of the intermetallic phase are substituted by neutral molecules. The mean bond lengths are d(W–W) = 2.878 Å, d(W–Cli) = 2.391 Å and d(W–Cla) = 2.447 Å. They will be discussed in relation to analogous clusters. The two crystallographically independent DMSO molecules (d(S–O) = 1.53–1.55 Å, d(S–C) = 1.65–1.78 Å) form a 3 D net of condensed < 4864 > dodecahedra which envelopes the clusters. 相似文献
3.
1INrnODUCTIoNlnthepreviouspapers,wehavereportedthesynthesisandcrystalstructureofseveralcrownetherpolyoxometalates"-",nowwestudythestructureofthetitlecomplexandcompareitwithsomeothercrownetherpolyoxometalatecomplexes.2EXPERmENTALToal5OmLaqueoussolutioncontaining32g(1OOmol)Na,WO#.2H,Opre-justedtopH=3.5withchloricacid,14g(4Ommol)(n-Bu)'NBrwasadded,thenwhitepowderwasformed.ThewhiteprecipitateobtainedwithafiltrationwaskeptasthenewmaterialAinnextstep.AmixtureoflgAandO.3g(O.8mmol)DB18… 相似文献
4.
Unusual Coordination Polyhedra around Oxygen in Li4Cl(OH)3 The pseudobinary system LiOH/LiCl was investigated by X-ray methods. Two compounds, Li4Cl(OH)3 and Li2Cl(OH), were obtained. The crystal structure of Li4Cl(OH)3 solved by single-crystal methods is delt with. For Li2Cl(OH) powder diffraction data are given: Li4Cl(OH)3: P21/m, Z = 2, a = 5.4096(8) Å, b = 7.382(2) Å, c = 6.2076(8) Å, β = 94.40(1)°, Z(Fo) with (Fo)2 ≧ 3σ(Fo)2 = 483, Z (parameter) = 50, R/Rw = 0.022/0.025 Li2Cl(OH): Pmma, Z = 2, a = 7.680(8) Å, b = 4.001(7) Å, c = 3.899(6) Å The hydroxide rich compound crystallizes in a new type of structure which contains puckered layers [Li4(OH)3+] connected via chloride ions. 相似文献
5.
NIU Mei-Ju ② DOU Jian-Min WANG Da-Qi LI Da-Cheng 《结构化学》2006,25(6):757-760
1 INTRODUCTION Since the report about unusual coordination num- bers and arrangements to metal ions of crown ether compounds by Pedersen[1], the crown ether compounds have attracted much attention. Due to their novel coordination modes, crown ethers have been widely used in catalyst, solvent extraction, iso- tope separation, bionics, material chemistry, host- guest chemistry and supramolecular chemistry[2~5]. So it is vital to study the synthesis of new crown ethers and their crystal stru… 相似文献
6.
The tetra(2, 4-dichlorobenzyl)tin was synthesized and characterized by elementary analysis, IR and
1H NMR. The crystal and molecular structure were determined by X-ray single crystal diffraction. The crystal of the title compound belongs to triclinic, space group
P1 with a=1.089 7(3) nm, b=1.050 33(4) nm, c=1.858 5(4) nm, α=96.822(4)°, β=94.477(4)°, γ=94.636(3)°, V=3.001 3(12)
nm3, Z=4, Dc=1.679 Mg·m-3, μ(Mo Kα)=1.582 mm-1, S=1.005, F(000)=1 496,
R1=0.040 7, wR2=0.076 3. In compound, the tin atom has a distorted tetrahedral coordination configuration. The molecules are packed in one-dimensional chain polymer through a weak interaction between the chlorine atoms from adjacent molecules, respectively. CCDC: 286106. 相似文献
7.
SynthesisandCrystalStructureofNovelFe_3ClusterCompound¥LuQing-Wei;WangYi-Bing;WuBao-Shan;SuoQuan-Ling;LiuShu-Tang;HuXiang;(De?.. 相似文献
8.
