The complex {[Mn(H2O)4(3, 3?azpy)](3, 3?azpy)3(PF6)2}n (3, 3?azpy = 3, 3? azobispyridine) has been synthesized and characterized. The crystal (C40H40F12MnN16O4P2, Mr = 1153.76) belongs to the triclinic system, space g...The complex {[Mn(H2O)4(3, 3?azpy)](3, 3?azpy)3(PF6)2}n (3, 3?azpy = 3, 3? azobispyridine) has been synthesized and characterized. The crystal (C40H40F12MnN16O4P2, Mr = 1153.76) belongs to the triclinic system, space group P with the following crystallographic parameters: a = 10.761(2), b = 11.040(2), c = 23.365(4) ? a = 85.52(1), b = 82.69(1), g = 70.44(1)? V = 2592.5(8) 3, Dc = 1.478 g/cm3, m(MoKa) = 4.16 cm-1, F(000) = 1174, Z = 2, final R = 0.0493 and wR = 0.1158 for the observed reflections (I > 2.00s(I)). The X-ray analysis revealed that manganese(Ⅱ) cation coordination environment is a distorted octahedral geometry, and the Mn2+ cation is coordinated by four oxygen atoms of water in the equatorial plane, while the two nitrogen atoms of 3, 3?azpy occupy the axial positions. The complex forms a one-dimensional chain structure via 3, 3?azpy bridging ligand.展开更多
The title complex [Cu2(bipy)2OAcClOH]TsTausH3H2O(C31H37Cl- Cu2N5O11S2) has been synthesized by the reaction of 2,2?bipyridine(bipy), N-P-tolysulfony taurine (TsTausH) and copper acetate in water-ethanol solution, and ...The title complex [Cu2(bipy)2OAcClOH]TsTausH3H2O(C31H37Cl- Cu2N5O11S2) has been synthesized by the reaction of 2,2?bipyridine(bipy), N-P-tolysulfony taurine (TsTausH) and copper acetate in water-ethanol solution, and its crystal structure was determined by X-ray diffraction method. The crystal belongs to triclinic, space group P with a = 0.74485(14), b = 1.6094(3), c = 1.7472(3) nm, a = 114.662(4), b = 99.997(4), g = 93.218(4), V = 1.8551(6) nm3, Mr = 882.31, Z = 2, Dc = 1.580 g/cm3, m = 1.395 mm-1 and F(000) = 906. The complex is a binuclear copper compound, and the two copper ions nearly have the same coordination environment. There exists MM bond in the complex. The distance of Cu(1)Cu(2) is 0.29747(7) nm. The two ions form two distorted octahedral geometries.展开更多
In this paper,a new type of photonic crystal fiber with high birefringence is proposed and analyzed with a full-vector model based on the super-lattice and the plane-wave expansion model.Due to the two different sizes...In this paper,a new type of photonic crystal fiber with high birefringence is proposed and analyzed with a full-vector model based on the super-lattice and the plane-wave expansion model.Due to the two different sizes of the holes introduced into the cladding of the PCF,the fiber is two-fold rotational symmetry and appears to be with high birefringence.Numerical results demonstrate that a modal birefringence at wavelength 1.31 μm is 1.8×10-3 in the PCF withΛ=2.55 μm, d1/Λ=0.3and d2/Λ=0.833. A near 200 nm SPSM region within the wavelength range from 1.4 μm to 1.6 μm is obtained.展开更多
By the reactions of [Rh2Co2(CO)12] 1 with functionally substituted alkyne ligands HC≡CR 2 (R = FeCp2) and 3 (R = 2-OH-C6H4COOCH2), respectively in n-hexane at room temperature, two new cluster derivatives [Rh2Co2(CO)...By the reactions of [Rh2Co2(CO)12] 1 with functionally substituted alkyne ligands HC≡CR 2 (R = FeCp2) and 3 (R = 2-OH-C6H4COOCH2), respectively in n-hexane at room temperature, two new cluster derivatives [Rh2Co2(CO)6(-CO)4(4, 2-HC≡CR)] 4 (R = FeCp2) and 5 (R = 2-OH-C6H4COOCH2) were obtained respectively. The alkyne was inserted into the CoCo bond of cluster 1 to give two butterfly clusters. Cluster 4 has been determined by single-crystal X-ray diffraction. Crystallographic data: C22H10Co2FeO10Rh2, Mr = 813.83, orthorhombic, space group P212121, a = 11.5318(7), b = 12.6572(7), c = 17.018(1) ? V = 2483.9(3) 3, Z = 4, Dc = 2.176 g/cm3, F(000) = 1568, = 3.233 mm-1, the final R = 0.0366 and wR = 0.0899 for 5367 observed reflections with I > 2(I). The two clusters have also been characterized by elemental analysis, IR and 1H-NMR spectroscopy.展开更多
