Diaza Crown ethers are versatile complexing reagents, their complexing abilities are dramatically modified by the electron donating atoms on substituents attached to the nitrogen if they can give a three-dimensional c...Diaza Crown ethers are versatile complexing reagents, their complexing abilities are dramatically modified by the electron donating atoms on substituents attached to the nitrogen if they can give a three-dimensional cavity as in cryptates. Hence the synthesis and characterization of bibracchial lariat ethers (BIBLES) have received much attention. In the preparation of new BIBLES, a complex Ⅱ was unexpectedly obtained.展开更多
The novel complex [K(18-C-6)]_2 [Cd(mnt)_2] [18-C-6 = 18-crown-6, mnt =1,2-dicyanoethene-1,2-dithiolate, C_2S_2-(CN)_2^(2-)] was synthesized and characterized by elementalanalysis, IR spectrum and X-ray diffraction an...The novel complex [K(18-C-6)]_2 [Cd(mnt)_2] [18-C-6 = 18-crown-6, mnt =1,2-dicyanoethene-1,2-dithiolate, C_2S_2-(CN)_2^(2-)] was synthesized and characterized by elementalanalysis, IR spectrum and X-ray diffraction analysis. The complex displays two-dimensional networkstructure of [K(18-C-6)] complex segments and [Cd(mnt)_2] complex segment bridged by S-K-S, S-K-Nand N-K-N interactions between adjacent [K(18-C-6)] and [Cd(mnt)_2] units.展开更多
A chiral liquid crystal crown ether containing diaza-18-crown-6 was synthesized with the help of CPK atomic model and in the meantime a nonchiral liquid crystal crown ether of alike structure was also synthesized for ...A chiral liquid crystal crown ether containing diaza-18-crown-6 was synthesized with the help of CPK atomic model and in the meantime a nonchiral liquid crystal crown ether of alike structure was also synthesized for comparison, indicating that only the former was asymmetric. The present work represents the first attempt of the investigation in chiral liquid crystal crown ether, thus providing basis for further research into problems as such.展开更多
3,3′-Dimethyl-dibenzo-18-crown-6 was synthesized and characterized by elemental analysis, FT-IR, ^1H NMR, UV, MS spectra and X-ray single-crystal diffraction. It belongs to orthorhombic, space group Pna21 with a = 8....3,3′-Dimethyl-dibenzo-18-crown-6 was synthesized and characterized by elemental analysis, FT-IR, ^1H NMR, UV, MS spectra and X-ray single-crystal diffraction. It belongs to orthorhombic, space group Pna21 with a = 8.0790(18), b = 16.780(4), c = 15.222(3) .A, Z= 4, V= 2063.6(8) A3 Dc = 1.250 g/cm^3,μ = 0.090 mm^-1, F(000) = 832, R = 0.0474 and wR = 0.1103. According to structural analysis, the title compound possesses a boat-like configuration.展开更多
Dibenzo-1 , 4 , 10 , 13-tetraselena-7 , 16-dioxacyclo-octadeca-2 , 11-diene was synthesized by the condensation of poly (o-diselenobenzene) with bis (2-chloroethyl) ether in the presence of potassium borohydride. The ...Dibenzo-1 , 4 , 10 , 13-tetraselena-7 , 16-dioxacyclo-octadeca-2 , 11-diene was synthesized by the condensation of poly (o-diselenobenzene) with bis (2-chloroethyl) ether in the presence of potassium borohydride. The molecular structure was examined by IR, MS and  ̄1H NMR spectra, and confirmed by an X-ray diffraction study. The molecule in the crystal has a centrosymmetry and shows a chair conformation. The dihedral angle between the plane containing the four Se atoms and the benzene ring is 104. 1 (2)°. All geometrical parameters of the molecule are unexceptional. Crystal data : C_20H_24O_2Se_4, M_r= 612. 26, monoclinic, space group P2_1/c, a=8. 866(2) , b=5. 349(1). c=22. 315(3) A, β=96. 04(2)°, V=1052. 3 A ̄3, Z=2,D_c=1.932 g/cm ̄-3 , μ(MoKα) = 69. 15 cm ̄-1, F(000) = 592, T= 297K, R= 0. 038for 1270 observed reflections and 154 refined parameters.展开更多
