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1.
Reaction of iron(III) thiocyanate with isonicotinamide (inia) in ethanol leads to formation of a dark red, air stabile crystalline iron(III) compound of composition [iniainia][Fe(inia)2(NCS-N)4]. Single-crystal X-ray diffraction analysis shows the triclinic P1 space group with unit cell parameters: a?=?8.2440(4)?Å, b?=?9.5540(3)?Å, c?=?11.2590(5)?Å, α?=?93.945(4)°, β?=?95.554(4)°, γ?=?96.285(3)°, and Z?=?1. The iron compound contains [iniainia]+ cations and [Fe(inia)2(NCS-N)4] anions, which are held together by ionic interactions and hydrogen bonding. The Fe(III) is octahedrally coordinated by six nitrogens, four from NCS in the equatorial plane and two from inia occupying axial positions. The [iniaH]Cl has been formed by reaction of inia with hydrochloric acid. [iniaH]Cl crystallized in the monoclinic C2/c space group with unit cell parameters: a?=?25.156(5)?Å, b?=?5.095(1)?Å, c?=?12.747(3)?Å, and Z?=?8. Both compounds have also been characterized by elemental analyses and infrared spectroscopy. Structural and infrared spectral data are compared with data of similar compounds in the literature.  相似文献   

2.
Polymeric dioxomolybdenum(VI) complexes, [MoO2L]n (L?=?L1?=?N′-(2-hydroxybenzylidene)nicotinohydrazide for 1, L?=?L2?=?N′-(2-hydroxy-5-methoxybenzylidene)isonicotinohydrazide for 2), were prepared and characterized by physico-chemical, spectroscopic methods, and single-crystal X-ray determination. Complex 1 crystallizes in the orthorhombic space group P212121 with a?=?7.6568(4), b?=?11.6315(7), c?=?15.2211(9)?Å, V?=?1355.59(13)?Å3, Z?=?4, R 1?=?0.0181, wR 2?=?0.0464, and S?=?1.097. Complex 2 crystallizes in the monoclinic space group P2 1 /n with a?=?11.2516(6), b?=?11.8134(7), c?=?12.4371(6)?Å, β?=?116.2210(10)°, V?=?1483.02(14)?Å3, Z?=?4, R 1?=?0.0399, wR 2?=?0.0874, and S?=?1.096. X-ray analysis indicates that Mo in each complex is octahedral with two oxo groups and N2O2 donor set of the nicotinohydrazone or isonicotinohydrazone. The complexes are efficient catalysts for oxidation of olefins.  相似文献   

3.
The complexes [NO2BzPz]2[Ni(mnt)2] (1) and [BrBzPz]2[Pd(mnt)2] (2) have been prepared by reaction of Na2mnt, NiCl2·6H2O or PdCl2, and the corresponding 1-(R-benzyl)pyrazinium bromide salt (R = 4′-nitro, R = 4′-bromo). Crystallographic data for 1: monoclinic, P21/n, a = 7.3494(15), b = 15.223(3), c = 15.054(3)?Å, β = 102.42(3)°, V = 1644.8(6)?Å3, Z = 2. Data for 2: monoclinic, P21/n, a = 7.399(2), b = 19.024(4), c = 12.224(2)?Å, β = 94.62(3)°, V = 1715.0(7)?Å3, Z = 4. In both complexes, the [M(mnt)2]2? anion has a centre of symmetry at the metal atom and two cations are related to each other by the symmetry centre. The [M(mnt)2]2? anion exhibits a quasi-planar structure in both complexes, which show similar crystal packing.  相似文献   

4.
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   

5.
6.
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   

7.
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   

8.
A 2-D coordination polymer, (C7N4H16)2{NH(CH3)3}[{K(H2O)}4Na(H2O)5{Co4(H2O)2(B-α-PW9O34)2}]·2H2O (1), was hydrothermally synthesized and structurally characterized by IR spectroscopy, elemental analysis, X-ray powder diffraction, and X-ray single-crystal crystallography. Crystal structure analysis shows a triclinic space group Pī with a?=?12.4677(8)?Å, b?=?12.5054(8)?Å, c?=?18.5745(1)?Å, α?=?73.3220(1)°, β?=?87.1890(1)°, γ?=?62.2710(1)°, and V?=?2443.4(3)?Å3. Sandwich-type tetra-cobalt(II)-substituted [Co4(H2O)2(B-α-PW9O34)2]10? of 1 consists of two trivacant Keggin [B-α-PW9O34]9? moieties and a rhomb-like Co4O16 unit. Each sandwich-type polyoxotungstate subunit connects 12 K(1) and K(2) centers from two adjacent 1-D K-chain units resulting in an interesting 2-D layer framework. Magnetic properties of 1 have been investigated.  相似文献   

