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1.
Nanostructures of a new coordination polymer of divalent lead with the ligand 2, 9‐dimethyl‐1, 10‐phenanthroline (dmp) containing the first Pb2‐(μ‐ClO4)2 motif, [Pb2(dmp)2(μ‐N3)2(μ‐ClO4)2]n ( 1 ), was synthesized by a sonochemical method that produces the coordination polymers at nano size. The new nanostructure was characterized by scanning electron microscopy, X‐ray powder diffraction, IR, 1H NMR and 13C NMR spectroscopy, and elemental analysis. Compound 1 was structurally characterized by single‐crystal X‐ray diffraction and the single‐crystal X‐ray data shows that the coordination number of PbII ions is six, (PbN4O2), with two N‐donor atoms from aza‐aromatic base ligands and four O‐donors from two perchlorate anions and two N‐donors from two azide anions. It has a “stereo‐chemically active” electron lone pair, and the coordination sphere is hemidirected. The supramolecular features in these complexes are guided and controlled by weak directional intermolecular interactions. The chains interact with each other through π–π stacking interactions creating a 3D framework. The structure of the title complex was optimized by density functional theory calculations. Calculated structural parameters and IR spectra for the title complex are in agreement with the crystal structure. The PbO nanoparticles were obtained by thermolysis of 1 at 180 °C with oleic acid as a surfactant. The average diameter of the nanoparticles was estimated by the Scherrer equation to be 23 nm. The morphology and size of the prepared PbO samples were further observed using SEM.  相似文献   

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A novel 1D polymeric lead(II) complex containing the first Pb2‐(μ‐N3)2 motif, [Pb(phen)(μ‐N3)(μ‐NO3)]n (phen = 1,10‐phenanthroline), has been synthesized and characterized. The single‐crystal X‐ray data showed the coordination number of Pb2+ ions to be eight (PbN4O4) with the Pb2+ ions having “stereo‐chemically active” electron lone pairs; the coordination sphere is hemidirected. The chains interact with each other via π‐π interactions to create a 3D framework.  相似文献   

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A novel 3D polymeric heteropolynuclear sodium(I) lead(II) complex containing different ligands, [NaPb(ClO4)(en)(NO2)2] was synthesized and characterized by elemental analysis and IR, and 1H‐, 13C‐, and 207Pb‐NMR spectroscopy. The single‐crystal X‐ray data of [NaPb(ClO4)(en)(NO2)2]n established that the complex is a three‐dimensional polymer, [(en)Pb(μ3‐ONO)2Na(μ3‐ONO)2Na(μ‐O2ClO2)Na]n. The Pb and Na atoms have four‐ and eight‐coordinate geometry, respectively. The lone pair of electrons at the PbII atom is ‘stereochemically active’.  相似文献   

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A new 3D hemidirected mixed‐ligand lead(II) coordination polymer with the ligand 1,2‐di(4‐pyridyl)ethane bpa) and the two metal coordinated anions nitrate and thiocyanate, [Pb2(bpa)2(SCN)3(NO3)]n ( 1 ), has been synthesized and characterized by CHN elemental analysis, IR‐, 1H‐ and 13C NMR spectroscopy. The single crystal X‐ray data of compound 1 show that the complex is a three‐dimensional coordination polymer with two different Pb atoms with stereoactive electron lone pairs and six‐ and five‐coordinate hemidirected geometries, respectively.  相似文献   

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A new mercury(II) complex of 1,2‐bis(4‐pyridyle)ethene (bpe) with anionic acetate and thiocyanate ligands has been synthesized and characterized by elemental analysis, IR, 1H NMR and 13C NMR spectroscopy. The single crystal X‐ray analysis shows that the complex is a two‐dimensional polymer with simultaneously bridging 1,2‐bis(4‐pyridyle)ethane, acetate and thiocyanate ligands and basic repeating dimeric [Hg2(μ‐bpe)(μ‐OAc)2(μ‐SCN)2] units. The two‐dimensional system forms a three‐dimensional network by packing via ππ stacking interactions.  相似文献   

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The title compound, [Cu2(C7H5O2)4(C7H10N2)2], is a crystallographically centrosymmetric binuclear complex, with Cu atoms [Cu...Cu = 2.6982 (4) Å] bridged by four benzoate ligands. Each of the Cu atoms in this bunuclear copper(II) acetate hydrate analogue is present in an approximately square‐pyramidal environment, with four O atoms in a plane and the pyridine N atom at the apical site. Selected geometric parameters are compared with values for related tetrabenzoate complexes of copper(II).  相似文献   

