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Zhao Q Freeman JL Wang J Zhang Y Hamilton TP Lawson CM Gray GM 《Inorganic chemistry》2012,51(4):2016-2030
A series of bithiophene derivatives that are either symmetrically disubstituted with two Ph(2)(X)P groups (X = O, S, Se) or monosubstituted with one Ph(2)(X)P group (X = O, S, Se) and an organic functional group (H, CHO, CH(2)OH, CO(2)Me) have been synthesized. The X-ray crystal structures of Ph(2)(Se)P(C(4)H(2)S)(2)P(Se)Ph(2), Ph(2)(O)P(C(4)H(2)S)(2)H, Ph(2)(S)P(C(4)H(2)S)(2)H, and Ph(2)(O)P(C(4)H(2)S)(2)CH(2)OH exhibit very different solid-state structures depending on the type of intermolecular π-π interactions that occur. The compounds have been characterized by electronic absorption and fluorescence studies. Of particular interest is that the quantum yields of Ph(2)(O)P(C(4)H(2)S)(2)H, Ph(2)(O)P(C(4)H(2)S)(2)P(O)Ph(2), Ph(2)(O)P(C(4)H(2)S)(2)CO(2)Me, and Ph(2)(O)P(C(4)H(2)S)(2)CH(2)OH are significantly larger than that of bithiophene (factors of 13, 14, 14, and 22, respectively). This behavior is quite different from that of analogously substituted terthiophenes in which substitution results in only modest increases in the quantum yields over that of terthiophene (factors of 0.94, 2.7, 1.3, and 1.5, respectively). DFT studies of the emission process suggest that modifying the Ph(2)(X)P group affects both the fluorescence and nonradiative rate constants while modifications of the organic substituents primarily affect the nonradiative rate constants. The higher quantum yields of the substituted bithiophenes make them promising for application in organic light-emitting devices (OLED). The optical power limiting (OPL) performances of these Ph(2)(X)P-substituted bithiophenes were evaluated by nonlinear transmission measurements in the violet-blue spectral region (430-480 nm) with picosecond laser pulses. The OPL performances are enhanced by heavier X groups and when by higher solubilities. Saturated chloroform solutions of Ph(2)(O)P(C(4)H(2)S)(2)H and Ph(2)(S)P(C(4)H(2)S)(2)H exhibit significantly stronger nonlinear absorption than any previously reported compounds and are promising candidates for use in broadband optical power limiters. 相似文献
3.
Jie Ling 《Journal of solid state chemistry》2009,182(2):402-7933
Five hybrid organic-inorganic uranyl selenates have been synthesized, characterized and their structures have been determined. The structure of (C2H8N)2[(UO2)2(SeO4)3(H2O)] (EthylAUSe) is monoclinic, P21, a=8.290(1), b=12.349(2), c=11.038(2) Å, β=104.439(4)°, V=1094.3(3) Å3, Z=2, R1=0.0425. The structure of (C7H10N)2[(UO2)(SeO4)2(H2O)]H2O (BenzylAUSe) is orthorhombic, Pna21, a=24.221(2), b=11.917(1), c=7.4528(7) Å, V=2151.1(3) Å3, Z=4, R1=0.0307. The structure of (C2H10N2)[(UO2)(SeO4)2(H2O)](H2O)2 (EDAUSe) is monoclinic, P21/c, a=11.677(2), b=7.908(1), c=15.698(2) Å, β=98.813(3)°, V=1432.4(3) Å3, Z=4, R1=0.0371. The structure of (C6H22N4)[(UO2)(SeO4)2(H2O)](H2O) (TETAUSe) is monoclinic, P21/n, a=13.002(2), b=7.962(1), c=14.754(2) Å, β=114.077(2)°, V=1394.5(3) Å3, Z=4, R1=0.0323. The structure of (C6H21N4)[(UO2)(SeO4)2(HSeO4)] (TAEAUSe) is monoclinic, P21/m, a=9.2218(6), b=12.2768(9), c=9.4464(7) Å, β=116.1650(10)°, V=959.88(12) Å3, Z=2, R1=0.0322. The inorganic structural units in these compounds are composed of uranyl pentagonal bipyramids and selenate tetrahedra. In each case, tetrahedra link bipyramids through vertex-sharing, resulting in chain or sheet topologies. The charge-density matching principle is discussed relative to the orientations of the organic molecules between the inorganic structural units. 相似文献
4.
