共查询到19条相似文献,搜索用时 171 毫秒
1.
以间苯二甲酰肼、取代水杨醛和有机锡前体化合物进行一锅溶剂热法反应,合成了5个双(取代水杨醛)间苯二甲酰腙有机锡配合物m-Ph (CONH-N=CH (o-O) PhR1)(SnR2)2:R1=Naphth,R2=Cy (1); R1=3-t-Bu,R2=n-Bu (2); R1=5-F,R2=Ph (3); R1=4-Cl,R2=Ph (4); R1=3-t-Bu,R2=Ph (5)。经元素分析、红外光谱、(1H、13C和119Sn)核磁共振谱表征,并用X射线衍射方法确证了配合物1~5的晶体分子结构。配合物1~4为三斜晶系P1空间群,配合物5为单斜晶系P21空间群。中心锡与配位原子组成五配位畸形三角双锥构型。将水杨醛酰腙链与有机锡配位形成远离中心苯环的构型称为"反式",将与中心苯环取向相同的构型称为"顺式"。通过C1-C2或C4-C8单键旋转,中心苯环上的2个配位链发生构型翻转。配合物1形成"反-反"式构型,配合物2形成"顺-顺"式构型,配合物3、4和5形成"顺-反"式构型。荧光研究表明,配合物具有发光性能,特别是配合物1和4的有机溶液具有很强的荧光性能。 相似文献
2.
以间苯二甲酰肼、取代水杨醛和有机锡前体化合物进行一锅溶剂热法反应,合成了5个双(取代水杨醛)间苯二甲酰腙有机锡配合物m-Ph (CONH—N=CH (o-O) PhR1)(SnR2)2: R1=Naphth,R2=Cy (1); R1=3-t-Bu,R2=n-Bu (2); R1=5-F,R2=Ph (3); R1=4-Cl,R2=Ph (4); R1=3-t-Bu,R2=Ph (5)。经元素分析、红外光谱、(1H、13C和119Sn)核磁共振谱表征,并用X射线衍射方法确证了配合物1~5的晶体分子结构。配合物1~4为三斜晶系P>1空间群,配合物5为单斜晶系P21空间群。中心锡与配位原子组成五配位畸形三角双锥构型。将水杨醛酰腙链与有机锡配位形成远离中心苯环的构型称为“反式”,将与中心苯环取向相同的构型称为“顺式”。通过C1—C2或C4—C8单键旋转,中心苯环上的2个配位链发生构型翻转。配合物1形成“反-反”式构型,配合物2形成“顺-顺”式构型,配合物3、4和5形成“顺-反”式构型。荧光研究表明,配合物具有发光性能,特别是配合物1和4的有机溶液具有很强的荧光性能。 相似文献
3.
利用3,5-二氨基苯甲酸配体合成了2种新的配合物[Cd(diaba)(phen)2]NO3·H2O(1)和[Zn(diaba)(2,2’-bipy)2](2)(H2diaba=3,5-diaminobenzoicacid;phen=1,10-phenanthroline,2,2’-bipy=2,2’-bipyridine),并对其进行了元素分析、红外光谱和X射线单晶衍射测定。配合物1属于正交晶系,空间群为Fddd,a=1.42581(7)nm,b=2.56462(13)nm,c=3.09247(17)nm。配合物2属于单斜晶系,空间群为C2/c,a=1.27362nm,b=1.59278nm,c=1.51935nm,β=107.334°。配合物1和2都为单核晶体。配合物1的结构单元由1个CdⅡ、1个3,5-二氨基苯甲酸和2个phen构成。配合物2的结构单元由1个ZnⅡ、1个3,5-二氨基苯甲酸和2个2,2’-bipy构成。两种配合物再通过氢键或π-π堆积形成三维超分子网络。研究了配合物的热稳定性和荧光性质。 相似文献
4.