A novel complex, chlorodi(p-chlorbenzyl)tin dithiotetrahydropyrrolocarbamate, has been synthesized. The crystal structure has been determined by X-ray single crystal diffraction. The crystal of the complex belongs to monoclinic with space group C2/c, a=3.070 0(19) nm, b=0.787 9(5) nm, c=2.374 9(15) nm, β=119.63(9) °, Z=8, V=4.993(5) nm3, Dc=1.515 g·cm-3, μ=1.521 mm-1, R1=0.047 4, wR2=0.097 2. The structure of the complex consists of discrete molecule containing five-coordinate tin atom in a seriously distorted trigonal bipyramidal configuration. The molecules are packed in the unit cell in one-dimensional chain polymer through a weak interaction between the chlorine atoms of the adjacent molecules. CCDC: 220743. 相似文献
9.
A cluster compound V2S6O2Cu6(3-MePy)6(3-MePy = 3-methyl pyridine) has been synthesized by using skiving method and the crystal structure was characterized by X-raydiffraction: space group P1, Z = 1, a = 9.7278(4), b = 10.4180(5), c = 11.9230(6) , α = 108.240(3), β = 98.120(2), γ = 99.500(2)o, R = 0.052 and wR = 0.104. The NLO properties were studied by Z-scan technique with 8 ns pulsed laser at 532 nm. The cluster exhibits strong NLO absorptive ability(α2 = 1.7 × 10–10 m·W–1) and effective self-focusing performance(n2 = 1.27×10–18 m2·W–1) in a 1.58 × 10–4 mol·dm–3 DMF solution. 相似文献
10.
Reaction of a preformed cluster [{(η5-C5Me5)WS3}3Cu7(MeCN)9](PF6)4
(1) in MeCN with LiCl and PPh3 gave rise to a tetranuclear cationic cluster [(η5-C5Me5)WS3{Cu(PPh3)}3Cl](PF6)
(2). The title compound 2 was characterized by elementary analysis, IR, UV-Vis,
1H NMR, and its crystal structure was determined by X-ray single crystal diffraction. It belongs to monoclinic, space group
P21/c with a=1.799 8(4) nm, b=2.083 6(4) nm, c=1.913 5(4) nm, β=113.63(3)°, V=6.574(3)
nm3, Z=4. The cluster cation [(η5-C5Me5)WS3{Cu(PPh3)}3Cl]+ of
2 contains a strongly distorted, cubane-like structure [WS3Cu3Cl] in which one Cl weakly fills into the void of the nido-like
[WS3Cu3] fragment with three relatively long Cu-Cl distances. CCDC: 270415. 相似文献
11.
(I) is prepared in high yield by reaction of Zr, B, RbCl, and ZrCl4 in a sealed Ta container at 850 °C. It crystallizes in the space group Pmna with Z=2. 相似文献
12.
Xiaoyu Dong Liang Cui Yunjing Shi Shilie Pan Zhongxiang Zhou Zhihua Yang Bingbing Zhang Xiangzhan Jiang Yun Yang Zhaohui Chen Zhenjun Huang 《无机化学与普通化学杂志》2013,639(6):988-993
The single crystals of Ba2Cd(B3O6)2 were grown by the spontaneous crystallization method for the first time. They crystallize in the centrosymmetric trigonal space group R$\bar{3}$ with a = 7.143(3) Å, c = 17.405(16) Å, and Z = 3. The structure is characterized by isolated B3O6 units, and the Ba2+ and Cd2+ cations connect with B3O6 rings to form three dimensional structure. The TG/DSC and XRD results reveal that Ba2Cd(B3O6)2 melts congruently. First‐principles electronic structure calculation performed with the density functional theory (DFT) method shows that the calculated bandgaps are 4.66 eV, which is in good agreement with the UV/Vis/NIR experimental value 4.59 eV. The calculation shows that the Ba2Cd(B3O6)2 crystal has a large birefringence (Δn = 0.0875–0.0569 from 270 nm to 2600 nm), which demonstrates that Ba2Cd(B3O6)2 is a potential birefringence crystal. 相似文献
13.
