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1.
Reaction of 1,3-thiazolidine-2-thione with tellurium(IV) in hydrobromic acid medium gave the hexabromotellurate, [C6H9N2S3]22+[TeIVBr6]2− (3). Reaction of 1-methylimidazoline-2-(3H)-thione (L″) with tellurium(IV), in hydrobromic acid medium, gave the mixed-ligand tellurium(II) complex [TeIIL″3Br]+Br− (4). The structures of [C6H9N2S3]22+[TeIVBr6]2− (3) and [TeIIL″3Br]+Br− were determined by single crystal X-ray diffraction methods. In 3 the unit cell contains [TeBr6]2− anions and two [C6H9N2S3]+ cations. There is no direct bonding between the metal atom and the cations. In the anion only slight angular deviations from the perfect octahedral geometry are observed. The lone pair of electrons on tellurium(IV) is found to be stereochemically inert. In the cation the two five-membered heterocyclic rings adopt different conformations. In complex 4, in the solid state, the planar [TeIIL″3Br]+ cation and Br− anion are held together by ionic interactions. In the cation, L″ is bonded to the central tellurium atom through the sulphur atom. 相似文献
2.
Elena Bermejo Alfonso Castieiras Douglas X. West 《Journal of Molecular Structure》2003,650(1-3):93-97
Condensation of thiosemicarbazide or N(4)-ethylthiosemicarbazide with 1,2,8,9-tetraphenyl-3,7-diazanona-1,9-dione in the presence of copper(II) acetate in 96% ethanol leads to Δ6-5,6-diphenyl-5-methoxy-1,2,4-triazacyclohexene-3-thione, C16H15N3OS, or Δ6-4-methyl-5,6-diphenyl-5-ethoxy-1,2,4-triazacyclohexene-3-thione, C18H19N3OS. For C16H15N3OS the crystal data are monoclinic, P21/c, a=9.7780(7), b=8.5120(3), c=18.2210(13) Å, β=100.958(3)°, V=1488.89(16) Å3, and Z=4 in agreement with an earlier report. For C18H19N3OS the crystal data are orthorhombic, P212121, a=8.6940(3), b=12.9946(3), c=15.5139(5) Å, V=1752.68(9) Å3, and Z=4. 相似文献
3.
新型金属-双二硫杂戊烯(M-BDT)配合物的合成、表征及X射线的指标化 总被引:2,自引:0,他引:2
合成了4个新型NiBDT配位化合物,BDT为具有9个S原子的杂戊烯.元素分析、IR谱、UV谱确定这4个新配合物的化学式分别为[(CH3)4N]2[Ni(C5S9)2](1),[(C2H5)4N]2·[Ni(C5S9)2](2),[(C4H9)4N]2[Ni(C5S9)2](3),[(C6H5)(CH3)3N]2[Ni(C5S9)2](4).采用Ito法对配合物1的X射线粉末图进行了指标化,确定该晶体属单斜晶系,简单晶格,晶胞参数:a=0.680nm,b=0.714nm,c=2.302nm,γ=111.4°,Z=2. 相似文献
4.
硫代嘧啶碱基是光动力疗法潜在的重要光敏剂,其最低单重激发态的光物理研究已有广泛报道。然而,其较高激发态的跃迁性质和反应动力学研究较为稀少。因此,本文采用共振拉曼光谱和密度泛函理论计算方法研究2,4-二硫代尿嘧啶的紫外光谱和几个较高单重激发态的短时结构动力学。首先,基于共振拉曼光谱强度与电子吸收带振子强度f的关系,将紫外光谱去卷积成四个吸收带,分别为358 nm(f=0.0336)中等强度吸收带(A带),338 nm(f=0.1491)、301 nm(f=0.1795)和278 nm(f=0.3532)强而宽的吸收带(B、C和D带)。这一结果既吻合密度泛函理论计算结果,又符合共振拉曼光谱强度模式对紫外光谱带的预期。据此,去卷积得到的四个吸收带被分别指认为S0→S2跃迁、S0→S6跃迁、S0→S7跃迁和S_0→S_8跃迁。同时,分别对B,C和D带共振拉曼光谱进行了详细的指认,获得了短时动力学信息。结果表明,S_8态短时动力学的显著特征是在Franck-Condon区域或附近发生了S8(ππ~*)/S(nπ~*)势能面交叉引发的、伴随超快结构扭转的非绝热过程。S7和S6态短时动力学的主要特征是反应坐标的多维性,它们分别沿C_5C_6/C_2S_8/C_4S_(10)/N_2C_3+C_4N_3H_9/N_1C_2N_3/C_2N_1C_6/C_6N_1H_7/C_5C_6H_(12)和C_5C_6/N_3C_2/C_4S_(10)/C_2S_8+C_6N_1H_7/C_5C_6H_(12)/C_5C_6N_1/C_5C_6H_(12)/C_2N_1C_6/N_1C_2N_3/C_4N_3H_9/N_1C_2N_3等内坐标演化。 相似文献
5.