The mononuclear copper(I) complex, [Cu(dppe)2](PF6)(CH3COCH3) [dppe = bis-(diphenylphosphino)ethane] has been synthesized and characterized by X-ray crystallography. The crystal belongs to monoclinic, Mr=1062.3, space...The mononuclear copper(I) complex, [Cu(dppe)2](PF6)(CH3COCH3) [dppe = bis-(diphenylphosphino)ethane] has been synthesized and characterized by X-ray crystallography. The crystal belongs to monoclinic, Mr=1062.3, space group P21/n with cell parameters a =14.741(2), b =19.354(8), c =18.587(3) ? = 91.41(1)°, V = 5301.5 3, Z = 4, Dc=1.302 g/cm3, F(000)= 2200, = 6.16cm-1, R=0.062, Rw = 0.068. A total of 9679 independent reflections were collected, of which 4574 reflections with I >3σ(I) were observed. The central Cu atom is coordinated by four P atoms from dppe to form a distorted tetrahedral environment. In the coordination sphere the bond lengths of CuP(1), CuP(2), CuP(3) and CuP(4) are 2.298(2), 2.305(2), 2.311(2) and 2.295? respectively; and the PCuP bond angles vary from 87.52(9) to 120.12(9)?展开更多
A new copper complex, Cu2（pba）（bpy）2Cl2·4H2O （here pba was propylenebis （oxamic acid）, bpy was bipyridine）, was synthesized. Crystal structure of the title complex was determined. It belongs to the tetrag...A new copper complex, Cu2（pba）（bpy）2Cl2·4H2O （here pba was propylenebis （oxamic acid）, bpy was bipyridine）, was synthesized. Crystal structure of the title complex was determined. It belongs to the tetragonal system, molecular formula Cu2Cl2O 10N6C 27H 32, Mr=798.58, space group P41212, a=b=9.484（4）, c=35\^918（9）, V=3235（2）3, Dx=1.64gcm -3 and F（000）=1568, μ=1\^546mm -1 for Z=4. The crystal structure was solved by direct methods for final R=0\^048 and Rw=0.060 for 1992 observed reflections with I>3σ（I）. The complex has a C2 symmetry. A chloride anion, two nitrogen atoms from bipyridine and two oxygen atoms from the oxamide carbonyl and carboxyl coordinated to the Cu II ion forming a square pyramidal geometry. In each molecule, two bpy are almost parallel.展开更多
The reduction of an aqueous solution of sodium molybdate by iron powder at low pH value (～0.83), in the presence of ethylenediaminetetraacetate (EDTA) ligand, gives the title compound [Fe(H 2O) 6][Mo 2O 4(EDTA)]·...The reduction of an aqueous solution of sodium molybdate by iron powder at low pH value (～0.83), in the presence of ethylenediaminetetraacetate (EDTA) ligand, gives the title compound [Fe(H 2O) 6][Mo 2O 4(EDTA)]·5H 2O 1, which was characterized by elemental analysis, IR and X ray single crystal diffraction techniques. Compound 1 crystallizes in monoclinic system, space group P2 1/c, C 10 H 34 N 2FeMo 2O 23 , M r=798.12, a=8.781(1), b=14.081(1), c=21.353(1) , β= 92\^688(1)°, V = 2637.2(3) 3, Z = 4, D c = 2.010 g·cm -3 , μ = 1.579 mm -1 , F (000)=1608, the final R =0.0530 and wR =0.1271 for 3312 observed reflections. The binuclear oxomolybdenum(V) anion and the six coordinated Fe(II) cation are linked to infinite three dimensional network through several hydrogen bonds towards different directions between crystal waters, Fe(II) cation and Mo(V) anion.展开更多
C_(10)H_8N_2O_2S_2, Mr=252. 32,monoclinic,P2_(1/c),a=7.165(5).b=7.659(3),c=19.543(8)A,β=96. 76(5)°,V=1065.0(9) A,Z=4,D_c=1. 57 g/cm￣3.The structure was solved by direct methods and refined to final R(R_w)=0.051...C_(10)H_8N_2O_2S_2, Mr=252. 32,monoclinic,P2_(1/c),a=7.165(5).b=7.659(3),c=19.543(8)A,β=96. 76(5)°,V=1065.0(9) A,Z=4,D_c=1. 57 g/cm￣3.The structure was solved by direct methods and refined to final R(R_w)=0.051(0.057) for 1446 observed reflections with I≥3σ(Ⅰ).The sulfur-sulfur bond length is found to be 2. 019(2) A with a dihedral angle CSSC of 93.29°.展开更多
