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1.
1 INTRODUCTION Polyaza-macrocyclic compounds with functional substituents have been extensively investigated recen- tly because of their potential applications in radioac- tive therapy, recovery of metal ions, biomimetic che- mistry, and catalysis[1, 2]. With various structures and distinctive properties, they have become significant building blocks for further chemical studies[3~6]. As far as the preparation method is concerned, metal template condensation reactions are shown to be effec…  相似文献   

2.
Two new polyoxomolybdate compounds,namely CuII2(HL)3]2[Mo8O26]·(H2O)4(1) and [NiII(HL)3]2(Mo8O26)·(H2O)3(2)(HL = 3-(2-pyridyl)pyrazole),were designed and synthesized under hydrothermal conditions.X-ray diffraction analyses reveal that compound 1 consists of one β-Mo8O264-cluster and a Cu2 dimer which is built from two Cu(II) ions linked by three 3-(2-pyridyl)pyrazole ligands.Compound 2 is generated by two kinds of polyoxomolybdate clusters of α-[Mo8O26]4-and β-[Mo8O26]4-.In complexes 1 and 2,the multi-dimensional frameworks are con-structed with the help of hydrogen-bonding links between the terminaloxygen atoms of [Mo8O26]4-,water molecules,and 3-(2-pyridyl)pyrazole ligands.Crystal data of 1:C24H25Cu2Mo4N9O15,Mr = 1190.37,monoclinic,space group P21/c,a = 10.850(2),b = 18.510(4),c = 17.230(3) ,β = 100.57(3)°,V = 3401.6(12) 3,Z = 4,Dc = 2.324 g/cm3,F(000) = 2312,μ = 2.742 mm-1,R = 0.0302 and wR = 0.0775(Ⅰ 2σ(Ⅰ));Crystal data for 2:C48H48Mo8N18Ni2O29,Mr = 2225.98,monoclinic,space group P21/n,a = 20.799(2),b = 14.7970(13),c = 23.141(2) ,β = 91.6180(10)°,V = 7119.0(11) 3,Z = 4,Dc = 2.077 g/cm3,F(000) = 4344,μ = 1.968 mm-1,R = 0.0309 and wR = 0.0696(Ⅰ 2σ(Ⅰ)).  相似文献   

3.
Four cobalt supramolecular architectures with Hmtyaa(2-(5-methyl-1,3,4-thiadiazol-2-ylthio)acetic acid) ligand have been synthesized.[Co(mtyaa)2(H2O)4]·4(H2O)(1):triclinic,space group P1 with a = 6.7537(18),b = 8.591(2),c = 10.615(3) ,α = 96.495(4),β = 99.955(5),γ = 103.615(5)°,V = 581.9(3) 3,Z = 1,Mr = 581.52,Dc = 1.659 g/m3,μ = 1.158 mm-1,F(000) = 301,Rint = 0.0557,R = 0.0377 and wR = 0.1056 for 1854 observed reflections with Ⅰ 2σ(Ⅰ);{[Co(4,4'-bipy)(H2O)4]·2(mtyaa)·2(H2O)}n(2):triclinic,space group P1 with a = 7.669(2),b = 8.840(3),c = 11.521(4) ,α = 79.912(5),β = 73.954(5),γ = 86.612(6)°,V = 738.9(4) 3,Z = 1,Mr = 701.67,Dc = 1.577 g/m3,μ = 0.924 mm-1,F(000) = 363,Rint = 0.0636,R = 0.0498 and wR = 0.1311 for 2155 observed reflections with Ⅰ 2σ(Ⅰ);{[Co(4,4'-bipy)(mtyaa)(H2O)3](mtyaa)·2(H2O)}(3):monoclinic,space group Pc with a = 7.7832(17),b = 11.527(3),c = 31.483(7) ,β = 91.952(4)°,V = 2822.9(11) 3,Z = 4,Mr = 683.65,Dc = 1.609 g/m3,μ = 0.963 mm-1,F(000) = 1412,Rint = 0.0758,R = 0.0609 and wR = 0.1095 for 5841 observed reflections with I 2σ(I);{[Co(bpe)(mtyaa)2(H2O)2]}n(4):monoclinic,space group C2/c with a = 19.290(11),b = 12.027(7),c = 14.865(8) ,β = 125.648(8)°,V = 2802(3)3,Z = 4,Mr = 657.66,Dc = 1.559 g/m3,μ = 0.959 mm-1,F(000) = 1356,Rint = 0.0456,R = 0.0332 and wR = 0.0985 for 2299 observed reflections with Ⅰ 2σ(Ⅰ).  相似文献   

