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The compound [{Pt4(en)4(NHCOtBu)4}{Tl(18-crown-6)}2](PF6)6 has been synthesized by a simple one-pot multicomponent reaction. Its structure was determined by X-ray single crystal diffraction analysis. The cation of the compound consists of one linearly arranged [Pt4(en)4(NHCOtBu)4]4+ chain and two [Tl(18-crown-6)]+ ions located at the two ends of the platinum chain. The complex crystallizes in a triclinic P1 with a=1.060 5(1), b=1.252 3(1), c=2.015(2) nm, α=107.430(2)°, β=91.032(2)°, γ=101.910(2)°, V=2.489 6(4) nm3, Z=2, R1=0.074 4, wR2(I>2σ(I))=0.222 5, S=1.062. CCDC: 294083. 相似文献
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[Cu(NBOCTB)](ClO4)2·2DMF的合成、晶体结构和热分解过程研究 总被引:2,自引:0,他引:2
李晓燕 《高等学校化学学报》1994,15(11):1597-1601
制备了二(N,N-二甲基甲酰胺)-高氯酸N,N,N'',N''-四[(1''-苄基-2''-苯并咪唑)甲基]-1,2-环己二胺合铜(Ⅱ){[Cu(NBOCTB)](ClO4)2·2DMF}.X射线测定表明其晶体属三斜晶系,空间群P1,晶胞参数α=1.1851(5)nm,b=1.2255(3)nm,c=2.5237(5)nm;α=92.37(2)°,β=98.01(2)°,γ=107.82(3)°,V=3.442(4)nm3,M=1403.93,Z=2,Dx=1.36g/cm3,μ=4.60cm(-1),F(000)=1470.TG-DTG技术研究结果表明,配合物的热分解过程分为以下4个阶段:(19941106-1597-1.jpg) 相似文献
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The title compound was synthesized by reaction of Cu(ClO4)2, picolinic acid and carbamide in C2H5OH/CH3CN solution, and characterized by single-crystal X-ray diffraction. It crystallizes in the orthorhombic system, space group Pbca with a=14.0481(8), b=9.0130(5), c=18.626(1)?, V=2358.3(2)?3, Z=4, Dx=1.771g·cm-3, μ=1.235mm-1 and F(000)=1276. The final R factor is 0.0440 for 1434 observed reflections. The X-ray analysis revealed that the copper(Ⅱ) atom is coordinated by two picolinic ligands in the equatorial plane, while the two oxygen atoms of perchlorate occupy the axial positions of octahedron with lengthened Cu-O distances, resulting in a 4+2 elongated octahedral environment. In the compound, there also exist two protonated carbamide cations for charge balance. CCDC: 195354. 相似文献
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The mixed-valence manganese(Ⅲ/Ⅳ) complex [Mn2(cyclen)2(μ-O)2](ClO4)3-4H2O (1) (cyclen=1,4,7,10-tetraazacyclododecan) with chemical formula C16H48Cl3Mn2N8O18 has been synthesized and characterized by single crystal X-ray diffraction analysis, elemental analysis, IR and electronic spectra. The results showed that the manganese(Ⅲ/Ⅳ) ions were six-coordinated by four nitrogen atoms from cyclen and two oxygen atoms from the oxygen bridge, forming a distorted octahedron geometry. There were two very strong peaks in the range of 400-700 nm in electronic spectrum, which was similar to Mn catalase and Mn ribonucleotide reductase extracted from organisms.Electrochemical study indicated that the complex underwent a quasi-reversible one-electron reduction and oxidation at E1/2=0.827 V in acetonitrile. 相似文献
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[Cu(TO)2(H2O)4](PA)2 was prepared by mixing the aqueous solution of 1,2,4-triazol-5-one(TO) and Cu(PA)2. The molecular structure and crystal structure of the title complex was determined by X-ray single crystal diffraction method. The crystal is triclinic, space group with a=0.7321(1)nm,b=0.7474(2)nm,c=1.3649(3)nm;α=88.65(2)°,β=85.63(1)°,γ=63.35(1)°;V=0.6655(2)nm3,Z=1. The Cu2+ coordinated with two TO molecule through its 2-nitrogen atom and four water molecules and showed an octahedral configuration. 相似文献
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The γ-hydroxypropyl-functionalised diiron dithiolate complex [Fe2(CO)6(μ-SCH2CH2CH2OH)2] is prepared upon thermolysis of Fe3(CO)12 and HO(CH2)3SH and further reaction with dppm (dppm = Ph2PCH2PPh2) affords [Fe2(CO)4(μ-dppm)(μ-SCH2CH2CH2OH)2]. From the reaction of Fe3(CO)12 with dppm(S2) a minor product is the tetrairon cluster, [{Fe2(CO)6(μ-SCH2CH2CH2OH)}2(μ4-S)], the mode of formation of which is unclear. It has been crystallographically characterised and adopts a μ4-S bridged double butterfly structure which is compared with other crystallographically characterised complexes of this type.
