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1.
Reactions of lead(Ⅱ) nitrate or perchlorate with bis(3,5-dimethylpyrazolyl)methane (dmpzm), produced two new Pb(Ⅱ) chelated complexes [Pb(dmpzm)2X2] (X=NO3^- 1, ClO4^- 2). Both compounds were structurally characterized by elemental analysis, IR spectroscopy, thermal analysis, and single crystal X-ray diffraction. Both compounds are mononuclear with a distorted square antiprismatic PbN4O4 coordination geometry incorporating a pair of O,O'-bidentate anions and N,N'-bidentate dmpzm ligands. In the crystals of 1 or 2, the methyl or methylene groups of dmpzm ligand interact with the oxygen atoms of nitrates or perchlorates to afford intra- and intermolecular hydrogen bonding, thereby forming a two-dimensional network 1 or a three-dimensional structure 2. 相似文献
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通过双吡唑基甲基锂与二苯基乙烯基碘化锡的反应, 合成了桥头碳上带有乙烯基锡修饰的双吡唑甲烷配体。在回流的THF中这些乙烯基锡修饰的双吡唑甲烷配体(R3SnCHPz2, R3Sn为三乙烯基锡或二苯基乙烯基锡;Pz代表取代吡唑)与M(CO)5THF (M = Mo或W)反应产生杂双金属化合物R3SnCHPz2M(CO)3。在这些化合物中,一个乙烯基以h2方式配位到金属钼或钨上,双吡唑甲烷表现为一个三齿k3-(p,N,N)配体。(CH2=CH)3SnCH(3,5-Me2Pz)2W(CO)3和Ph2(CH2=CH)SnCH(3,5-Me2Pz)2W(CO)3与I2的反应也被研究。前者给出化合物CH2(3,5-Me2Pz)2W(CO)4,而后者随着有机锡的丢失产生四元金属杂环化合物CH(3,5-Me2Pz)2W(CO)3I。用PhSNa处理该四元金属杂环化合物导致碘负离子被取代,得到化合物CH(3,5-Me2Pz)2W(CO)3SPh。 相似文献
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杂环化合物1 苯基 3 甲基 4 吡唑啉 5 酮(HPMP)为β 二酮,不仅可用作金属离子的萃取剂,还可用于核磁共振的位移试剂,也可用于激光、催化、生化、医学等领域[1-4]。我们从PMP出发,合成了它的Co(Ⅱ),Ni(Ⅱ),Cu(Ⅱ)和Zn(Ⅱ)的络合物[5,6]。利用单晶X 射线衍射分析方法报道了标题化合物的晶体结构。1 实验部分在合成PMP席夫碱化合物的过程中,得到标题化合物的单晶体。元素分析结果(括号内为计算值)C%:69 87(69 98),H%:5 62(5 59),N:15 61(15 55)。红外光谱(KBr):1645和1637cm-1的强吸收峰归属为羰基的伸缩振动,… 相似文献
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对双吡唑烷ⅥB金属羰基配合物的电化学特性进行了系统研究,结果表明,吡唑环上的取代基极大的影响双吡唑烷ⅥB金属羰基配合物金属中心的峰电位E1/2。给电子代取代基增强配体的配位能力且使金属中心的E1/2减小,而吸电子取代基减弱配体的配位能力使金属中心的E1/2增大。 相似文献
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4-酰基-双(1,3-二苯基-5-吡唑啉酮)铽(Ⅲ)配合物的和成及荧光性质 总被引:2,自引:0,他引:2
合成了3种4-酰基-双(1,3-二苯基-5-吡唑啉酮),1,5-双(1′,3′-二苯基-5′-吡唑啉酮-4′-基)-1,5-戊二酮;1,6-双(1′,3′-二苯基-5′-吡唑啉酮-4′-基)-1,6-己二酮和1,10-双(1′,3′-二苯基-5′-吡唑啉酮-4′-基)-1,10-癸二酮,通过元素分析,红外光谱和核磁共振氢谱对产物组成进行了表征,合成了它们的Tb(Ⅲ)二元和三元[1,10-二氮杂菲(Phen)或2,2′-联吡啶(Dipy)]配合物,测定了配合物的荧光光谱,对其荧光性质进行了研究,结果表明,配合物发射Tb(Ⅲ)的特征荧光,4-酰基0双(1,3-二苯基-5-吡唑啉酮)配体的三重态能级与Tb(Ⅲ)的最低激发态(5D4)能级匹配较好,配合物荧光强度随4-酰基-双(1,3-二苯基-5-吡唑啉酮)配体2个吡唑环间碳链的增长而减弱,第2配体Phen和Dipy具有荧光增强作用,且前者优于后者。′ 相似文献