Siama Basharat Robert Palgrave Derek A. Tocher 《Journal of organometallic chemistry》2008,693(10):1787-1796
Structural studies by X-ray crystallography have been carried out for a range of diorganoalkoxogallanes incorporating donor-functionalized ligands. The compounds [Et2Ga(μ-OR)]2 (1, R = CH2CH2NMe2; 2, R = CH(CH3)CH2NMe2; 3, C(CH3)2CH2OMe; 4, R = CH(CH2NMe2)2) adopt dimeric structures with a planar Ga2O2 ring, and each gallium atom is coordinated in a distorted trigonal bipyramidal geometry. Low pressure chemical vapor deposition (CVD) of 2 and 4 resulted in the formation of oxygen deficient gallium oxide thin films on glass. However, the reaction of Et3Ga and ROH (R = CH2CH2NMe2, CH(CH3)CH2NMe2, C(CH3)2CH2OMe, CH(CH2NMe2)2) in toluene under aerosol assisted (AA)CVD conditions afforded stoichiometric Ga2O3 thin films on glass. This CVD technique offers a rapid, convenient route to Ga2O3, which involves the in situ formation of diethylalkoxogallanes, of the type [Et2Ga(μ-OR)]2, the structures of which are described in this paper. The gallium oxide films were deposited at 450 °C and analyzed by scanning electron microscopy (SEM), X-ray powder diffraction, wavelength dispersive analysis of X-rays (WDX), X-ray photoelectron spectroscopy (XPS) and Raman spectroscopy. 相似文献
5.
Ruibiao Fu 《Journal of solid state chemistry》2011,184(1):159-163
A 1,4-Butanediamine has been introduced as a structure-directing agent to synthesize two 3D zinc phosphonates under hydrothermal conditions, [(H3N(CH2)4NH3) Zn2((O3PCH2)2NCH2PO3H)(Cl)] (1) and [(H3N(CH2)4NH3)Zn3(O3P(CH2)2PO3)2] (2). Compounds 1∼2 were characterized by single-crystal X-ray diffraction along with powder XRD, EA, IR and TGA. Compound 1 is a 3D open-framework consisting of tetranuclear units and 16-membered-ring channel. In compound 2, each trinuclear unit contacts with surrounding six trinuclear units through O-P-O groups into a single hybrid layer, which is further pillared by O3P(CH2)2PO3 groups to form a 3D open-framework with 1D channel. In both compounds, 1,4-butanediamines are protonated and encapsulated into the channel through hydrogen bondings. Solids 1 and 2 are thermally stable up to 300 and 350 °C under air atmosphere, respectively. The luminescent properties of solids 1 and 2 are also studied in detail. 相似文献
6.
Lyhs B Bläser D Wölper C Schulz S 《Chemistry (Weinheim an der Bergstrasse, Germany)》2011,17(17):4914-4920
Antimony(III) complexes of the general type LSbF(2) (3: L(1) =[tBuC(NiPr)(2)]; 4: L(2) =[tBuC(NDipp)(2) , Dipp=2,6-iPr(2)C(6)H(3)) and LSb(N(3))(2) (6: L(1); 7: L(2)) were prepared in high yields and characterized by elemental analyses, NMR and IR spectroscopy and single-crystal X-ray diffraction. Moreover, the solid-state structures of [L(2)SbF(2)][L(2)Li] (5), [L(2) AlH(2)] (1), and [L'H][L'K(thf)(3)] (2; L'=HC(NDipp)(2)) are described, in which the Li (5) and K atoms (2) adopt rather unusual coordination modes. 相似文献
7.
