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1.
Two new cobalt(II) supramolecular complexes [Co(4,4'-bipy)2(H2O)4]·[Co2(4,4'-bipy)3(H2O)8]·2TST·2(4,4'-bipy)·4H2O 1 and [Co(4,4'-bipy)2(H2O)4]DSNT·4,4'-bipy 2 based upon the assembly of Co(II), 4,4'-bipyridine (4,4'-bipy) and two new multifunctional organic ligands, 2,4,6-tris(4-sulfophenyl- amino)-1,3,5-triazine (H3TST) and 2,4-bis(p-sulfanilato)-6-diethylamino-1,3,5-triazine (H2DSNT), have been prepared by hydrothermal method and characterized by elemental analysis, IR spectrum, and single-crystal X-ray diffraction. The crystal structure of 1 is of monoclinic, space group P21/n with a = 13.599(4), b = 18.988(6), c = 22.995(7) A, β = 90.273(6)°, V = 5938(3)A^3, Z = 4, C56H59Co1.5N13O17S3, Mr = 1370.74, Dc = 1.533 g/cm^3, μ = 0.613 mm^-1, F(000) = 2842, GOOF = 1.018, the final R = 0.0796 and wR = 0.1498 for 9019 observed reflections with I 〉 2σ(I). The crystal structure of 2 belongs to the monoclinic system, space group C2/c with a = 18.864(6), b = 14.283(5), c = 20.246(7)A, β = 107.799(6)°, V = 5194(3)A^3, Z = 4, C49H52CoN12O10S2, Mr = 1092.08, Dc = 1.397 g/cm^3, μ = 0.480 mm^-1, F(000) = 2276, GOOF = 1.059, the final R = 0.0665 and wR = 0.1900 for 4887 observed reflections with I 〉 2σ(I). The results of X-ray crystal structure analysis revealed that complexes 1 and 2 exhibit layered supramolecular frameworks stabilized by electrostatic interactions, π-π interactions and hydrogen bonds.  相似文献   

2.
A binicotinic biscarbohydrazone compound,2,2'-bipyridyl-3,3'-bis(N,N'-disali- cylidene)-formyhydrazone,1 has been prepared and characterized by elemental analysis,FT-IR,1H- NMR,ESI-MS and single-crystal X-ray diffraction analysis. The crystal belongs to triclinic,space group P1 with a = 9.419(3),b = 11.745(4),c = 12.035(5)A,V = 1178.8(7)A^3,Z = 2,Dc = 1.354 g/cm^3,μ = 0.095 mm^-1,F(000) = 500,λ(MoKα) = 0.71073 ,C26H20N6O4,Mr = 480.48,the final R = 0.0480 and wR = 0.1084 for 3634 observed reflections with I 〉 2σ(I). Single-crystal X-ray diffraction analysis reveals that a 1D supramolecular structure of 1 has been constructed by multiply intermolecular N–H···N and O–H···O H-bonding interactions. Besides,compound 1 exhibits a strong green-light emission in the solid state at room temperature.  相似文献   

3.
A novel compound of chiral spiro{1-bromo-4-hydroxy-5-N-cyclohexyl-butyro-lactam-6-oxo-dirings[3.1.0]hexane-2,3'-(4'-diphenylcarbinol-5'-menthyloxy-butyrolatone)} was synthesized via tandem nucleophilic substitution reaction under mild conditions, and its structure was determined by IR, ^1H NMR, elemental analysis and X-ray diffraction. The crystal structure of this compound is of monoclinic system, space group P21 with a = 9.7356(9), b = 12.2760(12), c = 14.9577(14) A, β = 101.0300(10)°, Mr = 680.66, Z = 2, V = 1754.6(3) A^3, Dc = 1.288 g/cm^3, p(MoKα) = 1.216 mm^-1, F(000) = 716, the final R = 0.0434 and wR = 0.0996.  相似文献   

