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(C5H4SiMe2tBu)2LnnBu reacted with 1 equiv. of elemental sulfur in toluene at ambient temperature to yield the corresponding lanthanocene thiolates [(C5H4SiMe2tBu)2Ln(m-SnBu)]2 (Ln = Y (1), Er (2)). Complexes 1 and 2 have been characterized by elemental analysis, IR, mass spectros- copy and X-ray single-crystal diffraction analysis. Both complexes are of monoclinic with space group P21/c, formula C52H94S2Si4Y2 1 (C52H94S2Si4Er2 2) Mr = 1073.57 (1230.27), a = 8.495(2) (8.41(2)), b = 26.913(8) (26.67(7)), c = 13.756(4) (13.68(4)) (A), α = 90(90), β = 101.184(5) (101.57(4)), γ = 90 (90)°, V = 3085.1(15) (3007(14))(A)3, Dc = 1.156 (1.359) g·cm-3, Z = 2 (2), F(000) = 1144 (1260), μ = 2.046 (2.951) cm-1, R = 0.0687 (0.0749) and wR = 0.1306 (0.1507) for observed reflections with I > 2σ(I). X-ray structures of 1 and 2 definitively prove that only one sulfur atom is inserted into the Ln-C(nBu) bond, forming a thiolate ligand. 相似文献
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Eduard Bernhardt David J. Brauer Martin Köckerling Prof. Dr. Gottfried Pawelke Dr. 《无机化学与普通化学杂志》2007,633(7):947-954
Trimethylamine‐tris(pentafluoroethyl)borane [(C2F5)3BNMe3] ( 1 ) reacts at 190 °C with water under displacement of the trimethylamine ligand to yield the hydroxy‐tris(pentafluoroethyl)borate [(C2F5)3BOH]? ( 2 ). In tributylamine 1 reacts with alkynes HC≡CR to form novel ethynyl‐tris(pentafluoroethyl)borate anions [(C2F5)3BC≡CR]? – R = C6H5 ( 3 ), C6H4CH3 ( 4 ), Si(CH(CH3)2)3 ( 5 ) – in moderate yields. Compound 3 adds water across the triple bond to form the novel anion [(C2F5)3BCH2(CO)C6H5]? ( 6 ). The structures of [(C2F5)3BNMe3], [NMe4][(C2F5)3BOH] and K[(C2F5)3BCH2(CO)C6H5] have been determined by x‐ray crystallography. 相似文献
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在甲醇溶剂中利用(C6H5)3SnCl和三乙胺水解得到一种新型有机锡聚合物[(C6H5)3SnO]n。用元素分析、IR及X-射线衍射法表征配合物。晶体结构用直接法解出,并用全矩阵最小二乘法进行修正。该晶体属于正交晶系,空间群为P212121,晶胞参数为:a=0.8339(15)nm,b=1.040(2)nm,c=1.8067(4)nm,Z=4,V=1.5668(5)nm3,Mr=365.99,Dc=1.552g/cm3,mμ=1.623mm-1,F(000)=724,S=1.065,R=0.0278,wR=0.0511配合物的中心锡原子呈五配位畸变三角双锥构型。 相似文献
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New Benzyl Complexes of the Lanthanides. Synthesis and Crystal Structures of [(C5Me5)2Y(CH2C6H5)(thf)], [(C5Me5)2Sm(CH2C6H5)2K(thf)2]∞, and [(C5Me5)Gd(CH2C6H5)2(thf)] YBr3 reacts with potassium benzyl and [K(C5Me5)] in THF to give KBr and the monobenzyl compound [(C5Me5)2 · Y(CH2C6H5)(thf)] 1 . The analogous reaction with SmBr3 in THF leads to the polymeric product [(C5Me5)2Sm(CH2C6H5)2 ∞ K(thf)2]∞ 2 , with GdBr3 to [(C5Me5)Gd(CH2C6H5)2(thf)] 3 . The structures of 1–3 were determined by X-ray single crystal structure analysis:
- Space group P1 , Z = 2, a = 851.2(4) pm, b = 952.7(4) pm, c = 1858.6(8) pm, α = 79.90(4)°, β = 77.35(4)°, γ = 73.30(3)°.
- Space group P1 , Z = 2, a = 903.3(2) pm, b = 1375.9(3) pm, c = 1801.1(4) pm, α = 100.92(3)°, β = 100.77°, γ = 98.25(3)°.
- Space group P21/n, Z = 8, a = 1458.2(5) pm, b = 927.8(3) pm, c = 3792.9(15) pm, β = 96.83(3)°.