A mononuclear copper(II) complex, [Cu(bipy)(naph)(ClO4)] (where bipy is bipyridine and naph is 2-hydroxy-1-naphthaldehyde), was synthesized and characterized by X-ray single-crystal structure analysis. The crystal is ...A mononuclear copper(II) complex, [Cu(bipy)(naph)(ClO4)] (where bipy is bipyridine and naph is 2-hydroxy-1-naphthaldehyde), was synthesized and characterized by X-ray single-crystal structure analysis. The crystal is triclinic, space group P ?with a = 9.245(4), b = 9.962(4), c = 10.809(7) ? a = 84.83(5), b =82.35(4), g = 81.02(4), V = 972.1 ?, C21H15ClCuN2O6 Mr = 490.36, Z = 2, F(000) = 498, Dx = 1.68 g/cm3, m = 13.05 cm-1, R = 0.078, Rw = 0.081 for 2295 observed reflections with I > 3s(I). The copper(II) ion is coordinated by two nitrogen atoms of bipy and two oxygen atoms of naph in the equatorial plane, with an axial perchlorate oxygen-copper(II) bond to copper(II) ion to form square-pyramidal coordination geometry. The coordination environment of copper(II) is similar to the active site of galactose oxidase and this compound may also be considered as the structural model of galactose oxidase.展开更多
A novel complex [Cd2(phen)4(fca)2](ClO4)2(H2O)2 (fca = dianion of 3-ferrocenyl- 2-crotonic acid, phen = 1,10-phenanthroline) has been synthesized and characterized by X-ray single-crystal structure analysis. It crysta...A novel complex [Cd2(phen)4(fca)2](ClO4)2(H2O)2 (fca = dianion of 3-ferrocenyl- 2-crotonic acid, phen = 1,10-phenanthroline) has been synthesized and characterized by X-ray single-crystal structure analysis. It crystallizes in triclinic system, space group P?with a = 11.6297(5), b = 12.5165(5), c = 13.8986(6) ? a = 63.345(1), b = 87.747(1), g = 71.862(1), V = 1706.20(1) ?, Z = 1, Dc = 1.673 g/cm3, F(000) = 868 and m(MoKa) = 1.185 mm-1 (l = 0.71073 ). R = 0.0800 and wR = 0.1793 for 7653 observed reflections (I > 2s(I)). The structure consists of a dinuclear cation [Cd2(phen)4(fca)2]2+, two discrete perchlorate anions and two water molecules. The cationic part of the complex shows a tetrametallic core in which two fca groups act as the (O, O) bridging ligands between two cadmium(Ⅱ) ions with a distorted octahedral environment. The Cd…Cd intradimer distance is 4.128 ?展开更多
The binuclear complex [Ag2(m-Ph2PNHPPh2)3](ClO4)2CH2Cl2CH3OH (Ph2PNHP- Ph2 = bis(diphenylphosphino)amine) was prepared from the reaction of AgClO4 with bis- (diphenylphosphino)amine in equimolar ratio through self-ass...The binuclear complex [Ag2(m-Ph2PNHPPh2)3](ClO4)2CH2Cl2CH3OH (Ph2PNHP- Ph2 = bis(diphenylphosphino)amine) was prepared from the reaction of AgClO4 with bis- (diphenylphosphino)amine in equimolar ratio through self-assembly. The coordination cation affords a triply-bridging [Ag2L3]-type coordination moiety. The silver atom is in a trigonal planar environment with P3 coordination chromophore. The complex (C74H69Cl4N3O9P6Ag2) crystallizes in monoclinic, space group Cc with a = 18.3738(1), b = 20.0207(4), c = 20.5422(4) ? b = 95.829(1), V = 7517.5(2) 3, Z = 4, Mr = 1687.68, Dc = 1.491 g/cm3, F(000) = 3432, m = 0.848 mm-1, the final R = 0.0460 and wR = 0.0935 for 7005 observed reflections with I > 2s(I).展开更多
The title compound 4, 5-bis ( 2,-dinitrophenylthio )-1, 3-dithiole-2-thione [C3S5(C6H3N2O4)2] crystallizes in the orthogonal system, space group P212121,with a=10. 134(3) , b=20. 488(4), c=9. 656(3)A , V=2005. 1 A3, D...The title compound 4, 5-bis ( 2,-dinitrophenylthio )-1, 3-dithiole-2-thione [C3S5(C6H3N2O4)2] crystallizes in the orthogonal system, space group P212121,with a=10. 134(3) , b=20. 488(4), c=9. 656(3)A , V=2005. 1 A3, D_c=1. 76 g/cm￣3 , Z=4, M.=530. 56, λ=0. 71069 A, F(000)= 1072 , μ=6.1 cm￣(-1), T=296K.Final R= 0. 038, R.= 0. 045 for 1799 reflections with I≥3.5σ(I). In this nonplanar neutral molecule both nitrobenzol rings are approximately perpendicular to the dithiole ring with an asymmetric configuration.展开更多
The new uranyl complex UO2(NO3)2[PhN(CH3)C(O)(CH3)NPh]2 was synthesized and its crystal structure has been determined by single-crystal X-ray diffraction. Crystal data: C30H32N6O10U, triclinic, space group P with a = ...The new uranyl complex UO2(NO3)2[PhN(CH3)C(O)(CH3)NPh]2 was synthesized and its crystal structure has been determined by single-crystal X-ray diffraction. Crystal data: C30H32N6O10U, triclinic, space group P with a = 7.772(1), b = 9.267(1), c = 12.644(1) ? a = 68.246(8), b = 73.871(9), g = 84.99(1)o, V = 812.4(2) ?, Mr = 874.65, Z = 1, Dc = 1.788 g/cm3, F(000) = 426, m = 5.062 mm-1, the final R = 0.022 and wR = 0.059 for 3571 observed reflections (I > 2s(I)). The central uranyl ion is coordinated by six oxygen atoms, two from the carbonyl groups of N,N-dimethyl-N,N-dibenzenyl-urea molecules and the other four from two nitrate groups.展开更多
