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1.
A. A. Karasik A. V. Krashilina A. T. Gubaidullin I. A. Litvinov V. K. Cherkasov O. G. Sinyashin G. A. Abakumov 《Russian Chemical Bulletin》2000,49(10):1782-1788
Two new 3,6-di-tert-butyl-o-benzosemiquinone complexes of copper(i) (2a and2b) with 1,3,5,7-tetraphenyl-1,5-diaza-3,5-diphosphacyclooctane (1a) and 1,5-dibenzyl-3,7-diphenyl-1,5-diaza-3,7-diphosphacyclooctane (1b), respectively, were synthesized. Their structures in solution and in the crystalline state were studied. According to the
results of X-ray diffraction analysis, the copper(i) atom in molecules2a and2b is in a pseudotetrahedral environment and is directly coordinated to two P atoms of the diazadiphosphacyclooctane ligand
and two O atoms of the benzosemiquinone ligand. In complex2a, ligand1a adopts a chair-boat conformation typical of all complexes with eight-membered cyclic 1,5-donors studied previously. Unlike
ligand1a, the ligand in complex2b adopts a chair-chair (crown) conformation identical with that of the free ligand. Both complexes are paramagnetic in the
solid state and in solutions. The parameters of the isotropic ESR spectra of complexes2a and2b are typical of four-coordinateo-semiquinone copper(i) complexes with bidentate bisphosphine ligands. Based on analysis of the isotropic ESR spectra, it was suggested that compound2b in solutions exists as two isomers, which differ in the conformation of the eight-membered heterocycle (chair-boat or chair-chair).
Published inIzvestiya Akademii Nauk. Seriya Khimicheskaya, No. 10, pp. 1806–1812, October, 2000. 相似文献
2.
设计、合成了一种新的主体分子2,6-二(α-苯基苄基)-1,5-萘二酚 (1). 它可与许多有机小分子形成配位包合物. 用IR和1H NMR表征了配位包结物, 并测定了主客体分子的摩尔比: 1•DMF (1∶1), 1•DMSO (1∶2), 1•吡啶 (1∶1), 1•喹啉(1∶2), 1•N-甲基吡咯烷酮(1∶1). 用单晶X衍射分析了包结物 (1)•DMF的晶体结构, 属三斜晶系, 晶胞参数为P-1, a=0.9085(9) nm, b=0.9501(6) nm, c=2.0995(6) nm, α=99.59(3)°, β=90.13(4)°, γ=96.20(7)°, V=1.776(2) nm3, Dc=1.898 g•cm-3. 结果表明, 主体分子间的CH/π弱氢键在决定主体分子的层状框架结构和客体分子在层间的填充方式中发挥了重要作用; 两种不等效的客体分子与主体分子的作用方式是不同的, 一种客体分子是通过CH/π, CH/O弱氢键与同层的不同主体分子相互作用, 另一种是通过CH/π, CH/O弱氢键与相邻层的不同主体分子相互作用. 相似文献
3.
采用准刚性的双吡啶化合物3,7-di(3-pyridyl)-1,5-dioxa-3,7-diazacyclooctane(L),合成了4个过渡金属配合物[Co(NO3)(H2O)2(L)2]NO3(1)、[Co2Cl4(L)2]·CH2Cl2(2)、[Cd2(AcO)4(L)2]·4CH3OH(3)和[Cd2(NO3)2(CH3OH)2(H2O)2(L)2](NO3)2·2H2O(4)。单晶衍射分析表明,配合物1是单核结构,配合物2是24-元环状双核结构,而配合物3和4为多边形双核结构。在这些配合物中,双吡啶配体分别采用了单齿、trans-和cis-桥连3种不同配位方式。配合物经过了元素分析、红外、热重和X射线单晶结构分析表征。 相似文献
4.