9.
Two new binuclear complexes, [Mn2(μ-dmpo)2(SCN)4(H2O)2] (1) (where dmpo?=?3,5-dimethylpyridine N-oxide), [Mn2(μ-po)2(H2O)6I2]I2 (2) (where po?=?pyridine N-oxide), have been synthesized and their crystal structures determined by X-ray crystallography. Complexes 1 and 2 crystallize in monoclinic, space group P21/c, with unit cell dimensions a?=?8.8836(18)?Å, b?=?15.450(3)?Å, c?=?15.484(3)?Å, β?=?91.020(3)° for 1, and a?=?8.8352(13)?Å, b?=?17.927(3)?Å, c?=?8.3338(12)?Å, β?=?103.765(2)° for 2. In each binuclear complex two Mn(II) were bridged by two 3,5-dimethylpyridine N-oxides or by two pyridine N-oxides and the distances between the bridged Mn(II) ions are 3.599?Å for 1 and 3.552?Å for 2. Variable temperature (4–300?K) magnetic measurements were performed for 1 and the susceptibility data were fitted by using a binuclear Mn(II) magnetic coupling formula producing the 2J?=??2.17?cm?1.  相似文献   

10.
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   

11.
A new ion-pair complex, [BrBzMeQl][Ni(mnt)2] (1) ([BrBzMeQl]+?=?1-(4′-bromobenzyl)-2-methylquinolinium; mnt2??=?maleonitriledithiolate), has been prepared and characterized. X-ray diffraction analysis shows that the Ni(mnt)2 anion and [BrBzMeQl]+ cations of 1 form completely segregated stacking columns, with the Ni?···?Ni distances alternating between 3.717 and 4.466?Å?in the Ni(mnt)2 stacking column. The variable-temperature magnetic susceptibilities of 1 have been measured over the range 75–300?K and the results reveal that the complex exhibits antiferromagnetic behavior.  相似文献   

12.
Two new compounds, [Zn(phen)3]2[γ-As8V14O42(H2O)]?·?4H2O (1) and [Cd(phen)3]2[γ-As8V14O42(H2O)]?·?2H2O (2) (phen?=?1,10′-phenanthroline), have been hydrothermally synthesized and structurally characterized by single-crystal X-ray diffraction, infrared spectrum, and thermogravimetric analysis. Compound 1 crystallizes in the triclinic space group P 1 with a?=?11.429(4)?Å, b?=?15.760(5)?Å, c?=?15.952(5)?Å, α?=?108.825(5)°, β?=?92.194(5)°, γ?=?104.155(5)°, V?=?2615.6(15)?Å3, Z?=?1; 2 crystallizes in the triclinic space group P 1 with a?=?11.450(4)?Å, b?=?15.629(6)?Å, c?=?16.302(6)?Å, α?=?109.177(5)°, β?=?92.628(5)°, γ?=?104.251(4)°, V?=?2644.8(17)?Å3, Z?=?1. Single-crystal structural analysis shows that both 1 and 2 consist of a new type of [γ-As8V14O42(H2O)]4? cluster anion.  相似文献   

13.
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   

14.
15.
Two cobalt complexes [NaCoII(nta)(H2O)] n (H3nta?=?nitrilotriacetic acid) (1) and NH4[CoIII(ida)2]?·?2H2O (H2ida?=?iminodiacetic acid) (2) have been synthesized and characterized by single-crystal X-ray diffraction analysis. Compound 1 crystallizes in the orthorhombic system, space group P212121 with a?=?7.9770(12)?Å, b?=?9.7613(15)?Å, c?=?12.1945(18)?Å, V?=?949.5(2)?Å3, Z?=?4, and R 1?=?0.0705 for 1597 observed reflections. Compound 2 crystallizes in the monoclinic system, space group P2(1)/c with a?=?5.1801(3)?Å, b?=?11.2073(6)?Å, c?=?12.2891(7)?Å, V?=?707.09(7)?Å3, Z?=?2, and R 1?=?0.0349 for 1143 observed reflections. In compound 1, the Co is coordinated by a nitrogen and five oxygen atoms in a distorted octahedral geometry {CoNO5}, and the Na is coordinated by one water molecule and four carboxyl oxygen atoms in slightly distorted square pyramidal geometry. The entire structure shows a three-dimensional network. In compound 2, Co atom is equatorially coordinated by two ida ligands in a distorted octahedral geometry {CoN2O4}. The discrete [Co(ida)2]2? anions are linked by hydrogen bonding to a three-dimensional supramolecular network.  相似文献   