Crystal structure of the title compound C 16 H 25 O 2NS 2 has been determined by X-ray diffraction method. Its crystallographic data were as follows: M r=327.51, triclinic, space group P1, a=8.864(3), b=10.127(4), c=1...Crystal structure of the title compound C 16 H 25 O 2NS 2 has been determined by X-ray diffraction method. Its crystallographic data were as follows: M r=327.51, triclinic, space group P1, a=8.864(3), b=10.127(4), c=10.390(3) , α=105.94(3), β=103.10(2), γ=90.96(3)°, V=870.3(7) 3, Z=2, D c=1.250g.cm -3 , μ(MoKα)=2.966cm -1 , F(000)=176, a total of 3275 reflections measured (2θ max =50°), 2246[I5σ(I)] used in the refinement, R=0.067, R w=0.082. The result shows that the distances of N(1)-C(2) and N(1)-C(3) are longer than that of N(1)-C(11), which indicates that the interaction of C Ar -N sp 2 is stronger than that of C sp 3 -N sp 2 . Oxygen, nitrogen and sulfur atoms of the ring in the same plane was deduced from the least\|squares planes and the dihedral angles.展开更多
The title compound C18 H25 NC4ClBr2Cu crystallizes in space group P 1 with a = 1.0105(2)nm b=1.0821(1) nm, c=1. 1007(2) nm, a=80. 00(1)°,β=80. 26(1)° γ=77. 83(1)°. Z=2, D = 1. 831 g/cm3, μ=62. 658 cm...The title compound C18 H25 NC4ClBr2Cu crystallizes in space group P 1 with a = 1.0105(2)nm b=1.0821(1) nm, c=1. 1007(2) nm, a=80. 00(1)°,β=80. 26(1)° γ=77. 83(1)°. Z=2, D = 1. 831 g/cm3, μ=62. 658 cm-1(Mok(?)). The final refinement converged to R=0. 031 for 2547 independent observed reflections. The complex molecule consists of two cationic moieties (HL)+ and an anion which appears as a bromide-bridged copper dimer (Cu2Br6)2-. This structural characterization seems to be rare in metal complexes with crown-ether.展开更多
The reactions of 18 crown 6 with each of K 2(M=Zn, Hg; mnt=1,2 dicyanoethene 1,2 dithiolate, C 2S 2(CN) 2- 2) were studied and novel complexes [K(18 C 6)] 2[Zn(mnt) 2](1) and [K(18 C 6)] 2[Hg(mnt)...The reactions of 18 crown 6 with each of K 2(M=Zn, Hg; mnt=1,2 dicyanoethene 1,2 dithiolate, C 2S 2(CN) 2- 2) were studied and novel complexes [K(18 C 6)] 2[Zn(mnt) 2](1) and [K(18 C 6)] 2[Hg(mnt) 2](2) were characterized by elemental analysis, IR spectrum and X ray diffraction analysis. Complex 1 displays a one dimensional chain of [K(18 C 6)] 2[Zn(mnt) 2] bridged by K O interactions between adjacent [K(18 C 6)] + units. Complex 2 is also a one dimensional chain of [K(18 C 6)] 2[Hg(mnt) 2] bridged by K...S weak interactions between adjacent [K(18 C 6)] + and [Hg(mnt) 2] 2- .展开更多
Double-armed crown ether 15,16-bis((4-nitrophenoxy)methyl)-2,3,5,6,8,9,11,12-octahydrobenzo[b][1,4,7,10,13] pentaoxacyclopentadecine F.W. 570.54 was synthesized by dibromomethyl benzo-15-crown-5 with 4-nitrophenol...Double-armed crown ether 15,16-bis((4-nitrophenoxy)methyl)-2,3,5,6,8,9,11,12-octahydrobenzo[b][1,4,7,10,13] pentaoxacyclopentadecine F.W. 570.54 was synthesized by dibromomethyl benzo-15-crown-5 with 4-nitrophenol in the presence of anhydrous K2CO3, characterized by spectroscopic techniques and confirmed by X-ray crystal structure analysis. The title compound crystallizes in monoclinic, space group P21/c with a = 12.840(4), b = 9.425(3), c = 22.447(7), β = 98.128(7)° and Z = 4. The structure exhibits intermolecular hydrogen bonding of C-H···O type.展开更多
4',5'-Dibromo-o-xylyl-17-crown-5 ether (2BrB17C5) was synthesized,starting from 1,2-dibromo-4,5-bis(bromomethyl)-benzene and tetraethylene glycol,and was characterized by 1H NMR,MS and elemental analysis.Pale ...4',5'-Dibromo-o-xylyl-17-crown-5 ether (2BrB17C5) was synthesized,starting from 1,2-dibromo-4,5-bis(bromomethyl)-benzene and tetraethylene glycol,and was characterized by 1H NMR,MS and elemental analysis.Pale yellow prismatic single crystal obtained from anhydrous ethanol was investigated by X-ray structural analysis.The complexation properties toward alkali metal ions were examined using the solvent extraction method and UV absorption spectroscopy.The crown ether was found to be conformationally deformed and oblate-like and is highly selective for lithium ion.展开更多
