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1.
Two new structurally similar molybdenum(VI) complexes, [MoO2L1(CH3OH)] (1) and [MoO2L2(CH3OH)] (2), where L1 is the dianionic form of N′-(2-hydroxy-5-nitrobenzylidene)-2-methylbenzohydrazide and L2 is the dianionic form of N′-(2-hydroxy-4-methoxybenzylidene)-2-methylbenzohydrazide, were prepared and structurally characterized by elemental analysis, infrared spectra, and single-crystal X-ray diffraction. 1 crystallizes in the monoclinic space group P21/c, with unit cell dimensions a?=?7.941(1), b?=?14.337(2), c?=?15.141(2)?Å, β?=?92.782(2)°, V?=?1721.8(4)?Å3, Z?=?4, R1?=?0.0286, wR2?=?0.0650, GOOF?=?1.028. 2 crystallizes in the triclinic space group P-1, with unit cell dimensions a?=?8.003(1), b?=?10.608(1), c?=?10.880(1)?Å, α?=?95.745(2)°, β?=?97.627(2)°, γ?=?105.762(2)°, V?=?872.0(2)?Å3, Z?=?2, R1?=?0.0226, wR2?=?0.0595, GOOF?=?1.116. X-ray analysis indicates that Mo in the complexes are coordinated by the phenolate oxygen, imino nitrogen, and enolate oxygen of the benzohydrazone, methanol, and two oxo groups, generating octahedral coordination. The oxidation of olefins with the complexes as catalysts was evaluated, indicating that the complexes showed excellent catalytic efficiency in oxidation of most aliphatic and aromatic substrates under mild conditions using tert-butyl hydrogen peroxide as oxidant.  相似文献   

2.
Two structurally similar vanadium(V) complexes, [VOL1L] (1) and [VOL2L] (2), where L1 is the dianionic form of N′-(3,5-dibromo-2-hydroxybenzylidene)-4-methoxybenzohydrazide, L2 is the dianionic form of N′-(3,5-dibromo-2-hydroxybenzylidene)nicotinohydrazide, and L is benzohydroxamate, were prepared and characterized by elemental analysis, infrared spectra, and single crystal X-ray diffraction. 1 crystallizes in the monoclinic space group P21/c, with unit cell dimensions a?=?12.0262(7), b?=?16.5629(9), c?=?12.3449(8)?Å, β?=?105.160(2)°, V?=?2373.4(2)?Å3, Z?=?4, R1?=?0.0376, wR2?=?0.0844, GOOF?=?1.058; 2 crystallizes in the monoclinic space group P21/c, with unit cell dimensions a?=?10.6439(7), b?=?16.1968(9), c?=?13.1108(8)?Å, β?=?104.180(2)°, V?=?2191.4(2)?Å3, Z?=?4, R1?=?0.0521, wR2?=?0.1142, GOOF?=?1.018. X-ray analysis indicates that vanadium in the complexes are coordinated by phenolate oxygen, imino nitrogen, and enolate oxygen of the hydrazone, two oxygens of the benzohydroxamate, and one oxo, generating octahedral coordination. Oxidations of olefins with the complexes as catalysts were evaluated. The complexes showed effective catalytic efficiency in oxidation of several aliphatic and aromatic substrates under mild conditions, using tert-butyl hydrogen peroxide as oxidant.  相似文献   

3.
Three new complexes (13) have been synthesized and characterized by X-ray single crystal determination and evaluated for inhibitory activity on jack bean urease. All the complexes contained a new cinnamic acid derivative as the ligand (C11H12O4), (E)-3-(3,4-dimethoxyphenyl)acrylic acid, and crystallized in monoclinic C2/c space group. Complex 1 (C11H11O4)4(C3N2H8)2Cu2 (C3N2H8?=?1,2-diaminopropane) was obtained with a?=?20.488(2), b?=?19.596(2), c?=?15.2500(13), β?=?93.502(2)°, V?=?6111.2(10)?Å3, Z?=?4, R 1 ?=?0.0616, and wR 2 ?=?0.2059. Complex 2 (C11H11O4)4(C3N2H8)2Cu2 (C3N2H8=1,3-diaminopropane) was obtained with a?=?20.2494(12), b?=?19.5732(12), c?=?14.8940(8), β?=?96.884(2)°, V?=?5860.6(6)?Å3, Z?=?4, R 1 ?=?0.0409, and wR 2 ?=?0.1107. Complex 3 (C11H11O4)2(C2N2H6)2Ni2·H2O (C2N2H6?=?ethylenediamine) was obtained with a?=?28.359(2), b?=?6.5422(5), c?=?16.8587(14), β?=?101.359(2)°, V?=?3066.5(4)?Å3, Z?=?4, R 1 ?=?0.0422, and wR 2 ?=?0.1190. It was found that copper(II) complexes 1 [IC50?=?4.71?μM] and 2 [IC50?=?3.15?μM] showed strong inhibitory activity against jack bean urease compared with acetohydroxamic acid [IC50?=?10.01?μM] as a positive reference. Unfortunately, 3 exhibited no inhibitory activity.  相似文献   