Electronic supplementary material The online version of this article (doi:) contains supplementary material, which is available to authorized users. 相似文献
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Reactions of [(dtc)2Mo2(S)2(μ-S)2] with one or two equivalents of CuBr in CH2Cl2 afforded two new heterobimetallic sulfide clusters, [(dtc)2Mo2(μ3-S)(μ-S)3(CuBr)] (1) and [(dtc)2Mo2(μ3-S)4(CuBr)2] (2). Both compounds were characterized by elemental analysis, IR, UV-vis and X-ray analysis. Compound 1 contains a butterfly-shaped Mo2S4Cu core in which one CuBr unit is coordinated by one bridging S and two terminal S atoms of the [(dtc)2Mo2(S)2(μ-S)2] moiety. In the structure of 2, one [(dtc)2Mo2(S)2(μ-S)2] moiety and two CuBr units are held together by six Cu-μ3-S bonds, forming a cubane-like Mo2S4Cu2 core. 相似文献
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Oxo/hydoxo zirconium(IV) complex of the general formula [Zr6(μ3-O)4(μ3-OH)4(OOCCH2tBu)9(μ2-OH)3]2 has been isolated, when Zr(OiPr)4 reacted with a 2-fold excess of 3,3-dimethylbutyric acid. Single crystal X-ray diffraction data, collected at 103 and 153 K, showed that the studied compound crystallizes in hexagonal system (P63/m (no. 176)). Structure consists of dimers composed of [Zr6(μ3-O)4(μ3-OH)4(OOCCH2tBu)9] sub-units, linked by six μ2-OH bridges. Infrared spectroscopic studies proved the presence of hydroxo groups in the structure of studied clusters and formation of different types of oxo/hydroxo bridges. The application of variable temperature infrared spectroscopy and differential scanning calorimetry revealed that the structure of this complex undergoes the phase transitions at 143–183 and 203–293 K. Comparison of spectral and crystallographic data suggests that these phase transitions might be related to changes in the strength of Zr–O bonds of μ2-OH bridges linking complex sub-units, and change in symmetry of the crystal lattice (from hexagonal to trigonal). Analysis of thermogravimetric data showed that decomposition of [Zr6(μ3-O)4(μ3-OH)4(OOCCH2tBu)9(μ2-OH)3]2 proceeds with complete conversion to ZrO2 (monoclinic form) between 603 and 803 K. 相似文献
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The compounds [{VO(O2)2(NH3)}2{μ-Cu(NH3)4}] (1) and [Zn(NH3)4][VO(O2)2(NH3)]2 (2) were prepared and characterized by elemental analysis and infrared spectra. The single crystal X-ray study revealed that the structure of 1 consists of trinuclear complex molecules [(NH3)OV(O2)2{μ-Cu(NH3)4}(O2)2VO(NH3)] with a rare heterobimetalic peroxo bridge: copper(II)–peroxo