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1.
ZHAO  Pei-Liang ZHOU  Zhong-Zhen 《结构化学》2010,29(8):1280-1283
The crystal structure of the title compound 2-ethoxycarbonylmethyl-8-chloro-3a,4-dihydro-3a-methyl-chromeno[4,3-c]pyrazol-3(2H)-one(C15H15ClN2O4,Mr = 322.74) has been prepared and determined by single-crystal X-ray diffraction.The crystal is of orthorhombic,space group Pccn with a = 16.7246(10),b = 19.6626(12),c = 9.3013(6) ,V = 3058.7(3) 3,Z = 8,Dc = 1.402 g/cm3,μ = 0.269 mm-1,F(000) = 1344,the final R = 0.0506 and wR = 0.1464 for 2568 reflections with I 2σ(I).In addition,disordered C(14) and C(15) atoms exist in the crystal structure.  相似文献   

2.
Two new Schiff base complexes of nickle(Ⅱ) [C18H20NiN2O4]·1.5H2O(1) and [C18H20N2NiO4]·H2O(2) were synthesized and characterized by elemental analysis,IR,UV-Vis and X-ray crystal structure analysis.Both 1 and 2 crystallize in the orthorhombic system.Crystal 1:space group Pbcn with a = 12.8591(19),b = 14.779(2),c = 19.749(3) ,V = 3753.3(10) 3,C18H23N2NiO5.5,Mr = 414.07,Z = 8,Dc = 1.445 g/cm3,μ = 1.067 mm-1,F(000) = 1712,S = 1.037,the final R = 0.0741 and wR = 0.2101 for 4353 observed reflections(I > 2σ(I)) and R = 0.1157 and wR = 0.2380 for all data.Crystal 2:space group P21 with a = 9.4673(17),b = 11.559(2),c = 16.347(3) ,V = 1788.9(6) 3,C18H22N2NiO5,Mr = 405.07,Z = 4,Dc = 1.497 g/cm3,μ = 1.116 mm-1,F(000) = 840,S = 1.085,the final R = 0.0330 and wR = 0.0869 for 3151 observed reflections(I > 2σ(I)) and R = 0.0362 and wR = 0.0887 for all data.Each Ni atom of 1 and 2 is six-coordinated with two nitrogen atoms and four oxygen atoms from two salicylidene-2-ethanolamine ligands yielding a distorted octahedral geometry.Dimer structure is observed in the packing diagram of 1.The thermal stability of complex 2 is also studied.  相似文献   

3.
The title compound(C26H18N4O4) has been synthesized via a three-component reaction and it was characterized by means of IR and 1H NMR.Its crystal and molecular structures were determined by X-ray diffractometry.It belongs to the triclinic system,space group P1 with a = 7.7288(15),b = 11.168(2),c = 12.645(3) ,α = 107.02(3),β = 90.85(3),γ = 101.93(3)°,V = 1017.9(3) 3,Mr = 450.44,Z = 2,Dc = 1.470 g/cm3,λ = 1.54178 ,μ = 0.836 mm-1,F(000) = 468,the final R = 0.0488 and wR = 0.1180.A total of 11903 reflections were collected,of which 3642 were independent(Rint = 0.0377) and 3025 were observed with I > 2σ(I).  相似文献   

4.
A novel organic polycarboxylate N-cyclohexylaziridines-2R,3S-dicarboxylic acid was synthesized and reacted with Ni2(OH)2CO3.As a result,a coordination polymer was obtained.It crystallizes in orthorhombic,space group Pbca with a = 8.6325(10),b = 10.5414(13),c = 27.644(3) ,Z = 4,V = 2515.5(5) 3,C20H34N2Ni2O12,Mr = 611.91,Dc = 1.616 g/cm3,μ = 1.562 mm-1,F(000) = 1280,the final R = 0.0320 and wR = 0.0677 for 2854 independent reflections with Rint = 0.0390.Crystal structure shows that the coordination environment around the Ni(Ⅱ) ion can be described as a slightly distorted octahedron.The ligands act as a bridge through the carboxyl O atoms and join the Ni atoms into an infinite 1D chain structure.The 1D chain forms a 2D network through intermolecular O-H…O hydrogen bonds.The magnetic susceptibility measurements(2~300 K) agree with a weak antiferronmagnetic interaction between neighboring Ni ions in the chain.  相似文献   