4.
The title compound 3,3'-(2,2'-(ethane-1,2-diylbis(oxy))bis(ethane-2,1-diyl))bis(2- (4-chlorophenylamino)quinazolin-4(3H)-one) 3 (C34H30CI2N604, Mr = 657.54) has been synthesized and its crystal structure was determined by single-crystal X-ray diffraction analysis. It crystallizes in space group P1 with a = 9.9185(8), b = 10.6124(9), c = 15.4064(13) A, α = 92.896(2),β = 103.813(2), γ= 94.635(2)°, V= 1565.5(2) A3, Z = 2, Dc = 1.395 g/cm^3,μ = 0.257 mm^-1, F(000) = 684, the final R = 0.0580 and wR = 0.1284 for 3400 observed reflections (I〉 2σ(I). It remains triclinic in the crystal. Intra- and intermolecular N(3)-H(3A)…O(2), N(6)-H(6A)…O(3) and C(19)-H(19A)…O(4) #1 (#1: 1-x, 1-y, -z) hydrogen bonds are observed in the title compound. A two-dimensional chain network is formed from the dimmers and intermolecular π-π interactions in the crystal structure. This open network has solvent-accessible voids (10A3).  相似文献   

5.
The compound, N-(pyrimidin-2-yl)-N'-methoxycarbonyl-thiourea, has been synthesized. The single crystal structure has been determined by an X-ray diffractometer. The crystal belongs to triclinic with space group P-1 and a=0.72152(4) nm, b=0.8056(4) nm, c=0.90772(5) nm, α= 105.141(4)°, β=94.588(4)°, γ= 115.415(4)°, F(000)= 220, the unit cell volume V=0.45704(4) nm^3, the molecule number in one unit cell Z=2, the absorption coefficient μ=0.333 mm^-1, the calculated density Dc= 1.542 g/cm^3. The theoretical investigation of the title compound was carried out with B3LYP/6-311G, HF/6-311G and MP2/6-311G methods, and the atomic charges and natural bond orbital analysis were also discussed.  相似文献   

6.
The reaction of 2,6-diformyl-4-methylphenol, ethylenediamine and Cu(Ⅱ) in the proportion of 3:2:2 yields a new tetranuclear copper(Ⅱ) complex, [Cu2L]2(ClO4)2.2H2O(H3L= N,N'-bis(4-(3'-formyl-5'-methylsalicyclidene)iminoethyl)-4-methyl-2,6-bimethyliminophenol). The complex has been characterized by ES-MS, IR and X-ray diffraction analysis, and its crystal crystallizes in the triclinic system, space group P1 with a = 10.8673(11), b = 12.0829(12), c = 14.4834(15) А, α= 111.946(2), β= 105.828(2), γ = 99.583(2)°,V= 1618.5(3) А^3, Dc = 1.605 g/cm^3, Z = 2, Mr = 1564.26, F(000) = 800.0,μ(MoKa) = 1.460/mm, S = 1.063, R = 0.0612 and wR = 0.1163 for 6245 observed reflections (I 〉 2σ(I)). The complex is a dimer of dinuclear copper(Ⅱ) acylic enantiomorph subunit [Cu2L]ClO4.H_2O, held together by π…π weak coordination and hydrogen bonding interactions. In addition, the π…π interactions related to phenyl moieties as well as CH=N…π interactions were also found to stabilize the supramolecular architectures in the solid state.  相似文献   

7.
A new copper(II) complex Cu2(L)a(2,2'-bipy)2(H2O)2 (1) has been synthesized with 2-benzoylbenzoic acid (HL) and 2,2'-bipyridin as ligands. The crystal belongs to a monoclinic system with space group Cc, a = 13.9979(II), b = 15.9888(13), c = 30.306(3) A, β = 100.8700(10)°, V= 6661.1(10) A3, Dc= 1.372 g/cm3, Z = 8, F(000) = 2840, the final GOOF = 1.018, R= 0.0685, and wR= 0.1731. There are two mononuclear Cu(L)2(2,2'-bipy)(H20) units in the crystal of 1. Each Cu(II) cation is coordinated by five atoms. The magnetic and fluorescent properties of 1 were studied. The results show that 1 exhibits weak paramagnetism, and when the excitation wavelength is at 616 nm, it has an intense fluorescent emission band around 482 nm.  相似文献   