Thermal decomposition of mixed ligand thymine (2,4-dihydroxy-5-methylpyrimidine) complexes of divalent Ni(II) with aspartate, glutamate and ADA (N-2-acetamido)iminodiacetate dianions was monitored by TG, DTG and DTA analysis in static atmosphere of air. The decomposition course and steps of complexes [Ni(C5H6N2O2)(C4H5NO4)2−(H2O)2]·H2O, [Ni(C5H6N2O2)(C5H7NO4)2−(H2O)2]·H2O and [Ni(C5H6N2O2)(C6H8N2O5)2−(H2O)2]·1.5H2O were analyzed. The final decomposition products are found to be the corresponding metal oxides. The kinetic parameters namely, activation energy (E*), enthalpy (ΔH*), entropy (ΔS*) and free energy change of decomposition (ΔG*) are calculated from the TG curves using Coats–Redfern and Horowitz–Metzger equations. The stability order found for these complexes follows the trend aspartate > ADA > glutamate. 相似文献
6.
(C6H(14)N2)[NH4(ClO4)3] is a newly developed porous hybrid inorganic-organic framework material with easy access and excellent detonation performances,however,its thermal properties is still unclear and severely hampered further applications.In this study,thermal behaviors and non-isothermal decomposition reaction kinetics of(C6H(14)N2)[NH4(ClO4)3] were investigated systematically by the combination of differential scanning calorimetry(DSC) and simultaneous thermal analysis methods.In-situ FTIR spectroscopy technology was applied for investigation of the structure changes of(C6H(14)N2) NH4(ClO4)3]and some selected referents for better understanding of interactions between different components during the heating process.Experiment results indicated that the novel molecular perovskite structure renders(C6H(14)N2)[NH4(ClO4)3] better thermal stability than most of currently used energetic materials.Underhigh temperature s,the stability of the cage skeleton constructed by NH4^+and ClO4^-ions determined the decomposition process rather than organic moiety confined in the skeleton.The simple synthetic method,good detonation performances and excellent thermal properties make(C6H(14)N2)[NH4(ClO4)3] an ideal candidate for the preparation of advanced explosives and propellants. 相似文献
7.
Michael B. Hursthouse Richard L. Short Brian Piggott Alan Tucker Swee Fatt Wong 《Polyhedron》1986,5(12):2121-2122
Dissolution of Mo2O5((CH3)2NCH2CH2NHCH2CH2S)2 in dimethylformamide results in the formation of a species without coordinated sulphur, as indicated by 95Mo NMR spectroscopy. Subsequent crystallization of this solution yielded the compound Mo4O12(C12H30N4S2)2(C3H7ON)2 which X-ray crystallography shows to consist of a novel Mo4O12 core, containing an eight-membered Mo4O4 ring with the two pairs of diagonal molybdenum atoms linked by disulphido-containing groups. 相似文献
8.
Two new open-framework gallium phosphites formulated as (C2N2H10)0.5Ga2(OH)(H2O)(HPO3)3(1) and (C3N2H5)2(C3N2H6)Ga8(H2O)6(HPO3)14(2) were hydrothermally synthesized in the presence of ethylenediamine(en) and imidazole as structure directing agents(SDA), respectively. Structural analyses reveal that the 3D structures of compounds 1 and 2 are both built up from the linkage of GaO6, GaO5(H2O) and HPO32? units by sharing vertices. The structure of compound 2 is constructed from well-known 4.6.12-net connecting layers in the AAAA stacking sequence, which are penetrated by the 1D Ga-O-P chains to form a 3D pillared-layered structure. 相似文献
9.
