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1.
Reaction of the dinuclear complex [Pd{κ2-N2′,C1-2-(2′-NH2C6H4)C6H4}Cl]2 (1) with ligands (L = 4-picoline, sym-collidine) gave the six-membered palladacycles [Pd{κ2-N2′,C1-2-(2′-NH2C6H4)C6H4}Cl(L)] (2). The complex 1 reacted with AgX (X = CF3SO3, BF4) and bidentate ligands [L–L = phen (phenanthroline), dppe (bis(diphenylphosphino)ethane), bipy(2,2′-bipyridine) and dppp
(bis(diphenylphosphino)propane)] giving the mononuclear orthopalladated complexes [Pd{κ2-N2′,C1-2-(2′-NH2C6H4)C6H4}(L–L)] (3) [L–L = phen, dppe, bipy and dppp]. These compounds were characterized by physico-chemical methods, and the structure of
[Pd{κ2-N2′,C1-2-(2′-NH2C6H4)C6H4}Cl(L)] (L = sym-collidine) was determined by single-crystal X-ray analysis. 相似文献
2.
The ortho-metalated complex [Pd(x){κ
2
(C,N)-[C6H4CH2NRR′ (Y)}] (2a–4a and 2b–3b) was prepared by refluxing in benzene equimolecular amounts of Pd(OAc)2 and secondary benzylamine [a, EtNHCH2Ph; b, t-BuNHCH2Ph followed by addition of excess NaCl. The reaction of the complexes [Pd(x){κ
2
(C,N)-[C6H4CH2NRR′ (Y)}] (2a–4a and 2b–3b) with a stoichiometric amount of Ph3P=C(H)COC6H4-4-Z (Z = Br, Ph) (ZBPPY) (1:1 molar ratio), in THF at low temperature, gives the cationic derivatives [Pd(OC(Z-4-C6H4C=CHPPh3){κ
2
(C,N)-[C6H4CH2NRR′(Y)}] (5a–9a, 4b–6b, and 4b′–6b′), in which the ylide ligand is O-coordinated to the Pd(II) center and trans to the ortho-metalated C(6)H(4) group, in an “end-on
carbonyl”. Ortho-metallation, ylide O-coordination, and C-coordination in complexes (5a–9a, 4b–6b, and 4b′–6b′) were characterized by elemental analysis as well as various spectroscopic techniques. 相似文献
3.
Shinya Hayami Yoshihiro Kojima Daisuke Urakami Kazuchika Ohta Katsuya Inoue 《Monatshefte für Chemie / Chemical Monthly》2009,34(4):829-838
Abstract
Metal complexes with long alkyl chains [Co(C16-terpy)3](BF4)2 (1), [Fe(C16-terpy)2](BF4)2 (2), [Co(C16-terpy)2](BPh4)2 (3), [Co(C14-terpy)2](BF4)2 (4), and [Fe(C12C10C5-terpy)2](BF4)2 (5) were synthesized and their physical properties characterized, where C16-terpy, C14-terpy, and C12C10C5-terpy are 4′-hexadecyloxy-2,2′:6′,2′′-terpyridine, 4′-tetradecyloxy-2,2′:6′,2′′-terpyridine, and 4′-5′′′-decyl-1′′′-heptadecyloxy-2,2′:6′,2″-terpyridine, respectively. Complexes 1, 2, and 5 exhibited liquid–crystal properties in the temperature ranges of 371–528 K and 466–556 K, and 88–523 K, respectively. Variable-temperature magnetic susceptibility measurements revealed that the Co(II) complexes 1 and 4 exhibited unique spin transitions (T 1/2↓ = 217 K and T 1/2↑ = 260 K for 1 and T 1/2↓ = 250 K and T 1/2↑ = 307 K for 4), so-called ‘reverse spin transition,’ induced by structural phase transitions. Complex 3 exhibited gradual spin-crossover behavior (T 1/2 = 160 K.), and complex 5 exhibited spin transitions (T 1/2↑ = 288 K and T 1/2↓ = 284 K) at the liquid crystal transition temperature. Compounds with multifunction, i.e., magnetic and liquid–crystal properties, are important in the development of molecular materials. 相似文献4.