4.
A lanthanide coordination complex [Eu(PAA)2(phen)(NO3)]2 (PAA?=?phenylacetic acid, phen?=?1,10-phenanthroline) has been synthesized by the hydrothermal method. Single crystal X-ray diffractions show that it forms a dimeric molecular structure. The title complex crystallizes in the triclinic system, space group P 1, with lattice parameters a?=?8.9473(8)?Å, b?=?13.3659(12)?Å, c?=?13.4745(12)?Å, α?=?60.7590(10)°, β?=?89.5100(10)°, γ?=?71.9850(10)°, V?=?1317.3(2)?Å3, D c?= 1.675?Mg?m?3, Z?=?1, F(000)?=?660, GOF?=?1.003, R 1?=?0.0206, wR 2?=?0.0575. The fluorescence excitation and emission spectra have been investigated.  相似文献   

5.
A new two-dimensional compound C12H14O16Zn3 (1), containing seven-coordinate zinc atoms was prepared by the hydrothermal technique. The compound obtained was characterized by TG-DTA, single crystal X-ray diffraction, elemental analysis and FT-IR analysis. Single-crystal X-ray diffraction analysis shows that compound 1 crystallizes with monoclinic symmetry in the space group P21/c, a?=?6.1552(13)?Å, b?=?14.546(3)?Å, c?=?9.581?Å, β?=?102.66(2)°, V?=?836.9(4)?Å3, Z?=?2, R1?=?0.0311, wR2?=?0.0830.  相似文献   

6.
Four transition metal complexes with Schiff base and 1,10-phenanthroline, [Cu(L)(phen)]2·C2H5OH (1), [Zn(L)(phen)]2·C2H5OH (2), [Ni(L)(phen)]2·C2H5OH (3), and [Co(L)(phen)]2·C2H5OH (4) (H2L?=?1-((2-hydroxynaphthalen-1-yl)methylene)thiosemicarbazide; phen?=?1,10-phenanthroline) were synthesized and characterized by physico-chemical methods. The crystal structure of 1 was determined by X-ray single-crystal diffraction analysis. 1 crystallizes in the orthorhombic space group Pbca with a?=?15.008(9), b?=?16.100(10), c?=?37.54(2)?Å, V?=?9070(10)?Å3, Z?=?8, GOOF?=?1.002, R 1?=?0.0626, and wR 2?=?0.0912. The fluorescence and urease inhibitory activities of the compounds were tested. The enzymatic activity study indicated that 3 possessed potent inhibition against jack bean urease, with IC50?=?1.2?±?0.1?μM, and about 35 times more than 42.1?±?0.4 acetohydroxamic acid as positive reference. This suggests that inhibitory efficiency of these complexes can be strongly influenced by different transition metal ions.  相似文献   

7.
Two complexes [CuL2(H2O)2] (1) and [ZnL2(H2O)2] (2) (L?=?3-carboxyl-1,2,4-triazole (L)) have been synthesized and characterized by single-crystal X-ray diffraction analysis. Compound 1 crystallizes in the monoclinic space group P 2(1)/n, a?=?8.632(8)?Å, b?=?9.153(8)?Å, c?=?6.991(7)?Å, β?=?94.279(12)°, Z?=?2, R 1?=?0.0296, wR 2?=?0.0918. Compound 2 also crystallizes in the monoclinic space group P 2(1)/n, a?=?4.937(3)?Å, b?=?18.107(10)?Å, c?=?6.344(4)?Å, β?=?106.839(7)°, Z?=?2, R 1?=?0.0230, wR 2?=?0.0556. Extensive intermolecular hydrogen bonds assemble 1 and 2 into three-dimensional (3D) supramolecular architectures, with eight-member H-bonded synthons. Compounds 1 and 2 were also characterized by element analysis, FT–IR, luminescence and EPR studies.  相似文献   