新颖四核W-Cu-S簇合物[(η5-C5Me5)WS3Cu3Br(Py)3(dppm)](PF6)的合成和晶体结构 总被引:1,自引:0,他引:1
In the presence of NH4PF6, reaction of [PPh4][(η5-C5Me5)WS3Cu3Br(dppm)] with excess pyridine afforded red prismatic crystals, [(η5-C5Me5)WS3Cu3Br(Py)3(dppm)](PF6) (1). It was characterized by elemental analy-sis, IR, UV-vis and 1H NMR spectroscopy and X-ray diffraction. 1 crystallizes in an orthorhombic system with space group Pna21 and unit cell parameters a=2.1124(4)nm, b=1.8944(4)nm, c=1.3338(2)nm, V=5.3375(19)nm3, Z=4, Dc=1.807g·cm-3,Mr=1452.42, F(000)=2864, μ=4.342mm-1, R1=0.0487, wR2=0.1027. The structure of the cluster cation contains an incomplete cubane-like WS3Cu3 core where Cu(1) and Cu(2) atoms are bridged by a dppm ligand. Each of the three Cu atoms adopts a distorted tetrahedral coordi-nation geometry. The W-Cu(1), W-Cu(2) and W-Cu(3) distances are 0.27698(17)nm, 0.2772(17)nm, and 0.27065(9)nm, respectively. CCDC: 199845. 相似文献
14.
SynthesisandCrystalStructureofDinuclearCopperClusterCompound[Cu(dtp)PPh_3]_2ChenQiu-Hua;LuShao-Fang;HuangXiao-Ying(StatekeyLab... 相似文献
15.
One-electron oxidized zirconium chloride clusters were obtained from solid state precursors Rb5Zr6Cl18B and K3Zr6Cl15Be by dissolution in CH3CN in the presence of Et4NCl and isolated as the salts (Et4N)4Zr6Cl18B · 2 CH3CN and (Et4N)5Zr6Cl18Be · 3 CH3CN. (Et4N)4Zr6Cl18B · 2 CH3CN crystallizes in the space group P1 (#2) with a = 12.329(5) Å, b = 12.657(6) Å, c = 13.136(8) Å, α = 118.28(4)°, β = 93.45(4)°, γ = 105.54(3)°, V = 1696(2) Å3, and Z = 1. (Et4N)5Zr6Cl18Be · 3 CH3CN was refined in the space group C2/c (# 15) with a = 24.166(11) Å, b = 13.265(6) Å, c = 25.86(2) Å, β = 104.21(4)°, V = 8037(7) Å3, and Z = 4; the space group reflects the pseudo-symmetry of the crystal, the true symmetry of the structure is lower. The removal of one electron from the Zr? Zr bonding HOMO of both clusters results in cluster expansion of similar magnitude in both compounds. Moisture from the added Et4NCl is the likely oxidant, but the possibility that acetonitrile may be reduced by [(Zr6Be)Cl18]6? is not ruled out. 相似文献
16.
Ln3UO6Cl3 (Ln=La, Pr, Nd) — The First Oxochlorouranates of the Rare Earths . The new compounds Ln3UO6Cl3 (Ln=La, Pr, Nd) were prepared by heating stoichiometric amounts of LnOCl/Ln2O3/U3O8 (7 : 1 : 1) (Ln=La, Nd) and PrOCl/Pr6O11/U3O8 (12 : 1 : 2) in silica ampoules (5 d, 1000°C, Ln=La; 9 d 800°C, Ln=Pr, Nd) in the presence of an excess of chlorine [p(Cl2, 25°C)=1 atm]. Single crystals were obtained by chemical transport reactions using chlorine [p(Cl2, 25°C)=1 atm] as transport agent [T2=1000°C→T1=900°C (Ln=La); T2=840°C→T1=780°C (Ln=Pr, Nd)]. Crystals of Ln3UO6Cl3 (Ln=La, Pr, Nd) were investigated by X-ray diffraction methods and La3UO6Cl3 additionally by high resolution electron microscopy. The compounds Ln3UO6Cl3 crystallize in the hexagonal spacegroup P63/m (No. 176) with Z=2 formula units per unit cell. Isotypical structure refinements resulted in R=3.04% respectively Rw=1.91% (Ln=La), R=4.72% respectively Rw=3.80% (Ln=Pr) and R=3.99% respectively Rw=2.49% (Ln=Nd). Uranium is coordinated with six oxygen atoms forming a trigonal prism. Lanthanide ions are 10-coordinated (6 oxygen atoms, 4 chlorine atoms). 相似文献
17.