利用不同过渡金属盐在溶剂热中合成了2个新型杂核化合物{[CuEu2(INAIP)3(HCOO)(H2O)3]·3H2O}n(1)和{[NiEu2(INAIP)4(H2O)4]·4H2O}n(2)(INAIP=异烟酰胺吡啶基异酞酸根),并对其进行了元素分析、IR及X-射线衍射法表征。晶体结构研究表明:配合物1和2都属于三斜晶系,P1空间群。晶胞参数:配合物1a=1.0887(3)nm,b=1.5158(4)nm,c=1.5644(2)nm,V=2.3332(10)nm3,Z=2,Dc=1.955g·cm-3,μ=3.203mm-1,F(000)=1352,Rint=0.027,R1=0.0505,wR2=0.1309。配合物2a=1.0134(3)nm,b=1.0836(6)nm,c=1.3741(2)nm,V=1.4530(9)nm3,Z=1,Dc=1.878g·cm-3,μ=2.554mm-1,F(000)=818,Rint=0.0458,R1=0.0341,wR2=0.0869。配合物1是由配体异烟酰胺吡啶基异酞酸连接而成的三维二重贯穿sqc27拓扑结构,而配合物2是由配体异烟酰胺吡啶基异酞酸连接稀土铕离子形成二维层状结构,该二维层通过Ni-O和Ni-N键连接成三维非贯穿网络结构。配合物1和2具有典型的稀土铕离子红色荧光和高的热稳定性。 相似文献
5.
选择刚性的1,2,4,5-均苯四甲酸(H4L)为主配体,以1,3-双(1H-咪唑-1-基甲基)苯(1,3-bib)为辅助配体,在水热条件下,与过渡金属离子Cd2+配位合成了配合物[Cd(L)0.5(1,3-bib)(H2O)]·H2O(1)。利用元素分析、红外光谱、X射线单晶衍射、热重和X射线粉末衍射对其结构进行了表征,并研究了化合物的荧光性质。结果表明:配合物1属正交晶系,空间群Pbca,a=0.857 08(4)nm,b=1.912 23(10)nm,c=2.451 60(12)nm。配合物1中Cd2+与L4-配体的羧基通过双齿螯合配位,通过1,3-bib连接形成三维网状结构。配合物1具有较强的荧光,其对丙酮溶剂、MnO4-、Hg2+离子有一定的荧光猝灭。 相似文献
6.
甲醇中三环己基氢氧化锡分别与呋喃-2-甲酸、2,4,6-三甲基苯甲酸反应,合成了2个三环己基锡芳香羧酸酯Cy3SnO2CC4H3O(1)和Cy3SnO2CC6H2Me3(2)(Cy为环己基)。通过IR、1H和13C NMR、元素分析及X-射线单晶衍射表征结构。(1)和(2)均属单斜晶系,配合物(1)空间群P21,晶体学参数:a=0.82304(2)nm,b=1.11119(3)nm,c=1.28390(3)nm,β=101.090(2)°,Z=2,V=1.15227(5)nm3,Dc=1.381g·cm-3,μ(Mo Kα)=1.127mm-1,F(000)=496,R1=0.0529,wR2=0.1387。配合物(2)空间群P21/c,晶体学参数:a=0.99962(2)nm,b=1.41597(2)nm,c=1.97359(3)nm,β=94.0420(10)°,Z=4,V=2.78653(8)nm3,Dc=1.266g·cm-3,μ(Mo Kα)=0.937mm-1,F(000)=1112,R1=0.0540,wR2=0.1619。配合物(1)和(2)的中心锡原子均为畸变四面体构型。通过分子间氢键作用,配合物(1)形成二维网状结构。试验表明,配合物(1)和(2)具有良好的热稳定性,对人癌细胞Colo205、HepG2、MCF-7、Hela、NCI-H460增殖均有较强的抑制作用。 相似文献
7.
以3,3’,5,5’-(1,3-苯基)-联苯四羧酸(H4btb)与1,10-菲咯啉(phen)为配体,分别与硝酸镉和硝酸锌在水热条件下反应合成2个一维[Cd(H2btb)(phen)]n(1)和二维{[Zn2(btb)(phen)]·1.5H2O}n(2)配位聚合物,并对其进行了元素分析、红外光谱、热重分析和X-射线单晶衍射测定。配合物1属于单斜晶系,空间群为C2/c,晶胞参数:a=2.82845(13)nm,b=1.08554(5)nm,c=1.81768(8)nm,β=96.4850(10)°,V=5.5453(4)nm3,Z=8,Dc=1.670Mg·m-3,F(000)=2800,R1=0.0339,wR2=0.0718[I >2σ(I)],配体H4btb的2个羧基分别采取μ1-η1:η1、μ2-η2:η1配位模式连接镉原子形成一维带状结构。化合物2也属于单斜晶系,空间群为P21/c,晶胞参数:a=1.7471(3)nm,b=1.2511(2)nm,c=2.1870(3)nm,β=120.911(11)°,V=4.1014(11)nm3,Z=4,Dc=1.491Mg·m-3,F(000)=1876,R1=0.0673,wR2=0.1749[I>2σ(I)],全部去质子的H4btb配体的4个羧基分别采取μ1-η1:η0、μ1-η1:η1、μ2-η1:η1配位模式连接锌原子形成一维链,链间通过μ2-η1:η1桥连羧基扩展为(3,5)-连接的二维(42·67·8)(42·6)网状结构。同时研究了2个配合物的荧光性质。 相似文献
8.