Gordana P. Radi? Verica V. Glo?ovi? Goran N. Kalu?erovi? Frank W. Heinemann Sre?ko R. Trifunovi? 《Transition Metal Chemistry》2011,36(4):331-336
The reaction of K2[PdCl4] with [(S,S)-H2(Et)2eddv]Cl2 diester (O,O′-diethyl-(S,S)-ethylenediamine-N,N′-di-2-(3-methyl)butanoate) (1) resulted in [PdCl2{(S,S)-(Et)eddv-κ2
N,N′,κO}] (2) complex with one hydrolyzed ester group. The compound was characterized by spectroscopic methods and it was found that the
reaction is diastereoselective (1H and 13C NMR; one diastereoisomer of four possible). In addition, the structure of 2 was confirmed by X-ray diffraction analysis, indicating that the product is the (R,R)–N,N′-configured isomer. DFT calculations support the formation of one diastereoisomer of 2. 相似文献
5.
Ronald Lindner Goran N. Kaluđerović Reinhard Paschke Christoph Wagner Dirk Steinborn 《Polyhedron》2008
Reactions of [PtMe3(OCMe2)3](BF4) and [(PtMe3I)4] with pyrazole (pzH) afforded mononuclear pyrazole platinum(IV) complexes [PtMe3(pzH)3](BF4) (1) and [PtMe3I(pzH)2] (2), respectively. The formation of dinuclear pyrazolato bridged platinum(IV) complexes (PPN)[(PtMe3)2(μ-pz)3] (3), (PPN)[(PtMe3)2(μ-I)(μ-pz)2] · 1/2Et2O (4) and [K(18C6)][(PtMe3)2(μ-I)(μ-pz)2] (5) was achieved by the reaction of each 1 and 2 with [PtMe3(OCMe2)3](BF4) in the presence of KOAc followed by reaction with (PPN)Cl (PPN+ = bis(triphenylphosphine)iminium cation) and 18C6, respectively. The reaction of complex 4 with AgO2CCF3 followed by addition of RSR′ (R/R′ = Me/Me, Me/Ph) resulted in the formation of complexes [(PtMe3)2(μ-pz)2(μ-RSR′)] (R/R′ = Me/Me, 6; Me/Ph, 7). All complexes were characterized unambiguously by microanalysis and NMR (1H, 13C) spectroscopic investigations. Additionally, crystal structures of complexes 3 and 4 as well as DFT calculation are presented. Furthermore, in vitro studies on the anti-proliferative activity of complexes 2 and 5 were carried out. 相似文献
6.
Shinya Hayami Yoshihiro Kojima Daisuke Urakami Kazuchika Ohta Katsuya Inoue 《Monatshefte für Chemie / Chemical Monthly》2009,140(7):829-838
Abstract Metal complexes with long alkyl chains [Co(C16-terpy)3](BF4)2 (1), [Fe(C16-terpy)2](BF4)2 (2), [Co(C16-terpy)2](BPh4)2 (3), [Co(C14-terpy)2](BF4)2 (4), and [Fe(C12C10C5-terpy)2](BF4)2 (5) were synthesized and their physical properties characterized, where C16-terpy, C14-terpy, and C12C10C5-terpy are 4′-hexadecyloxy-2,2′:6′,2′′-terpyridine,
4′-tetradecyloxy-2,2′:6′,2′′-terpyridine, and 4′-5′′′-decyl-1′′′-heptadecyloxy-2,2′:6′,2″-terpyridine, respectively. Complexes
1, 2, and 5 exhibited liquid–crystal properties in the temperature ranges of 371–528 K and 466–556 K, and 88–523 K, respectively. Variable-temperature
magnetic susceptibility measurements revealed that the Co(II) complexes 1 and 4 exhibited unique spin transitions (T
1/2↓ = 217 K and T
1/2↑ = 260 K for 1 and T
1/2↓ = 250 K and T
1/2↑ = 307 K for 4), so-called ‘reverse spin transition,’ induced by structural phase transitions. Complex 3 exhibited gradual spin-crossover behavior (T
1/2 = 160 K.), and complex 5 exhibited spin transitions (T
1/2↑ = 288 K and T
1/2↓ = 284 K) at the liquid crystal transition temperature. Compounds with multifunction, i.e., magnetic and liquid–crystal properties,
are important in the development of molecular materials.
Graphical Abstract
相似文献
Shinya HayamiEmail: |
7.