以磷钼酸、2-氨基吡啶、五氧化二钒、氯化锌和氯化镍等为主要原料,采用水热方法合成了2个簇基超分子化合物[H3PMo12O40]2[C5H6N2]6(1)和[H2PMo12V2O42][C5H6N2]5·3H2O(2)(C5H6N2=2-氨基吡啶).通过元素分析、红外光谱、紫外-可见光谱、X射线光电子能谱、热重分析、X射线单晶衍射及X射线粉末衍射等手段对化合物进行了结构表征.结构分析显示,簇单元不同的2个超分子化合物以各自独特的堆积方式形成三维超分子网络.利用苯乙烯的环氧化反应研究了2个化合物的催化性能. 相似文献
10.
The hexaaquacobalt(II)bis(phthalhydrazidato)tetrahydrate, [Co(H2O)6](C8N2O2H5)2·4H2O is examined using single crystal X-ray diffraction analysis. The crystals are triclinic, space group , with a = 9.757(1), b = 10.955(2), c = 11.106(1), = 100.79(2), β = 90.35(3), γ = 91.54(1) and Z = 2. In [Co(H2O)6](C8N2O2H5)2·4H2O, the cobalt(II) is coordinated by six water ligands and the [Co(H2O)6]2+ is associated with the two O-deprotonated phthalhydrazidato ions only by hydrogen bonds. The infrared and Raman spectra of phthalhydrazide (PH) and infrared spectra of deuterated derivative phthalhydrazide (PD) and of [Co(H2O)6](C8N2O2H5)2·4H2O are reported. The theoretical wavenumbers, infrared intensities and Raman scattering activities have been calculated using density functional (B3LYP) method with the 6-311++G(d,p) basis set. The calculated potential energy distribution has proved to be of great help in assigning the spectra PH, its deuterated derivative and [Co(H2O)6](C8N2O2H5)2·4H2O. The results from natural bond orbital (NBO) analysis for keto-hydroxy form of PH are presented. 相似文献
11.
Antony J. Deeming Caroline Whittaker Alejandro J. Arce Ysaura De Sanctis 《Journal of organometallic chemistry》1997,540(1-2):67-76
The cluster [Os3(CO)10(MeCN)2] reacts with indazole (C7H6N2) to give two isomeric products [0s3(μ-H)(μ-C7H5N2)(CO)10] in which the five-membered ring has been metallated with N-H cleavage to give an N,N-bonded isomer or with C-H cleavage to give a C,N-bonded isomer. These two isomers have very similar X-ray structures but can be clearly distinguished by 1H NMR methods. They are shown to correspond to related clusters derived from pyrazole. Benzotriazole (C6H5N3) also reacts (as shown earlier by others) to give two isomers: an N,N-bonded species [Os3(μ-H)(μ-C6H4N3)(CO)10] coordinated only through the five-membered ring and a minor C,N-bonded isomer [Os3(μ-H)(μ-C6H4N3)(CO)10], metallated at the C6 ring and coordinated through both rings. The former isomer reacts with Me3NO in acetonitrile to give [Os3(μ-H)(μ-C6H4N3)(CO)9(MeCN)] which thermally looses MeCN to produce the coupled product [Os6(μ-H)2(μ3-C6H4N3)2(CO)18] which was shown by X-ray structure determination to have all six nitrogen atoms coordinated to osmium, a novel situation for coordinated benzotriazole. The two Os3 units are linked together by an OsNNOsNN ring in a boat conformation with the whole cluster adopting C2 symmetry. 相似文献
12.
R. Bruce King 《Journal of organometallic chemistry》1995,500(1-2):187-194
The aryldiazenido ligands provide the fourth member of the isoelectronic series CO, NO+, RNC, RN2+ of ligands for transition metal complexes. The first aryldiazenido metal complex was reported in 1964 when p-CH3OC6H4N2Mo(CO)2C5H5 was prepared by the reaction of NaMo(CO)3C5H5 with p-CH3OC6H4N2+BF4−. This review surveys the development of organometallic aryldiazenido chemistry since that time. Such organometallic aryldiazenido derivatives, including RN2M(CO)2C5H5, RN2M(CO)2(Pz3BH) (M = Cr, Mo, W), [(η6-Me6C6)Cr(CO)2N2Ar]+, [(MeC15H4)M′(CO)2N2Ar]+ M′ = Mn, Re), [trans-PhN2Fe(CO)2(PPh3)2]+, and PhN2M′(CO)2(PPh3)2(PPh3)2 can be obtained by reactions of arenediazonium salts with suitably chosen transition metal nucleophiles. Analogous methods cannot be used to prepare alkyldiazenido transition metal complexes because of the instability of alkyldiazonium salts. However, the alkyldiazenido derivatives RCH2N2M(CO)2C5H5 (R = H or Me3Si) can be obtained from HM(CO)3C5H5 and the corresponding diazoalkanes. Important aspects of the chemical reactivity of RN2M(CO)2Q derivatives (Q = C5H5, Pz3BH) include CO substitution reactions, coordination of the second nitrogen in the RN2 ligand to give heterobimetallic complexes such as C5H5Mo(CO)2(μ-NNC6H4Me)(CO)2C5H5, oxidative addition rections with X2 X = Cl, Br, I), SnX4, RSSR, and CINO, and reactions with further RN2+ to give bis(aryldiazenido) derivatives (RN2)2MQL+ (L = CO, X−, etc.). Dearylation of an aryldiazenido ligand to a dinitrogen ligand can be effected by reaction of [(MeC5H4)M′(CO)2N2Ar]+ with certain nucleophiles to give (MeC5H4)M′(CO)2N2. 相似文献
13.