5.
The reactions of Co(ClO4)2·6H2O and Co(NO3)2·6H2O with the di-Schiff base ligand N,N'-bis-(1-benzimidazo-2-yl-ethylidene)-ethane-1,2-diamine (LA) in ethanol have been investigated. The reactions of LA with excess amount of cobalt salts yield the six-coordinate complexes [CoL2](ClO4)2·H2O 1 and [CoL2](NO3)2·H2O 2 as isolatable products (L = N-(1-benzimidazo-2-yl-ethylidene)-ethane-1,2-diamine), where L is a tri-dentate mono-Schiff base ligand, resulting from the hydrolysis of the precursor di-Schiff base LA. Both complexes were characterized by X-ray crystallography. Crystal data for complex 1: monoclinic, space group P21/c, a = 11.9214(10), b = 23.5828(17), c = 14.0387(12) , β = 135.219(4)o, C22H30Cl2CoN8O9, Mr = 680.37, V = 2780.1(4) 3, Z = 4, Dc = 1.625 g/cm3, μ(MoKα) = 0.876 mm-1, F(000) = 1404, the final R = 0.0725 and wR = 0.1530 for 5726 observed reflections (I > 2σ(I)). Crystal data for complex 2: monoclinic, space group P21/c, a = 18.2162(16), b = 10.0610(6), c = 18.593(2) , β = 130.099(3)o, C22H30CoN10O7, Mr = 605.49, V = 2606.5(4) 3, Z = 4, Dc = 1.543 g/cm3, μ(MoKα) = 0.722 mm-1, F(000) = 1260, the final R = 0.0619 and wR = 0.1429 for 5194 observed reflections (I > 2σ(I)). X-ray diffraction analysis reveals that each cobalt atom in the two complexes is chelated by six nitrogen atoms from two tridentate ligands L, exhibiting a slightly distorted octahedral coordination sphere. In both complexes, the strong hydrogen-bonding interactions between the lattice waters and N-H groups of the ligands result in 1D chains which are further connected by ClO4-(or NO3-) groups to form a 3D framework. In complex 2, the strong π-π interactions increase the stability of the structure.  相似文献   

6.
WANG  Yan-Qin GAO  En-Qing 《结构化学》2010,29(9):1331-1336
Two complexes with a zwitterionic dicarboxylate ligand,Mn(L)2(H2O)4 1 and Co(L)2(H2O)4 2(L = 1-carboxymethylpyridinium-4-carboxylate),were synthesized and structurally characterized.Complex 1 crystallizes in monoclinic,space group P21 with a = 6.490(2),b = 19.210(7),c = 7.813(3) ,β = 92.716(5)o,V = 972.9(6) 3,Z = 2,Mr = 487.28,Dc = 1.663 g/cm3,F(000) = 502,μ = 0.749 mm-1,S = 1.060,the final R = 0.0377 and wR = 0.0893 for 3292 observed reflections with I 2σ(I).Complex 2 is isomorphous with 1,with a = 6.478(2),b = 19.052(7),c = 7.742(3) ,β = 92.690(4)o,V = 954.6(6) 3,Z = 2,Mr = 491.28,Dc = 1.709 g/cm3,F(000) = 506,μ = 0.971 mm-1,S = 1.035,the final R = 0.0425 and wR = 0.0809 for 3289 observed reflections with I 2σ(I).In the compounds,the mononuclear [M(L)2(H2O)4] units with trans-octahedral coordination geometry are linked into 3D architectures via hydrogen bonding(or second-sphere coordination) involving carboxylate groups and coordinated water molecules.The 3D networks illustrate a 3,8-connected net with Schlfli symbol(4·62)2(42·623·83).  相似文献   