The title compound 2,5-bis(morpholino)-3,4-bis(p-chlorophenyl) thiophene 2 was obtained by the reaction of -thio-p-chlorobenzoyl thioformmorpholine 1 with trimethyl phosphite in refluxing xylene. The crystal is of tri...The title compound 2,5-bis(morpholino)-3,4-bis(p-chlorophenyl) thiophene 2 was obtained by the reaction of -thio-p-chlorobenzoyl thioformmorpholine 1 with trimethyl phosphite in refluxing xylene. The crystal is of triclinic, space group P?with unit cell constants: a = 6.0740(1), b = 10.3250(1), c = 19.779(2) , ?= 76.740(1), = 87.110(1), = 74.920(1), C24H24Cl2N2O2S, Mr = 475.41, Z = 2, V = 1165.7(3) ?, Dc = 1.354 g/cm3, (MoK) = 0.71073, = 0.392 mm-1, F(000) = 496, the final R = 0.0324 and wR = 0.0819 for 3102 observed reflections (I > 2(I)). X-ray analysis reveals that the two morpholinyl groups are located at the -position of thiophene, and the two p-chlorophenyl groups at the -position. Therefore, the title compound is a new symmetric thiophene derivative.展开更多
The title complex was prepared from the reaction of 1,2-bis(phenylthiomethyl)- benzene L with K2PtCl4 at room temperature and its structure has been determined by single-crystal X-ray diffraction. There exist two inde...The title complex was prepared from the reaction of 1,2-bis(phenylthiomethyl)- benzene L with K2PtCl4 at room temperature and its structure has been determined by single-crystal X-ray diffraction. There exist two independent cis-[1,2-bis(phenylthiomethyl)benzene]dichloro- platinum(Ⅱ) [PtCl2L] molecules without significant structural difference and a molecule of acetonitrile in one crystallographic asymmetric unit. Crystallographic data: triclinic, space group Pī, a = 11.010(3), b = 12.080(3), c = 16.095(4) ? = 94.728(5), = 90.129(5), = 99.274(5)? C20H18Cl2NPtS20.5CH3CN, Mr = 608.98, V = 2105(1) ?, Z = 4, Dc = 1.921 g/cm3, (Mo-K) = 7.122 mm1, F(000) = 1172, R = 0.0503 and wR = 0.0848 for 3929 observed reflections with I > 2s(I). The title complex is a neutral molecule in which the central Pt(Ⅱ) ion is four-coordinated with two S-donors of the ligand and two Cl anions, forming a distorted square planar geometry. In the crystal, there exist two kinds of molecular packing patterns. One [PtCl2L] molecule is connected to the other one through the weak interactions of Pt…Pt, Pt…S and Pt…Cl, forming a supramolecular quasi-dimer. The other one complex molecule is connected with the CH3CN molecule by weak Cl…N interaction.展开更多
A novel binuclear copper (Ⅱ) complex,namely [Cu 2｛Ph 3P(CH 2) 2CO 2｝ 4(NO 3) 2]·(NO 3) 2 1,has been synthesized from the reaction of Cu(NO 3) 2·4H 2O with Ph 3P +(CH 2) 2CO - 2 L.The si...A novel binuclear copper (Ⅱ) complex,namely [Cu 2｛Ph 3P(CH 2) 2CO 2｝ 4(NO 3) 2]·(NO 3) 2 1,has been synthesized from the reaction of Cu(NO 3) 2·4H 2O with Ph 3P +(CH 2) 2CO - 2 L.The single crystal X ray structural analysis of 1 indicates that the compound crystallizes in space group P1(No.2) with a=12.652(3),b=18.983(4),c=9.102(3),α=97.26(2)°,β=107.38(2)°,γ=102.22(2)° and Z=1.In complex 1,a pair of Cu(Ⅱ) atoms are bridged by carboxylate groups of four ligand molecules with a Cu…Cu distance of 2.738 to form a tetrakis (carboxylato O,O) bridge dimetal core,and the apical coordination positions are occupied by monodentate nitrato anions,which is rare in the structures of similar Cu(Ⅱ) complexes in which the apical ligands are usually neutral molecules.The result shows that introducing the anionic ligands into the coordination sphere of the Cu(Ⅱ) atom significantly increases the Cu…Cu distance.展开更多