Gary Y. Peters William P. Jensen James J. Worman Robert A. Jacobson David A. Nelson 《Journal of heterocyclic chemistry》1977,14(5):769-772
The crystal structure of 3,7-dihydroxy-1,5-bis(p-brornophenyl)octahydro-1,5-diazocine ( 4 ) has been determined from the three dimensional x-ray diffraction data. This infers a similar structure for 3,7-dihydroxy-1,5-diphenyloetahydro-1,5-diazocine ( 1 ). The molecules are in a twist crown conformation and the configuration of the hydroxyl groups on the 3,7-positions is cis. 相似文献
5.
A. Kakanejadifard L. Mahmodi A. Yari A. Mohajeri 《Journal of heterocyclic chemistry》2006,43(6):1695-1697
6.
Kuznetsov R. M. Balueva A. S. Litvinov I. A. Gubaidullin A. T. Nikonov G. N. Karasik A. A. Sinyashin O. G. 《Russian Chemical Bulletin》2002,51(1):151-156
The reaction of bis(hydroxymethyl)phenylphosphine with 4,4"-diaminodiphenylmethane in DMF afforded 1,1",5,5"-bis[methylenedi(p-phenylene)]di(3,7-diphenyl-1,5-diaza-3,7-diphosphacyclooctane) (1) whose structure was established by X-ray diffraction analysis. Sulfurization and oxidation of macrocyclic tetraphosphine 1 gave rise to products 2 and 3, respectively, compound 3 being obtained as a stable hexahydrate. The reaction of bis(hydroxymethyl)phenylphosphine with bis(4-N-methylaminophenyl)methane in DMF followed by sulfurization yielded monocyclic bis{methylenedi[p-phenylene(N-methyl)aminomethyl]}di(P-phenyl)phosphine sulfide (4). 相似文献
7.
V. R. Akhmetova N. N. Murzakova G. R. Khabibullina T. V. Tyumkina Z. A. Starikova I. S. Bushmarinov L. F. Korzhova 《Russian Chemical Bulletin》2012,61(1):141-147
Heterocyclization of hydrazine with aldehydes R-CHO (R = Me, Et, Prn, Bun, n-C5H11, Ph, 4-MeOC6H4, 3-Py) and H2S leads to stereoisomeric 2,4,6,8-tetrasubstituted 3,7-dithia-1,5-diazabicyclo[3.3.0]octanes, which were separated by column chromatography. The trans-transoid-trans-configuration of tetramethyl(-ethyl,-propyl)-3,7-dithia-1,5-diazabicyclo-[3.3.0]octanes was inferred from the X-ray diffraction and 1H and 13C NMR spectroscopic data. 相似文献
8.
Aarti Gupta Pragati Devi Priyanka Chaudhary Dharma Kishore 《Phosphorus, sulfur, and silicon and the related elements》2013,188(7):808-821
Abstract The synthetic potential of 2,3,4,5-tetrahydrobenzo[b] [1,5]thiazepine-1,1,4-trione-2-carbohydrazide (5) which resulted from ethyl-4-oxo-2,3,4,5-tetrahydrobenzo[b] [1,5]thiazepine-2-carboxylate (3), on its oxidation with H2O2/AcOH followed by treatment with NH2NH2.H2O, was exploited to provide an access to 2-triazolo, 2-oxadiazolo, and 2-pyrazolo substituted derivatives of 1,5-benzothiazepin-4-oxo-1,1-dioxides (6–10), respectively. 相似文献
9.
A series of methylenebis(phenyl-1,5-benzothiazepine)s 4 and methylenebis(benzofuryl-1,5-benzothiazepine)s 5 were prepared by the reaction of methylene-bis-chalcones 3 with 2-aminothiophenol for 4 and followed by the condensation with chloroacetone for 5. The structures of the synthesized compounds have been confirmed by their IR, 1H NMR, 13C NMR, MS and elemental analyses. All the synthesized compounds were tested for their antimicrobial activity against Gram-positive, Gram-negative bacteria and fungi. To elucidate the essential structural requirements for the antimicrobial activity, the preliminary structure-activity relationship has been described. Among the compounds tested, the dimeric compounds 4f, 4g, 5f and 5g were found to be most active against Bacillus subtilis, Bacillus sphaericus, Staphylococcus aureus, Klebsiella aerogenes and Chromobacterium violaceum. Similarly these dimeric compounds showed potent antifungal activity against Candida albicans, Aspergillus fumigatus, Trichophyton rubrum, and Trichophyton mentagrophytes. It is interesting to note that the dimeric compounds with substituents of heterocyclic ring at the 4th position of benzothiazepine system displayed notable antibacterial activity equal to that of streptomycin and penicillin. Further, the activity of all the dimeric compounds was compared with that of their monomeric compounds, and it is interesting to note that almost all the dimeric compounds showed enhanced activity than their monomeric compounds. 相似文献
10.