7.
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   

8.
WEN  Li-Rong WANG  Li-Juan LI  Ming 《结构化学》2011,30(6):867-871
The title compound(C25H16Cl2N3O3S),as a thiopyran derivative,has been synthe-sized by the cyclization of an organic intermediate obtained from Baylis-Hillman adducts with a β-aroylthioamide using copper(I) salt as the catalyst.The crystal belongs to the monoclinic system,space group P21/c with a = 13.668(3),b = 8.4803(17) c = 21.999(4) ,β = 113.57(3)°,V = 2337.2(10) 3,Z = 4,Mr = 510.38,Dc = 1.451 g/cm3,μ = 0.401 mm-1,F(000) = 1048,the final R = 0.0487 and wR = 0.1079 for 3678 observed reflections with I > 2σ(I).  相似文献   

9.
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   

10.
Two novel complexes,[(C9H18NS2)3Sb(III)](1) and [(C9H18NS2)3Bi(III)](2),were synthesized and characterized by elemental analysis,IR,TG and X-ray single-crystal diffraction.Both 1 and 2 crystallize in the monoclinic system,P21/c space group.The data for 1:a = 1.6964(3),b = 1.02149(17),c = 2.5650(3) nm,β = 121.824(8)°,Z = 4,V = 3.7766(10) nm3,Dc = 1.293 g·cm-3,F(000) = 1536,μ = 1.082 mm-1,the final R = 0.0500,wR = 0.1562 and S =1.072.The data for 2:a = 1.6802(9),b = 1.0256(6),c = 2.5083(10) nm,β = 121.77(3)°,Z = 4,V = 3.675(3) nm3,Dc = 1.486 g·cm-3,F(000) = 1664,μ = 5.159 mm-1,the final R = 0.0481,wR = 0.1055 and S =1.076.The coordinated geometry of the central M(III) with six sulfur atoms from three ligands is a distorted pentagonal pyramid configuration.The dimer structural system is formed by the weak interactions of M…S and C-H…S between two molecules.The complexes were valued for their antibacterial activities by agar-streak method.It was found that 1 is active against the four test bacterial organisms.  相似文献   

11.
A new inorganic-organic hybrid supramolecular compound [Habo]6[V10O28]·solvents and its crystal structure was reported as follows: monoclinic, space group P21/n, a =11.419(9), b = 16.811(16), c = 15.521(12) (A), β= 102.98(2)°, V= 2903(4) (A)3, Z = 4, C15H46N3O19V5,Mr = 827.25, Dc = 1.893 g/cm3, λ(MoKα) = 0.71073 A,μ = 1.636 mm-1, F(000) = 1696, the final R =0.0696 and wR = 0.1361 for 4641 observed reflections with I > 2σ(I). The compound is based on decavanadate clusters [V 1oO28]6-. The hydrogen bonding interactions among Habo+ cations, solvents and decavanadate clusters extend 1 into a three-dimensional supramolecular architecture.  相似文献   

12.
Under hydrothermal conditions, two new ribbon-like structures, [Cu(C14H9O4)-analysis revealed that these structures were constructed by mixed ligands. The coordination polymer forms the basic architecture while the weak interactions extend the framework into a secondary structure. The whole structures of them are governed by collaboration of the strong and weak interactions. Compound 1 crystallizes in monoclinic, space group C2/c with a = 17.0485(3), b =1 1.0558(3), c = 22.7623(4) A, β = 102.465(1)°, V = 4189.2(2) A3, Z = 4, Mr = 915.44, Dc = 1.451g/mL, F(000) = 1900 andμ(MoKα) = 0.587 cm-1. The final R and wR are 0.0030 and 0.1022,respectively for 3037 observed reflections with I > 2σ(I). Compound 2 crystallizes in monoclinic,space group P21/c with a = 11.5963(4), b = 11.7004(5), c = 17.1254(5) A,β = 95.620(1)°, V =2312.4(1) A3, Z = 4, Mr = 556.35, Dc = 1.598 g/mL, F(000) = 1132 andμ(MoKα) = 0.912 cm-1The final R and wR are 0.0431 and 0.1050, respectively for 2629 observed reflections with I > 2σ(I).  相似文献   