Heterometallic Cluster Complexes of the Types Re2(μ-PR2)(CO)8(HgY) and ReMo(μ-PR2)(η5-C5H5)(CO)6(HgY) (R = Ph, Cy; Y = Cl, W(η5-C5H5)(CO)3) Dinuclear complexes Re2(μ-H)(μ-PR2)(CO)8 and ReMo(μ-H)(μ-PR2)(η5-C5H5)(CO)6 (R = phenyl, cyclohexyl) were deprotonated and reacted as anions with HgCl2 to compounds of the both types Re2(μ-PR2)(CO)8HgCl) and ReMo(μ-PR2)(η5-C5H5)(CO)6(HgCl). The heterometallic three-membered cluster complexes correspond to an isolobal exchange of a proton against a cationic HgCl+ group. For one of the products ReMo(μ-PCy2)(η5-C5H5)(CO)6(HgCl) has been shown its conversion with NaW(η5-C5H5)(CO)3 to ReMo(μ-PCy2)(η5-C5H5)(HgW(η5-C5H5)(CO)3) under substitution of the chloro ligand, par example. The newly prepared compounds were characterized by means of IR, UV/VIS and 31P NMR data. A complete determination of the molecular structure by single crystal analyses was done in the case of Re2(μ-PCy2)(CO)8(HgCl) and of ReMo(μ-PCy2)(η5-C5H5)(CO)6(HgCl) which both are dimer because of the presence of an asymmetric dichloro bridge, and of ReMo(μ-PCy2)(η5-C5H5)(CO)6(HgW(η5-C5H5)(CO)3). The structural study illustrates through comparison the influence of various metal types on an interaction between centric and edge-bridged frontier orbitals in three-membered metal rings. 相似文献
18.
The structure and stability of Be6, Be, and Be clusters have been investigated at the B3LYP, B3PW91, and second‐order Møller–Plesset (MP2) levels of theory, along with the 6‐311G* basis set for neutral and cationic clusters and the 6‐311+G* basis set for anion clusters. CCSD(T)/6‐311+G* has also been used to calculate some neutral structure to find the most stable structure. Twelve Be6, six Be, and eight Be isomers are identified. The distortion octahedron structure, pentagonal pyramids structure, and trapezoidal bipyramid structure are found to be the most stable structure on the neutral, cationic, and anionic surface, respectively. They are in agreement with the results reported previously. Natural bond orbital (NBO) analysis, molecular orbital (MO) pictures, and the nucleus independent chemical shift (NICS) values suggest aromatic of the neutral and cationic clusters and antiaromatic of the anionic cluster. The multi‐center σ bonds and delocalized π bonds play important role in the bonding of the beryllium clusters. © 2006 Wiley Periodicals, Inc. Int J Quantum Chem, 2007 相似文献
19.
Formation and Crystal Structure of Tribarium Tetradecaphosphide‐Ammonia(1/18) Ba3P14_.18NH3 Tribarium tetradecaphosphide‐ammonia(1/18) Ba3P14_.18NH3 was prepared by the reduction of red phosphorus with a solution of Ba in liquid NH3. It contains heptaphosphanortricyclane anions P73–, which are joined via P–Ba contacts resulting in <$>^1_\infty<$>[Ba2(P7)2]2–‐chains separated by barium octaammine complexes Ba(NH3)82+. 相似文献
20.
Ba3N2 reacts at 950°C under pure N2 with Zr to yield dark red, air-sensitive Ba[ZrN2]. This new compound crystallizes in the tetragonal space group P4/nmm with a = 416.10(2), c = 839.2(1) pm and Z = 2. The crystal structure was solved and refined using X-ray and neutron powder diffraction data. In the nitrido zirconate [ZrN2]2? the Zr atoms exhibit a square-pyramidal coordination by five N atoms at distances of 201(3) and 220.2(2) pm. The pyramids share all the edges in the basal plane to form layers parallel to (001) with their apices alternately pointing up and down. The Ba2+ cations are integrated into these layers at the levels of the pyramidal apices. The structure can be interpreted as a stuffed PbFCl type. Ba2[NbN3] is formed by the reaction of Ba3N2 and NbN or of Ba and Nb at 1 000°C under N2. Isostructural to Ba2[TaN3] it crystallizes in the monoclinic space group C2/c with a = 613.2(3), b = 1 176.8(3), c = 1 322.9(4) pm, β = 91.65(2)°, Z = 8. The nitrido niobate anions form chains of corner sharing NbN4 tetrahedra with distances Nb? N between 188(1) and 199.9(9) pm. 相似文献