ligand–vanadium(V). The structure of 2 is composed of tetraamminezinc(II) cations and ammineoxodiperoxovanadate(V) anions. In course of thermal decomposition of 1 performed up to 620 °C, the following intermediate products: [Cu(NH3)2(VO3)2], and subsequently a mixture of V2O5 with monoclinic β-Cu2V2O7, were gradually formed. The final product of decomposition is Cu(VO3)2. The thermal decomposition of 2 is a two-step process. In the first stage, [Zn(NH3)3(VO3)2] as supposed intermediate was formed, which transformed at higher temperatures by release of ammonia molecules to the monoclinic modification of Zn(VO3)2. 相似文献
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混合价双核锰配合物[(bipy)2Mn(μ-O)2Mn(bipy)2](ClO4)3的合成晶体结构及性能 总被引:4,自引:0,他引:4
[Mn3O(O2CCH2Cl)6(C5H5N)2(H2O)]·CH2ClCOO·H2O在pH=4.5的HOAcNaOAc的缓冲水溶液中和2,2′联吡啶(bipy)反应,制得了混合价双核锰配合物[(bipy)2Mn(μ-O)2Mn(bipy)2](ClO4)3·1.5H2O。该配位化合物的X射线单晶衍射表明,该晶体属单斜晶系,空间群P21/c,晶胞参数:a=1.3854(3),b=1.3943(3),c=2.4225(5)nm,β=103.30°,V=4.554(2)nm3,Z=4,Dc=1.448g·cm-3。其紫外可见光谱在640nm处有一个峰,可指派为桥配体O2-到Mn(Ⅲ)的电荷迁移光谱.循环伏安实验说明,此配合物在半波电位E1/2为1.25V处,有一个可逆的氧化还原峰,这相应于(Ⅲ,Ⅳ)态氧化为(Ⅳ,Ⅳ)态,另外在0.37V处有一阴极峰,相应于(Ⅲ,Ⅳ)态还原为(Ⅲ,Ⅲ)态,在0.81V处有一氧化峰,相应于(Ⅲ,Ⅲ)态氧化为(Ⅲ,Ⅳ)态,这两个峰是不可逆的。 相似文献
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Thermodynamical data of rare earth complexes with amino acid are important for engineering chemistry and fundamental chemistry.
However, they have rarely been reported. In this work, a series of crystalline complexes of rare earth perchlorate coordinated
with glutamic acid have been synthesized in water medium, and their thermodynamical data, including the heat capacity in low
temperature range and the standard enthalpy of formation, were determined. These complexes were identified to be [RE2(Glu)2(H2O)8](ClO4)4·H2O (RE = Nd, Eu, Dy) by using thermogravimetric analysis (TG), differential thermal analysis (DTA), and chemical and elementary
analyses. Their purity has been determined. No melting points were observed for all the three complexes. The heat capacity
of the complexes was measured by an adiabatic calorimeter from 79 to 370 K. Abnormal heat capacity values were detected for
two of the complexes and the decomposition range of one complex was found. The temperature, enthalpy change and entropy change
of the decomposition processes of the three complexes were calculated. The polynomial equations of heat capacity in the experimental
temperature range have been obtained by least squares fitting. The standard enthalpy of formation was determined by an isoperibol
reaction calorimeter at 298.15 K.