Two new polymeric erbium(Ⅲ) complexes of two flexible double betaine ligands have been synthesized and characterized by X-ray analysis. In {[Er(L1)(H2O)4)Cl3 H2O}n (1) (L1 = 4, 4’ -trimethylenedipyridinio-N, N’-dia...Two new polymeric erbium(Ⅲ) complexes of two flexible double betaine ligands have been synthesized and characterized by X-ray analysis. In {[Er(L1)(H2O)4)Cl3 H2O}n (1) (L1 = 4, 4’ -trimethylenedipyridinio-N, N’-diacetate ), the erbium(Ⅲ) ions form a two-dimensional metal carboxylate layer in which each pair of Er(Ⅲ) atoms is bridged by two syn-anti μ-carboxylato-o,o’ groups, Adjacent layers arecross-linked through hydrogen bonds among aqua ligands, lattice water molecules andchloride ions to form a three-dimensional network. Complex l, C17 H28 N2 O9 ErC13 (Mr =676.0) is monoclinic, space group C2, with a= 27. 408(4), b= 9. 645 (3), c= 9. 423(2) A, p=1loo. 85(1)’, V=2446. 2(9) A’, Z=4, D=l. 836 g/cm’, F(OOO) =1332, μ(MoKa) = 38.06 cm-1, R=0. 048 for 2451 reflections with I>2σ(I). { [Er(L2 ) (H2O)4]Cl3. 5H2O}. (2) (L2=1, 3-bis (pyridinio-4-carboxylato) propane) comprises lanthanide carboxylate chains built from centrosymmetric dimeric units crosslinked by a pair of L2 ligands, discrete anions and lattice water molecules. In the dimeric unit of complex 2, each pair of metal ions is bridged by four syn-syn μ-carboxylatoO, O’ groups that are oriented nearly perpendicular to each other about the metal-metalaxis. The metal carboxylate chains of complex 2 are further cross-linked by hydrogenbonds to form a three-dimensional network. Complex 2, C15 H32 N2O13 ErCl3 (Mr=722.0) belongs to the monoclinic space group C2/m with a=16. 564 (3), b=15. 839(3), c=11. 792(4) , β=122. 27(1)°, V=2616(1), Z=4, Dc=1.833 g/cm3,F(000) =1436, μ (MoKa) = 35. 75 cm-1, R =0.043 for 2436 observed reflectionswithI>2σ(I).展开更多
基金Supported by the funds of Organic Syntheses Key Laboratory of Jiangsu Province
文摘The complex {[Mn(H2O)4(3, 3?azpy)](3, 3?azpy)3(PF6)2}n (3, 3?azpy = 3, 3? azobispyridine) has been synthesized and characterized. The crystal (C40H40F12MnN16O4P2, Mr = 1153.76) belongs to the triclinic system, space group P with the following crystallographic parameters: a = 10.761(2), b = 11.040(2), c = 23.365(4) ? a = 85.52(1), b = 82.69(1), g = 70.44(1)? V = 2592.5(8) 3, Dc = 1.478 g/cm3, m(MoKa) = 4.16 cm-1, F(000) = 1174, Z = 2, final R = 0.0493 and wR = 0.1158 for the observed reflections (I > 2.00s(I)). The X-ray analysis revealed that manganese(Ⅱ) cation coordination environment is a distorted octahedral geometry, and the Mn2+ cation is coordinated by four oxygen atoms of water in the equatorial plane, while the two nitrogen atoms of 3, 3?azpy occupy the axial positions. The complex forms a one-dimensional chain structure via 3, 3?azpy bridging ligand.
基金This work was supported by the NSF of Guangxi Province (0339034) and the Science Research Foundation of Guangxi Universities
文摘The title complex [Cu2(bipy)2OAcClOH]TsTausH3H2O(C31H37Cl- Cu2N5O11S2) has been synthesized by the reaction of 2,2?bipyridine(bipy), N-P-tolysulfony taurine (TsTausH) and copper acetate in water-ethanol solution, and its crystal structure was determined by X-ray diffraction method. The crystal belongs to triclinic, space group P with a = 0.74485(14), b = 1.6094(3), c = 1.7472(3) nm, a = 114.662(4), b = 99.997(4), g = 93.218(4), V = 1.8551(6) nm3, Mr = 882.31, Z = 2, Dc = 1.580 g/cm3, m = 1.395 mm-1 and F(000) = 906. The complex is a binuclear copper compound, and the two copper ions nearly have the same coordination environment. There exists MM bond in the complex. The distance of Cu(1)Cu(2) is 0.29747(7) nm. The two ions form two distorted octahedral geometries.
文摘In this paper,a new type of photonic crystal fiber with high birefringence is proposed and analyzed with a full-vector model based on the super-lattice and the plane-wave expansion model.Due to the two different sizes of the holes introduced into the cladding of the PCF,the fiber is two-fold rotational symmetry and appears to be with high birefringence.Numerical results demonstrate that a modal birefringence at wavelength 1.31 μm is 1.8×10-3 in the PCF withΛ=2.55 μm, d1/Λ=0.3and d2/Λ=0.833. A near 200 nm SPSM region within the wavelength range from 1.4 μm to 1.6 μm is obtained.