Clovis Piovezan Fábio da Silva Lisboa Fábio Souza Nunes Sueli Maria Drechsel 《Transition Metal Chemistry》2011,36(1):79-85
We report the reactivity of three binuclear non-heme Fe(III) compounds, namely [Fe2(bbppnol)(μ-AcO)(H2O)2](ClO4)2 (1), [Fe2(bbppnol)(μ-AcO)2](PF6) (2), and [Fe2(bbppnol)(μ-OH)(Cl)2]·6H2O (3), where H3bbppnol = N,N′-bis(2-hydroxybenzyl)-N,N′-bis(2-methylpyridyl)–1,3-propanediamine-2-ol, toward the hydrolysis of bis-(2,4-dinitrophenyl)phosphate as models for phosphoesterase
activity. The synthesis and characterization of the new complexes 1 and 3 was also described. The reactivity differences observed for these complexes show that the accessibility of the substrate
to the reaction site is one of the key steps that determinate the hydrolysis efficiency. 相似文献
8.
Synthesis, crystal structures and DNA-binding properties of two new mononuclear copper(II) complexes
Two mononuclear copper(II) complexes, [Cu(bpy)2(CH3OH)](pic)2 (1) and [Cu(Me2bpy)2(H2O)](pic)2 (2) (bpy = 2,2′-bipyridine; Me2bpy = 4,4′-dimethyl-2,2′-bipyridine; Hpic = 2,4,6-trinitrophenol), were synthesized and characterized by elemental analyses,
conductivity measurements, IR, UV–Visible spectroscopy and single crystal X-ray analyses. Both complexes 1 and 2 are mononuclear compounds. The copper atom in complex 1 is in a distorted square pyramidal geometry with a CuN4O chromophore as revealed from the τ value (0.25), while the Cu(II) ion in complex 2 displays a distorted trigonal bipyramidal stereochemistry with τ = 0.72. Hydrogen bonding interactions and π–π stacking interactions
link the mononuclear copper complex 1 or 2 into a 1D infinite chain. The interactions of the two mononuclear complexes with herring sperm DNA (HS-DNA) have been studied by UV–visible absorption titration, fluorescence titration and ethidium bromide (EB) displacement
experiments. The results suggest that both complexes might bind to DNA by intercalation. 相似文献
9.
Yan Ding Hongli Chen Weilin Chen Enbo Wang Jingxin Meng 《Transition Metal Chemistry》2009,34(3):281-288
Four novel organic–inorganic hybrid compounds [Cu5
I(4,4′-bpy)3(2,2′-bpy)4][BW12O40] · H2O (1), [Ni0.5(2,2′-bpy)1.25][Ni(2,2′-bpy)3][Ni(2,2′-bpy)2(H2O)(SiW11VIWVO40)] · 0.5H2O (2), [H2bpy]2[Zn(2,2′-bpy)3]2[Si2W18O62] · 1.5H2O (3) and [CuII(2,2′-bpy)2]2[SiW12O40] · 2H2O (4) (2,2′-bpy = 2,2′-bipyridine, 4,4′-bpy = 4,4′-bipyridine) have been synthesized under hydrothermal conditions and characterized
by elemental analysis, IR spectroscopy, thermal gravimetric analysis, electrochemical measurements and single-crystal X-ray
diffraction. Compound (1) is a novel [BW12O40]5− polyoxoanion bisupported by copper(I) coordination cations with mixed 2,2′-bpy and 4,4′-bpy ligands. Compound (2) is constructed from the [SiW11VIWVO40]5− polyoxoanions supported by [Ni(2,2′–bpy)2]2+. Compound (3) is composed of a novel [Si2W18O62]8− cluster and [Zn(2,2′–bpy)3]2+ complexes, which held together into a three-dimensional (3D) supramolecular network through hydrogen-bonding interactions.
Compound (4) shows a 2D layer framework constructed from a bisupporting Keggin polyoxoanion cluster and [Cu(2,2′–bpy)2]2+ coordination polymer fragments, resulting in 3D networks via supramolecular interactions.
Electronic supplementary material The online version of this article (doi:) contains supplementary material, which is available to authorized users. 相似文献
10.