8.
Two metal complexes, [NiII(mscinn)2(pda)2] (1) and [CdII(mscinn)2(dmeda)2·2H2O] (2) (mscinn?=?4-methylsulfonyl cinnamate, pda?=?propane-1,3-diamine, dmeda?=?N′,N′-dimethylethane-1,2-diamine), were synthesized by reacting 4-methylsulfonyl cinnamate with the diamines and metal salts. Their structures were determined by single-crystal X-ray diffraction analysis. Crystal parameters of 1: C26H38N4NiO8S2, M?=?657.43, monoclinic, P21/c, a?=?16.6123(8)?Å, b?=?8.5956(4)?Å, c?=?11.2047(5)?Å, β?=?107.423(1)°, V?=?1526.54(12)?Å3, Z?=?2, D calcd?=?1.430?g?cm?3, F(000)?=?692, μ?=?0.825?mm?1, R 1?=?0.0257, wR 2?=?0.0669. Crystal data of 2: C28H42CdN4O8S2?·?2(H2O), M?=?775.24, monoclinic, P21/c, a?=?9.8278(4)?Å, b?=?11.6611(5)?Å, c?=?15.3972(7)?Å, β?=?96.195(1)°, V?=?1754.26(13)?Å3, Z?=?2, D calcd?=?1.468?g?cm?3, F(000)?=?804, μ?=?0.798?mm?1, R 1?=?0.0299, wR 2?=?0.0770. Antimicrobial activities for 1 and 2 against Escherichia coli, Pseudomonas putida, Bacillus subtilis, and Bacillus cereus had better antibacterial activity than their parent carboxylic acid against Gram-positive bacteria (B. subtilis and B. cereus). The cadmium complex of the cinnamate displayed high inhibitory activity with an MIC value of 5?µg?mL?1 against P. putida, while the nickel complex also exhibited good inhibitory potency with an MIC value of 5?µg?mL?1 against B. subtilis.  相似文献   

9.
This article reports the hydrothermal synthesis and characterization of two new phosphonate compounds NaCo[O3PCH(OH)CO2] (1) and NaMn[O3PCH(OH)CO2] (2) based on 2-hydroxyphosphonoacetic acid (H3L). Their structures have been characterized by single-crystal X-ray diffraction as well as with elemental analysis, infrared spectroscopy and thermogravimetric analysis. The two isomorphous compounds crystalline in the orthorhombic, space group Pbca: Crystal data for 1: a?=?10.1827(8)?Å, b?=?9.6673(8)?Å, c?=?10.7853(9)?Å, V?=?1061.70(15)?Å3, Z?=?8, R 1?=?0.0252, wR 2?=?0.0577; Crystal data for 2: a?=?10.4309(18)?Å, b?=?9.7913(17)?Å, c?=?10.9012(19)?Å, V?=?1113.4(3)?Å3, Z?=?8, R 1?=?0.0194, wR 2?=?0.0536. In the two compounds, the metal atoms are octahedrally coordinated; all oxygen atoms from the H3L ligand are involved in coordination. The overall structures can be described as a 3D open framework with channels running along the a axis and the charge-compensating Na+ cations being located at the intersections of these channels.  相似文献   

10.
The hydrothermal reaction of 1,3-dicyanobenzene, 1,10-phenanthroline (phen) and Pb(CH3COO)2 yields a new 1D coordination polymer, {Pb[C6H4(COO)2][phen]} n . The 1,3-benzenecarboxylate anion found in the final product was generated in situ during the synthesis by hydrolysis of 1,3-dicyanobenzene. X-ray diffraction shows that complex 1 crystallizes in the triclinic system, space group P 1, a?=?7.5442(2)?Å, b?=?9.7962(3)?Å, c?=?13.1505(4)?Å, α?=?69.739(2)?Å, β?=?80.597(2)?Å, γ?=?71.377(2)?Å, v?=?862.48(4)?Å3, Z?=?2, D c?=?2.124 Mg?m?3. Complex 1 emits strong blue fluorescent light (λem(max)?=?482.4?nm) when excited by UV light in the solid state at room temperature.  相似文献   