使Zn(OAc)2·2H2O或Cd(OAc)2·2H2O与邻羧基苯甲酰二茂铁钠(o-OOCC6H4COFcNa;Fc=(η5-C5H5)Fe(η5-C5H4))和1,10-邻菲咯啉(phen)在甲醇中反应,合成了含有混合配体的单核配合物[Zn(o-OOCC6H4COFc)2(phen)(H2O)]·CH3OH (1)和双核配合物{[Cd(η2-o-OOCC6H4COFc)( μ2-o-OOCC6H4COFc)(phen)]·CH3OH2·H2O}2 (2)。晶体结构表明:在1中,单核的结构单元通过分子间氢键形成了一维的长链结构;在2中,o-FcCOC6H4COO-以及phen均双齿螯合中心Cd(II)离子,随后在o-FcCOC6H4COO-的双齿桥联下,形成一个双核结构。研究了这2个配合物在DMF溶液中的电化学性能。 相似文献
9.
在不同反应条件下反应得到了两种1,2,3-三唑衍生物的配合物[Co(H2O)6][Co(L1)3]2·4H2O(1)和Cu(L2)2(2)(HL1=5-methyl-1-phenyl-1H-1,2,3-triazole-4-carboxylic acid;HL2=1-(4-iodophenyl)-5-methyl-1H-1,2,3-triazole-4-carboxylic acid)。通过X射线单晶衍射和红外光谱确定了晶体结构,同时对配合物1和2进行了表面作用分析(Hirshfeld surface analysis),在二维指纹图谱中可以清楚的看到配合物中的主要分子间作用。 相似文献
10.
Cp3Ln与邻氨基苯甲酰胺在甲苯中反应,之后在HMPA和甲苯中结晶,以中等到高收率得到四核稀土有机配合物[CpLn( μ-η2:η2-NHC6H4CONH)( μ3-η1:η1:η2-NHC6H4CONH)LnCp(HMPA)}2(Ln=Yb,1a;Er,1b;Y,1c)。化合物 1与4倍物质的量的PhNCO在甲苯中反应形成1,3-喹唑啉二氧基(Quo)双负离子稀土配合物[Cp2Ln( μ3-η2:η2:η1-Quo)]3Ln(HMPA)2(Ln=Yb,2a;Er,2b;Y,2c),表明化合物1中的Ln-NHAr键和ArCONH-Ln键能与异氰酸酯分子发生连续加成/胺消除反应,形成1,3-喹唑啉二氧基骨架。但化合物1a~1c与iPrN=C=NiPr反应,仅得到ArNH基单加成产物{Cp2Ln[ μ-η1:η1:η2-iPrNC(NHiPr)NC6H4CONH]}3Ln(HMPA)3 (Ln=Yb,3a;Er,3b;Y,3c)。而Cp3Ln与邻氨基苯甲酰胺和iPrN=C=NiPr在甲苯中进行“一锅”反应,则形成双核配合物{CpLn[ μ-η1:η2:η2-NHCOC6H4 NC(NHiPr)NiPr]}2(Ln=Yb,4a;Er,4b;Y,4c)。值得注意的是,HMPA 能够诱导配合物4发生配体重排反应,转化成化合物3。 相似文献
11.
Fritz Theil 《Angewandte Chemie (International ed. in English)》1999,38(16):2345-2347
A breakthrough in the synthesis of diaryl ethers has been achieved as shown in Equation (1). The coupling of phenols with aryl boronic acids in the presence of copper(II ) acetate and a base proceeds under very mild conditions (room temperature) as described simultaneously by Evans et al. and Chan et al. Examples: R1=2-Cl, 2-I, 2-OMe, 4-tBu, 4-CH2CH(NHCOOtBu)CO2Me, 3,5-tBu2; R2=2-Me, 3-OMe, 3-NO2, 4-H, 4-F, 4-OMe. 相似文献
12.