A new energetic organic potassium salt bis(dinitromethyl)difurazanyl ether potas- sium salt [K2(BDFE)] was synthesized, and structurally characterized by elemental analysis, IR spectra, t3C NMR and single-crystal ...A new energetic organic potassium salt bis(dinitromethyl)difurazanyl ether potas- sium salt [K2(BDFE)] was synthesized, and structurally characterized by elemental analysis, IR spectra, t3C NMR and single-crystal X-ray diffraction. K2(BDFE) crystallizes in monoclinic system, space group C2/c with a = 17.342(3), b = 12.6943(17), c = 8.0972(11) A, β = 110.630(2)°, V = 1668.3(4) A3, Z = 4, Dc = 2.000 g/cm3, F(000) = 1000,μ= 0.675 mm-1, S = 1.058, the final R = 0.0499 and wR = 0.1452. The K ion is eight-coordinated with eight O atoms from one water molecule and four bis(dinitromethyl)difurazanyl ethers (BDFE), forming a distorted dodecahedral structure. Thermal decomposition of the title complex was studied by using DSC and TG-DTG. There are primarily two exothermic decomposition processes between 200 and 370 ℃.展开更多
Two charged donor-acceptor [2]catenanes were synthesized by the cyclization of the π-acceptor 1,1 '-[1, 4-phenylenebis-(methylene)]bis(4,4'-bipyridinium)bis(hexafluorophosphate)(2) and bis(bromomethyl)ben...Two charged donor-acceptor [2]catenanes were synthesized by the cyclization of the π-acceptor 1,1 '-[1, 4-phenylenebis-(methylene)]bis(4,4'-bipyridinium)bis(hexafluorophosphate)(2) and bis(bromomethyl)benzene with the templates of the π-donor phenylene-diacetylene crown ethers la and lb in the yields of 31%, 35%, respectively. The mass spectra, 1H and 13C NMR spectra confirm that the phenylene-diacetylene crown ethers, with a nonaromatic ~r-system, successfully template the cyclization of CBPQT4+. The X-ray crystallography analysis shows that the CBPQT4+ ring encircles around the phenylene motif of the crown ethers, leaving the 1,3-butadiyne fragment out of the cavity of CBPQT4+ ring. The mechanically interlocked structure of [2]catenanes was stabilized by the cooperative effects of π-stacking and hydrogen bonding interactions.展开更多
The preparation and X-ray crystal structures of the adducts of 10-thiabenzo-15-crown-5 and 10-selenabenzo-15-crown-5 with PdCl2 are reported. [PdCl2(C14H20O4S)2] (1): or-thorhombic, space group Pbca with cell dimensio...The preparation and X-ray crystal structures of the adducts of 10-thiabenzo-15-crown-5 and 10-selenabenzo-15-crown-5 with PdCl2 are reported. [PdCl2(C14H20O4S)2] (1): or-thorhombic, space group Pbca with cell dimensions of a=17.285(5), 6=8.354(3), c=21.689(4) A, K=3131.9 A3, Z=4;R=0.0330 for 2301 reflections with I > 3o(I), [PdCl2(C14H2oO4Se)2] (2): monoclinic, space group P21/n with cell dimensions of a=18.928(4), b=8.912(3), c=9.813(2) A, β=96.90(2)0, V=1643.4 A3, Z=2; R=0.0289 for 2617 reflections with I> 3σ(I), Both complexes are monomeric, square-planar palladiurn(Ⅱ) compounds with the Pd(Ⅱ) ion situating on a crystal-lographic inversion centre, and the crown ligands all adopt the axial coordination with the Pd-S bond of 2.3233(7) A and the Pd-Se bond of 2.4357(3) A. Their complexing characteristics are discussed in brief.展开更多
The preparation method of [Na ( DB18C6) (CH_3OH )]_2Mo_6O_(19)·(DB18C6)·(CH_3OH) , where DB18C6 is dibenzo-18-crown-6, is described. Thecrystal and molecular structure of the title complex has been determine...The preparation method of [Na ( DB18C6) (CH_3OH )]_2Mo_6O_(19)·(DB18C6)·(CH_3OH) , where DB18C6 is dibenzo-18-crown-6, is described. Thecrystal and molecular structure of the title complex has been determined crystallographically. The title complex crystallizes in the monoclinic system,space group P2_1/c ,a=18. 727(6) ,b=19. 555(6) , c=22. 827(7) ,β=112. 84(3)°, V=7704(4)  ̄3 ,M_r = 2102. 9 , Z = 4 , F (000 ) = 4224 , μ= 1 . 028 mm  ̄(-1), D_c = 1.813 g/cm ̄3 . final R =0. 075 and R_w= 0. 078 based on 4463 observed reflections with F>6. 0σ(F) . The complex consists of [Mo_6O_(19)] ̄(2-) ,[Na(DB18C6)] ̄+ and CH_3OH, which are linked by long distance interaction through O-Na-O bond.展开更多