8.
The title compound [Co(5-NH2-bdc)(4,4'-dpdo)(H2O)]n 1 (5-NH2-bdc = 5-aminoiso- phthalic acid,4,4'-dpdo = 4,4'-bipyridrl-N,N'-dioxide) crystallizes in triclinic,space group P1 with a = 4.999(1),b = 10.072(2),c = 13.028(3) A,α = 107.72(3),β = 92.58(3),γ = 98.11(3)°,V = 615.9(3) A^3,F(000) = 356,Rint = 0.0186,Z = 2,R = 0.0333,wR = 0.0721,S = 1.032 and (Δ/σ)max = 0.001. In the molecule of 1,the Co(II) cation is coordinated by three O-atoms of two 5-NH2-bdc ligands,one N-atom of another 5-NH2-bdc ligand,one O-atom of 4,4'-dpdo and one terminal O-atom of water molecule. The molecules construct a 2-D network through bridging 5-NH2-bdc and 4,4'-dpdo ligands,and further form a 3-D network through N–H and O–H hydrogen bonds. The network topology of 1 can be simplified as a rare 2D (3,6)-connected (426381) net.  相似文献   

9.
The title compound (Z)-1-(3-fluorobenzyl)-5-((3-fluorobenzylimino)(2-hydroxy-4- methoxyphenyl)methyl)pyridin-2(1H)-one (C27H22F2N2O3,Mr = 460.47) was synthesized and crystallized. The crystal belongs to the triclinic system,space group P1 with a = 9.951(6),b = 10.059(6),c = 12.927(7)A,α = 109.828(7),β = 102.304(7),γ = 104.898(7)°,Z = 2,V = 1110.2(11)A^3,Dc =1.377 Mg/m^3,μ(MoKα) = 0.102 mm^-1,F(000) = 480,the final R = 0.0449 and Rw = 0.1250 for 4595 observed reflections (I 〉 2σ(I)). X-ray analysis reveals that both m-fluorobenzyl groups are diorientationally disordered because of the rotation of C–C single bond which was represented as F(1),F(2) and F(1'),F(2'). The diorientational disorder was refined and gave the occupancies of 0.665(4) and 0.335(4) for F(1) and F(1'),0.631(3) and 0.369(3) for F(2) and F(2'). Hydrogen bonds existing in the cell link different components to stabilize the crystal structure. The active data proved that the title compound has good anti-HBV activity.  相似文献   

10.
A one-dimensional chain coordination polymer [Co(Ⅱ)(C6H5CH--CHCOOH)2(4,4'- bipy)(H20)5]n has been synthesized with cinnamylic acid, 4,4'-bipy and cobaltous chloride as raw materials. Crystal data for this complex: monoclinic, space group P21/c, a = 1.1481(3), b = 1.1230(2), c = 1.1759(3) nm, β = 97.054(4)^o, V= 1.5046(6) nm^3, Mr= 617.50, Dc = 1.363 g/cm^3, Z = 2, ,u(MoKa) = 0.627 mm^-1, F(000) = 646, S = 1.062, R 0.0443 and wR = 0.1178. The crystal structure shows that two neighboring cobalt(ID ions are linked together by one 4,4'-bipy, and the whole complex molecule adopts a one-dimensional chain structure. Each cobalt(H) ion is coordinated with two nitrogen atoms from two 4,4'-bipy molecules and four oxygen atoms from four water molecules, giving a distorted octahedral coordination geometry. The electrochemical properties were analyzed by combining with the crystal structure.  相似文献   