Otto J. Scherer Matthias Flörchinger Karin Göbel Jürgen Kaub William S. Sheldrick 《欧洲无机化学杂志》1988,121(7):1265-1270
Element-Organic Amine/Imine Compounds, XXXI. - Cyclometallation with N-tert-Butyl-Phosphorus-Nitrogen Iridium Complexes The interaction of R1R2N–PNR3 ( 1 ) (R1 SiMe3, tBu, iC3H7; R2 R3 SiMe3, tBu) with [M(COD)(μ-Cl)]2 ( 2 ), M Rh, Ir, affords the amino(imino)phosphane complexes 3 , whose PN bond adds methanol with formation of the diamidophosphite complexes 4 . Already below 0°C the iridium compounds of 4 undergo cyclometallation of a tBu methyl group (R2) with formation of the hydrido-iridium metallaheterocycles 5 . The structures of 4b and 5a are elucidated by X-ray analyses. 相似文献
13.
The synthesis,structure, and ethylene polymerization of dimeric salicylaldiminato titanium complexes
《Journal of Coordination Chemistry》2012,65(20):3652-3660
A series of dimeric titanium complexes bearing salicylaldiminates, [4-R-6-tBu-2-(CH=NnBu)C6H2OTiCl2(µ-Cl)]2 [R?=?H (1); R?=?tBu (2); R?=?NO2 (3)], have been synthesized in high yield (>90%) by the reaction of corresponding 4-R-6-tBu-2-(CH=NnBu)C6H2OSiMe3 with TiCl4. The molecular structure of 2 has been confirmed by single-crystal X-ray diffraction analysis. When activated with methylaluminoxane, these complexes exhibit good catalytic activity for ethylene polymerization. 相似文献
14.
A. V. Piskunov I. A. Aivazyan G. A. Abakumov V. K. Cherkasov O. V. Kuznetsova G. K. Fukin E. V. Baranov 《Russian Chemical Bulletin》2007,56(2):261-266
The exchange reactions of tin diorganohalides R2SnCl2 (R = Et, But, or Ph) with lithium amidophenolate APLi2 (AP is the 4,6-di(tert-butyl)-N-(2,6-diisopropylphenyl)-o-iminobenzo-quinone dianion) in tetrahydrofuran produced the new five-coordinate (Et2SnAP(THF) (3)) and four-coordinate (R2SnAP (R = But, Ph)) tin(IV) complexes. The reaction of Ph2SnCl2 with APLi2 in a nonpolar solvent (hexane or toluene) is accompanied by the additional redox process giving rise to the paramagnetic
complex Ph2Sn(ImSQ)Cl (6) (ImSQ is the 4,6-di(tert-butyl)-N-(2,6-diisopropylphenyl)-o-iminobenzoquinone radical anion). The molecular structures of complexes 3 and 6 were established by X-ray diffraction.
Published in Russian in Izvestiya Akademii Nauk. Seriya Khimicheskaya, No. 2, pp. 253–258, February, 2007. 相似文献
15.
通过乳酸衍生物和3-溴-4-羟基苯甲酸的组合得到对映体3-溴-4-(((1R)-1-羧基乙基)氧基)苯甲酸(R-H2bba)和3-溴-4-(((1S)-1-羧基乙基)氧基)苯甲酸(S-H2bba)。以其为手性合成子在水热条件下分别与1,3-二(吡啶-4-基)丙烷(1,3-dpp)和Ni2+反应,构建了对映手性配位聚合物{[Ni(R-bba)(1,3-dpp)(H2O)0.5]·1.5H2O}n(HU12-R)和{[Ni(S-bba)(1,3-dpp)(H2O)0.5]·1.5H2O}n(HU12-S)。结构分析揭示HU12-R和HU12-S是具有dia网络特征的三维螺旋骨架。在骨架中,阴离子配体R-bba2-和S-bba2-分别与Ni2+中心连接在一起围绕2,螺旋轴得到一对小的对映螺... 相似文献
16.
通过乳酸衍生物和3-溴-4-羟基苯甲酸的组合得到对映体3-溴-4-(((1R)-1-羧基乙基)氧基)苯甲酸(R-H2bba)和3-溴-4-(((1S)-1-羧基乙基)氧基)苯甲酸(S-H2bba)。以其为手性合成子在水热条件下分别与1,3-二(吡啶-4-基)丙烷(1,3-dpp)和Ni2+反应,构建了对映手性配位聚合物{[Ni(R-bba)(1,3-dpp)(H2O)0.5]·1.5H2O}n (HU12-R)和{[Ni(S-bba)(1,3-dpp)(H2O)0.5]·1.5H2O}n (HU12-S)。结构分析揭示HU12-R和HU12-S是具有dia网络特征的三维螺旋骨架。在骨架中,阴离子配体R-bba2-和S-bba2-分别与Ni2+中心连接在一起围绕21螺旋轴得到一对小的对映螺旋链,而1,3-dpp与Ni2+中心则围绕41螺旋轴构建出另外一对大的对映螺旋链。电化学测试显示HU12-R属n型半导体,具有低阻抗性质,对紫外可见光有很强的吸收能力。进一步光催化实验证实在紫外光照射下所得配合物对染料降解有明显催化效果。 相似文献
17.