The interaction of lanthanum(Ⅲ) chloride with 12-crown-4 in MeCN/MeOH mixed solvent produces an anhydrous complex,LaCl3(12-crown-4)(MeOH)(complex Ⅰ),C9H20O5LaCl3(Mr= 453.6),in which the La(Ⅲ) ion is 8-coordinated b...The interaction of lanthanum(Ⅲ) chloride with 12-crown-4 in MeCN/MeOH mixed solvent produces an anhydrous complex,LaCl3(12-crown-4)(MeOH)(complex Ⅰ),C9H20O5LaCl3(Mr= 453.6),in which the La(Ⅲ) ion is 8-coordinated by three Cl anions,four oxygen atoms from a crown ligand and a methanol oxygen atom,the complex molecules were connected into a dimer by two O(MeOH)…Cl hydrogen bonds.Reaction of complex Ⅰ with phen(1,10-phenanthroline) gives the crystallization of[LaCl3 (phen)2(H2O)]·MeOH(complex Ⅱ),C25H22O2N4LaCl3(Mr= 655.8) in which the crown ligand is totally replaced by two phen molecules.Cell parameters for the two complexes are a= 9.389(3)[13.228 (5)],b=11.382(4)[10.767(3)],c=7.542(3)[18.520(6) ];α=94.32(3)[90.0],β=102.10(2)[102.01(3)],γ=91. 83(3)[90. 0]°with space group P1[P21/α];V=784.5(5)[2580(1)3,Z=2[4];μ(MoKα)=32.8[20. 2]cm-1;F (000)=444[1296];R=0.042[0.045];Rω=0.044[0.036] for 2398 [2345] observed reflections withⅠ>3σ(Ⅰ).The La(Ⅲ) ion in complex Ⅱ is 8-coordinated by three Cl anions,four N atoms of two phen molecules and one water molecule.The methanolmolecule forms a hydrogen bond with Cl(3) atom.展开更多
Single crystals of complex BiCl3(15-crown-5) were synthesized by gel method, and the structure was solved from X-ray diffraction data by direct and Fourier methods. The crystal is orthorhombic, space group is P212121 ...Single crystals of complex BiCl3(15-crown-5) were synthesized by gel method, and the structure was solved from X-ray diffraction data by direct and Fourier methods. The crystal is orthorhombic, space group is P212121 with unit cell parameters:a = 7. 677(4), 6=13. 254(6) and c= 15. 911(6) A , and 2=4. The final structural refinement converged with unweighted and weighted factors of 0. 053 and 0. 063 respectively for 1290 observed reflections. The structure consists of discrete BiCl3(15-crown-5) molecules in which bismuth atom is sandwiched between two essentially parallel planes, one of which contains five oxygen atoms and the other contains three chlorine atoms.展开更多
The supennolecular based on sodium molybdate(Ⅵ) and sulfate, dibenzo-18-crown-6 was synthesized in acetonitrile and characterized by elemental analysis, IR,^1H NMR, single crystal X-ray diffraction, indicating that...The supennolecular based on sodium molybdate(Ⅵ) and sulfate, dibenzo-18-crown-6 was synthesized in acetonitrile and characterized by elemental analysis, IR,^1H NMR, single crystal X-ray diffraction, indicating that it contains [S2M018062]^4+ and [Na(DB18Cr)(H2O)]^+, where each sodium ion is deviated from the plane defined by the oxygen atoms in the corresponding crown ether. The compound crystallizes in the monoclinic space group C2/c with a=3.29332(10) nm, b= 1.90917(6) nm, c=2.63132(7) nm, β= 121.6630(10)°, V=14081.8(7) nm^3, Z=8, T=293(2) K, and R1(wR2)=0.0177 (0.1525). The compound exhibits a novel organic-inorganic structure, in which the crown ether-sodium complexes are coordinated to the terminal oxygen atoms of Mo18054 and the oxygen atoms of water molecule.展开更多
The crystal structure of the title compound (C18H18N4O, Mr = 306.36) has been determined by single-crystal X-ray diffraction. The crystal is of triclinic, space group P1 with α = 4.783(0), b = 13.577(1), c = 13...The crystal structure of the title compound (C18H18N4O, Mr = 306.36) has been determined by single-crystal X-ray diffraction. The crystal is of triclinic, space group P1 with α = 4.783(0), b = 13.577(1), c = 13.830(1) A, α = 63.581(2), β = 88.326(2), γ = 86.161(2)°, V= 802.5(1) A3, Z= 2, Dc = 1.268 g/cm^3, F(000) = 324, μ(MoKa) = 0.082 mm^-1, the final R = 0.0497 and wR = 0.1199 for 3094 observed reflections (I 〉 2σ(I)). The dihedral angles between the phenyl (C(1)-C(4)-(6)) and triazole, the phenyl (C(13)-C(15)-C(18)) and triazole, and the two phenyl rings are 7.9(1), 69.9(1) and 67.8(1)°, respectively. Strong C-H…π interaction joins molecules into a chain along the c axis and contributes to the stability of the structure. Preliminary bioassay results show that the title compound possesses excellent and selective fungicidal activity against Colletotrichum gossypii but displays moderate to weak insecticidal activity against aphides.展开更多