13.
Two new compounds containing triarylamine and benzoic hydrazide units, 4-[N,N-di(4-toyl)amino]benzaldehyde-N-(4-ethoxylphenyl)-formyl hydrazone 3a and 4-[N,N-di(4-toyl) amino]benzaldehyde-N-(2-ethoxylphenyl)-formyl hydrazone 3b, have been synthesized and their crystal structures (C30H29N3O2, Mr = 463.56) were interpreted by a combination technique of 1HNMR, IR, elemental analysis, mass spectra, UV-Vis spectra and X-ray crystallography, respec- tively. The crystal of 3a belongs to monoclinic, space group P21/n with a = 9.321(3) A, b = 11.046(4) A, c = 24.335(9) A, β=92.649(7)°, V = 2502.7(16) A3, Z = 4,μ =0.078 mm-1, Dc =1.230 g/cm3, F(000) = 984, the final R = 0.0590 and wR = 0.1316 for 4367observed reflections with I > 2σ(I). The crystal of 3b belongs to monoclinic, space group P21/c with a = 10.637(4) A, b = 24.138(10) A, c = 10.398(4) A, β= 104.913(8)°, V= 2579.8(17) A3, Z = 4,μ = 0.075 mm-1, Dc = 1.194 g/cm3, F(000) = 984, the final R =0.0631 and wR =0.1006 for 4463 observed reflections with I > 2σ(I). X-ray crystallography revealed that the nitrogen atom in the triarylamine moiety is of sp2 hybridization with the three phenyl rings twisted to each other.  相似文献   

14.
The crystals of the title compounds (H3O)(C3H5N2)[Mn(OH)6Mo6O18]·3.5H2O 1 and (H3O)3[Co(OH)6Mo6O18]·7H2O 2 have been prepared and structurally determined by X-ray single-crystal diffraction. Compound 1 crystallizes in monoclinic, space group C2/c with a = 21.5018(9), b = 10.9331(5), c = 11.8667(5)A,β = 95.3570(10)o, V = 2777.5(2)A3, Z = 4, Dc = 2.802 g/cm3, Mr = 1171.80,μ(MoKα) = 3.173 mm-1, F(000) = 223, the final R = 0.0458 and wR = 0.1041 for 2093 observed reflections (I>2σ(I)); Compound 2 crystallizes in monoclinic, space group P21/c with a = 11.4042(12), b = 10.9481(11), c = 11.6722(12)A, β= 99.948(2)o, V = 1435.4(3)A3, Z = 2, Dc = 2.794 g/cm3, Mr = 1207.80,μ(MoKα) = 3.223 mm-1, F(000) = 1160, the final R = 0.0544 and wR = 0.1066 for 1906 observed reflections (I > 2σ(I)). Both compounds 1 and 2 adopt the Anderson structure, in which the anion is of centrosymmetry and formed by six octahedral edge-sharing MoO6 units surrounding the central MO6 (M = Mn or Co) octahedron.  相似文献   

15.
1 INTRODUCTION The design and synthesis of metal-organic frame- work structures have been extensively studied due to their unexpected properties for potential applications as functional materials as well as the intriguing ar- chitectures and topologies[1~4]. When rigid bifunc- tional ligands are used to connect metal centers, to- pology of the network is usually determined by the coordination geometry of the central metal prefer- ence. Contrary to rigid ligands, the bifunctional fle- xib…  相似文献   