基金the National Natural Science Foundation of China (29871061)
文摘By the reactions of [Rh2Co2(CO)12] 1 with functionally substituted alkyne ligands HC≡CR 2 (R = FeCp2) and 3 (R = 2-OH-C6H4COOCH2), respectively in n-hexane at room temperature, two new cluster derivatives [Rh2Co2(CO)6(-CO)4(4, 2-HC≡CR)] 4 (R = FeCp2) and 5 (R = 2-OH-C6H4COOCH2) were obtained respectively. The alkyne was inserted into the CoCo bond of cluster 1 to give two butterfly clusters. Cluster 4 has been determined by single-crystal X-ray diffraction. Crystallographic data: C22H10Co2FeO10Rh2, Mr = 813.83, orthorhombic, space group P212121, a = 11.5318(7), b = 12.6572(7), c = 17.018(1) ? V = 2483.9(3) 3, Z = 4, Dc = 2.176 g/cm3, F(000) = 1568, = 3.233 mm-1, the final R = 0.0366 and wR = 0.0899 for 5367 observed reflections with I > 2(I). The two clusters have also been characterized by elemental analysis, IR and 1H-NMR spectroscopy.
基金We thank NSFC(No.29871009) Henan Province Outstanding Youth Science Foundation Natural Science Foundation for the financial support of this research.
文摘The mononuclear copper(I) complex, [Cu(dppe)2](PF6)(CH3COCH3) [dppe = bis-(diphenylphosphino)ethane] has been synthesized and characterized by X-ray crystallography. The crystal belongs to monoclinic, Mr=1062.3, space group P21/n with cell parameters a =14.741(2), b =19.354(8), c =18.587(3) ? = 91.41(1)°, V = 5301.5 3, Z = 4, Dc=1.302 g/cm3, F(000)= 2200, = 6.16cm-1, R=0.062, Rw = 0.068. A total of 9679 independent reflections were collected, of which 4574 reflections with I >3σ(I) were observed. The central Cu atom is coordinated by four P atoms from dppe to form a distorted tetrahedral environment. In the coordination sphere the bond lengths of CuP(1), CuP(2), CuP(3) and CuP(4) are 2.298(2), 2.305(2), 2.311(2) and 2.295? respectively; and the PCuP bond angles vary from 87.52(9) to 120.12(9)?
文摘A new copper complex, Cu2（pba）（bpy）2Cl2·4H2O （here pba was propylenebis （oxamic acid）, bpy was bipyridine）, was synthesized. Crystal structure of the title complex was determined. It belongs to the tetragonal system, molecular formula Cu2Cl2O 10N6C 27H 32, Mr=798.58, space group P41212, a=b=9.484（4）, c=35\^918（9）, V=3235（2）3, Dx=1.64gcm -3 and F（000）=1568, μ=1\^546mm -1 for Z=4. The crystal structure was solved by direct methods for final R=0\^048 and Rw=0.060 for 1992 observed reflections with I>3σ（I）. The complex has a C2 symmetry. A chloride anion, two nitrogen atoms from bipyridine and two oxygen atoms from the oxamide carbonyl and carboxyl coordinated to the Cu II ion forming a square pyramidal geometry. In each molecule, two bpy are almost parallel.
文摘The reduction of an aqueous solution of sodium molybdate by iron powder at low pH value (～0.83), in the presence of ethylenediaminetetraacetate (EDTA) ligand, gives the title compound [Fe(H 2O) 6][Mo 2O 4(EDTA)]·5H 2O 1, which was characterized by elemental analysis, IR and X ray single crystal diffraction techniques. Compound 1 crystallizes in monoclinic system, space group P2 1/c, C 10 H 34 N 2FeMo 2O 23 , M r=798.12, a=8.781(1), b=14.081(1), c=21.353(1) , β= 92\^688(1)°, V = 2637.2(3) 3, Z = 4, D c = 2.010 g·cm -3 , μ = 1.579 mm -1 , F (000)=1608, the final R =0.0530 and wR =0.1271 for 3312 observed reflections. The binuclear oxomolybdenum(V) anion and the six coordinated Fe(II) cation are linked to infinite three dimensional network through several hydrogen bonds towards different directions between crystal waters, Fe(II) cation and Mo(V) anion.
文摘C_(10)H_8N_2O_2S_2, Mr=252. 32,monoclinic,P2_(1/c),a=7.165(5).b=7.659(3),c=19.543(8)A,β=96. 76(5)°,V=1065.0(9) A,Z=4,D_c=1. 57 g/cm￣3.The structure was solved by direct methods and refined to final R(R_w)=0.051(0.057) for 1446 observed reflections with I≥3σ(Ⅰ).The sulfur-sulfur bond length is found to be 2. 019(2) A with a dihedral angle CSSC of 93.29°.
基金Supported by the National Natural Science Foundation of China (No. 29971017) the Teaching and Research Award Program for Outstanding Young Teachers in Higher Education Institutions of MOE China.
文摘A mononuclear copper(II) complex, [Cu(bipy)(naph)(ClO4)] (where bipy is bipyridine and naph is 2-hydroxy-1-naphthaldehyde), was synthesized and characterized by X-ray single-crystal structure analysis. The crystal is triclinic, space group P ?with a = 9.245(4), b = 9.962(4), c = 10.809(7) ? a = 84.83(5), b =82.35(4), g = 81.02(4), V = 972.1 ?, C21H15ClCuN2O6 Mr = 490.36, Z = 2, F(000) = 498, Dx = 1.68 g/cm3, m = 13.05 cm-1, R = 0.078, Rw = 0.081 for 2295 observed reflections with I > 3s(I). The copper(II) ion is coordinated by two nitrogen atoms of bipy and two oxygen atoms of naph in the equatorial plane, with an axial perchlorate oxygen-copper(II) bond to copper(II) ion to form square-pyramidal coordination geometry. The coordination environment of copper(II) is similar to the active site of galactose oxidase and this compound may also be considered as the structural model of galactose oxidase.