The interaction of lanthanum(Ⅲ) chloride with 12-crown-4 in MeCN/MeOH mixed solvent produces an anhydrous complex,LaCl3(12-crown-4)(MeOH)(complex Ⅰ),C9H20O5LaCl3(Mr= 453.6),in which the La(Ⅲ) ion is 8-coordinated b...The interaction of lanthanum(Ⅲ) chloride with 12-crown-4 in MeCN/MeOH mixed solvent produces an anhydrous complex,LaCl3(12-crown-4)(MeOH)(complex Ⅰ),C9H20O5LaCl3(Mr= 453.6),in which the La(Ⅲ) ion is 8-coordinated by three Cl anions,four oxygen atoms from a crown ligand and a methanol oxygen atom,the complex molecules were connected into a dimer by two O(MeOH)…Cl hydrogen bonds.Reaction of complex Ⅰ with phen(1,10-phenanthroline) gives the crystallization of[LaCl3 (phen)2(H2O)]·MeOH(complex Ⅱ),C25H22O2N4LaCl3(Mr= 655.8) in which the crown ligand is totally replaced by two phen molecules.Cell parameters for the two complexes are a= 9.389(3)[13.228 (5)],b=11.382(4)[10.767(3)],c=7.542(3)[18.520(6) ];α=94.32(3)[90.0],β=102.10(2)[102.01(3)],γ=91. 83(3)[90. 0]°with space group P1[P21/α];V=784.5(5)[2580(1)3,Z=2[4];μ(MoKα)=32.8[20. 2]cm-1;F (000)=444[1296];R=0.042[0.045];Rω=0.044[0.036] for 2398 [2345] observed reflections withⅠ】3σ(Ⅰ).The La(Ⅲ) ion in complex Ⅱ is 8-coordinated by three Cl anions,four N atoms of two phen molecules and one water molecule.The methanolmolecule forms a hydrogen bond with Cl(3) atom.展开更多
基金Supported by the National Natural Science foundation of China Laboratory of Magnetic Resonance and Atomic and Molecular Physics, Wuhan Institute of Physics, Academic Soinica, Wuhan
文摘Diaza Crown ethers are versatile complexing reagents, their complexing abilities are dramatically modified by the electron donating atoms on substituents attached to the nitrogen if they can give a three-dimensional cavity as in cryptates. Hence the synthesis and characterization of bibracchial lariat ethers (BIBLES) have received much attention. In the preparation of new BIBLES, a complex Ⅱ was unexpectedly obtained.
文摘The novel complex [K(18-C-6)]_2 [Cd(mnt)_2] [18-C-6 = 18-crown-6, mnt =1,2-dicyanoethene-1,2-dithiolate, C_2S_2-(CN)_2^(2-)] was synthesized and characterized by elementalanalysis, IR spectrum and X-ray diffraction analysis. The complex displays two-dimensional networkstructure of [K(18-C-6)] complex segments and [Cd(mnt)_2] complex segment bridged by S-K-S, S-K-Nand N-K-N interactions between adjacent [K(18-C-6)] and [Cd(mnt)_2] units.
文摘A chiral liquid crystal crown ether containing diaza-18-crown-6 was synthesized with the help of CPK atomic model and in the meantime a nonchiral liquid crystal crown ether of alike structure was also synthesized for comparison, indicating that only the former was asymmetric. The present work represents the first attempt of the investigation in chiral liquid crystal crown ether, thus providing basis for further research into problems as such.
基金This project was supported by the Natural Science Foundation of Shandong Province (No.Y2003 D01)
文摘3,3′-Dimethyl-dibenzo-18-crown-6 was synthesized and characterized by elemental analysis, FT-IR, ^1H NMR, UV, MS spectra and X-ray single-crystal diffraction. It belongs to orthorhombic, space group Pna21 with a = 8.0790(18), b = 16.780(4), c = 15.222(3) .A, Z= 4, V= 2063.6(8) A3 Dc = 1.250 g/cm^3,μ = 0.090 mm^-1, F(000) = 832, R = 0.0474 and wR = 0.1103. According to structural analysis, the title compound possesses a boat-like configuration.
文摘Dibenzo-1 , 4 , 10 , 13-tetraselena-7 , 16-dioxacyclo-octadeca-2 , 11-diene was synthesized by the condensation of poly (o-diselenobenzene) with bis (2-chloroethyl) ether in the presence of potassium borohydride. The molecular structure was examined by IR, MS and  ̄1H NMR spectra, and confirmed by an X-ray diffraction study. The molecule in the crystal has a centrosymmetry and shows a chair conformation. The dihedral angle between the plane containing the four Se atoms and the benzene ring is 104. 1 (2)°. All geometrical parameters of the molecule are unexceptional. Crystal data : C_20H_24O_2Se_4, M_r= 612. 26, monoclinic, space group P2_1/c, a=8. 866(2) , b=5. 349(1). c=22. 315(3) A, β=96. 04(2)°, V=1052. 3 A ̄3, Z=2,D_c=1.932 g/cm ̄-3 , μ(MoKα) = 69. 15 cm ̄-1, F(000) = 592, T= 297K, R= 0. 038for 1270 observed reflections and 154 refined parameters.
