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1.
以大环铜配合物[CuL](ClO_4)_2(L=5,7,7,12,14,14-六甲基-1,4,8,11-四氮杂环十四-4,11-二烯)与NH_4VO_3反应合成了一个新的钒氧多酸桥联大环铜配合物[CuL]_2[H_2V_(10)O_(28)]·7H_2O(1),其结构经IR,元素分析和X-射线单晶衍射表征。1(CCDC:1510831)属单斜晶系,P2(1)/n空间群,晶胞参数a=11.512(3),b=18.170(4),c=14.534(3),β=102.997(4)°,V=2 962.3(11)~3,Dc=1.986 mg·cm~(-3),Z=2,μ=2.300mm~(-1),R_1=0.047 2,wR_2=0.118 2。  相似文献   

2.
设计合成了一个铜(I)的配合物[Cu(Triphos)(PPh3)](BF4)(1),通过红外、核磁氢谱和磷谱、紫外光谱、X-射线单晶衍射等对其进行结构表征。晶体结构研究表明,该晶体属于单斜晶系,P2(1)/c空间群;晶胞参数为a=12.8072(4),b=14.3693(4),c=25.8438(8),V=4756.0(2)3,Z=4。配合物1中的铜(I)原子同时与单齿配体PPh3和三齿配体Triphos的P原子配位,形成一个扭曲的四面体构型。配合物通过C-H…π、π…π堆积作用力形成三维网状结构。在室温下,配合物1的乙腈溶液在265 nm有紫外吸收峰,在399 nm有荧光发射峰。CCDC:1017906。  相似文献   

3.
牛磺酸和邻香草醛在甲醇中于0℃反应4 h制得牛磺酸缩邻香草醛席夫碱(TMSSB);以TMSSB和邻啡罗啉(phen)为混合配体经水溶液法合成了一个新型配合物{[Co(TMSSB)(phen)2]·5H2O(1)},其结构经IR和X-射线单晶衍射表征。1属单斜晶系,空间群C2/c,晶胞参数a=16.478(5),b=20.600(7),c=22.327(7),β=95.775(5)°,V=7538(4)3,Z=8,R1=0.092 9,wR2=0.163 1。1的中心Co(Ⅱ)与两个phen分子的4个氮原子,TMSSB上一个亚氨基氮原子及一个脱质子羟基氧原子配位,形成六配位的变形八面体构型;1分子间通过氢键和π-π堆积作用形成三维结构。  相似文献   

4.
罗世霞  陈晓靓  朱淮武  张笑一  卫钢 《化学通报》2014,77(11):1098-1102
以吡啶-2,6-二甲酸为起始原料,经酯化后与N-(3-氨基丙基)咪唑反应合成了有机配体分子吡啶-2,6-二[N-(1'-咪唑基丙基)甲酰胺](L)及其锌(Ⅱ)、镉(Ⅱ)配合物。配体L的结构经1H NMR、13C NMR、IR、UV和元素分析表征,并采用单晶X-射线衍射方法确定了L的晶体结构,L属于正交晶系,Pbcn空间群,晶胞参数a=25.03(2),b=8.933(7),c=20.101(16),α=β=γ=90°,V=4495(6)3,Z=8,Dc=1.287g·cm-3,μ=0.095mm-1,F(000)=1856。通过元素分析确定锌(Ⅱ)、镉(Ⅱ)配合物的组成分别为(C19H23N7O2)2Zn2(ClO4)2·(CH3O)2·2H2O和(C19H23N7O2)2Cd2(ClO4)·(CH3O)3·2H2O,并采用对比分析的方法讨论了配位前后游离配体L和两种配合物的红外吸收光谱和紫外吸收光谱的谱学性质。  相似文献   

5.
外消旋大环锌配合物[Zn(rac-L)](Cl O4)2(L=5,5,7,12,12,14-六甲基-1,4,8,11-四氮杂环十四烷)与L-苯丙氨酸(L-Phe)在弱碱性条件下反应制得单手性配合物[Zn(RR-L)(L-Phe)](Cl O4)(2),其结构经IR,元素分析,圆二色光谱和X-射线单晶衍射表征。2(CCDC:1 491 999)属四方晶系,空间群P41,晶胞参数a=12.647(11),b=12.647(11),c=18.295(3),β=90°,V=2 926.2(6)3,Dc=1.393 g·cm-3,Z=4,μ=0.977 mm-1,R1=0.040 7,wR2=0.081 5。  相似文献   

6.
本文通过恒温水浴法和溶剂热法分别合成了两种配合物Fe(3PCA)2(H2O)2(1)和[Cu(3PCA)(Im)]n(2)(3PCA=pyrazole-3-carboxylic acid,Im=imidazole),并用X-射线单晶衍射仪测定了它们的晶体结构。结果表明:配合物(1)属于单斜晶系,空间群为P21/c,晶胞参数为:a=5.11446(19),b=11.4930(4),c=9.4084(3),β=95.692(4)°,V=550.30(3)3,Z=2;配合物(2)属于单斜晶系,空间群为P21/c,晶胞参数为:a=11.7198(4),b=8.5094(3),c=8.9703(3),β=111.765(4)°,V=830.82(5)3,Z=4。对配合物(2)进行了磁性质研究,结果表明,铜离子之间存在反铁磁相互作用。  相似文献   