11.
12.
13.
Two new arsenic–vanadate compounds [Co(C4H13N3)2]2[As8V14O42(H2O)]?·?3.5H2O (1) and (C2N2H9)2(C2N2H10)[As8V14O42(H2O)]?·?2.33H2O (2) have been hydrothermally synthesized and characterized by X-ray single crystal diffraction, IR spectra and thermogravimetric analysis. Compound 1 crystallizes in the monoclinic space group P 2(1)/c, a?=?24.649(9)?Å, b?=?13.364(5)?Å, c?=?22.463(8)?Å, β?=?104.008(5)°, V?=?7180(5)?Å3, Z?=?4, R 1?=?0.0787, and wR 2?=?0.1859. Compound 2 crystallizes in rhombohedral system with space group R3c, a?=?b?=?c?=?22.2405(5)?Å, α?=?β?=?γ?=?110.4030(10)°, V?=?8163.4(3)?Å3, Z?=?6, R 1?=?0.0341 and wR 2?=?0.0941. The structural analyses show that both compounds have the same discrete cluster anion [As8V14O42(H2O)]4?. Moreover, in 1, the polyanions are connected through van der Waals forces to generate soft channels that are filled by [Co(C4H13N3)2]2+ cations and water. In 2, water and organic molecules link cluster anions to create the supramolecular assembly through hydrogen bonding.  相似文献   

14.
A novel isopolyoxomolybdate complex (C10H18N)4Mo8O26·6(CH3)2SO 1 was synthesized, purified and characterized by means of elemental analysis, IR and 1H NMR spectra and single-crystal X-ray diffraction. It crystallizes in a triclinic system with a?=?11.5090(6), b?=?12.8399(3), c?=?14.774(13)?Å, α?=?105.390(16), β?=?93.09(4), γ?=?106.100(10)°, V?=?2003.1(2)?Å3, Z?=?2, R1?=?0.0789, wR2?=?0.2190. Complex 1 is constructed from [Mo8O26]4?, (C10H18N)+ and (CH3)2SO and extends to form a two-dimensional network via hydrogen bonds and weak interactions in the ab plane. Chicken embryo experiments show that Compound 1 has high antiviral activity in vitro.  相似文献   

15.
A new ion-pair complex, [TTF][Pd(mnt)2] (1), where TTF+ =?tetrathiafulvalene and mnt2??=?maleonitriledithiolate, was synthesized and characterized structurally. Compound 1 crystallizes in triclinic space group P-1, with a?=?8.008(5)?Å, b?=?11.333(8)?Å, c?=?11.373(6)?Å, α?=?108.112(7)°, β?=?91.550(5)°, γ?=?95.232(5)°, and V?=?975.2(11)?Å3. The [TTF]+ cations (C) and [Pd(mnt)2]? anions (A) form mixed stacks in …AACCAACC… fashion, and the neighboring mixed stacks are held together via van der Waals forces in the crystal. Compound 1 shows weak Curie/Weiss-type magnetic behavior from 2 to 370?K; theoretical investigation disclosed the existence of strongly antiferromagnetic coupling in both [Pd(mnt)2]2 2? and [TTF]2 2+ dimer pairs via frontier orbitals overlap mechanism and weakly ferromagnetic coupling between the face-to-face overlapped [TTF]+ and [Pd(mnt)2]? via spin polarization mechanism within a mixed stack. The powdered pellet electrical conductivity measurement indicated that 1 shows semiconductor character with activation energy of 1.1(3)?eV.  相似文献   

16.
The chiral dinuclear heterometallic complexes [Cu(dach)2][Pt(CN)4]?·?2H2O (1), [Ni(dach)3][Pt(CN)4]?·?2DMF?·?H2O (2), and [Pd(dach)4][Pt(CN)4]?·?H2O (3) (dach?=?1R,2R-cyclohexanediamine) have been prepared and characterized by X-ray diffraction analysis. Crystal data: 1, monoclinic, P21, a?=?8.108(3), b?=?15.552(6), c?=?9.914(4)?Å, β?=?110.931(6)°, V?=?1167.6(8)?Å3, Z?=?2, R 1?=?0.0420, wR 2?=?0.1122; 2, monoclinic, P21, a?=?13.264(11), b?=?9.285(7), c?=?16.211(13)?Å, β?=?111.640(9)°, V?=?1856(3)?Å3, Z?=?2, R 1?=?0.0276, wR 2?=?0.0698; 3, monoclinic, P21, a?=?6.887(2), b?=?12.809(4), c?=?12.975(4)?Å, β?=?94.865(4)°, V?=?1140.6(6)?Å3, Z?=?2, R 1?=?0.057, wR 2?=?0.156. In complex 1, the Pt and Cu atoms are linked by a CN bridge that presents a very bent C=N–Cu angle [136.8(8)°].  相似文献   