文摘Crystal structure of the title compound C 16 H 25 O 2NS 2 has been determined by X-ray diffraction method. Its crystallographic data were as follows: M r=327.51, triclinic, space group P1, a=8.864(3), b=10.127(4), c=10.390(3) , α=105.94(3), β=103.10(2), γ=90.96(3)°, V=870.3(7) 3, Z=2, D c=1.250g.cm -3 , μ(MoKα)=2.966cm -1 , F(000)=176, a total of 3275 reflections measured (2θ max =50°), 2246[I5σ(I)] used in the refinement, R=0.067, R w=0.082. The result shows that the distances of N(1)-C(2) and N(1)-C(3) are longer than that of N(1)-C(11), which indicates that the interaction of C Ar -N sp 2 is stronger than that of C sp 3 -N sp 2 . Oxygen, nitrogen and sulfur atoms of the ring in the same plane was deduced from the least\|squares planes and the dihedral angles.
基金This work was supported by the National Natural Science Foundation of China.
文摘The title compound C18 H25 NC4ClBr2Cu crystallizes in space group P 1 with a = 1.0105(2)nm b=1.0821(1) nm, c=1. 1007(2) nm, a=80. 00(1)°,β=80. 26(1)° γ=77. 83(1)°. Z=2, D = 1. 831 g/cm3, μ=62. 658 cm-1(Mok(?)). The final refinement converged to R=0. 031 for 2547 independent observed reflections. The complex molecule consists of two cationic moieties (HL)+ and an anion which appears as a bromide-bridged copper dimer (Cu2Br6)2-. This structural characterization seems to be rare in metal complexes with crown-ether.
文摘The reactions of 18 crown 6 with each of K 2(M=Zn, Hg; mnt=1,2 dicyanoethene 1,2 dithiolate, C 2S 2(CN) 2- 2) were studied and novel complexes [K(18 C 6)] 2[Zn(mnt) 2](1) and [K(18 C 6)] 2[Hg(mnt) 2](2) were characterized by elemental analysis, IR spectrum and X ray diffraction analysis. Complex 1 displays a one dimensional chain of [K(18 C 6)] 2[Zn(mnt) 2] bridged by K O interactions between adjacent [K(18 C 6)] + units. Complex 2 is also a one dimensional chain of [K(18 C 6)] 2[Hg(mnt) 2] bridged by K...S weak interactions between adjacent [K(18 C 6)] + and [Hg(mnt) 2] 2- .
基金supported by the Natural Science Foundation of Hebei Province (No. B2009000670)the Foundation of the Education Department of Hebei Province (No. 2009117)
文摘Double-armed crown ether 15,16-bis((4-nitrophenoxy)methyl)-2,3,5,6,8,9,11,12-octahydrobenzo[b][1,4,7,10,13] pentaoxacyclopentadecine F.W. 570.54 was synthesized by dibromomethyl benzo-15-crown-5 with 4-nitrophenol in the presence of anhydrous K2CO3, characterized by spectroscopic techniques and confirmed by X-ray crystal structure analysis. The title compound crystallizes in monoclinic, space group P21/c with a = 12.840(4), b = 9.425(3), c = 22.447(7), β = 98.128(7)° and Z = 4. The structure exhibits intermolecular hydrogen bonding of C-H···O type.
基金Project supported by the National Natural Science Foundation ot China.
文摘4',5'-Dibromo-o-xylyl-17-crown-5 ether (2BrB17C5) was synthesized,starting from 1,2-dibromo-4,5-bis(bromomethyl)-benzene and tetraethylene glycol,and was characterized by 1H NMR,MS and elemental analysis.Pale yellow prismatic single crystal obtained from anhydrous ethanol was investigated by X-ray structural analysis.The complexation properties toward alkali metal ions were examined using the solvent extraction method and UV absorption spectroscopy.The crown ether was found to be conformationally deformed and oblate-like and is highly selective for lithium ion.