Senem Karahan Pelin Kose Elif Subasi Huseyin Alp Hamdi Temel 《Transition Metal Chemistry》2008,33(7):849-854
The hitherto unknown complexes, [M2(CO)6(μ-CO)(μ-L)], [M = Cr; 1, Mo; 2, W; 3] and [M2(CO)6(μ-CO)(μ-L′)], [M = Cr; 4, Mo; 5, W; 6] have been synthesized by the photochemical reactions of photogenerated intermediate, M(CO)5THF (M = Cr, Mo, W) with thio Schiff base ligands, N,N′-bis(2-aminothiophenol)-1,4-bis(2-carboxaldehydephenoxy)butane (H
2
L) and N,N′-bis(2-aminothiophenol)-1,7-bis(2-formylphenyl)-1,4,7-trioxaheptane (H
2
L′). The complexes have been characterized by elemental analysis, LC-mass spectrometry, magnetic studies, FT-IR and 1H NMR spectroscopy. The spectroscopic studies show that H
2
L and H
2
L′ ligands are converted to benzothiazole derivatives, L and L′ after UV irradiation and coordinated to the central metal as bridging ligands via the central azomethine nitrogen and sulphur
atoms in 1–6. 相似文献
11.
Abstract
Four complexes of 3,3-diphenylpropanoate (L) and 4,4′-bipyridine as auxiliary bridging ligands were synthesized and characterized, namely [Zn(L)2(4bpy)(EtOH)2]∞ (1), [Co(L)2(4bpy)(EtOH)2]∞ (2), [Ni(L)2(4bpy)(EtOH)2]∞ (3), and [Cu(L)2(4bpy)(H2O)]∞ (4) (4bpy = 4,4′-bipyridine). X-ray single-crystal diffraction analyses show that complexes 1–4 all take one-dimensional (1D) fishbone-like structures incorporating bridging 4bpy ligands. The complexes show different supramolecular frameworks interlinked via intermolecular hydrogen bonds, π···π stacking, and/or C–H···π supramolecular interactions. Complex 3 only has a simple one-dimensional fishbone-like chain, whereas complexes 1 and 2 show two-dimensional supramolecular structures by interchain C–H···O hydrogen bonds. Complex 4 is assembled into two-dimensional layers and then an overall three-dimensional framework by a combination of interchain O–H···O hydrogen bonds and C–H···π supramolecular interactions. The luminescent properties of the ligands and their complexes were investigated. 相似文献12.
Ruthenium complexes [Ru(κ3−tpy)(AsPh3)2C1]PF6 · 0.42H2O (tpy =2,2′:6′,2′′-terpyridine) (1) and a new crystal form of [Ru(κ3−tpy)(AsPh3)2Cl]BF4 (2), which crystallized without water solvate, and their comparative studies on spectral, structure and stability aspects are
reported. The complexes have been characterized by elemental analyses, FAB-MS, i.r., 1H n.m.r. and electronic spectral studies. In these complexes weak C—H···Fπ and face-to-face π–π interactions lead to a single helical motif while, C—H···FX (X=F, Cl) interactions result in linear chains. Various studies on the stability of the complexes suggested that the compound
containing the counter anion PF6- is more stable than the other containing BF4- as the counterpart. 相似文献
13.
Dong-Yu Lv Zhu-Qing Gao Jin-Zhong Gu Jian-Zhao Liu Wei Dou 《Transition Metal Chemistry》2011,36(3):275-281
Two Mn(II) coordination polymers, namely [Mn(bpda)]
n
(1) and [Mn(bpda)(bpy)0.5]
n
(2) (H2bpda = 1,1′-biphenyl-3,3′-dicarboxylic acid and bpy = 4,4′-bipyridine), have been synthesized from H2bpdc, bpy, and MnSO4·2H2O under hydrothermal conditions. The complexes were characterized by physicochemical and spectroscopic methods, as well as
by X-ray crystallography. Compound 1 possesses a 3D structure consisting of carboxylate-bridged edge-sharing Mn–O–Mn double chains. Compound 2 features a 3D open structure with a dinuclear Mn(II) secondary building unit. Magnetic susceptibility measurements of compounds
1 and 2 exhibit antiferromagnetic interactions between the nearest Mn(II), with J = –11.3 cm−1 and g = 2.12 for 1, and J = –13.5 cm−1 and g = 2.12 for 2. 相似文献
14.