17.
Two Cd(II) coordination polymers have been synthesized with derivatives of pyrazine-1,4-dioxide and thiocyanate anion as bridging ligands and structurally determined by X-ray crystallography. Complex 1, [Cd(μ1,3-SCN?)21,6-L1)] n (L1?=?2,5-dimethylpyrazine-1,4-dioxide), belongs to the triclinic, space group P 1 with a?=?5.7627(18)?Å, b?=?7.182(2)?Å, c?=?7.509(2)?Å, α?=?74.042(3)°, β?=?84.766(4)°, γ?=?88.162(4)°; complex 2, [Cd21,3-SCN?)44-L2)] n (L2?=?2,3,5,6-tetramethylpyrazine-1,4-dioxide), crystallizes in a monoclinic system with space group C2/m with a?=?10.194(4)?Å, b?=?13.491(6)?Å, c?=?8.140(3)?Å, β?=?120.372(4)°. Complex 1 shows a two-dimensional sheet structure, and in a direction the Cd(II) ions were coordinated by μ1,3-SCN? forming the one-dimensional chain and the L1 bridging ligand made the chains connect in the c direction leading to formation of a two-dimensional sheet on the ac plane. For 2 the one-dimensional chains in the a axis were constructed by coordination of μ1,3-SCN? bridging ligands with the Cd(II) ions, and in b and c directions the chains were joined by L2 bridging ligands leading to a three-dimensional structure. In 2 L2 displays a μ4-bridging coordination mode. Both complexes exhibit strong fluorescence emission.  相似文献   

18.
Three new complexes [CuL(N3)2] (1), [CuL(SCN)2] (2), and [CoL(SCN)3] (3) (L?=?1,4,7-tribenzyl-1,4,7-triazacyclononane) have been synthesized and structurally characterized. Complex 1 crystallizes in monoclinic space group P2(1)/n with unit cell parameters a?=?14.105(7), b?=?8.999(5), c?=?21.603(11)?Å, β?=?100.470(7)°. While 2 crystallizes in triclinic space group P-1 with unit cell parameters a?=?9.6380(16), b?=?10.6993(18), c?=?15.798(3)?Å, α?=?106.636(3), γ?=?116.478(3)°. Complex 3 crystallizes in trigonal space group P–3c1 with unit cell parameters a?=?14.744(3), b?=?14.744(3), c?=?16.098(4)?Å, γ?=?120°. Elemental analysis, IR, UV-vis spectra of complexes 13 and ESR spectra of complexes 12 were also determined.  相似文献   

19.
A novel supramolecular complex, [Na2(2,3-naphtho-15-crown-5)2(NO3)][Cu(NO3)3(H2O)] (1), has been prepared and characterized by X-ray single crystal diffraction. The complex crystallizes in the triclinic system, space group Pī, with a?=?11.233(6), b?=?13.342(7), c?=?16.601(8)?Å, α?=?89.836(7), β?=?79.132(8), γ?=?66.545(7)°, V?=?2234(2)?Å3, Z?=?2 and final R 1(wR 2)?=?0.0467(0.1164). Novel coordination features and supramolecular architectures are found in the solid state of 1. Two [Na(2,3-naphtho-15-crown-5)]+ cations containing two different sodium coordination numbers (six and seven) are bridged by a tridentate nitrate group, to form a larger complex cation, [Na2(2,3-naphtho-15-crown-5)2(NO3)], which is assembled into a novel 1D zigzag chain-like structure through aromatic C–H?···?π interactions.  相似文献   

20.
Two one-dimensional linear coordination polymers, [Mg(L)?·?4(H2O)] (H2L?=?olsalazine) and 2 [Ca(L)?·?4(H2O)] were obtained from self-assembly of CaCl2 or MgSO4 with olsalazine and their structures determined by single crystal X-ray diffraction. Both complexes are one-dimensional polymers, for complex 1 with crystal data: P2(1)/c, a?=?9.5224(18), b?=?11.309(2), c?=?16.211(3)?Å, β?=?106.648(3)°, V?=?1672.6(6)?Å3, Z?=?4, R 1?=?0.0695, wR 2?=?0.2183, for complex 2 with crystal data: P4(3)2(1)2, a?=?10.4006(2), b?=?10.4006(2), c?=?32.0746(10)?Å, V?=?3469.59(14)?Å3, Z?=?8, R 1?=?0.0332, wR 2?=?0.1015. In the complexes, Mg and Ca adopt totally different coordination modes. Alkaline-earth Mg is six-coordinate octahedronal geometry, however, in 2, the local coordination geometry around calcium atom can be best described as a slightly distorted pentagonal bipyramid crystallizing in a homo-chiral space group. Olsalazine in both compounds also adopts dissimilar coordination modes.  相似文献   

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