4.
<正>Two new isomeric Au complexes,Au(PPh_3)(bmt),have been synthesized via the reaction of Au(PPh_3)Cl with 2-benzimidazolethiol(Hbmt)in dichloromethane(CH_2Cl_2)solution. Their crystal structures were determined by elemental analysis and single-crystal X-ray diffraction studies.Complex 1 crystallizes in the monoclinic system,space group C2/c with a=19.589(2),b= 21.1368(15),c=23.424(2)(?),β=108.346(4)°,V=9206.1(14)(?)~3,M_r=1216.85,D_c=1.756 g/cm~3,μ=6.566 mm~(-1),F(000)=4704,Z=8,the final R=0.0563 and wR=0.1028 for 8125 reflections with I2σ(I).Complex 2 crystallizes in the monoclinic system,space group P2_l/n with a= 9.627(3),b=21.384(8),c=22.308(8)(?),P=92.068(6)°,V=4590(3)(?)~3,M_r=1216.85,D_c=1.761 g/cm~3,μ=6.585 mm~(-1),F(000)=2352,Z=4,the final R=0.0500 and wR=0.0883 for 10477 reflections with I2σ(I).X-ray diffraction studies reveal that complexes 1 and 2 both feature a 1D chain along the a axis.  相似文献   

5.
温德才  刘世雄 《结构化学》2007,26(11):1281-1286
Two complexes,Cu(HnicO)2 1 and Ni(HnicO)2(H2O)2 2 (H2nicO=2-hydroxy-nicolinic acid),were synthesized by hydrothermal reactions and structurally characterized. Complex 1 crystallizes in monoclinic,space group P21/n,with a=8.314(7),b=6.275(4),c=11.283(7),β =98.32(3)°,V=582.5(7)3,Z=2,Mr=339.74,Dc=1.937 g/cm3,F(000)=342,μ=1.908 mm-1,S =1.097,the final R=0.0284 and wR=0.0781 for 1177 observed reflections with I > 2σ(I). Complex 2 crystallizes in monoclinic,space group P21/c,with a=7.438(5),b=12.22(1),c=7.537(5),β=100.07(3)°,V=674.3(8)3,Z=2,Mr=370.95,Dc=1.827 g/cm3,F(000)=380,μ =1.487 mm-1,S=1.041,the final R=0.0335 and wR=0.0779 for 1202 observed reflections with I > 2σ(I). There are extended 3D framework structures in complexes 1 and 2 due to the N–H…O and C–H…O hydrogen bonds. The copper atom in 1 has square planar coordination,while the nickel atom in 2 adopts octahedral coordination geometry. The TG curve shows that complex 2 is stable in solid state to 150 ℃.  相似文献   