16.
The reaction of VO(acac)2 with 2-hydroxyl-1-naphthaldehyde isonicotinyl hydrazone and amines (ethylenediamine or diethylenetriamine) in CH3OH yields crystals of novel vanadium compounds characterized by IR, NMR spectroscopic methods and X-ray single-crystal structure determination. Two different vanadium units exist in the crystal cell of [VO2(C17H11N3O2)][VO- (C4H13N3)(C6H5N3O)](C2H5OH) which crystallizes in the triclinic system, space group P1 with a = 8.0104(17), b = 13.898(3), c = 14.955(3)A, α = 89.103(4), β = 79.551(4), γ = 78.352(4)°, V = 1603.3(6)A^3, Mr = 723.54, Dc = 1.499 g/cm^3, Z = 2, λ(MoKα) = 0.71073 ]A,μ= 0.644 mm^-1, F(000) = 748, the final R = 0.0547 and wR = 0.0997 for 8920 observed reflections with I 〉 2σ(I). According to structure analysis, two different molecules are arranged in the lattice and the two vanadium atoms adopt octahedral and square pyramidal coordination geometries, respectively. The interactions between DNA and vanadium complexes have been investigated by UV-Vis absorption spectro- photometry.  相似文献   

17.
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   

18.
Two new iron-sulfur carbonyl complexes, [Fe2(SC6H4Cl)2(CO)6]·0.5(Et2O) 1 and [Fe3(SC6H4NH2)6(CO)6]·2(MeOH) 2, have been prepared and characterized by elemental analysis, IR spectra and single-crystal X-ray diffraction. Crystal data for 1: monoclinic, C2/c, a = 18.4439(8), b = 11.0999(5), c = 25.1830(10)(A), β = 97.0370(10)o, V = 5116.8(4)(A)3, Z = 8, C20H13Cl2Fe2O6.50S2, Mr = 604.02, Dc = 1.568 g/cm3, μ = 1.540 mm-1, F(000) = 2424, the final R = 0.0545 and wR = 0.1454 for 3443 observed reflections with I > 2σ(I); 2: monoclinic, P21/n, a = 12.350, b = 26.3050(11), c = 16.057(A),β = 97.891(3)°, V = 5166.9(2)(A)3, Z = 4, C44H44Fe3N6O8S6, Mr = 1144.76, Dc = 1.472 g/cm3, μ = 1.128 mm-1, F(000) = 2352, the final R = 0.0442 and wR = 0.1197 for 7978 observed reflections with I > 2σ(I). Complex 1 contains one iron dimer, in which two tricarbonyliron(I) fragments are bridged together by two 4-chlorophenylthiolate ligands, whereas complex 2 contains a linear tri-iron cluster, in which two terminal tricarbonyliron(II) fragments and the central Fe(II) atom are linked together by six 4-aminophenylthiolate bridging ligands.  相似文献   

19.
A new dinuclear copper(Ⅱ) polymer [Cu2(bipy)2(Hbtc)2(H2O)2]·(H2O)1/2 1 (bipy=2,2'-bipyridine, H3btc = benzene-1,3,5-tricarboxylic acid) was obtained by the hydrothermal single-crystal X-ray diffraction analysis and identified using elemental analysis and IR spectrum.The title complex crystallizes in monoclinic system, space group P21/c with a = 7.2880(5), b =18.4778(13), c = 13.5465(10)(A), β = 95.9580(10)°, C19H14.50CuN2O7.25, Mr = 450.37, V= 1814.4(2)(A)3, Z=4, Dc = 1.649 g/cm3, μ = 1.253 mm-1, F(000) = 918, Rint = 0.0185, the final R = 0.0271and wR = 0.0710 for 2773 observed reflections (I>2σ(I)). The study results reveal that a pair of distorted square-pyramidal Cu2+ ions are interlinked by bis-monodentate bridging Hbtc2- ligands to constitute a 16-membered ring.  相似文献   

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