Adrian B. Chaplin Zoltán Béni Christian G. Hartinger Hisham Ben Hamidane Andrew D. Phillips Rosario Scopelliti Paul J. Dyson 《Journal of Cluster Science》2008,19(1):295-309
The new mixed-metal complex {anti-[(p-cymene)RuCl]-μ-[κ
2-P,P′;κ
1-P′′-(PPh2CH2)3CMe]-[AuCl]}PF6 and its cluster derivative {anti-[(p-cymene)RuCl]-μ-[κ
2-P,P′;κ
1-P′′-(PPh2CH2)3CMe]-[AuPt3(CO)3(PCy3)3]}(PF6)2 have been prepared and characterized. Notably, NMR spectroscopy and high resolution FT-ICR mass spectrometry, including a
tandem mass spectrometric analysis, demonstrated the formation of these compounds that was also confirmed by single crystal
X-ray diffraction analysis. 相似文献
15.
Giuseppe Tresoldi Santo Di Pietro Dario Drommi Santo Lanza 《Transition Metal Chemistry》2010,35(2):151-158
The solvento species obtained by the treatment of cis-RuCl2(N,N-L)2 [L = di-2-pyridyl sulfide (dps), di-2-pyrimidyl sulfide (dprs)] with AgPF6, reacted with dithioethers L′ [L′ = 2,6-bis(2-pyridylthiomethyl)pyridine (pytmp), 2,6-bis(2-pyrimidylthiomethyl)pyridine (prtmp) and 2,6-bis{2-(4-methyl)pyrimidylthiomethyl}
pyridine (mprtmp)] to afford the compounds [Ru(N,N-L)2(N,S-L′)][PF6]2. The 1H NMR spectra indicate that L′ is chelated through S and N atoms with the formation of a four-membered ring. As a consequence, the ruthenium and sulfur
atoms are stereogenic centers with ∆ and Λ and (R) and (S) configurations, respectively. NMR spectra, at low temperatures, show that two invertomers, of similar abundance, as enantiomeric
couples ∆S, ΛR and ∆R, ΛS are present. In the methylene region, four AB systems are observed that in both the species contain
two non-equivalent methylene groups. Variable-temperature NMR spectra and EXSY experiments show that the sulfur inversion
produces an exchange between the invertomers. The one-dimensional band-shape analysis of the exchanging methylene signals
showed that the energy barriers for the process are in the 43–52 kJ mol−1 range. The possible mechanisms of the sulfur inversion are discussed. 相似文献
16.
Diacetylplatinum(II) complexes [Pt(COMe)2(N^N)] (N^N = bpy, 3a; 4,4′-t-Bu2-bpy, 3b) were found to undergo oxidative addition reactions with organyl halides. The reaction of 3a with methyl iodide and propargyl bromide led to the formation of the cis addition products (OC-6-34)-[Pt(COMe)2(R)X(bpy)] (R = Me, X = I, 4a; CH2C≡CH, X = Br, 4k). Analogous reactions of 3a with ethyl iodide, benzyl bromide, and substituted benzyl bromides, 3-(bromomethyl)pyridine, 2-(bromomethyl)thiophene, allyl
bromide, and cyclohex-2-enyl bromide led to exclusive formation of the trans addition products (OC-6-43)-[Pt(COMe)2(R)X(bpy)] (X = I, R = Et, 4b; X = Br, R = CH2C6H5, 4c; CH2C6H4(o-Br), 4d; CH2C6H4(p-COOH), 4e; CH2-3-py (3-pyridylmethyl), 4f; CH2-2-tp (2-thiophenylmethyl), 4g; CH2CH=CH2, 4h; c-hex-2-enyl (cyclohex-2-enyl), 4i). All complexes 4 were characterized by microanalysis, 1H and 13C NMR and IR spectroscopy. Additionally, complexes 4a, 4f, and 4g were characterized by single-crystal X-ray diffraction analyses. Reactions of 3a and 3b with o-, m- and p-bis(bromomethyl)benzene, respectively, led to the formation of dinuclear platinum(IV) complexes [{Pt(COMe)2Br(N^N)}2-{μ-(CH2)2C6H4}] (5). These complexes were characterized by microanalysis, IR spectroscopy, and depending on their solubility by 1H and 13C NMR spectroscopy, too. A single-crystal X-ray diffraction analysis of complex [{Pt(COMe)2Br(bpy)}2{μ-m-(CH2)2C6H4}] (5b) confirmed its dinuclear composition. The solid-state structures of 4a, 4f, 4g, and 5b are discussed in terms of C–H···O and O–H···O hydrogen bonds as well as π–π stacking between aromatic rings. 相似文献
17.