11.
Compounds [Zn(2,2'-bipy)(L)Cl]2 1 and [Zn(phen)(L2)]2 2 (2,2'-bipy = 2,2'-bipyridine, HL = 3-methylbenzoic acid, phen = 1,10-phenanthroline) have been synthesized under hydrothermal conditions. 1: monoclinic, space group C2/c, a = 20.240(4), b = 9.2960(19), c = 17.904(4)A, β = 92.63(3)°, V = 3365.1(12) A^3, C36H30Cl2N4O4Zn2, Mr = 784.32, Z = 4, Dc = 1.548 g/cm^3, μ = 1.631 mm^-1, F(000) = 1600, the final R = 0.0367 and wR = 0.1289 for 3867 observed reflections (I 〉 2σ(I)). 2: monoclinic, space group C2/c, a = 23.035(5), b = 9.0395(18), c = 23.799(5) A, β = 98.55(3)°, V = 4900.6(17)A^3, C56H44N4O8Zn2, Mr = 1031.73, Z = 4, Dc = 1.398 g/cm^3, μ = 1.039 mm^-1, F(000) = 2128, the final R = 0.0540 and wR = 0.1287 for 5002 observed reflections (I 〉 2σ(I)). The two compounds have the same space group and similar isolated dinuclear structure, but different space packing structures are formed by different weak intermolecular interactions. Mo- reover, IR and luminescence spectra are also employed to study the crystal structures and pro- perties of these two compounds.  相似文献   

12.
A manganese(Ⅱ) complex (tataH)2[Mn(pydc)2]·4H2O (C20H28MBN14O12, Mr = 711.50, tata = 2,4,6-triamino-1,3,5-triazine, pydcH2 = pyridine-2,6-dicarboxylic acid) has been synthesized and its crystal structure was determined by single-crystal X-ray diffraction. The crystal belongs to the triclinic system, space group P1^-, with a = 9.9847(3), b = 10.9813(3), c = 15.2616(5)A, a = 101.5310(10), β = 90.2610(10), γ = 116.4600( 10)% V = 1459.44(8)A^3, Z = 2, Dc = 1.619 g/cm^3,μ = 0.539 mm^-1, F(000) = 734, the final R = 0.0292 and wR = 0.0745. In the crystal the Mnn atom is six-coordinated by four carbonyl oxygen atoms and two pyridine nitrogen atoms from two tridentate pydc ligands to furnish a distorted octahedral geometry. The complex shows the A…D…D'…A' H-bonded tetramer. The molecules are packed in a three-dimensional framework structure by the combination of O-H…O, N-H…O and N-H…N hydrogen bonds between (tataH)^+, [Mn(pydc)2]^2- and crystal water.  相似文献   

13.
A new nickel(II) complex [NiL2](DMF)4 (HL = 2'-[4-N,N'-(dimethylamino- benzylidene)]-3,5-dihydroxybenzoylhydrazide) has been synthesized and its structure was characterized by IR,UV-Vis,1H NMR and elemental analysis. The fluorescence emission mechanism of the complex was discussed by fluorimetric spectra. The single-crystal structure was determined by X-ray diffraction analysis. The crystal belongs to the triclinic system,space group P1 with a = 0.9918(4),b = 1.1297(4),c = 1.1331(4) nm,α = 76.860(7),β = 75.105(6),γ = 89.022(7)°,V = 1.1936(8) nm^3,Z = 1,μ = 0.472 mm^-1,Dc = 1.319 g/cm^3,F(000) = 502 and Rint = 0.0913. In the title compound,the nickel(II) atom is four-coordinated with two nitrogen atoms from amide and two oxygen atoms from keto group. The complex is centrosymmetric with nickel located at the center.  相似文献   

14.
The new title compound N-(5-(4-chloro-2-(trifluoromethyl)phenyl)furan-2-carbon-yl)- N'-(4,6-dimethylpyrimidin-2-yl)thiourea (C19H14C1F3N4O2S) has been synthesized, and its crystal structure and biological behaviors were studied. The title compound crystallizes in the monoclinic system, space group P21/c with a = 7.932(5), b = 33.46(2), c = 7.556(5) A, β = 98.058(9)°, V = 1986(2) A^3 Mr = 454.85, Z = 4, Dc = 1.521 g/cm^3, μ = 0.349 mm^-1 and F(000) = 928. The structure was solved by direct methods and refined to R = 0.0724 and wR= 0.1429 for 3494 observed reflections (I 〉 2σ(I)). Intermolecular hydrogen bonds along the b axis together with the continuous π-π interactions construct the three-dimensional architecture of the title compound. The preliminary biological tests show definite herbicidalactivity for the title compound.  相似文献   