基金supported by the National Natural Science Foundation of China(No.21243007)National Defense Fundamental Scientific Research(No.B09201100051)
文摘A new energetic organic potassium salt bis(dinitromethyl)difurazanyl ether potas- sium salt [K2(BDFE)] was synthesized, and structurally characterized by elemental analysis, IR spectra, t3C NMR and single-crystal X-ray diffraction. K2(BDFE) crystallizes in monoclinic system, space group C2/c with a = 17.342(3), b = 12.6943(17), c = 8.0972(11) A, β = 110.630(2)°, V = 1668.3(4) A3, Z = 4, Dc = 2.000 g/cm3, F(000) = 1000,μ= 0.675 mm-1, S = 1.058, the final R = 0.0499 and wR = 0.1452. The K ion is eight-coordinated with eight O atoms from one water molecule and four bis(dinitromethyl)difurazanyl ethers (BDFE), forming a distorted dodecahedral structure. Thermal decomposition of the title complex was studied by using DSC and TG-DTG. There are primarily two exothermic decomposition processes between 200 and 370 ℃.
基金National Natural Science Foundation of China,the Natural Science Foundation of Guangdong Province of China
文摘Two charged donor-acceptor [2]catenanes were synthesized by the cyclization of the π-acceptor 1,1 '-[1, 4-phenylenebis-(methylene)]bis(4,4'-bipyridinium)bis(hexafluorophosphate)(2) and bis(bromomethyl)benzene with the templates of the π-donor phenylene-diacetylene crown ethers la and lb in the yields of 31%, 35%, respectively. The mass spectra, 1H and 13C NMR spectra confirm that the phenylene-diacetylene crown ethers, with a nonaromatic ~r-system, successfully template the cyclization of CBPQT4+. The X-ray crystallography analysis shows that the CBPQT4+ ring encircles around the phenylene motif of the crown ethers, leaving the 1,3-butadiyne fragment out of the cavity of CBPQT4+ ring. The mechanically interlocked structure of [2]catenanes was stabilized by the cooperative effects of π-stacking and hydrogen bonding interactions.
基金supported by the National Natural Science Foundation of China and the Doctoral Special Grant from the State Education Commission of China.
文摘The preparation and X-ray crystal structures of the adducts of 10-thiabenzo-15-crown-5 and 10-selenabenzo-15-crown-5 with PdCl2 are reported. [PdCl2(C14H20O4S)2] (1): or-thorhombic, space group Pbca with cell dimensions of a=17.285(5), 6=8.354(3), c=21.689(4) A, K=3131.9 A3, Z=4;R=0.0330 for 2301 reflections with I > 3o(I), [PdCl2(C14H2oO4Se)2] (2): monoclinic, space group P21/n with cell dimensions of a=18.928(4), b=8.912(3), c=9.813(2) A, β=96.90(2)0, V=1643.4 A3, Z=2; R=0.0289 for 2617 reflections with I> 3σ(I), Both complexes are monomeric, square-planar palladiurn(Ⅱ) compounds with the Pd(Ⅱ) ion situating on a crystal-lographic inversion centre, and the crown ligands all adopt the axial coordination with the Pd-S bond of 2.3233(7) A and the Pd-Se bond of 2.4357(3) A. Their complexing characteristics are discussed in brief.
文摘The preparation method of [Na ( DB18C6) (CH_3OH )]_2Mo_6O_(19)·(DB18C6)·(CH_3OH) , where DB18C6 is dibenzo-18-crown-6, is described. Thecrystal and molecular structure of the title complex has been determined crystallographically. The title complex crystallizes in the monoclinic system,space group P2_1/c ,a=18. 727(6) ,b=19. 555(6) , c=22. 827(7) ,β=112. 84(3)°, V=7704(4)  ̄3 ,M_r = 2102. 9 , Z = 4 , F (000 ) = 4224 , μ= 1 . 028 mm  ̄(-1), D_c = 1.813 g/cm ̄3 . final R =0. 075 and R_w= 0. 078 based on 4463 observed reflections with F>6. 0σ(F) . The complex consists of [Mo_6O_(19)] ̄(2-) ,[Na(DB18C6)] ̄+ and CH_3OH, which are linked by long distance interaction through O-Na-O bond.
文摘The interaction of lanthanum(Ⅲ) chloride with 12-crown-4 in MeCN/MeOH mixed solvent produces an anhydrous complex,LaCl3(12-crown-4)(MeOH)(complex Ⅰ),C9H20O5LaCl3(Mr= 453.6),in which the La(Ⅲ) ion is 8-coordinated by three Cl anions,four oxygen atoms from a crown ligand and a methanol oxygen atom,the complex molecules were connected into a dimer by two O(MeOH)…Cl hydrogen bonds.Reaction of complex Ⅰ with phen(1,10-phenanthroline) gives the crystallization of[LaCl3 (phen)2(H2O)]·MeOH(complex Ⅱ),C25H22O2N4LaCl3(Mr= 655.8) in which the crown ligand is totally replaced by two phen molecules.Cell parameters for the two complexes are a= 9.389(3)[13.228 (5)],b=11.382(4)[10.767(3)],c=7.542(3)[18.520(6) ];α=94.32(3)[90.0],β=102.10(2)[102.01(3)],γ=91. 83(3)[90. 0]°with space group P1[P21/α];V=784.5(5)[2580(1)3,Z=2[4];μ(MoKα)=32.8[20. 2]cm-1;F (000)=444[1296];R=0.042[0.045];Rω=0.044[0.036] for 2398 [2345] observed reflections withⅠ>3σ(Ⅰ).The La(Ⅲ) ion in complex Ⅱ is 8-coordinated by three Cl anions,four N atoms of two phen molecules and one water molecule.The methanolmolecule forms a hydrogen bond with Cl(3) atom.