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IntroductionPoly(pyrazol 1 yl)alkanes,especiallybis(pyrazol 1 yl)alkanes ,havebeenoneofpopularpolydentatenitrogendonorligandssinceTrofimenko’sfirstreport1andJulia’slatermodification .2 Ithasbeenfoundthatthecoordinationbehavioroftheseligandscaneasilybeadjustedbychang ingtheelectronicandstericcharacteristicsofsubstituentsonthepyrazolering .Recentinvestigationshavealsoshownthatthecentralcarbonatomoftheseligandscanbemodifiedbythevariousfunctionalgroupstoformversatileheteroscorpionateligands ,wh… 相似文献
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用 X射线方法测定了二 (对氯苄基 )二氯化锡的晶体结构,该化合物晶体属单斜晶系,空间群为 C2/c,晶体学参数: a=2.8010(3), b=0.4882(2), c=1.2174(3)nm,β =111.71(1)°, V=1.5467(7) nm3, Z=4, Dx=1.893g· cm- 3,μ (MoKα )=23.24cm- 1, F(000)=856.00, R=0.025, Rw=0.038, Sn C键长为 0.2148(3)nm, Sn Cl键长为 0.23754(9)nm。空间构型为畸变四面体构型的单分子有机锡化合物。 相似文献
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不对称取代双(吡唑)甲烷VIB羰基金属化合物的合成及表征 总被引:1,自引:0,他引:1
3-苯基吡唑与二溴甲烷在相转移催化下反应,得到(3-苯基吡唑-5'-苯基吡唑)甲烷(1)和双(3-苯基吡唑)甲烷(2)的混合物.当该混合配体与M(CO)6(M=Cr,Mo,W)在光照下反应时,分离得到了不对称取代的(3-苯基吡唑-5'-苯基吡唑)甲烷四羰基铬(3),钼⑷和钨(5).用X-射线衍射测定了化合物5的晶体结构.结果表明,该晶体属于单斜晶系,P2(1)/n空间群,a=1.7976(7) rnn,b=1.3210(5) nm, c=1.8681(7) nm;β=98.293(8)°, V=4.390(3) nm3, Z=8,最终结构偏离因子[I>2σ(I)]=0.0516, Rw=0.0898, GOF=0.879.两个苯基分别处于两个吡唑的3位及5'位. 相似文献
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通过三苯基锡基-双(3,5-二甲基吡唑)甲烷与羰基钼的反应合成了钼锡键合的四元金属杂环化合物CH(3,5- Me2Pz)2Mo(CO)3SnPh3 (Pz=1-吡唑基). 当用叔丁基异腈处理该化合物及其钨类似物时, 伴随着有机锡结构单元的丢失, 金属钼(钨)上发生还原消除并分解得到化合物CH2(3,5-Me2Pz)2M(CO)3(CNBu-t) (M为Mo或W). 另外, 该化合物与三苯基膦或亚磷酸甲酯及异丙酯反应时, 只发生羰基取代反应得到化合物CH(3,5-Me2Pz)2Mo(CO)2(PR3)SnPh3 (R为苯基、甲氧基及异丙氧基). 而用亚磷酸苯酯与之反应, 除得到羰基取代产物外, 还伴随着P-O/C键的交换, 得到金属钼上还原消除的产物(PhO)2PCH(3,5-Me2Pz)2Mo(CO)3. 相似文献
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Liang-Fu Tang Wen-Li JiaZhi-Hong Wang Ji-Tao WangHong-Gen Wang 《Journal of organometallic chemistry》2002,649(2):152-160
The reaction of 3(5)-methylthio-5(3)-phenylpyrazole with dibromomethane under phase-transfer catalytic conditions only affords a new ligand, bis(3-phenyl-5-methylthiopyrazol-1-yl)methane. However, the reaction of 3(5)-methylthio-5(3)-p-methoxyphenylpyrazole or 3(5)-methylthio-5(3)-tert-butylpyrazole with dibromomethane under the same conditions yields three isomers, respectively, indicating that the substituents significantly affect the steric and electronic properties of pyrazole ring during the formation of ligands. Treatment of these potential polydentate ligands with M(CO)6 (M=Cr, Mo or W) under UV irradiation at room temperature affords (NN)M(CO)4 derivatives, in which some complexes contain asymmetric substituted bis(pyrazol-1-yl)methane ligands. The X-ray crystal structure analyses indicate that the sulfur atoms in these complexes do not take part in the coordination to the metal centers, and S-rich bis(pyrazol-1-yl)methanes actually act as bidentate chelating ligands by two nitrogen atoms. It is also interesting that in order to reduce the repulsion of methyl groups with carbonyls, the methyl groups in these complexes are oriented away from the metal centers. 相似文献