基金the grants from the State Key Program of China the National Natural Science Foundation of China (29871001 20071001) and the Committee of Education of Anhui province
文摘A novel complex [Cd2(phen)4(fca)2](ClO4)2(H2O)2 (fca = dianion of 3-ferrocenyl- 2-crotonic acid, phen = 1,10-phenanthroline) has been synthesized and characterized by X-ray single-crystal structure analysis. It crystallizes in triclinic system, space group P?with a = 11.6297(5), b = 12.5165(5), c = 13.8986(6) ? a = 63.345(1), b = 87.747(1), g = 71.862(1), V = 1706.20(1) ?, Z = 1, Dc = 1.673 g/cm3, F(000) = 868 and m(MoKa) = 1.185 mm-1 (l = 0.71073 ). R = 0.0800 and wR = 0.1793 for 7653 observed reflections (I > 2s(I)). The structure consists of a dinuclear cation [Cd2(phen)4(fca)2]2+, two discrete perchlorate anions and two water molecules. The cationic part of the complex shows a tetrametallic core in which two fca groups act as the (O, O) bridging ligands between two cadmium(Ⅱ) ions with a distorted octahedral environment. The Cd…Cd intradimer distance is 4.128 ?
基金This work was supported by NNSFC (No. 20171044) and the project for "undred Talents from" the Chinese Academy of Sciences
文摘The binuclear complex [Ag2(m-Ph2PNHPPh2)3](ClO4)2CH2Cl2CH3OH (Ph2PNHP- Ph2 = bis(diphenylphosphino)amine) was prepared from the reaction of AgClO4 with bis- (diphenylphosphino)amine in equimolar ratio through self-assembly. The coordination cation affords a triply-bridging [Ag2L3]-type coordination moiety. The silver atom is in a trigonal planar environment with P3 coordination chromophore. The complex (C74H69Cl4N3O9P6Ag2) crystallizes in monoclinic, space group Cc with a = 18.3738(1), b = 20.0207(4), c = 20.5422(4) ? b = 95.829(1), V = 7517.5(2) 3, Z = 4, Mr = 1687.68, Dc = 1.491 g/cm3, F(000) = 3432, m = 0.848 mm-1, the final R = 0.0460 and wR = 0.0935 for 7005 observed reflections with I > 2s(I).
文摘The title compound 4, 5-bis ( 2,-dinitrophenylthio )-1, 3-dithiole-2-thione [C3S5(C6H3N2O4)2] crystallizes in the orthogonal system, space group P212121,with a=10. 134(3) , b=20. 488(4), c=9. 656(3)A , V=2005. 1 A3, D_c=1. 76 g/cm￣3 , Z=4, M.=530. 56, λ=0. 71069 A, F(000)= 1072 , μ=6.1 cm￣(-1), T=296K.Final R= 0. 038, R.= 0. 045 for 1799 reflections with I≥3.5σ(I). In this nonplanar neutral molecule both nitrobenzol rings are approximately perpendicular to the dithiole ring with an asymmetric configuration.
基金This work was supported by the Funds of the Key Laboratory of Organic Syntheses of Jiangsu province (No. KJS01018) and the Funds of Young Teachers of Suzhou University
文摘The new uranyl complex UO2(NO3)2[PhN(CH3)C(O)(CH3)NPh]2 was synthesized and its crystal structure has been determined by single-crystal X-ray diffraction. Crystal data: C30H32N6O10U, triclinic, space group P with a = 7.772(1), b = 9.267(1), c = 12.644(1) ? a = 68.246(8), b = 73.871(9), g = 84.99(1)o, V = 812.4(2) ?, Mr = 874.65, Z = 1, Dc = 1.788 g/cm3, F(000) = 426, m = 5.062 mm-1, the final R = 0.022 and wR = 0.059 for 3571 observed reflections (I > 2s(I)). The central uranyl ion is coordinated by six oxygen atoms, two from the carbonyl groups of N,N-dimethyl-N,N-dibenzenyl-urea molecules and the other four from two nitrate groups.
基金The project was supported by the Natural Science Foundation of Jiangsu Education Committee (99KJB 150001)
文摘The title compound 2,5-bis(morpholino)-3,4-bis(p-chlorophenyl) thiophene 2 was obtained by the reaction of -thio-p-chlorobenzoyl thioformmorpholine 1 with trimethyl phosphite in refluxing xylene. The crystal is of triclinic, space group P?with unit cell constants: a = 6.0740(1), b = 10.3250(1), c = 19.779(2) , ?= 76.740(1), = 87.110(1), = 74.920(1), C24H24Cl2N2O2S, Mr = 475.41, Z = 2, V = 1165.7(3) ?, Dc = 1.354 g/cm3, (MoK) = 0.71073, = 0.392 mm-1, F(000) = 496, the final R = 0.0324 and wR = 0.0819 for 3102 observed reflections (I > 2(I)). X-ray analysis reveals that the two morpholinyl groups are located at the -position of thiophene, and the two p-chlorophenyl groups at the -position. Therefore, the title compound is a new symmetric thiophene derivative.