15.
The title compound, N,N'-bis-[3-chloro-5-S-(l-menthyloxy)-2(5H)-4-furanon-yl]- propane-l,3-diamine (C31H48Cl2N2O6, Mr = 615.61), has been synthesized and characterized by IR, 1H NMR, MS, elemental analysis and single-crystal X-ray diffraction. The crystal crystallizes in the monoclinic system, space group C2 with a = 16.1091(4), b = 11.1880(3), c = 19.2854(5) A, β = 106.297(2)°, V = 3336.12(15) A3, Z = 4, Dc = 1.226 mg/m3,μ = 0.237 mm^-1, F(000) = 1320, the final R = 0.0531 and wR = 0.0700 for 2760 observed reflections (I 〉 2σ(I)). X-ray analysis reveals that the title compound possesses four rings: two chiral five-membered furanone rings and two six-membered cyclohexane rings with chair conformation, containing eight chiral centers: C2(S), C3(R), C5(R), C10(S), C18(S), C21(R), C22(S) and C25(R). The structure is stabilized by N-H…O hydrogen bonding interaction.  相似文献   

16.
Three new inorganic-organic composite polyoxotungstates [Cu(2,2'-bpy)2]5[α-PW11.5Cu0.5O40]·2H2O 1, [Co(2,2'-bpy)2(N3)2]4H3[α-PW12O40]·3H2O 2 and [Cu(2,2'-bpy)2(4,4'-bpy)]2[α-GeW12O40]-4H2O 3 (2,2'-bpy = 2,2'-bipyridine, 4,4'-bpy = 4,4'-bipyridine) have been hydrothermally synthesized and structurally characterized. 1 crystallizes in the orthorhombic space group Pna21 with a = 27.847(3), b = 21.597(2), c = 20.1179(19)A, V= 12099(2)A^3, Z= 4, GOF= 1.038, R = 0.0427 and wR = 0.1035; 2 belongs to the triclinic space group P1^- with a = 12.31150(10), b = 16.1954(4), c = 19.36290(10)A, α = 99.366(11), β =105.168(8), γ = 111.836(8)°, V = 3309.98(9)A3, Z = l, GOF = 1.024, R = 0.0739 and wR = 0.2216; and 3 crystallizes in the monoclinic space group P21/n with a = 12.858(4), b = 20.943(6), c = 15.598(5)A, β = 102.338(5)°, V= 4103(2)A3, Z = 2, GOF = 1.026, R = 0.0557 and wR = 0.1316. The common structural features of 1-3 are that their molecular structures all consist of a saturated a-Keggin polyoxoanion and several discrete metal-organic moieties. Intriguingly, 2 and 3 are composed of metal-organic coordination moieties with two mixed ligands.  相似文献   

17.
A POMs-based 3D zeolike ionic crystal 1, {[Co(dpdo)2(CH3CN)(H2O)2]2(SiMo12O40)- (HEO)2}n (dpdo = 4,4'-bipyridine-N,N'-dioxide), was constructed via self-assembly by embedding Keggintype [SiMo12O40]^4- polyanions within the intercrystalline voids as pillars and structurally characterized. The crystal structure was determined by single-crystal X-ray diffraction. The crystal is of triclinic, space group P1 with a = 11.430(3), b = 12.242(3), c = 14.279(3)A, α = 106.196(4),β = 94.316(4), γ = 98.294(3)°, V = 1884.5(7)A^3 Z = 1, C44H50N10O54CoEMo12Si, Mr = 2880.17, Dc = 2.538 g/cm^3, p = 2.484 mm^-1,F(000) = 1388, the final R = 0.0383 and wR = 0.1096 for 7753 observed reflections with I 〉 2σ(I). Flack factor is 0.22(3). Compound 1 is a pillar-layered framework with the [SiMo12O40]^4- anions linearly located on the square voids between the 2D bilayers which are formed by the dpdo ligands and cobalt(II) ions.  相似文献   