6.
Three ZnⅡ coordination polymers, [Zn(py)(H2O)(dpa)]n 1, [Zn2(4,4'-bipy)2(dpa)2]n 2 and [Zn(bpe)(H2O)2(Hdpa)2]n 3 (py = pyridine, H2dpa = diphenic acid, 4,4'-bipy = 4,4'-bipyridine,bpe = 1,2-bis(4-pyridyl)ethane), were synthesized and characterized by X-ray single-crystal structure determination. 1 crystallizes in monoclinic, space group C2/c with a = 23.014(3), b = 8.7184(13), c = 18.091(3) (A), β = 95.964(3)°, V = 3610.2(9) (A)3, Z = 8, C19H15NO5Zn, Mr = 402.69,Dc= 1.482 g/cm3, F(000) = 1648, μ(MoKα) = 1.389 mm-1, the final R = 0.0431 and wR = 0.1120 for 4239 observed reflections with I > 2σ(Ⅰ). 2 crystallizes in orthorhombic, space group Fddd with a = 23.1613(5), b = 24.0324(6), c = 29.4785(1) (A), V= 16408.4(5) (A)3, Z = 32, C24H16N2O4Zn, Mr = 461.76, Dc= 1.495 g/cm3, F(000) = 7552, μ(MoKα) = 1.232 mm-1, the final R = 0.0542 and wR = 0.1724 for 3632 observed reflections with I > 2σ(Ⅰ). 3 crystallizes in orthorhombic, space group C2/c with a = 19.142(4), b = 13.862(3), c = 15.625(3) (A), β = 122.404(3)°, V = 3500.3(11) (A)3, Z = 8,C20H17NO5Zn0.50, Mr = 384.03, Dc= 1.457 g/cm3, F(000) = 1592,μ(MoKα) = 0.766 mm-1, the final R = 0.0400 and wR = 0.1210 for 4024 observed reflections with I > 2σ(Ⅰ).  相似文献   

7.
A Ni(Ⅱ) complex [Ni(bdpm)2(OAc)]2(N3)2·5H2O (bdpm = bis(3,5-dimethylpyrazol-1-yl)-methane) was synthesized and characterized by elemental analysis, IR and single-crystal X-ray diffraction. It crystallizes in the monoclinic system, space group P21/c with a = 18.630(2), b =16.6624(19), c = 19.821(2) (A), β = 90.146(2)°, V = 6152.9(12) (A)3, Z = 4, C48H8oN22Ni2O9, Mr =1226.76, Dc = 1.324 g/cm3, F(000) = 2600 andμ = 0.680 mm-1. The structure was refined to the final R = 0.0578 and wR = 0.1337 for 10848 independent reflections (Rint = 0.0311) and 6915 observed reflections (I > 2σ(Ⅰ)). The complex contains two asymmetric molecules in the cell with small difference in bond distances and bond angles. Each Ni(Ⅱ) ion is bound by four nitrogen atoms of two chelating bdpm groups in a six-membered boat conformation and two oxygen atoms from one chelating bidentate acetate group to form a distorted octahedral geometry. The complex also contains azide anion outside acting as counteranion and two crystalline water molecules to link two discrete mononuclear cations though hydrogen bonds.  相似文献   

8.
The mononuclear copper(Ⅱ) complex [Cu(L)(2-AP)] 1 and binuclear copper(Ⅱ)complex [Cu(L)(py)]2 2 (L = C1oH1 1O5NS, taurine o-vanillin, py = prydine, 2-AP = 2-aminopyridine)with mixed ligand have been synthesized and characterized by X-ray diffraction method. Crystal data for 1: orthorhombic, space group Pbca with a = 11.921(4), b = 15.816(6), c = 17.076(6) (A), V=3219.7(19) (A)3, C15H17CuN3O5S, Z = 8, Mr = 414.92, Dc = 1.712 g/cm3,μ(MoKα) = 1.520 mm-1,F(000) = 1704, the final R = 0.0300 and wR = 0.0705 for 2840 observed reflections with I > 2σ(I);and crystal data for 2: monoclinic, space group P21/c with a = 7.929(3), b = 17.038(5), c = 11.734(4)(A), β = 98.162(6)°, V = 1569.1 (9) (A)3, C15H16CuN2O5S, Z = 4, Mr = 399.90, Dc = 1.693 g/cm3, F(000)= 820,μ(MoKα) = 1.554 mm-1, the final R = 0.0351 and wR = 0.0848 for 2767 observed reflections (I > 2o(I)). The molecular structure of complex 1 consists of one tetra-coordinated Cu(Ⅱ) atom generating a slightly distorted square plane, and a one-dimensional chain structure is formed by intermolecular hydrogen bonds. Complex 2 consists of a diphenolic hydroxyl O-bridged binuclear copper(Ⅱ) structure. The crystal structures of complexes 1 and 2 reveal that the coordinate copper centers are bound to both nitrogen and oxygen atom donors. The usual N,O-trans arrangement of ligands is observed in both cases.  相似文献   