11.
G. R. Nasybullina V. V. Yanilkin A. Yu. Ziganshina V. I. Morozov E. D. Sultanova D. E. Korshin Yu. S. Spiridonova A. S. Balueva A. A. Karasik A. I. Konovalov 《Russian Chemical Bulletin》2013,62(10):2158-2170
The possibility of controlling the association of tetraviologen calix[4]resorcinol (MVCA-C5 8+) with 3,7-di(l-menthyl)-1,5-di(p-sulfonatophenyl)-1,5-diaza-3,7-diphosphacyclooctane (APCO-22?) in the electrochemical cycle of reduction-reoxidation of viologen units was shown. Reduction to tetra(radical cation) MVCA-C5 4+· transforms monomeric MVCA-C5 8+ and APCO-22- into the associate (π-polymer) (xAPCO-22?·yMVCA-C5 4+·) n , which is completely returned by reoxidation to the initial state. 相似文献
12.
New pyrazolo[1,5-a]quinazoline-3-carbonitriles 4a,b were obtained via cyclocondensation of 5-amino-3-cyanomethyl-1H-pyrazole-4-carbonitrile (1) with enaminones of 1,3-cyclohexanedione derivatives 2a,b in refluxing glacial acetic acid. Condensation of compounds 4a,b with various aromatic aldehydes furnished the corresponding arylidene derivatives 6a–j. On the other hand, condensation of 4a,b with o-hydroxybenzaldehydes yielded the polyheterocyclic compounds 10a–h. Coupling of compounds 4a,b with aryldiazonium chlorides led to formation of 2-arylhydrazono derivatives 12a–h. Also, reaction of compounds 4a,b with phenyl isothiocyanate, followed by addition of ethyl chloroacetate and chloroacetonitrile, afforded the polyheterocyclic compounds based on pyrazolo[1,5-a]quinazoline core. The reaction of compounds 4a,b with phenyl isothiocyanate and elemental sulfur gave the thiazole-2-thione derivatives 25a,b. The reaction of enamines of compounds 4a,b with each of hydrazine hydrate and guanidine hydrochloride afforded pyrazolo[4″,3″:5′,6′]pyrido[4′,3′:3,4]pyrazolo[1,5-a]quinazolin-8-ones 30a,b and pyrimido[5″,4″:5′,6′]pyrido[4′,3′:3,4]pyrazolo[1,5-a]quinazolin-9(10H)-ones 33a,b, respectively. The structures of all the newly synthesized compounds were elucidated by elemental analyses and spectral data. The plausible mechanisms have been postulated to account for their formation. 相似文献
13.
G. Tóth J. Halász A. Lévai B. Rezessy 《Monatshefte für Chemie / Chemical Monthly》1997,128(6-7):625-632
Summary Conformational analysis of 2,3-dihydro-2,2-dimethyl-1,4-benzoxazepines (1,3,5, and7) and their 1,5-isomers (2,4, and6) was performed by temperature dependent NMR measurements. The effect of substituents on the ring inversion was studied. The results obtained were corroborated by AMl calculations.Dedicated to Prof.Waldemar Adam on the occasion of his 60th birthday 相似文献
14.
15.