文摘Single crystals of complex BiCl3(15-crown-5) were synthesized by gel method, and the structure was solved from X-ray diffraction data by direct and Fourier methods. The crystal is orthorhombic, space group is P212121 with unit cell parameters:a = 7. 677(4), 6=13. 254(6) and c= 15. 911(6) A , and 2=4. The final structural refinement converged with unweighted and weighted factors of 0. 053 and 0. 063 respectively for 1290 observed reflections. The structure consists of discrete BiCl3(15-crown-5) molecules in which bismuth atom is sandwiched between two essentially parallel planes, one of which contains five oxygen atoms and the other contains three chlorine atoms.
文摘The supennolecular based on sodium molybdate(Ⅵ) and sulfate, dibenzo-18-crown-6 was synthesized in acetonitrile and characterized by elemental analysis, IR,^1H NMR, single crystal X-ray diffraction, indicating that it contains [S2M018062]^4+ and [Na(DB18Cr)(H2O)]^+, where each sodium ion is deviated from the plane defined by the oxygen atoms in the corresponding crown ether. The compound crystallizes in the monoclinic space group C2/c with a=3.29332(10) nm, b= 1.90917(6) nm, c=2.63132(7) nm, β= 121.6630(10)°, V=14081.8(7) nm^3, Z=8, T=293(2) K, and R1(wR2)=0.0177 (0.1525). The compound exhibits a novel organic-inorganic structure, in which the crown ether-sodium complexes are coordinated to the terminal oxygen atoms of Mo18054 and the oxygen atoms of water molecule.
基金Supported by NNSFC (20302002 and 20872046)the SRF for ROCS, SEM (No. [2007] 1108)
文摘The crystal structure of the title compound (C18H18N4O, Mr = 306.36) has been determined by single-crystal X-ray diffraction. The crystal is of triclinic, space group P1 with α = 4.783(0), b = 13.577(1), c = 13.830(1) A, α = 63.581(2), β = 88.326(2), γ = 86.161(2)°, V= 802.5(1) A3, Z= 2, Dc = 1.268 g/cm^3, F(000) = 324, μ(MoKa) = 0.082 mm^-1, the final R = 0.0497 and wR = 0.1199 for 3094 observed reflections (I 〉 2σ(I)). The dihedral angles between the phenyl (C(1)-C(4)-(6)) and triazole, the phenyl (C(13)-C(15)-C(18)) and triazole, and the two phenyl rings are 7.9(1), 69.9(1) and 67.8(1)°, respectively. Strong C-H…π interaction joins molecules into a chain along the c axis and contributes to the stability of the structure. Preliminary bioassay results show that the title compound possesses excellent and selective fungicidal activity against Colletotrichum gossypii but displays moderate to weak insecticidal activity against aphides.
文摘The interaction of lanthanum(Ⅲ) chloride with 12-crown-4 in MeCN/MeOH mixed solvent produces an anhydrous complex,LaCl3(12-crown-4)(MeOH)(complex Ⅰ),C9H20O5LaCl3(Mr= 453.6),in which the La(Ⅲ) ion is 8-coordinated by three Cl anions,four oxygen atoms from a crown ligand and a methanol oxygen atom,the complex molecules were connected into a dimer by two O(MeOH)…Cl hydrogen bonds.Reaction of complex Ⅰ with phen(1,10-phenanthroline) gives the crystallization of[LaCl3 (phen)2(H2O)]·MeOH(complex Ⅱ),C25H22O2N4LaCl3(Mr= 655.8) in which the crown ligand is totally replaced by two phen molecules.Cell parameters for the two complexes are a= 9.389(3)[13.228 (5)],b=11.382(4)[10.767(3)],c=7.542(3)[18.520(6) ];α=94.32(3)[90.0],β=102.10(2)[102.01(3)],γ=91. 83(3)[90. 0]°with space group P1[P21/α];V=784.5(5)[2580(1)3,Z=2[4];μ(MoKα)=32.8[20. 2]cm-1;F (000)=444[1296];R=0.042[0.045];Rω=0.044[0.036] for 2398 [2345] observed reflections withⅠ】3σ(Ⅰ).The La(Ⅲ) ion in complex Ⅱ is 8-coordinated by three Cl anions,four N atoms of two phen molecules and one water molecule.The methanolmolecule forms a hydrogen bond with Cl(3) atom.