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The platinum‐platinum attraction and the spectroscopic properties of [Pt3(μ‐CO)3(CO)3] (n = 3–5) were studied at the PBE level. Theoretical calculations are in agreement with experimental geometries. The absorption spectra of these platinum complexes were calculated by the single excitation time‐dependent (TD) density functional method. All complexes showed MLCT transitions interrelated with the intertriangular complexes. The values obtained at the PBE level are in agreement with the experimental color range. © 2008 Wiley Periodicals, Inc. Int J Quantum Chem, 2009  相似文献   

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The two complexes of composition Cu2(OAc)4(phen)(H2O)2 ( 1 ) andCu2(OAc)4(phen)2(H2O) ( 2 ) have been synthesized and characterized by chemical analysis and IR and electronic spectroscopies. Compound 2 has the structure of a dimer with a phenanthroline molecule and two monodentate acetate groups coordinated to each copper atom and a water molecule as the only bridging ligand between them. Each copper atom has a distorted square‐planar pyramidal coordination, determined by two oxygen atoms at 1.94(3) and 1.959(3) Å, two nitrogen atoms at 2.023(4) Å and the oxygen atom of the bridging water molecule at 2.289(2) Å. The distance between the two copper atoms is of 4.29 Å and the angle Cu(1)‐O(3)‐Cu(1A) 139.2(2)°. The water molecule is involved in two intramolecular hydrogen bonds with non coordinated oxygen atoms. The distance between the molecules of phenanthroline is 3.75 Å. Magnetic and EPR results for Cu2(OAc)4(phen)(H2O)2 ( 1 ), Cu2(OAc)4(phen)2(H2O) ( 2 ), Cu2(OAc)4(bipy) ( 3 ) and Cu2(OAc)4(bipy)2(H2O)2 ( 4 ) have been analysed and compared. For 1 and 3 an antiferromagnetic dimer unit [Cu2(μ‐OAc)4] with 2J = ?325 and ?292 cm?1, respectively, and other two copper atoms without significant magnetic interaction are present. Triplet signals are detected in the EPR spectra. In 2 and 4 there is no practically magnetic exchange and the orthorhombic signals are observed in the EPR spectra.  相似文献   

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The two title dinuclear copper(II) complexes, [Cu2Cl4(C17H20Cl2N2)2], (I), and [Cu2Cl4(C19H22N2O4)2], (II), have similar coordination environments. In each complex, the asymmetric unit consists of one half‐molecule and the two copper centres are bridged by a pair of Cl atoms, resulting in complexes with centrosymmetric structures containing Cu(μ‐Cl)2Cu parallelogram cores; the Cu...Cu separations and Cu—Cl—Cu angles are 3.4285 (8) Å and 83.36 (3)°, respectively, for (I), and 3.565 (2) Å and 84.39 (7)° for (II). Each Cu atom is five‐coordinated and the coordination geometry around the Cu atom is best described as a distorted square‐pyramid with a τ value of 0.155 (3) for (I) and 0.092 (7) for (II). The apical Cu—Cl bond length is 2.852 (1) Å for (I) and 2.971 (2) Å for (II). The basal Cu—Cl and Cu—N average bonds lengths are 2.2673 (9) and 2.030 (2) Å, respectively, for (I), and 2.280 (2) and 2.038 (6) Å for (II). The molecules of (I) are linked by one C—H...Cl hydrogen bond into a complex [10] sheet. The molecules of (II) are linked by one C—H...Cl and one N—H...O hydrogen bond into a complex [100] sheet.  相似文献   

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A new nanostructured coordination polymer of divalent lead with the ligand 2,9‐dimethyl‐1,10‐phenanthroline (dmp), [Pb(dmp)(μ‐N3)(μ‐NO3)]n ( 1 ), was synthesized by sonochemical methods. The polymer was characterized by scanning electron microscopy, X‐ray powder diffraction, IR, 1H NMR, and 13C NMR spectroscopy, and elemental analyses. Compound 1 was structurally characterized by single‐crystal X‐ray diffraction. The single‐crystal analysis shows that the coordination number of PbII ions is seven, (PbN4O3) has a “stereo‐chemically active” electron lone pair, and the coordination sphere is hemidirected. The chains interact with each other through π–π stacking interactions to create a 3D framework. The structure of the title complex was optimized by density functional calculations. The calculated structural parameters and the IR spectrum of the title complex are in agreement with the crystal structure.  相似文献   

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The structure of [Co2(μ‐OH)2(μ‐OAc)(OAc)2(dipyam)2]AcO · EtOH ( 1 ) has been determined by single‐crystal X‐ray analysis. The cationic complex may be described as a “di(μ‐hydroxo)(μ‐acetato)dicobalt(III)” core with chelating 2, 2′‐dipyridylamine and monodentate acetate ligands. The coordination polyhedron around each cobalt atom is a distorted octahedral. The dimers are linked in the crystal by N‐H···Oionic AcO and C‐H···Omonodentate AcO hydrogen bonds. Spectroscopic data are also presented.  相似文献   

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