《Journal of Coordination Chemistry》2012,65(1):181-194
Both [Cu(DAT)2(PA)2] (1) and [Cu(DAT)2(HTNR)2] (2) were prepared from 1,5-diaminotetrazole (DAT) and copper trinitrophenol, 1 for picrate (PA) and 2 for styphnate acid (2,4,6-trinitro resorcinol, TNR), and were characterized by elemental analysis, FT-IR spectroscopy, and single crystal X-ray diffraction. The space group of these compounds is P21/c (monoclinic). The lattice parameters are similar [a = 11.405(3) Å, b = 14.867(3) Å, c = 8.099(2) Å for 1 and a = 12.262(3) Å, b = 14.900(3) Å, c = 7.243(2) Å for 2], except the β = 106.257(3)° in 1 and β = 92.989(4)° in 2. Both have extended structures due to hydrogen bonds, but there are some differences because of the ligands induced effect. Differential scanning calorimetry analysis shows that two exothermic processes take place in both complexes, the first peak temperatures are 488.2 K for 1 and 519.2 K for 2. The kinetic parameters of the first exothermic process were studied by using Kissinger’s method and Ozawa’s method, in which the enthalpy of formation (?7346 and ?5706 kJ M?1), critical temperature of thermal explosion (475.0 and 515.8 K), entropy of activation (ΔS≠), enthalpy of activation (ΔH≠), and free energy of activation (ΔG≠) were calculated and obtained as ?117.25 J K?1 M?1, 140.64 kJ M?1, 196.44 kJ M?1 and ?219.1 J K?1 M?1, 383.56 kJ M?1, 495.34 kJ M?1 for 1 and 2, respectively. The sensitivity test results showed that both compounds were sensitive to impact (<5 J) and flame (>20 cm) rather than friction. 相似文献
16.
G. R. Nasybullina V. V. Yanilkin N. V. Nastapova A. Yu. Ziganshina D. E. Korshin Yu. S. Spiridonova A. A. Karasik A. I. Konovalov 《Russian Chemical Bulletin》2012,61(12):2295-2310
Binding of an amphiphilic dianion 1,5-bis(p-sulfonatophenyl)-3,7-diphenyl-1,5-diaza-3,7-diphosphacyclooctane (APCO2?) with an amphiphilic octacation tetra(methyl viologen) calix[4]resorcinol (MVCA8+) in media containing different amounts of water and DMSO using NaClO4 or NaCl as supporting electrolytes was shown for the first time by cyclic voltammetry and spectrophotometry. The stoichiometry of the complex depends on the MVCA8+: APCO2? ratio, medium, and supporting electrolyte. A 1: 1 charge-transfer complex is mainly formed (λmax = 480 nm) in 30% DMSO at a ratio of the compounds of 1: 1. A similar 1: 1 complex of APCO2? with a model compound methyl viologen MV2+ (λmax = 482 nm) is formed under these conditions. A donor-acceptor interaction occurs between the acceptor viologen units and nitrogen-centered electron-donating fragments of the APCO2? dianion. An increase in the content of APCO2? in the solution leads to an additional binding of one (30 vol.% DMSO, water, NaClO4) or two (30 vol.% DMSO, water, NaCl) particles of APCO2? with the hydrophobic fragments of MVCA8+. The complexes aggregate to form insoluble precipitates in aqueous and water-DMSO media. A selective reversible electroswitching from the bound to free state of one of the three bound APCO2? particles was performed when reducing MVCA8+ to MVCA4·+ in a 30 vol.% DMSO/NaCl medium. 相似文献
17.
A penta‐coordinated Ni(II) complex with a 1,5‐diazacyclooctane (DACO) ligand functionalized by two imidazole donor pendants, [NiL1Cl] (ClO4) H2O (1) (where L1 = 1,5‐bis (imidazol‐4‐ylmethyl)‐l,5‐diazacyclooctane) has been synthesized and characterized by X‐ray diffraction, infrared spectra, elemental analyses, conductance, thermal analyses and UV‐Vis techniques. Complex 1 crystallizes in triclinic crystal system, P‐l space group with a = 0.74782(7), b = 1.15082 (10), c = 1.23781(11) nm, α = 82.090(2), β = 73.011(2), γ = 83.462(2)°, V = 1.00603(16) nm3, M, = 486.00, Z = 2, Dc = 1.604 g/cm3, final R = 0.0435, and wR = 0.1244. The structures of 1 and its related complexes show that in all the three mononuclear complexes, each Ni(II) center is penta‐coordinated with a near regular square pyramid (RSP) to distorted square‐pyramidal (DSP) coordination environment due to the boat/chair configuration of DACO ring in these complexes, and the degree of distortion increases with the augment of the size of the heterocyclic pendants. In addition, the most striking feature of complex 1 resides in the formation of a two‐dimensional network structure through hydrogen bonds and stabilized by π‐π stacking. The solution behaviors of the Ni(II) complexes are also discussed in detail. 相似文献
18.