Limin Han Guangbin Zhang Ning Zhu Ruijun Xie Quanling Suo Meihua Luo Linhong Weng 《Journal of Cluster Science》2010,21(4):789-801
Two novel bimetallic complexes, [Cr(CO)3(η
6-C6H5)–C≡C–C6H4–Fc] (Fc = C5H5FeC5H4] (1) and [Cr(CO)3(η
6-C6H5)–C ≡ C–Fc–C(CH3)2–Fc] (3), were synthesized by the Sonogashira coupling reaction. By using of (1) and (3) as ligands to react with Co2(CO)8, two others novel polymetallic complexes, [Cr(CO)3(η
6-C6H5){Co2(CO)6-η
2-μ
2-C≡C–}–C6H4–Fc] (2) and [Cr(CO)3(η
6-C6H5){Co2(CO)6-η
2-μ
2-C≡C–}Fc–C(CH3)2–Fc] (4) were obtained. Four carbonyl complexes were characterized by elemental analysis, FT-IR, NMR and MS. The molecular structures
of complexes (1), (2) and (4) were determined by single crystal X-ray diffraction. The interactions among the ferrocenyl,
Cr(CO)3 and Co2(CO)6-η
2-μ
2-C≡C– units were investigated by cyclic voltammetry. 相似文献
18.
Abstract
Three new cadmium coordination polymers, [CdBr2(tmdp)2(μ-tmdp)2] n ·n(H2O) (1), [Cd(SCN)2(μ-tmdp)2] n ·2n(PhS) (2) and [Cd(SCN)2(μ-tmdp)2] n ·n(Ph2S2)·n(CH3CN) (3) (tmdp = 4,4′-trimethylenedipyridine), have been synthesized under solvothermal conditions and structurally characterized by single-crystal X-ray diffraction analysis. The geometry around cadmium is a slightly distorted octahedron with four tmdp and two Br- or SCN- ligands. Complex 1 represents a one-dimensional structure, whereas complexes 2 and 3 are two-dimensional coordination polymers. The rhombic channels of the coordination network of 2 and 3 are occupied by 1D polymeric (PhS) n and diphenyl disulfide (Ph2S2) molecules, respectively. The photoluminescent properties of coordination polymers 1–3 were investigated in solid state at room temperature. The TGA experiments showed that these three complexes were quite thermally stable. 相似文献19.
Yaqi Jiang Rong Yu Yuelin Bai Zhaoxiong Xie Lansun Zheng 《Transition Metal Chemistry》2008,33(8):1019-1026
Three novel coordination polymers, namely, [Mn(ndc)(bpy)]
n
· n(H2O) (1), [Mn(ndc)(phen)]
n
(2), and [Mn3(ndc)3(bpy)2]
n
(3) (H2ndc = 2,6-naphthalenedicarboxylic acid, bpy = 2,2′-bipyridine, phen = 1,10-phenanthroline) have been hydrothermally synthesized
and characterized by elemental analysis, IR, and single-crystal X-ray diffraction analysis. Complexes 1–3 exhibit three-dimensional metal-organic frameworks (MOFs); 1 and 2 are assemblies of the same secondary building units (SBUs), linear infinite chains {Mn(CO2)2}
n
, forming one-dimensional channel, while complex 3 is constructed by trinuclear clusters {Mn3(CO2)6} SBUs. Magnetic properties of complexes 1 and 3 are also discussed with respect to the bridging mode of the carboxylate groups. 相似文献
20.
Two new CuI coordination polymers, [CuI(TATP) (CN)]
n
(1) and [CuI(bpy)(SCN)]
n
(2) (TATP = 1,4,8,9-tetranitrogen-trisphene, bpy = 2,2′-bipyiridine), have been synthesized under hydrothermal conditions and
structurally characterized by elemental analysis, IR, and X-ray crystallography. In 1 and 2, the metal centers are linked by bridging CN−/SCN− to form one-dimensional chains in the crystals and are stabilized by interchain π–π stacking interaction. 相似文献