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1.
The complex of [Ag2(μ–L)2(μ–NO3)2]n, where L?=?2–methyl–5–(2–pyridyl)–1,3,4–oxadiazole, has been synthesized and characterized by single–crystal X–ray diffraction analysis. The crystals are in triclinic system with space group P–1. Complex [Ag2(μ–L)2(μ–NO3)2]n is a polymeric silver(I) complex bridged through the 1,3,4–oxadiazole rings and the nitrate ions, and the center Ag1(I) atoms have distorted trigonal bipyramidal geometries [AgN3O2].  相似文献   

2.

Abstract  

Two complexes [Cd2(dpe)3(H2O)8]·(dpe)·(hssal)2·(H2O)2 1, [Mn(dpe)2(Hpcmb)2·(H2O)2] 2, (dpe = trans-1,2-di(4-pyrindyl)ethylene; H2hssal = sulphosalicylic acid; H2pcmb = p-(carboxyl-methyloxy)-benzenecarboxylic acid) has been prepared, and was characterized by elemental analysis, FT-IR and single-crystal X-ray diffraction. Structure indicates in complex 1 that Cd(II) is a distorted octahedral coordination geometry. The hssal2− anions are localized between 2-D sheets {[Cd(dpe)2(H2O)4]2+(dpe)}n and {{[Cd(dpe)2(H2O)4]2+}n as count anions and bridge to further connect these 2-D sheets through hydrogen bond O–H···O to form 3-D structure. The complex 2 is a single molecule structure. In 2, Each Mn(II) atom is six-coordinated with a distorted octahedral coordination geometry. The single molecule units are extended into three-dimensional structure via π–π, hydrogen bonding interactions. The thermogravimetric behavior and luminescent property of complex 1 were investigated.  相似文献   

3.
Abstract These complexes have been characterized by X-ray crystallography, spectroscopic, and cyclic voltammetry. In 1, the copper(II) ion has a distorted square-pyramidal geometry with three nitrogen atoms of the dpa ligand and two oxygen atoms of the nitrate anions. The crystal structure of 2 shows that the copper(II) ions are bridged by tp anion to form a dinuclear complex, in which each copper(II) ion exhibits a distorted square-pyramid with three nitrogen atoms of the dpa ligand, water molecule, and the oxygen atom of the bridging tp ligand. Cyclic voltammetric data indicate that 1 undergoes irreversible one-electron oxidation to the CuIII and reversible one-electron reduction to the CuI, while 2 gives one reversible oxidation and two reversible and irreversible reduced processes. The electronic spectra and redox potentials of the complexes are influenced significantly by the anionic ligands. Graphical Abstract The reaction of [Cu(dpa)Cl2] with K(NO3)2 and Na2tp yields mononuclear and dinuclear copper(II) complexes [Cu(dpa)(NO3)2] (1) and [Cu2(dpa)2(H2O)2(μ-tp)](tp)·6H2O (2) (dpa = di-(2-picolyl)amine, tp = terephthalate).   相似文献   

4.
A new nicotinamide complex of Fe(II) cation was prepared by reaction between ferrous sulfate and nicotinamide in aqueous solution. The complex was characterized on the basis of elemental analysis, FT IR and UV–VIS spectroscopy, electrochemistry (cyclic voltammetry) and X–ray crystallography. The complex consists of the molecular composition of [Fe(nicotinamide)2(H2O)4]· [Fe(H2O)6]·(SO4)2·2H2O. The complex crystallizes in the monoclinic space group P 21/c [a = 12.862(3), b = 7.110(3), c = 16.382(3) Å; β = 95.79(2)°]. It has been proven that nicotinamide is coordinated to Fe(II) through the nitrogen atom of its heterocyclic ring. © 2006 WILEY‐VCH Verlag GmbH & Co. KGaA, Weinheim  相似文献   

5.
Two new transition metal complexes of [M(OH2)(HDPA)2]·3H2O (M=Mn(1); M=Co(2)) (H2DPA, 2,6-pyridine-dicarboxylic acid) have been prepared at room temperature from the reaction of MCl2·6H2O (M=Mn or Co) and H2DPA in the mixed solvent of H2O and EtOH in the presence of piperazine, and were characterized by X-ray analysis, elemental analysis. X-ray analysis reveals that the coordination geometries of Mn2+ and Co2+ are of octahedron and severely distorted square-based pyramid, respectively. Crystal data: [Mn(OH2)(HDPA)2]·3H2O (1), Mr=459.23, monoclinic, P2(1)/n, a=7.0056(3), b=(23.8125(12), c=10.7444(3) ?, β=99.834(2)°, Z=4, V=1766.28(13) ?3, R 1=0.0586, wR 2=0.1448 [I>2σ(I)]; Co(OH2)(HDPA)2]·3H2O (2), Mr=463.22, monoclinic, P2(1)/n, a=7.0014(2), b=23.8346(7), c=10.7212(4) ?, β=99.8540(10)°, Z=4, V=1762.71(10) ?3, R 1=0.0474, wR 2=0.1366 [I>2σ(I)].  相似文献   

6.