7.
以草酰胺铜配合物CuL(H_2L=2,3-二氧-5,6∶13,14-二联苯基-9,10-环己基-1,4,8,11-四氮杂十四环-7,12-二烯烃)为前驱配体,1,10-邻菲啰啉为端接配体,高氯酸锰为金属核心,经回流反应合成了一个新型的异双核配合物[CuLMn(phen)2](ClO_4)_2·2CH_3OH(1),其结构和性能经UV-Vis,IR,元素分析,X-射线粉末衍射和X-射线单晶衍射表征。结果表明:1(CCDC:1 445 582)属三斜晶系,空间群P-1,晶胞参数a=11.298(19),b=15.17(4),c=16.71(3),α=113.69(3),β=109.30(2),γ=93.08(4),V=2 417(9)3,Z=2。1在DMF中的最大吸收峰位于272 nm和361 nm。  相似文献   

8.
多吡啶配体H2L[N,N’-二(3-甲基吡啶基)-2,6-吡啶二酰胺]与Cu(OAc)2.H2O反应合成了一种新型的四核铜配合物——[Cu4L2(N3)2(μ2-N3)2].CH3OH(1),其结构经IR,XRD和元素分析表征。1属单斜晶系,空间群C2/m,晶胞参数a=15.774(3),b=15.062(3),c=10.724(2),β=114.91(3)°,V=2 344.0(8)3,Z=4,Dc=1.736 mg.cm-3,μ=1.869 mm-1,R1=0.120 1,ωR2=0.298 4。1中四个金属铜原子通过两个L2-配体,四个N3-基团连接在一起,形成了一个新颖的四核铜结构。  相似文献   

9.
以4-氨基苯甲酸和1,10-菲啰啉(phen)与高氯酸铁或硝酸镉反应,得到了两个邻菲啰啉的配合物:[Fe(phen)3]·2Cl O4·2CH2OH(1)和[Cd(phen)2(NO3)2](2)。并利用元素分析、红外光谱和X射线单晶衍射分析进行了表征。晶体结构分析表明,配合物(1)和(2)晶体属单斜晶系,C2/c空间群,其晶胞参数分别为:(1)a=35.708(3),b=15.903(2),c=12.204(1),β=102.504(6),V=6766(1)3,Z=8。(2)a=11.6887(6),b=15.2569(8),c=13.4630(10),β=105.9650(10),V=2310.5(2)3,Z=4。配合物(1)中phen上的氢原子与来自高氯酸根和乙二醇的氧原子形成氢键,并且相邻phen的吡啶环之间形成π~π堆积,从而使整个晶体扩展为三维网状超分子结构;配合物(2)中phen上氢原子与硝酸根的氧原子之间通过氢键使整个晶体扩展为三维网状超分子结构。  相似文献   

10.
H2L[N,N’-二(3-吡啶基)-2,6-吡啶羧酸二酰胺]与CuSO4.5H2O反应合成了新型大环双核铜配合物——[Cu2(H2L)2(SO4)2(H2O)6]·CH3OH·6H2O(1),其结构经IR,XRD和元素分析表征。1属单斜晶系,空间群P21/C,晶胞参数a=26.870(5),b=7.563 7(15),c=28.316(6),α=90°,β=114.91(3)°,γ=90°。1在催化2,6-二甲基苯酚氧化偶联反应时表现出较好的选择性及催化活性。  相似文献   

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A low barrier in the reaction pathway between the double Rydberg isomer of OH(3) (-) and a hydride-water complex indicates that the former species is more difficult to isolate and characterize through anion photoelectron spectroscopy than the well known double Rydberg anion (DRA), tetrahedral NH(4) (-). Electron propagator calculations of vertical electron detachment energies (VEDEs) and isosurface plots of the electron localization function disclose that the transition state's electronic structure more closely resembles that of the DRA than that of the hydride-water complex. Possible stabilization of the OH(3) (-) DRA through hydrogen bonding or ion-dipole interactions is examined through calculations on O(2)H(5) (-) species. Three O(2)H(5) (-) minima with H(-)(H(2)O)(2), hydrogen-bridged, and DRA-molecule structures resemble previously discovered N(2)H(7) (-) species and have well separated VEDEs that may be observable in anion photoelectron spectra.  相似文献   

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Summary Dichlorobis(methylsalicylato)titanium(IV) reacts with potassium or amine salts of dialkyl or diaryl dithiocarbamates in 11 and 12 molar ratios in anhydrous benzene (room temperature) or in boiling CH2Cl2 to yield mixed ligand complexes: (AcOC6H4O)2 Ti(S2CNR2)Cl (1) and (AcOC6H4O)2 Ti(S2CNR2)2 (2), R=Et, n-Pr, n-Bu, cyclo-C4H8 and cyclo-C5H10. These compounds are moisture sensitive and highly soluble in polar solvents. Molecular weight measurement in conjunction with i.r.,1H and13C n.m.r. spectral studies suggest coordination number 7 and 8 around titanium(IV) in (1) and (2) respectively.  相似文献   