XRD is used to determine the structure of Cp′Ir(cod) at a temperature of 150(2) K. Crystallographic data for C14H19Ir are: a = 10.8272(5) ?, b = 9.7746(4) ?, c = 10.9180(5) ?, β = 97.3310(10)°, monoclinic symmetry, space group P21/n, V = 1146.02(9) ?3, Z = 4, d
calc= 2.199 g/cm3, R = 0.0246. The structure is molecular, built of neutral molecules. The metal atom coordinates carbon atoms of two cyclic ligands:
5-methylcyclopentadienyl-ion (Cp′) and 1,5-cyclooctadiene (cod). Five Ir-CCp′ distances lie in the range of 2.21–2.28 ?; four Ir-Ccod distances differ insignificantly, and their average value is 2.114(13) ?. The C11C12C13C14C15 and C1C2C5C6 planes of ligand fragments are almost parallel, and the angle between normals is 1.9°. In the crystal, molecules are bonded
only by van der Waals interactions; in the structure, the eight shortest Ir...Ir distances are in the range of 5.608–7.257
?.
Original Russian Text Copyright ? 2009 by K. V. Zherikova, N. B. Morozova, and I. A. Baidina
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Translated from Zhurnal Strukturnoi Khimii, Vol. 50, No. 3, pp. 591–594, May–June, 2009. 相似文献
19.
According to the Ullman reaction mechanism, the synthesis of 1,5-di(o-anisidino)anthraquinone was achieved by the multiphase reaction of 1,5-dichloroanthraquinone in xylene and o-anisidine in the presence of copper metal powder and potassium acetate. The effects of various factors on the reaction, such
as the dosages of xylene and catalyst, molar ratios of raw materials, and reaction times were investigated. When the molar
ratio of 1,5-dichloroanthraquinone to o-anisidine and potassium acetate is 1:10:2.5 and the catalyst dosage based on 1,5-dichloroanthraquinone is 5.3%, the conversion
of 1,5-dichloroanthraquinone is 97.8% and the yield of 1,5-di(o-anisidino)anthraquinone is 80.6% after reflux for 10 h. Under these conditions, the recovery of the solvent is 86.0%. The
target compound was identified by MS, 1H NMR, IR and DSC.
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Translated from Journal of Dalian University of Technology, 2007, 47(2): 170–174 [译自: 大连理工大学学报] 相似文献
20.
A novel series of pyrazolo[1,5-a]pyrimidines 14a–j and pyrazolo[1,5-a]quinazolines 18a, b were synthesized via condensation of 5-amino-1H-pyrazoles 10a, b with 3-(dimethylamino)-1-aryl-prop-2-en-1-ones 11a–e and 2-((dimethylamino)methylene)-5,5-dimethylcyclohexane-1,3-dione (15), respectively, in glacial acetic acid. Finally, treatment of 10a, b with sodium nitrite (NaNO2) afforded pyrazolo[3,4-d]triazines 20a, b. Structures of compounds were confirmed by their spectral data. These compounds were screened for their in vitro cytotoxic activities against human cancer cell lines (HepG-2 and MCF-7) using 3-[4,5-dimethyl-2-thiazolyl)-2,5-diphenyl-2H-tetrazolium bromide (MTT) assay. The results reveal that, the compounds 14b and 14h were the most potent in comparison with doxorubicin. The structure–activity relationship was discussed. 相似文献