9.
The title compound [Cu(C11H29N5)](ClO4)2 was synthesized and characterized by elemental analysis,IR and X-ray single-crystal diffraction.The compound crystallizes in the monoclinic system,space group P21/n with a = 9.405(2),b = 14.495(3),c = 14.715(3)(A),β = 90.262(3)°,V =2006.1(7)(A)3,Mr = 493.83,Z= 4,F(000) = 1028,Dc= 1.635 g/cm3,T= 298(2) K,μ = 1.403 mm-1 and λ = 0.71073(A).The structure was refined to R = 0.0508 and wR = 0.1250 for 2293 observed reflections with I > 2σ(I).The Cu(Ⅱ)atom possesses a five-coordinate CuN5 environment which shows a slightly distorted square-pyramidal geometry.Antimicrobial activity study found that the complex is active against Salmonella species,Staphylococcus aureu,Bacillus pumilus and Bacillus coliforms.  相似文献   

10.
1 INTRODUCTION In recent years, the researches on tin sulfide ma- terials have drawn increasing attention of chemists owning to their potential applications as photo-vol- taic materials, holographic recording system[1, 2], so- lar control devices[3] and semiconductor materials. In the last decades, many finite adducts of tin (IV) thio- lates with organic amine ligands have been synthe- sized by self-assembly, such as cis-Sn(SPh)4(2,2?-bi- py)[4], cis-Sn(edt)2(ethyldimiane)[5], trans-Sn(…  相似文献   

11.
Three novel metal-organic complexes with formulas [Ni(C9N2O2H7)2(CH3OH)2](1),[Zn(C9N2O2H7)2(H2O)2](2) and [Cd(C9N2O2H7)2(CH3OH)2](3) were synthesized by the reactions of Ni,Zn and Cd salts with ethyl 2-benzimidazolylacetate under hydrothermal conditions or layering technique,and characterized by single-crystal X-ray diffraction analysis,IR spec-troscopy,solid-state luminescent properties and thermogravimetric(TG) analysis.The crystal data for these three complexes are as follows:for 1,monoclinic,space group P21/c,a = 9.384(3),b = 9.634(3),c = 11.292(3) ,β = 95.787(5)°,V = 1015.7(5) 3,Z = 2,F(000) = 492,Dc = 1.547 Kg/m3,μ = 1.002 mm-1,the final R = 0.0451 and wR = 0.0900 for 1833 observed reflections with Ⅰ 2σ(Ⅰ);for 2,orthorhombic,space group Pbca,a = 10.031(4),b = 10.379(4),c = 17.525(7),V = 1824.6(12) 3,Z = 4,F(000) = 928,Dc = 1.645 Kg/m3,μ = 1.392 mm-1,the final R = 0.0452 and wR = 0.0996 for 1661 observed reflections with Ⅰ 2σ(Ⅰ);for 3,monoclinic,space group P21/c,a = 9.9114(13),b =10.4852(15),c = 10.4120(14) ,β = 108.453(5)°,V = 1026.4(2) 3,Z = 2,F(000) = 532,Dc = 1.705 Kg/m3,μ = 1.110 mm-1,the final R = 0.0322 and wR = 0.0805 for 1822 observed reflections with Ⅰ 2σ(Ⅰ).In the three complexes,the ethyl 2-benzimidazolylacetate shows the same chelating mode,and the adjacent units are interlinked into a two-dimensional layer through hydrogen-bonds(O-H···O,N-H···O).  相似文献   