Jun-Ling Song 《Journal of solid state chemistry》2004,177(7):2557-2564
Hydrothermal reactions of lead(II) acetate with 5-sulfoisophthalic acid monosodium salt (NaH2BTS) and N-(phosphonomethyl)-N-methylglycine, MeN(CH2CO2H)(CH2PO3H2) (H3L1), or a new aminodiphosphonic acid, 3-Pyridyl-CH2N(CH2PO3H2)2 (H4L2), afforded two novel lead(II) phosphonate-sulfonate hybrids, namely, Pb3[L1][BTS][H2O]·H2O 1 and Pb2[HL3][BTS]·H2O 2 (H2L3=3-Pyridyl-CH2(Me)N(CH2PO3H2)). H2L3 was formed as a result of the decomposition of one phosphonate group in H4L2 during the reaction. Compound 1 crystallizes in the triclinic space group with a=9.9148(4) Å, b=10.4382(4) Å, c=10.6926(2) Å, α=96.495(2)°, β=110.599(2)°, γ=98.433(2)°, V=1008.31(6) Å3, and Z=2. The structure of compound 1 features a 3D network built from the interconnection of hexanuclear Pb6(L1)2 units and 1D double chains of lead(II) carboxylate-sulfonate. Compound 2 crystallizes in the monoclinic space group P21/c with a=9.5403(7) Å, b=11.6170(8) Å, c=19.7351(15) Å, β=97.918(2)°, V=2166.4(3) Å3, and Z=4. Compound 2 has a 3D network structure built by the cross-linkage of 1D double chains of lead(II) phosphonates and 2D layers of lead(II) carboxylate-sulfonate. 相似文献
8.
Copsey MC Panneerselvam A Afzaal M Chivers T O'Brien P 《Dalton transactions (Cambridge, England : 2003)》2007,(15):1528-1538
Reactions of Na(tmeda)[N((i)Pr(2)PTe)(2)] with CuCl, AgI or AuCl (in the presence of PPh(3)) in THF produced the coinage metal ditelluroimidodiphosphinate complexes {Cu[N((i)Pr(2)PTe)(2)]}(3), (5), {Ag[N((i)Pr(2)PTe)(2)]}(6) (6) and Au(PPh(3))[N((i)Pr(2)PTe)(2)] (7), respectively. Complexes 5, 6 and 7 were characterized in the solid state by X-ray crystallography. Complex 5 is trimeric and exhibits a highly distorted Cu(3)Te(3) ring. In contrast, the Ag(I) complex 6 is a hexamer, and forms a twelve-membered Ag(6)Te(6) ring. The replacement of the (i)Pr groups on phosphorus by Ph results in an intriguing structural change to a tetramer with a boat-shaped Ag(4)Te(4) ring in {Ag[N(Ph(2)PTe)(2)}(4).2THF (8). The gold(I) complex 7 is monomeric. Aerosol-assisted chemical vapour deposition (AACVD) of compounds 5, 6 and 7 yields CuTe, Ag(7)Te(4), AuTe(2) and Au films, respectively. The films were grown at temperatures of 300-500 degrees C and characterized by X-ray powder diffraction (XRD), scanning electron microscopy (SEM) and energy dispersive analysis of X-rays (EDAX). 相似文献
9.
Lan-Chang Liang Chih-Wei Yang Chen-Hsiung Hung 《Journal of organometallic chemistry》2003,679(1):135-142
Several pyrrolylaldiminate complexes of Group 1, 4 and 13 metals are reported. The reaction of 5-tert-butyl-2-[(2,6-diisopropylphenyl)aldimino]pyrrole (HL) with NaH produced LNa(THF) (1). In situ lithiation of HL followed by addition of one equivalent of MClx (M=Zr, x=4; M=Hf, x=4, M=Al, x=3) afforded the corresponding pyrrolylaldiminate complexes, MLCl2(μ-Cl)2Li(OEt2)2 (M=Zr, 3; Hf, 4) and AlLCl2 (5). Alkylation of 5 with MeMgBr generated AlLMe2 (6). In addition to the spectroscopic data, complexes 3-6 were characterized by X-ray crystallography. 相似文献
10.
Three new organically templated or organically bonded zinc selenates, namely, {H2bipy}Zn(SeO4)2(H2O)21 (bipy=4,4′-bipyridine), {H2pip}{Zn(SeO4)2(H2O)4}·2H2O 2 (pip=piprazine), and Zn(SeO4)(phen)(H2O)23 (phen=1,10-phenanthroline) have been synthesized by hydrothermal reactions. The structure of compound 1 features a 1D chain composed of [Zn(SeO4)2(H2O)2]2− anions. Compound 2 has a 2D layer structure built from {Zn(SeO4)2(H2O)4}2− anions that are cross-linked by doubly protonated piperazine cations via N-H?O hydrogen bonds. The structure of compound 3 contains a 1D chain of Zn(SeO4)(phen)(H2O)2, such chains are further interlinked by hydrogen bonds and π?π interactions to form a 〈200〉 layer. The different roles the templates played have also been discussed. 相似文献
11.