16.
Two rare-earth metal coordination compounds, (NH4)4[SmIII2(Httha)2]·16H2O (1) (H6ttha?=?triethylenetetramine-N,N,N,N′′,N′′′,N′′′-hexaacetic acid) and (NH4)4[SmIII2(dtpa)2]·10H2O (2) (H5dtpa?=?diethylenetriamine-N,N,N,N′′,N′′-pentaacetic acid), have been synthesized through reflux and characterized by FT-IR spectroscopy, thermal analysis, and single-crystal X-ray diffraction techniques. SmIII of (NH4)4[SmIII2(Httha)2]·16H2O (1) is nine-coordinate, forming tricapped trigonal prismatic coordination with three amine nitrogens and six oxygens, in which four oxygens are from one ttha and two from the other ttha. (NH4)4[SmIII2(Httha)2]·16H2O (1) crystallizes in the monoclinic crystal system with P2(1)/c space group. The crystal data are: a?=?13.9340(13) Å, b?=?22.890(3) Å, c?=?20.708(2) (14) Å, β?=?99.521(2)°, and V?=?6513.7(13) Å3. There are two –NH+– groups in the [SmIII2(Httha)2]4?. The polymeric (NH4)4[SmIII2(dtpa)2]·10H2O (2) also is nine-coordinate with tricapped trigonal prismatic conformation and crystallizes in the triclinic crystal system with P–1 space group. The cell dimensions are: a?=?9.8240(8) Å, b?=?10.0329(9) Å, c?=?13.0941(11) Å, β?=?77.1640(10)°, and V?=?1227.30(18) Å3. In (NH4)4[SmIII2(dtpa)2]·10H2O, there are two types of ammonium cations, which connect [SmIII2(dtpa)2]4? and lattice water through hydrogen bonds, leading to a 2-D ladder-like layer structure.  相似文献   

17.
Reaction of the monovacant heteropolyanions α-[SiW11O39]8? with PhCH2PO(OH)2 leads to the formation of the organophosphoryl derivative α-[Bu4N]3H[PhCH2P(O)]2SiW11O39 (1). Single-crystal X-ray diffraction analysis shows that the crystal is monoclinic with space group P21 /n and the unit cell parameters: a?=?14.386 (3)?Å, b?=?27.015 (5)?Å, c?=?25.480 (5)?Å, α?=?90°, β?=?91.44 (3)°, γ?=?90°, V?=?9899 (3)?Å3. Z?=?4, D c?=?2.467?g?cm?1, λ (Mo-Kα)?=?0.071073?nm, R 1?=?0.0638, wR 2?=?0.1364. The hybrid anion consists of an α-[SiW11O39]8? framework on which two equivalent organophosphoryl groups are grafted through P?O?W bridges; each of the two PhCH2P(O) groups are connected to two terminal oxygen atoms belonging to a triad and a diad, respectively.  相似文献   

18.
A new inorganic–organic hybrid material, [EtdiPy][Co(NCS)4] (1) ([EtdiPy]2+?=?1,1′-ethylene-2,2′-dipyridinium), was synthesized and characterized by elemental analysis, IR spectrum, UV-Vis spectrum, ESI-MS, and single-crystal X-ray diffraction. Compound 1 is monoclinic, space group P21/n, with a?=?21.691(5)?Å, b?=?8.639(2)?Å, c?=?21.748(5)?Å, β?=?90.124(3)°, V?=?4075.1(16)?Å3, D c?=?1.550?g cm?3, Z?=?8, F(000)?=?1928, and R 1?=?0.0435. The C–H···S hydrogen bond, short S···C, S···N interactions, p···π, and π···π interactions observed in the solid state of 1 give a 3-D structure. Magnetic measurements from 2 to 300?K have shown weak antiferromagnetic exchange with θ?=??0.892?K in 1.  相似文献   

19.
A Cu(II) complex with 2-(2′-pyridyl)benzimidazole and l-arginine has been synthesized and investigated by elemental analysis, molar conductivity, IR, UV/vis, and X-ray diffraction. The complex crystallizes in the triclinic space group P1 with six molecules in a unit cell of dimensions a?=?10.6397(5)?Å, b?=?19.2178(8)?Å, c?=?20.0387(9)?Å, α?=?75.3670(10)°, β?=?79.4670(10)°, γ?=?87.4470(10)°, V?=?3897.6(3)?Å3, R 1?=?0.0408, and wR 2?=?0.0502. The complex contains six crystallographically independent complexes, Cu1, Cu2, Cu3, Cu4, Cu5, and Cu6, which have a distorted square-pyramidal geometry. The complex was screened for its in vitro antibacterial activities against two Gram-positive (Bacillus subtilis and Staphylococcus aureus) and two Gram-negative (Escherichia coli and Salmonella) micro-organisms. The complex exhibited good antibacterial activities against the micro-organisms compared with HPB and Cu(ClO4)2. Interaction of the complex with DNA was studied by electronic absorption spectroscopy, fluorescence spectroscopy, circular dichroic spectroscopy, viscosity measurements, and agarose gel electrophoresis. Results suggest that the complex could bind to CT-DNA via partial intercalation, and cleave the plasmid DNA with involvement of hydroxyl radicals, and probably singlet oxygen-like copper-oxo species in the presence of ascorbate.  相似文献   

20.
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   

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