12.
1 INTRODUCTION The design of metal complexes of bipyridine is one of the most highlighting topics in molecular materials with specific optical, electronic and mag- netic properties. What studied and well-documented most widely are those of the d6 metal polypyridines, and so are the d8 and d10 metal complexes with rich luminescence behaviour[1] very recently, which can be beneficial to the design of unique functional ma- terials. Currently our interest is to design lumine- scent heteronuc…  相似文献   

13.
The self-assembly reactions of MIICl2 (M = Ni, Co) with the flexible bix ligand [bix = 1,4-bis(imidazole-1-ylmethyl)benzene] yielded a 2D network [NiII(bix)2Cl2]n 1 and a 1D chain [CoII(bix)Cl2]n 2. Their crystal structures have been determined by X-ray single-crystal diffraction analysis. Complex 1 characters a two-dimensional grid-type structure and crystallizes in monoclinic, space group P21/c with a = 7.7231(7), b = 12.7787(9), c = 13.9374(13) , β = 105.419(4)o, C28H28Cl2N8Ni, Mr = 606.19, Ζ = 2, V = 1326.0(2) 3, Dc = 1.518 g/cm3, μ = 0.969 mm-1, F(000) = 628, R = 0.0429 and wR = 0.0783 for 2503 observed reflections (I > 2σ(I)). Compound 2 is a one-dimensional chain and crystallizes in orthorhombic, space group Pbca with a = 11.3696(6), b = 10.2128(6), c = 14.4943(9) , C14H14Cl2CoN4, Mr = 368.12, Z = 4, V = 1683.01(17) 3, Dc = 1.453 g/cm3, μ = 1.334 mm-1, F(000) = 748, R = 0.0317 and wR = 0.0800 for 1778 observed reflections (I > 2σ(I)). Magnetic properties of the title complexes were also investigated.  相似文献   

14.
A mixed-valent hexanuclear complex [CuⅡCuⅠ2(pbi)2Br2]2 (pbi = (2-(2-pyridyl)-benzimidazole) exhibiting a dimeric unit bridged by two Br atoms was synthesized by hydrothermal reaction.Interestingly, there exist intramolecular and intermolecular π-πstacking interactions as well as metalaromatic ring interactions in the title complex. The crystal belongs to the monoclinic system, space group P-1, with a = 7.1061(9), b = 12.1008(13), c = 14.0711(17) (A), α = 91.742(8), β = 100.155(9), γ =90.486(7)°, V = 1190.3(2)(A)3, Z = 2, C48H32Br4Cu6N12, Mr = 1477.74, Dc= 2.061 g/cm3, F(000) = 718,μ(MoKα) = 6.039 mm-1, the final R = 0.0481 and wR = 0.0974 for 3426 observed reflections (I>2σ(I)).  相似文献   

15.
A new copper(Ⅱ) compound has been prepared and fully characterized by elemen-tal analysis,IR,TG and single-crystal X-ray diffraction.The compound [Cu(4-hba)2(inta)(H2O)]·H2O (4-hba=4-hydroxybenzoic acid,inta=isonicotinamide) 1 crystallizes in the monoclinic system,space group P21/c with a=7.590(5),b=11.027(5),c=23.761(5),β=102.5740(10)o,V=1974.1(16) 3,Mr=991.84,Z=2,Dc=1.669 g/cm3,F(000)=1020,μ=1.166 mm-1,R=0.0353 and wR=0.0604 for 3166 observed reflections (I 2σ(I)).In compound 1,the copper cation is penta-coordinated with two carboxylate oxygen atoms from two different 4-hba ligands,two oxygen atoms from two coordinated water molecules and one nitrogen atom from inta ligand,showing a slightly distorted square-pyramidal geometry.  相似文献   