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H
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0 values of the complex formation in water of benzo-18-crown-6 (B18C6) with K+, Tl+, and Pb2+ were determined and compared with those of 18-crown-6. The H0 values of B18C6 are negative. The stability in water of the B18C6-metal ion complex at 25°C is governed largely by the magnitude of the H
0 value. The B18C6-metal ion complex is less stable in water than the corresponding 18C6-metal ion complex. This is due largely to a less favorable enthalpic contribution of the B18C6-metal ion complex compared with the corresponding 18C6-metal ion complex. The two aromatic ether oxygen atoms of B18C6 are responsible for the larger H
0 value of the B18C6-metal ion complex compared with the corresponding 18C6-metal ion complex. 相似文献
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[(C6H5CH2C5H4)2GdCl.THF]2 (1) and (C6H5CH2C5H4)2ErCl.THF (2) were prepared by the reaction of LnCl3 (Ln? Gd, Er) with benzylcyclopentadienyl sodium in THF and characterized by elemental analysis, IR, 1H NMR, 13C NMR, MS and thermal gravimetry. The crystal structures of both compounds were determined. Complex 1 is dimeric and its structure belongs to the monoclinic, P21/c space group with a=1.1432(2), b=1.2978(2), c=1.7604(3) nm, β=108.75(2), V=2.4732(9) nm3, Z=2(four monomers), Dc“1.54 g.cm?3. R=0.0342 and Rw“0.0362. Complex 2 is monomer and its structure belongs to the orthorhombic, P212121 space group with a=0.8645(2), b=1.1394(3), c=2.5289(4) nm, V=2.4919(9) nm3, Z=4, Dc“1.56 g.cm?3. R=0.0514, Rw“0.0529. The determination of the crystal structure shows that in complex 1 the benzyl groups on the cyclopentadienyls coordinated to Gd3+ are located in the opposite direction (139°); in complex 2 the benzyl groups on the cyclopentadienyls coordinated to Er3+ are located in the same direction (6.5°). 相似文献
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《Journal of organometallic chemistry》1993,443(2):C39-C40
The thermally-stable cobalt(II) dialkyl compound CoR2 [R = C(SiMe3)2C5H4N-2] (1) has been prepared by reaction of [{LiR}2] with cobalt(II) chloride in ether. An X-ray structural study has revealed a centrosymmetric molecular skeleton (for two nearly identical independent molecules) in which a pair of sterically-hindered, functionalized pyridine ligands R− are trans-chelated to the central planar four-coordinate cobalt(II) atom, with mean CoCα and CoN distances of 2.094(6)Å and 1.919(4) Å respectively, and a CαCoN angle of 69.6(2)°. 相似文献
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Heavy Metal π-Complexes. IX. The Chain Polymers [(1,2- (CH3)2C6H4BiCl3)2], [(1,3- (CH3)2C6H4BiCl3)2] and [(1,4- (CH3)2C6H4BiCl3)2] In the crystal structures of the three solid state complexes (C6H4(CH3)2BiCl3 (C6H4(CH3)2 = o-xylene: 1 , m-xylene: 2 , p-xylene: 3 ) quasi-dimeric units of almost undistorted, arene coordinated BiCl3 fragments can be found that are further associated via additional Bi? Cl contacts to form one-dimensional polymeric chains. Whereas the chains of 2 and 3 are constituted by Bi2Cl2 four-membered rings only, further Cl-bridging in 1 leads to additional trigonal-bipyramidal arrangements with Bi atoms exhibiting coordination numbers of 3 + 3 + 1 and 3 + 2 + 1, respectively (prim. + sec. Cl contacts + arene). The arene-metal bonding is characterized by Bi-arene distances in the range from 297 – 306 pm, including ring slippages of 24 –41 pm and 73 pm with the Bi atoms being six and seven coordinated, respectively. The direction of this slipping with respect to the arene's methylation sites cannot be understood in terms of electronic influences but is shown to be caused by steric demands. The values IP1 of the arenes prove to determine the colours of the complexes. 相似文献
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在溶剂热体系中,以N,N-二乙基乙二胺为结构导向剂,合成了Al/P为3/4的层状磷酸铝[Al6P8O32][(C2H5)2NHCH2CH2NH3]2·[C2H5NH2CH2CH2NH2C2H5]单晶,并通过X射线单晶衍射结构分析.XRD,ICP,元素分析,差热-热重分析等手段进行了表征.该化合物属单斜晶系,P2(1)/c空间群,晶胞参数:a=0.90945(2)nm,b=1.46424(4)nm,c=1.87572(5)nm,β=102.672(2)°,Z=4.其阴离子层由AlO4四面体和PO3(=O)四面体单元交替连接构成,形成四、六、八元环拓扑结构,无机层以ABAB方式堆积,两种质子化的有机胺分子N,N-二乙基乙二胺及其重排产物N,N′-二乙基乙二胺填充在层间.用分子动力学模拟方法,考察了标题化合物中有机胺与无机层间的相互作用,讨论了这两种有机胺的共模板作用. 相似文献
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π‐Allyl (η3‐C3H5), a four‐electron donor, was used as a ligand model to replace η5‐C5Me4SiMe3 in DFT calculations on the tetranuclear yttrium polyhydrido complex (η5‐C5Me4SiMe3)4Y4H8 containing a Y4H8 tetrahedral core structure, which may separate the four π‐allyl groups and hence suppress the allyl ligand coupling during the computation. In terms of the calculated core geometry, isomerization energy barrier, charge population, and frontier orbital features of the complex, the η3‐C3H5 ligand model is comparable to η5‐C5H5. © 2006 Wiley Periodicals, Inc. Int J Quantum Chem, 2007 相似文献