18.
Homobinuclear complex (HCuL)2 (1) (H3L: N-3-carboxylsalicylidene-N'-salicylaldehyde-1,2-diaminoethane) was obtained from self-organization of the reported complex HCuL, and its crystal structure was determined through X-ray diffraction at room temperature. The crystal of complex 1 belongs to monolinic system, the space group Cc, a=2.5326(5) nm, b=0.88861(18) nm, c=1.3738(3) nm, β=96.95(3)°, Z=4, R1=0.0520, wR2=0.1185. (HCuL)2 is a dimeric molecule and has extended phenolic oxygen-bridged structure. In addition, using mononuclear complex HCuL as building blocks, Cu(Ⅱ)-Mg(Ⅱ)-Cu(Ⅱ) heterotrinuclear complex 2 was synthesized, and its crystal structure also has been determined by X-ray analysis. The crystal of complex 2 is of monoclinic system, space group Pc, a=1.1816(2) nm, b=1.5599(3) nm, c=1.9642 (4) nm, β=98.22°, Z=2, R1=0.0701, wR2=0.1498. Each dissymmetricai cell unit of complex 2 contains two heterotrinucler neutral molecules: {[CuL(H2O)]Mg[CuL(CH3OH)]} and {[CuL]Mg[CuL(H2O)]}.  相似文献   

19.
The 1-D chain coordination complex of {[Mn2(HCAM)3(H2bipy)]·5H2O}n (H3CAM = 4-hydroxypyridine-2,6-dicarboxylic acid, bipy = 4,4'-bipyridine) has been synthesized by the reaction of 4-hydroxypyridine-2,6-dicarboxylic acid, 4,4'-bipyridine and manganese carbonate under hydrothermal conditions, and its crystal structure was determined by X-ray diffraction method The crystal belongs to the monoclinic system, space group P21/n with a = 10.110(2), b = 20.159(4), c = 17.861(4)A,β = 99.67(3)°, V = 3.5884(12) nm3, Mr= 901.47, Z = 4, Dc= 1.669 g.cm^-3, μ= 0.798 mm^-1, F(000) = 1840, the final R = 0.0713 and ωR = 0.1853. The complex forms a 1-D chain bridged by HCAM, protonated 4,4-bipyridines link the 1-D chains to construct 2-D networks via N-H...O hydrogen bonds, and networks are further extended via π-π stacking and hydrogen bonds into 3-D supramolecular framework.  相似文献   

20.
The title compound N,N'-bis(5,5-dimethyl-2-phospha-2-thio-1,3-dioxan-2-yl) ethylene diamine (DPTDEDA, C12H26N2O4P2S2) was synthesized by the reaction of neopentyl glycol, phosphorus thio-chloride and 1,2-ethylenediamine, and characterized by elemental analysis, IR and ^1H NMR spectra. Its crystal structure was determined by single-crystal X-ray diffraction analysis and the thermal property was analyzed by TG analysis. The crystal structure belongs to monoclinic, space group P21/c, with a = 14.557(16), b = 11.299(12), c = 12.163(13)A,β = 98.707(19)^o, Dc = 1.305 g/cm^3, Z = 4, γ = 0.71073A,μ(MoKa) = 0.447 mm^-1, Mr = 388.41, V = 1977(4)A3, F(000) = 824, S = 1.107, the final R = 0.0478 and wR = 0.0810 for 1738 observed reflections (I 〉 2σ(I)). X-ray analysis reveals that the crystal structure is centrosymmetrically distributed through 1,2-ethylenediamine to join two distorted six-membered rings. The weak N-H…S interactions are observed and link the molecules into sheets. TG analysis shows that the title compound has good thermal stability and char-forming capability, which are required for an excellent intumescent fire retardant.  相似文献   

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