Tristram Chivers Robert W. Hilts Masood Parvez
Dusan Ristic-Petrovic
Kenneth Hoffman 《Journal of organometallic chemistry》1994,480(1-2):c4-c6The reaction of Ru(CO)4(C2H4) or Ru(CO)5 with 1,5-Ph4P2N4S2 in CH2Cl2/hexane at 23°C produces the dimer [Ru(CO)2(Ph4 P2N4S2)]2 (2), which was shown by X-ray crystallography to have a centrosymmetric structure in which the P2N4S2 ring is attached to one ruthenium atom through two (geminal) nitrogen atoms and the remote sulfur atom and serves as a bridge to the other ruthenium atom via the second sulfur atom. Crystals of 2 ·2(CH2Cl2) are triclinic, space group P
(No. 2), a = 12.901(1) Å, b = 13.072(1) Å, c = 10.123(1) Å, = 100.88(1)°, β = 98.90(1)°, γ = 67.50(1)°, V = 1542.4(3) Å, Z = 1 with final R and Rw values of 0.040 and 0.027, respectively. 相似文献
14.
The structures of the title compounds have been established by X-ray crystallography from diffractometer data. Crystals of the first (I), C4H8N4S, are monoclinic, space group P21/c, with a = 8.166(2), b = 10.481(1), c = 8.585(1) Å, β = 109.33(2)°, Z = 4, Dc = 1.381 g cm−3. Crystals of the second (II), C9H10N4S, are monoclinic, space group P21/c, with a = 11.850(4), b = 7.898(1), c = 23.981 (6) Å, β = 117.23(2)°, Z = 8, Dc = 1.373 g cm−3. Crystals of the third (III), C11H14N4S1 are also monoclinic, space group P21/c with a = 12.829(3), b = 8.348(1), c = 11.088(4) Å, β = 94.40(4)°, Z = 4, Dc = 1.314 g cm−3. The structures, determined by direct methods (I, III) and Patterson synthesis (II) were refined to R = 0.039 for 1070 reflections of I, R = 0.040 for 2792 reflections of II and R = 0.041 for 1900 reflections of III. The characteristic features of the planar five-membered rings are studied in comparison with the analogous 1,2,3-triazoles and imidazoles. It is shown that these planar rings exhibit only two patterns of the endocyclic bond angles induced dominantly by the number and relative position of the N-lone pairs. A similar effect of the double bonds (attached to C atoms) is also discussed. 相似文献
15.
Three small organic molecular co-crystal compounds (C3N6H6)·(C6H10O4)·H2O(1), C3H8N2O(3) and (H4btec)2·(4,4'-bipy)(4)(H4btec=1,2,4,5-benzenetetracarboxylic acid, 4,4'-bipy=4,4'-bipyridine) and one coordination supramolecular compound [Mn(C2O4)(H2O)2]·C6H11NO2(2) were synthesized by hydrothermal reaction. They were characterized by elemental analysis, infrared(IR) spectroscopy and single crystal X-ray diffraction(XRD). Structural analyses reveal that these 2D or 3D supramolecular networks of the compounds were formed by C―H···O, N―H···O, N―H···N, O―H···O and O―H···N hydrogen bonds. Therein, the functional groups of ―COOH, ―NH2 and ―OH play important roles in constructing supramolecular architectures. 相似文献
16.