基金This project was supported by the National Natural Science Foundation of China (No. 29971019)
文摘The title complex was prepared from the reaction of 1,2-bis(phenylthiomethyl)- benzene L with K2PtCl4 at room temperature and its structure has been determined by single-crystal X-ray diffraction. There exist two independent cis-[1,2-bis(phenylthiomethyl)benzene]dichloro- platinum(Ⅱ) [PtCl2L] molecules without significant structural difference and a molecule of acetonitrile in one crystallographic asymmetric unit. Crystallographic data: triclinic, space group Pī, a = 11.010(3), b = 12.080(3), c = 16.095(4) ? = 94.728(5), = 90.129(5), = 99.274(5)? C20H18Cl2NPtS20.5CH3CN, Mr = 608.98, V = 2105(1) ?, Z = 4, Dc = 1.921 g/cm3, (Mo-K) = 7.122 mm1, F(000) = 1172, R = 0.0503 and wR = 0.0848 for 3929 observed reflections with I > 2s(I). The title complex is a neutral molecule in which the central Pt(Ⅱ) ion is four-coordinated with two S-donors of the ligand and two Cl anions, forming a distorted square planar geometry. In the crystal, there exist two kinds of molecular packing patterns. One [PtCl2L] molecule is connected to the other one through the weak interactions of Pt…Pt, Pt…S and Pt…Cl, forming a supramolecular quasi-dimer. The other one complex molecule is connected with the CH3CN molecule by weak Cl…N interaction.
文摘A novel binuclear copper (Ⅱ) complex,namely [Cu 2｛Ph 3P(CH 2) 2CO 2｝ 4(NO 3) 2]·(NO 3) 2 1,has been synthesized from the reaction of Cu(NO 3) 2·4H 2O with Ph 3P +(CH 2) 2CO - 2 L.The single crystal X ray structural analysis of 1 indicates that the compound crystallizes in space group P1(No.2) with a=12.652(3),b=18.983(4),c=9.102(3),α=97.26(2)°,β=107.38(2)°,γ=102.22(2)° and Z=1.In complex 1,a pair of Cu(Ⅱ) atoms are bridged by carboxylate groups of four ligand molecules with a Cu…Cu distance of 2.738 to form a tetrakis (carboxylato O,O) bridge dimetal core,and the apical coordination positions are occupied by monodentate nitrato anions,which is rare in the structures of similar Cu(Ⅱ) complexes in which the apical ligands are usually neutral molecules.The result shows that introducing the anionic ligands into the coordination sphere of the Cu(Ⅱ) atom significantly increases the Cu…Cu distance.
文摘Two new polymeric erbium(Ⅲ) complexes of two flexible double betaine ligands have been synthesized and characterized by X-ray analysis. In {[Er(L1)(H2O)4)Cl3 H2O}n (1) (L1 = 4, 4’ -trimethylenedipyridinio-N, N’-diacetate ), the erbium(Ⅲ) ions form a two-dimensional metal carboxylate layer in which each pair of Er(Ⅲ) atoms is bridged by two syn-anti μ-carboxylato-o,o’ groups, Adjacent layers arecross-linked through hydrogen bonds among aqua ligands, lattice water molecules andchloride ions to form a three-dimensional network. Complex l, C17 H28 N2 O9 ErC13 (Mr =676.0) is monoclinic, space group C2, with a= 27. 408(4), b= 9. 645 (3), c= 9. 423(2) A, p=1loo. 85(1)’, V=2446. 2(9) A’, Z=4, D=l. 836 g/cm’, F(OOO) =1332, μ(MoKa) = 38.06 cm-1, R=0. 048 for 2451 reflections with I>2σ(I). { [Er(L2 ) (H2O)4]Cl3. 5H2O}. (2) (L2=1, 3-bis (pyridinio-4-carboxylato) propane) comprises lanthanide carboxylate chains built from centrosymmetric dimeric units crosslinked by a pair of L2 ligands, discrete anions and lattice water molecules. In the dimeric unit of complex 2, each pair of metal ions is bridged by four syn-syn μ-carboxylatoO, O’ groups that are oriented nearly perpendicular to each other about the metal-metalaxis. The metal carboxylate chains of complex 2 are further cross-linked by hydrogenbonds to form a three-dimensional network. Complex 2, C15 H32 N2O13 ErCl3 (Mr=722.0) belongs to the monoclinic space group C2/m with a=16. 564 (3), b=15. 839(3), c=11. 792(4) , β=122. 27(1)°, V=2616(1), Z=4, Dc=1.833 g/cm3,F(000) =1436, μ (MoKa) = 35. 75 cm-1, R =0.043 for 2436 observed reflectionswithI>2σ(I).