Supported by the Research Fund of Beijing Institute of Petro-Chemical Technology (N06-06) 相似文献
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The new dinuclear copper(I) complex, [Cu2((Me-Pk)2En)(PPh3)4](ClO4)2 · 2CHCl3 (I), where (Me-Pk)2En = N,N′-bis(1-pyridin-2-yl-ethylidene)ethane-1,2-diamine), has been synthesized and characterized by elemental analyses,
FT-IR, and single-crystal X-ray diffraction method. In this complex, two Cu(PPh3)2 units are connected by one (Me-Pk)2En bridging ligand. The coordination geometry around each copper(I) atom is a distorted tetrahedron formed by two N atoms
from (Me-Pk)2En and two P atoms from the PPh3 ligands. The distance between two copper atoms is 7.06(1) ?. 相似文献
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利用微波技术合成了配合物[Gd2(Gly)6(H2O)4](ClO4)6(H2O)5, 进行了化学成分分析、红外表征和热重分析. 应用X衍射仪测定其晶体结构, 该晶体为一维链结构, 属三斜晶系, P 空间群, 晶胞参数: a=1.1569(17) nm, b=1.4138(2) nm, c=1.5642(2) nm, α=96.910(2)°, β=102.735(2)°, γ=105.512(2)°, V=2.3606(6) nm3, Z=2, Dc=2.144 g•cm-3. 采用精密溶解-反应量热计, 通过设计热化学循环, 计算出了该配合物的标准摩尔生成焓为 -(7960.73±3.23) kJ•mol-1. 相似文献
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A Cu(Ⅰ) complex with mix ligands [Cu(HIm)2(PPh3)2](BF4) was synthesized and characterized by elemental analysis, IRspectroscopy and X-ray diffraction crystallography. The crystal belongs to monoclinic system and P21/c space group, with cell parameters, a=1.2836(3)nm, b=1.5089(3)nm, c=2.0661(4)nm, α=90°, β=101.464(4)°,γ=90°, V=3.9219(13)nm3, Z=4 and Dc=1.374mg·m-3. The Cu(Ⅰ) is coordinated by two Patoms from triphenylphosphine and two Natoms from imidazole to form the distorted tetrahedral geometry. 相似文献
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A new polymer azido-bridged copper(II) complex [Cu4(En)2(μ1,1-N3)4(μ1,1,1-N3)2(μ1,3-N3)2]
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(I) (En = ethylenediamine) has been synthesized and crystallography characterized. Complex I shows one-dimensional coordination polymeric structure based on a tetranuclear cluster unit [Cu4(En)2(μ1,1-N3)4(μ1,1,1-N3)2(μ1,3-N3)2], in which the azido ions display three different bridging modes. 相似文献
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合成了一种稀土高氯酸盐-谷氨酸配合物. 经TG/DTG、化学和元素分析、FTIR及与相关文献对比, 确定其组成为[Pr2(L-α-Glu)2(ClO4)(H2O)7](ClO4)3•4H2O, 纯度为99.0%以上. 利用显微熔点仪分析发现其没有熔点. 在78~370 K温区, 用精密绝热量热仪测量其低温热容, 在285~306 K温区发现一明显吸热峰, 归结为固-固相变过程. 通过相变温区三次重复热容测量, 得到相变温度Ttr、相变焓ΔtrHm和相变熵ΔtrSm分别为(297.158±0.280) K, (12.338±0.016) kJ•mol-1和(41.520±0.156) J•K-1•mol-1. 用最小二乘法将非相变温区的热容对温度进行拟合, 得到了热容随温度变化的两个多项式方程. 用此方程进行数值积分, 得到每隔5 K的舒平热容值和相对于273.15 K的热力学函数值. 根据TG/DTG结果, 推测了该配合物的热分解机理. 依据Hess定律, 选择1 mol•dm-3盐酸为量热溶剂, 利用等温环境溶解-反应量热计, 测定了该配合物的标准摩尔生成焓为: ΔfHm0=-(7223.1±2.4) kJ•mol-1. 相似文献
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The complex [Mn(bipy)3]·(ClO4)2 was synthesied and characterized by X-ray diffraction. X-ray diffraction result for the single crystal showed that the crystal belongs to triclinic, space group P1, a=0.8123(2),b=1.1024(2), c=1.8646(4)nm,α=102.30(3)°,β=91.00(3)°,γ=99.69(3)°,V=1.6056(6)nm3,Z=2,Dc=1.494g·cm-3. The thermal decomposition of [Mn(bipy)3](ClO4)2 occurred in a three steps pattern. The reaction mechanism of the first step decomposition was deduced as n(1-α)[-ln(1-α)](n-1)/n with the activation energy of 130kJ·mol-1. 相似文献