Kom-Bei Shiu Shin-Jay Yu Yu Wang Gene-Hsiang Lee 《Journal of organometallic chemistry》2002,650(1-2):37-42
Treatment of [Ru2(CO)4(MeCN)6][BF4]2 or [Ru2(CO)4(μ-O2CMe)2(MeCN)2] with uni-negative 1,1-dithiolate anions via potassium dimethyldithiocarbamate, sodium diethyldithiocarbamate, potassium tert-butylthioxanthate, and ammonium O,O′-diethylthiophosphate gives both monomeric and dimeric products of cis-[Ru(CO)2(η2-(SS))2] ((SS)−=Me2NCS2− (1), Et2NCS2− (2), tBuSCS2− (3), (EtO)2PS2− (4)) and [Ru(CO)(η2-(Me2NCS2))(μ,η2-Me2NCS2)]2 (5). The lightly stabilized MeCN ligands of [Ru2(CO)4(MeCN)6][BF4]2 are replaced more readily than the bound acetate ligands of [Ru2(CO)4(μ-O2CMe)2(MeCN)2] by thiolates to produce cis-[Ru(CO)2(η2-(SS))2] with less selectivity. Structures 1 and 5 were determined by X-ray crystallography. Although the two chelating dithiolates are cis to each other in 1, the dithiolates are trans to each other in each of the {Ru(CO)(η2-Me2NCS2)2} fragment of 5. The dimeric product 5 can be prepared alternatively from the decarbonylation reaction of 1 with a suitable amount of Me3NO in MeCN. However, the dimer [Ru(CO)(η2-Et2NCS2)(μ,η2-Et2NCS2)]2 (6), prepared from the reaction of 2 with Me3NO, has a structure different from 5. The spectral data of 6 probably indicate that the two chelating dithiolates are cis to each other in one {Ru(CO)(η2-Et2NCS2)2}fragment but trans in the other. Both 5 and 6 react readily at ambient temperature with benzyl isocyanide to yield cis-[Ru(CO)(CNCH2Ph)(η2-(SS))2] ((SS)=Me2NCS2− (7) and Et2NCS2− (8)). A dimerization pathway for cis-[Ru(CO)2(η2-(SS))2] via decabonylation and isomerization is proposed. 相似文献
12.
The reactions of [Li(2)[PhB(N(t)Bu)(2)]](2) with GaCl(3) in various stoichiometries yield [Li(thf)(4)][PhB(mu-N(t)Bu)(2)GaCl(2) x GaCl(3)] (1), [PhB(mu-N(t)Bu)(2)GaCl](2) (2), and [mu-Li(OEt(2))[PhB(N(t)Bu)(2)]Ga] (3a), a series of complexes in which the three chloride ligands are successively replaced by the dianion [PhB(N(t)Bu)(2)](2-). The X-ray structures of 1, 2, and 3a show that the boraamidinate ligand adopts an N,N'-chelating mode. In the ion-separated complex 1, one of the nitrogen atoms is coordinated to a GaCl(3) molecule. The related indium complexes [mu-LiCl(thf)(2)][PhB(mu-N(t)Bu)(2)InCl](2) (4) and [mu-Li(OEt(2))[PhB(mu-N(t)Bu)(2)]In] (3b) were obtained in a similar manner. Complex 4 is the indium analogue of 2 with the incorporation of a bissolvated LiCl molecule. In 3a and 3b the spirocyclic [[PhB(mu-N(t)Bu)(2)](2)M](-) (M = Ga, In) anions are N,N'-chelated to the [Li(OEt(2))](+) counterion. Prolonged reactions result in the formation of [PhB(mu-N(t)Bu)(2)GaCl][(t)BuN(H)GaCl(2)] (5) and [[PhB(mu-N(t)Bu)(2)InCl][(t)BuN(H)InCl(2)][mu-LiCl(OEt(2))(2)]] (6), respectively. The X-ray structures of 5 and 6 reveal bicyclic structures which formally involve the entrapment of the monomers (t)BuN(H)MCl(2) by a four-membered BN(2)M ring (M = Ga, In). The synthesis and X-ray structure of Cl(2)Ga[mu-N(H)(t)Bu](2)GaCl(2) are also reported. 相似文献
13.