Two novel phase transition materials,[C9H20N2] [Na(BF4)3] (1) and[C9H20N2] [(PF6)2] (2), were synthesized based on 1-isopropyl-1,4-diazabicyclo[2.2.2]octan-1-ium with sodium tetrafluoroborate and hexafluorophosphoric acid, respectively. Differential scanning calorimetry measurements detected that 1 and 2 underwent reversible phase transitions, which were confirmed by dielectric measurements. Single crystal X-ray diffraction data suggested that compound 1 changed from a high temperature phase with a space group of P63 to a low temperature one with a space group of P21/c, and that compound 2 transformed from the space group of Pbca at room temperature to P21/c at low temperature. Formation of hydrogen bonds and distortion of 1,4-diazabicyclo[2.2.2]octane rings may drive the transitions. 相似文献
17.
1-Methylpiperazine was employed to crystallize with 2,4-dihydroxybenzoic acid and 1,8-naphthalene acid, affording two multi-component hydrogen-bonding salts [(C5H14N2)2+·(C7H5O4)2-·H2O](1) and [(C5H14N2)2+(C12H6O4)2ˉ·2H2O](2). These two forms of salts are both monoclinic systems with space group P21/c(14). The lattice parameters of salts 1 and 2 are a=1.32666(10) nm, b=0.90527(7) nm, c=1.67107(13) nm, β=103.125(1)° and a=1.4950(2) nm, b=0.75242(15) nm, c=1.6563(3) nm, β=92.834(2)°, respectively. Expected classical hydrogen bonds N―H…O and O―H…O appear in the chargetransfer salts, and asymmetric units of these two forms both contain water molecules which play a significant role in building novel supramolecular architectures. Robust hydrogen-bond interactions between 1-methylpiperazine and aromatic acid provide sufficient driving force to direct the two crystals to three-dimensional structures. Weak interactions C―H…O emerging in salts 1 and 2 further enhance their crystal structures. As a consequence, hydrogen-bonding interactions in these compounds afford diverse 3D net supramolecular architectures. Thermal stability of these compounds was investigated by thermogravimetric analysis(TGA). 相似文献
18.
在水热和弱酸性反应条件下,螯合型表面活性剂前驱体乙二胺三乙酸分别与氯化锌、氯化钴反应,形成水合乙二胺三乙酸金属配合物[M(H2O)6][M(ED3A)(H2O)]2·2H2O[M=Zn(1),Co(2);H3ED3A=乙二胺三乙酸,C8H14N2O6]。 产物经元素分析、红外、热重、液体核磁共振和X射线单晶衍射结构表征。 乙二胺三乙酸和锌(Ⅱ)、钴(Ⅱ)五配位,并与水一起形成典型的[MN2O4]或[MO6]八面体结构。 13C核磁共振实验结果表明,溶液中乙二胺三乙酸与锌形成配合物在弱酸性条件下(pH值3~7)稳定存在,在酸性溶液中完全解离,乙二胺三乙酸进一步经分子内成环反应生成3-酮哌嗪二乙酸(H2kpda=C8H12N2O5)。 相似文献
19.
QU Xue-jian WANG Shuang ZHANG Dao-jun JING Xue-min ZHANG Li-rong LI Guang-hua HUO Qi-sheng LIU Yun-ling 《高等学校化学研究》2012,28(4):581-584
Two 1D coordination polymers Cu2I(C6N3H4)2(1) and CuII(C6N3H4)2·H2O(2) based on benzotriazole(Bta) were hydrothermally synthesized by controlling the crystallization temperature. Single-crystal X-ray diffraction (XRD) analyses reveal that compound 1 is a 1D tubular structure constructed from two types of 1D chains {-Cu-N=N-N-}n, where the Cu(I) ions adopt linear, triangular, and tetrahedral coordination modes to connect two types of Bta ligands via π-π interaction inside the tubular-like chain. For compound 2, the Cu(II) ions assume a quadrilateral coordination mode linking to the Bta ligands to give 1D straight chains, which stacks through π-π interactions to construct a 2D layer structure. Further characterizations including elemental analyses, infrared IR spectra, thermogravimetric(TG) analyses and luminescence properties have been done. 相似文献
20.
MoO2(C5H7O2)2, where C5H7O2 is 2,4-pentanedione (acac), reacts with 2-2′ pyridylbenzoxazole in acetone to give a product with stoichiometry, Mo3C24H16N6O12. This product dissolves readily in dimethylformamide to give a brown solution which on standing for several weeks yielded crystals. An X-ray structure determination showed these crystals to contain uncoordinated 2-2′pyridylbenzoxazole and [(CH3)2NH2]4+[Mo8O26]4−. 相似文献