16.
The coordination polymer {[Co(phth)(phen)(H2O)]·(C2H5OH)}n (phth = phthalate, phen = 1,10-phenanthroline) with formula C22H20CoN2O6 (Mr = 467.33) was synthesized by the solvothermal method under low temperature, and its crystal structure was determined by singlecrystal X-ray diffraction. The complex belongs to monoclinic system, space group P21/n with a =12.7352(16), b = 8.8125(11), c = 18.677(2) (A), β = 102.633(2)°, V = 2045.3(4) (A)3, Z = 4, Dc =1.518 g/cm3,μ = 0.882 mm-1, F(000) = 964, S = 1.053, the final R = 0.0401 and wR = 0.0984 for 3135 observed reflections (I > 2σ(I)). Single-crystal X-ray analysis revealed that the Co(Ⅱ) ion is six-coordinated. The cobalt complex forms a one-dimensional chain structure via phthalate bridging ligand. In the cobalt complex, a 3D network structure is formed by π-π stacking interaction of 1,10-phenanthroline as well as intermolecular hydrogen bonding interactions.  相似文献   

17.
1 INTRODUCTION Optically active oxazolines have been extensi- vely used as valuable chiral ligands for transition metals in asymmetric catalysis[1]. The design and syntheses of new chiral oxazoline ligands have inspired many scientists to work with great efforts during the recent years. Our interest has been focus- ed on the studies of enantioselective transition- metal catalysis of heterocyclic ligands. In the pre- sent work, we choose o-hydroxyphenyloxazoline ligand for it has a rigi…  相似文献   

18.
The title compound [Cd(Hq)2(Hdpa)2] (Hq = 8-hydroxyquinoline, H2dpa = diphenic acid) has been synthesized and characterized by single-crystal X-ray diffraction analysis. It crystallizes in monoclinic, space group C2/c with a = 20.6880(5), b = 14.2584(4), c = 13.4776(4) (A), β = 113.434(2)°, C46H28Cd1N2O10, Mr = 881.10, V = 3647.68(17) (A)3, Z = 4, Dc = 1.604 g/cm3, F(000) = 1784,μ = 0.668 mm-1, the final R = 0.0576 and wR = 0.1157 for 2631 observed reflections with I >2σ(Ⅰ). The centrosymmetric Cd(Ⅱ) ion is six-coordinated in a slightly distorted octahedral geometry.The intermolecular hydrogen bonds extend the mononuclear structure into a one-dimensional supramolecular framework. The fluorescence spectrum of the compound exhibits intense emission at 520 nm when excited at 330 nm in solid state at room temperature.  相似文献   

19.
1 INTRODUCTION Diazoles have both a pyridine-type nitrogen and a pyrrole-type nitrogen (imino group), so they can act as bifunctional groups to coordinate with many metal ions or Lewis acids giving a variety of products[1, 2]. Recently researches on the pyrazole ligand have been focused on the following three sections. (i) The first is that the ligand acts as a bridged ligand and coordinates to metal forming di- and polynuclear complexes. Such system arouses much interest mainly because o…  相似文献   

20.
Two novel cobalt(Ⅱ) compounds were obtained and characterized by X-ray single-crystal diffraction,IR,1H NMR and elemental analysis.Compound 1 crystallizes in monoclinic,space group P21/n,with a = 18.046(4),b = 11.335(3),c = 19.157(5) ,β = 92.707(3)o,Z = 4,V = 3914.4(16) 3,Mr = 968.56,Dc = 1.644 g/cm3,μ = 1.378 mm-1,F(000) = 1960,the final R = 0.0367 and wR = 0.0895.The crystal of compound 2 is of monoclinic,space group P21/c with a = 8.7253(10),b = 10.9031(13),c = 18.235(2) ,β = 93.2210(10)o,Z = 4,V = 1732.0(3) 3,Mr = 464.21,Dc = 1.780 g/cm3,μ = 1.560 mm-1,F(000) = 932,the final R = 0.0322 and wR = 0.0743.  相似文献   

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