《Journal of Coordination Chemistry》2012,65(19):3402-3411
Three coordination complexes with N-donor ligands, Ag2(L1)1.5(NO3)2 (1), Ag3(L2)2(NO3)3 (2), and Ag(L1)2NO3 (3) {L1?=?1,4-bis(pyrazole-1-ylmethyl)benzene, L2 = 4,4′-bis(pyrazole-1-ylmethyl)biphenyl}, have been synthesized and structurally characterized by elemental analysis, IR spectroscopy, TGA, and X-ray single crystal diffraction. Complex 1 shows a 3-D fsh-3,4-P21/c structure with brevity code {83}2{85·10}. Complex 2 has a 3-D framework with a 2-D layer penetrated by an infinite 1-D zigzag chain. Complex 3 exhibits a (4,4)-net racemizing layer structure with nitrate anions filling the cavity. The results indicate that L1 and L2 can adopt varied conformations in formation of the complexes, and the length of the ligands plays a key role in configuring and directing the corresponding structure of the complexes. 相似文献
14.
2,5-噻吩双酰腙的合成 总被引:1,自引:0,他引:1
酰腙可提供氧、氮、硫等配位原子,与生物环境比较接近,且能与许多金属形成稳定的配合物[1 3]。1982年,Johnson及其合作者报道了芳香腙对DNA的合成具有奇特的抑制效果,并能抑制啮齿细胞链的增长;1988年,Mohan合成了7个含双吡啶环的芳香腙,这些配体都具有明显的抗肿瘤活性[4]。考虑到噻吩等杂环化合物在自然界中具有广泛的生物活性,故把杂环引入酰腙,我们合成了七个2,5 噻吩双酰腙,旨在为人们开发新药奠定一定的基础,合成路线如下:1 实验部分1 1 仪器与试剂意大利CarloErba1106型元素分析仪;美国NicoletESP360型傅立叶变换红外光谱… 相似文献
15.
The triorganotin(IV) derivatives of 2-mercapto-4-quinazolinone (HSqualone) of the type, R3SnL (R = Ph 1, CH32, PhCH23, p-F-PhCH24, o-F-PhCH25, n-Bu 6), were obtained by the reaction of the R3SnCl and HSqualone with 1:1 molar ratio in benzene. All complexes 1-6 were characterized by elemental analyses, IR, 1H and 13C NMR spectroscopy and the crystal structures of complexes 1-3 were also confirmed by X-ray crystallography. The structure analyses reveal that the tin atoms of complexes 1-3 are all distorted tetrahedral geometries. Furthermore, the dimeric structures in complexes 1-3 have also been found linked by intermolecular O-H?N or N-H?O hydrogen bonding interaction. Interestingly, the dimers of complexes 2 and 3 are further linked into one-dimensional chain through intermolecular C-H?S and C-H?O weak hydrogen bonding interactions, respectively. 相似文献
16.
The syntheses, crystal structures and characterizations of two new divalent metal carboxylate-phosphonates, namely, Zn(H3L)·2H2O (1) and Pb(H3L)(H2O)2 (2) (H5L4-HO2C–C6H4–CH2N(CH2PO3H2)2) have been reported. Compound 1 features a 1D column structure in which the Zn(II) ions are tetrahedrally coordinated by four phosphonate oxygen atoms from four phosphonate ligands, and neighboring such 1D building blocks are further interconnected via hydrogen bonds into a 3D network. The carboxylate group of H3L anion remains non-coordinated. Compound 2 has a 2D layer structure. Pb(II) ion is 7-coordinated by four phosphonate oxygen atoms from four phosphonate ligands and three aqua ligands. The interconnection of Pb(II) ions via bridging H3L anions results in a 001 layer. The carboxylate group of the H3L anion also remains non-coordinated and is oriented toward the interlayer space. Solid state luminescent spectrum of compound 1 exhibits a strong broad blue fluorescent emission band at 455 nm under excitation at 365 nm at room temperature. 相似文献
17.