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18.
Huang FQ  Ibers JA 《Inorganic chemistry》2001,40(10):2346-2351
The alkali metal/group 4 metal/polychalcogenides Cs(4)Ti(3)Se(13), Rb(4)Ti(3)S(14), Cs(4)Ti(3)S(14), Rb(4)Hf(3)S(14), Rb(4)Zr(3)Se(14), Cs(4)Zr(3)Se(14), and Cs(4)Hf(3)Se(14) have been synthesized by means of the reactive flux method at 823 or 873 K. Cs(4)Ti(3)Se(13) crystallizes in a new structure type in space group C(2)(2)-P2(1) with eight formula units in a monoclinic cell at T = 153 K of dimensions a = 10.2524(6) A, b = 32.468(2) A, c = 14.6747(8) A, beta = 100.008(1) degrees. Cs(4)Ti(3)Se(13) is composed of four independent one-dimensional [Ti(3)Se(13)(4-)] chains separated by Cs(+) cations. These chains adopt hexagonal closest packing along the [100] direction. The [Ti(3)Se(13)(4-)] chains are built from the face- and edge-sharing of pentagonal pyramids and pentagonal bipyramids. Formal oxidation states cannot be assigned in Cs(4)Ti(3)Se(13). The compounds Rb(4)Ti(3)S(14), Cs(4)Ti(3)S(14), Rb(4)Hf(3)S(14), Rb(4)Zr(3)Se(14), Cs(4)Zr(3)Se(14), and Cs(4)Hf(3)Se(14) crystallize in the K(4)Ti(3)S(14) structure type with four formula units in space group C(2)(h)()(6)-C2/c of the monoclinic system at T = 153 K in cells of dimensions a = 21.085(1) A, b = 8.1169(5) A, c = 13.1992(8) A, beta = 112.835(1) degrees for Rb(4)Ti(3)S(14);a = 21.329(3) A, b = 8.415(1) A, c = 13.678(2) A, beta = 113.801(2) degrees for Cs(4)Ti(3)S(14); a = 21.643(2) A, b = 8.1848(8) A, c = 13.331(1) A, beta = 111.762(2) degrees for Rb(4)Hf(3)S(14); a = 22.605(7) A, b = 8.552(3) A, c = 13.880(4) A, beta = 110.919(9) degrees for Rb(4)Zr(3)Se(14); a = 22.826(5) A, b = 8.841(2) A, c = 14.278(3) A, beta = 111.456(4) degrees for Cs(4)Zr(3)Se(14); and a = 22.758(5) A, b = 8.844(2) A, c = 14.276(3) A, beta = 111.88(3) degrees for Cs(4)Hf(3)Se(14). These A(4)M(3)Q(14) compounds (A = alkali metal; M = group 4 metal; Q = chalcogen) contain hexagonally closest-packed [M(3)Q(14)(4-)] chains that run in the [101] direction and are separated by A(+) cations. Each [M(3)Q(14)(4-)] chain is built from a [M(3)Q(14)] unit that consists of two MQ(7) pentagonal bipyramids or one distorted MQ(8) bicapped octahedron bonded together by edge- or face-sharing. Each [M(3)Q(14)] unit contains six Q(2)(2-) dimers, with Q-Q distances in the normal single-bond range 2.0616(9)-2.095(2) A for S-S and 2.367(1)-2.391(2) A for Se-Se. The A(4)M(3)Q(14) compounds can be formulated as (A(+))(4)(M(4+))(3)(Q(2)(2-))(6)(Q(2-))(2).  相似文献   

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Pure, highly explosive CF(3)C(O)OOC(O)CF(3) is prepared for the first time by low-temperature reaction between CF(3)C(O)Cl and Na(2)O(2). At room temperature CF(3)C(O)OOC(O)CF(3) is stable for days in the liquid or gaseous state. The melting point is -37.5 degrees C, and the boiling point is extrapolated to 44 degrees C from the vapor pressure curve log p = -1875/T + 8.92 (p/mbar, T/K). Above room temperature the first-order unimolecular decay into C(2)F(6) + CO(2) occurs with an activation energy of 129 kJ mol(-1). CF(3)C(O)OOC(O)CF(3) is a clean source for CF(3) radicals as demonstrated by matrix-isolation experiments. The pure compound is characterized by NMR, vibrational, and UV spectroscopy. The geometric structure is determined by gas electron diffraction and quantum chemical calculations (HF, B3PW91, B3LYP, and MP2 with 6-31G basis sets). The molecule possesses syn-syn conformation (both C=O bonds synperiplanar to the O-O bond) with O-O = 1.426(10) A and dihedral angle phi(C-O-O-C) = 86.5(32) degrees. The density functional calculations reproduce the experimental structure very well.  相似文献   

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