Dr. Alain Carpy Jean -Michel Léger Danielle Roche Michel P. Madesclaire Pascale Besse Henri Veschambre 《Structural chemistry》1995,6(3):191-195
The X-ray crystal structures of (–)-syn-4-phenyl-3-bromo-2-butyl camphanate (I) and (+-anti-4-phenyl-3-bromo-2-butyl camphanate (II) have been determined. Thesyn diastereoisomer of bromohydrin has the (2S,3S) absolute configuration whereas theanti diastereoisomer has the (2S,3R) absolute configuration. The crystallized derivatives I and II have been obtained by the reaction of each stereoisomer of bromohydrin, synthesized by reduction with baker's yeast, with (1S)-camphanic chloride. Crystal data: (I) C20H25BrO4:M
w: 409.32; orthorhombic,P212121;a=11.245(3),b=12.086(1),c=14.512(4) å; Z=4; finalR=0.053 for 1819 observed reflections. (II) C20H25BrO4;M
w=409.32; monoclinic, P21;a=11.352(1),b=6.378(1),c=14.255(2) å,=110.38(1);Z=2; finalR=0.045 for 1672 observed reflections. 相似文献
18.
Abstract The solvothermal reactions of copper(I) tert-butylthiolate (CuS
t
Bu) with 1/3 equiv. of dppe [dppe = bis(diphenylphosphino)ethane] or bix [bix = 1,4-bis(imidalzole-1-ylmethyl)benzene] in
CH3CN led to the formation of two cluster-based coordination polymers [(CuS
t
Bu)4(dppe)]
n
(1) and [(CuS
t
Bu)6(bix)]
n
(2). Single-crystal X-ray diffraction studies reveal that 1 and 2 feature 1D zigzag polymeric chains which contain rare (CuS
t
Bu)4 or (CuS
t
Bu)6 clusters as connecting junctions and dppe or bix as linkers. The title compounds show optical transitions with band gaps
of ∼3.18 eV for 1 and ∼2.81 eV for 2. Compounds 1 and 2 exhibit strong photoluminescence with the peaks maximum at 603 and 629 nm respectively.
Graphical Abstract Two 1D zigzag polymers [(CuS
t
Bu)4(dppe)]
n
(1) and [(CuS
t
Bu)6(bix)]
n
(2) [dppe = bis(diphenylphosphino) ethane] or bix [bix = 1,4-bis(imidalzole-1-ylmethyl)benzene] have been synthesized by solvothermal
reactions using copper(I) tert-butylthiolate CuS
t
Bu as the starting material. Compounds 1 and 2 contain rare (CuS
t
Bu)4 and (CuS
t
Bu)6 clusters as connecting nodes and dppe or bix as bridging ligands. The title compounds show optical transitions with band
gaps of ∼3.18 eV for 1 and ∼2.81 eV for 2. Both 1 and 2 exhibit strong photoluminescence with the peak maximums at 603 and 629 nm, respectively.
The 1D zigzag polymer of [(CuS
t
Bu)6(bix)]
n
(2). 相似文献
19.
Josep M. Ribó Maria D. Masip Asuncion Vallès 《Monatshefte für Chemie / Chemical Monthly》1981,112(3):359-368
Deprotonation of 3,4-dimethyl-3-pyrrolin-2-on (1) int-butyl alcohol/potassiumt-butoxide solutions takes place on the N atom, as shown by1H/2H exchange andpK
a
determinations of1 (pK=17.1), 1,3,4-trimethyl-3-pyrrolin-2-one (pK
a
=17.6), and 3,4-dimethyl-5-methoxy-2H-pyrrole (pK
a
=16.7). The SCF-MO approximation MINDO/3 indicates, however, that in the gas phase deprotonation of1 should occur at the C atom.
1.Mitt.:Ribó, J. M., Trull, F., Mh. Chem.110, 201 (1979). 相似文献