Hydrothermal reactions of cadmium(II) chloride with three amino-diphosphonic acids, C6H5CH2N(CH2PO3H2)2 (H4L1), C6H5CH2CH2N(CH2PO3H2)2 (H4L2) and 4-CH3-C6H4CH2N (CH2PO3H2)2) (H4L3) resulted in three new metal amino-diphosphonates, namely, Cd(H3L1)2, 1 Cd(H3L2)2·2H2O 2 and Cd(H3L3)23. In all three complexes, the Cd(II) ion is octahedrally coordinated by six phosphonate oxygen atoms from six ligands. Complexes 1 and 3 have a similar structure in which the CdO6 octahedra are cross-linked by bridging ligands into a double chain along the c-axis, such double chains are further interlinked via hydrogen bonds between non-coordinated phosphonate oxygen atoms to form 〈100〉 and 〈200〉 layers with the phenyl groups of the ligands orientated toward the interlayer space. The structure of complex 2 features a 〈100〉 cadmium(II) diphosphonate layer. The effects of the substitute groups attached to the amine groups on the structures of the metal phosphonates are also discussed. 相似文献
18.
Guo Y Song X Li J Li Y Han Y Yu J Xu R 《Dalton transactions (Cambridge, England : 2003)》2011,40(36):9289-9294
Two heteroatom-containing open-framework aluminophosphates, (C(3)H(4)N(2))(2)FeAl(3)P(4)O(16) and (C(3)H(4)N(2))(2)CrAl(3)P(4)O(16) (denoted as MAPO-CJ50, M = Fe, Cr), have been synthesized by using imidazole as the template under solvothermal conditions. The structure of FeAPO-CJ50 is determined by single-crystal X-ray diffraction, and its analogous structure CrAPO-CJ50 is identified by powder X-ray diffraction. The 3-dimensional framework of MAPO-CJ50, constructed by MO(4)N(2) octahedra, AlO(4) tetrahedra, and PO(4) tetrahedra, contains interconnecting 10- and 8-ring channels. Imidazole molecules are coordinated with framework M(3+) ions and interact with each other through π-π stacking interactions in the channels. These two compounds show photoluminescent properties due to ligand-to-metal charge transfer. Magnetic measurements reveal that there are antiferromagnetic interactions between M(3+) ions in the frameworks of FeAPO-CJ50 and CrAPO-CJ50. 相似文献
19.
Singh S Ahn HJ Stasch A Jancik V Roesky HW Pal A Biadene M Herbst-Irmer R Noltemeyer M Schmidt HG 《Inorganic chemistry》2006,45(4):1853-1860
A series of organometallic compounds of group 13 metals supported by the sterically encumbered beta-diketiminate ligand containing hydrides, fluorides, chlorides, and bromide have been synthesized and structurally characterized. The synthetic strategy applied utilizes halide metathesis and reduction of metal chlorides to the corresponding hydrides. Thus, the reaction of LLi.OEt2 with MeMCl2 affords LM(Me)Cl (M = Al (1), Ga (2), In (3)) and LGaBr2 (4) with GaBr3. Reduction of LGa(Me)Cl with LiH.BEt3 leads to the formation of LGa(Me)H (10). Synthesis of LGaH(2) (12) has been accomplished by reacting LGaI2 (8) with LiH.BEt3. LAl(Me)Cl (1) and LAlH2 (6) have been converted to LAl(Me)F (5) and LAlF2 (7), respectively. The former was obtained in a reaction of LAl(Me)Cl with Me3SnF while the latter was isolated in a reaction of LAlH2 with BF3.OEt2. Similarly reaction of LGaI2 (8) with Me3SnF affords LGaF2 (9). Compounds reported herein have been characterized by elemental analyses, IR, NMR, EI-MS, and single-crystal X-ray diffraction techniques. 相似文献
20.
Dongwoon Jung 《Solid State Sciences》2010,12(4):466-470
The transition metal-doped zinc oxides, Zn1?xMxO (M = Cu, Mn and Fe) were synthesized by using solid-state reaction method and co-precipitation method. Samples prepared by co-precipitation method showed exactly same structure and properties compared to those made by solid-state reaction method. XRD, XRF and mapping analyses showed that Zn was successfully substituted with Cu, Mn and Fe by co-precipitation method. Zn1?xMxO samples exhibited new absorption shoulder in visible light region so that they showed photocatalytic activity in the visible light region. The highest photocatalytic activity under visible light was found in the Mn-substituted zinc oxide. 相似文献