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《Journal of Coordination Chemistry》2012,65(7):783-789
Reaction of M(CO)6 with 3,5-dimethyl-4-ferrocenylmethylpyrazole under UV irradiation yields monosubstituted group 6 metal carbonyl complexes M(CO)5L (M?=?Cr, Mo or W; L?=?3,5-dimethyl-4-ferrocenylmethylpyrazole). Their electrochemical behaviour, investigated by cyclic voltammetry, indicates that chromium and tungsten complexes exhibit two one-electron quasi-reversible couples corresponding to the ferrocenyl group and the chromium or tungsten centre, respectively, while the molybdenum complex has one quasi-reversible couple corresponding to the ferrocenyl group and one irreversible oxidation process for molybdenum. The crystal structure of W(CO)5L, determined by X-ray diffraction methods, shows that ferrocenylpyrazole acts as a monodentate ligand, and W is six-coordinate with quasi-octahedral coordination geometry. The complex is linked into a one-dimensional chain in the lattice through weak intermolecular hydrogen bonds with metal carbonyls acting as acceptors. 相似文献
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本文研究了羰基钼(钨)与双(1-甲基咪唑-2-基)甲酮和双(1-甲基咪唑-2-基)甲烷以及双(1-甲基咪唑-2-基)乙烯的反应,获得了6个双齿螯合的双(1-甲基咪唑-2-基)甲酮,双(1-甲基咪唑-2-基)甲烷和双(1-甲基咪唑-2-基)乙烯四羰基金属衍生物,以及1个单齿配位的双(1-甲基咪唑-2-基)乙烯五羰基钨化合物。它们的结构通过红外,核磁以及X-射线单晶衍射分析得到确证。所有这些新化合物的电化学测试表明,它们只存在一个不可逆的氧化过程。 相似文献
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合成了2-[1-(3-叔丁基)吡唑基甲基]吡啶(CH2(Py)(3-ButPz)),并研究了羰基钼(钨)与该配体及其类似物2-(1-吡唑基甲基)吡啶(CH2(Py)(Pz))和2-[1-(3,5-二甲基)吡唑基甲基]吡啶(CH2(Py)(3,5-Me2Pz))的反应,合成了6个含双齿螯合的2-(1-吡唑基甲基)吡啶类配体的四羰基金属衍生物CH2(Py)(3-ButPz)M(CO)4,CH2(Py)(Pz)M(CO)4和CH2(Py)(3,5-Me2Pz)M(CO)4(M=Mo或W)。当用SnCl4处理CH2(Py)(3,5-Me2Pz)M(CO)4时,Sn-Cl键对金属中心发生氧化加成得到2个杂双核金属有机化合物CH2(Py)(3,5-Me2Pz)M(CO)3(Cl)SnCl3。所有新化合物均通过了红外和核磁的表征,CH2(Py)(3-ButPz)W(CO)4和CH2(Py)(3,5-Me2Pz)W(CO)3(Cl)SnCl3的结构还得到了X-射线单晶衍射的确证。用循环伏安法测定了四羰基金属衍生物的电化学性质。 相似文献
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Two novel tricarbonyl rhenium complexes based on the bidentate heterocyclic N–N ligands [bis(pyrazol-1-yl)methane(bpzm) and bis(3,5-dimethylpyrazol-1-yl)methane(bdmpzm)] have been synthesized by heating at reflux [Re(CO)5Cl] with the appropriate N–N ligand in toluene. The compounds have been characterized by IR and UV–Vis spectroscopy and X-ray analysis. Density functional theory (DFT) and time-dependent (TD) DFT calculations have been carried out for the [Re(CO)3(bdmpzm)Cl] complex. 相似文献