A co-crystal of cobalt(II) complexes, Co(AMTTO)2(CH3CN)2]2+(NO3)2. [Co(AMTTO)2(H2O)2]2+(NO3)2, compound (1) was isolated from the reaction of Co(NO3)2?6H2O and 4-amino-3-mercapto-6-methyl-5-oxo-1,2,4-triazine (AMTTO) in acetonitrile as solvent. Isolated crystals were characterized by elemental analyses, IR spectroscopy as well as X-ray diffraction studies. Crystal data for 1 at 95 K revealed a monoclinic space group P21/n, a?=?11.7903(5), b?=?12.1279(5), c?=?14.1443(6) Å, β?=?99.244(4)°, Z?=?2, R1?=?0.0339. Compound 1 consists of two co-crystallized Co(II) complexes [Co(AMTTO)2(CH3CN)2]2+ and [Co(AMTTO)2(H2O)2]2+ and four nitrate counter anions In both complexes, cobalt(II) ions are in an octahedral arrangement. Two S, N bidentate AMTTO ligands are coordinated to both Co(II) ions. The coordination sphere of Co1 is completed by two acetonitrile molecules, and these positions are occupied by water molecules for Co2.

Graphic Abstract

A co-crystal of cobalt(II) compound was isolated from the reaction of Co(NO3)2?6H2O and 4-amino-3-mercapto-6-methyl-5-oxo-1,2,4-triazine in acetonitrile as solvent.

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7.
The structure of three complexes of bivalent metals (cobalt, nickel, and cadmium) with anions of benzoic (HL 1) and 2-(acetylamino)-5-nitrobenzoic (HL 2) acids, namely, [Co21 (H2O)2(μ-C4H4N2)] n (I), [NiL2(H2O)5]L2 · 2H2O (II), and [Cd(μ-L 2)2(H2O)2] n · 2nH2O (III), is determined. In chainlike structure I, cobalt atoms are connected by bridging pyrazine molecules; structure II contains isolated complexes. In structure III, centrosymmetric (CdOCO)2 cycles and polymeric ribbons are formed due to the coordination of the carboxylate group of the L 2 ligand to two cadmium atoms.  相似文献   

8.
A new basic Nd3+ nitrate, [Nd6O(OH)8(H2O)14(NO3)6](NO3)2 · 2H2O (I), is isolated in the crystal form and studied. Compound I differs from the basic Ln nitrates containing [Ln 6O(OH)8] clusters in that it involves a larger number of water molecules. The incorporation of additional water molecules is accompanied by changes in the coordination environment of one of the three crystallographically independent Nd3+ cations. Two cations have coordination polyhedra in the form of a monocapped tetragonal antiprism with a coordination number of 9, and the third cation has a polyhedron in the form of a bicapped tetragonal antiprism with a coordination number of 10. Original Russian Text ? I.A. Charushnikova, C. Den Auwer, 2007, published in Kristallografiya, 2007, Vol. 52, No. 2, pp. 248–251.  相似文献   

9.

Abstract  

The new complex with flexible heterocyclic carboxylate ligand, [Ba(HL)2(H2O)3]·H2O (H2L = 1-(4-Hydroxyphenyl)-5-thioacetatetetrazole), were synthesized and structurally determined by X-ray diffraction analysis. The complex belongs to the monoclinic system, space group C2/c. The center Ba(II) is nine-coordinated by six carboxylate oxygen atoms from four HL-ligands and three water molecules in a distorted monocapped square trans-prism geometry. The ligand serves as a bridge to link two adjacent Ba(II) atoms into a chain structure which are further assembled into the final three-dimensional supramolecular architecture with microporous open channel via hydrogen bonds.  相似文献   

10.
Cs[VO2(NO3)2] (I), MoO2(NO3)2 (II), and Cs[MoO2(NO3)3] (III) complexes have been obtained by crystallization from nitric solutions and studied by single-crystal X-ray diffraction. Complexes I and II contain infinite zigzag chains of similar compositions, [VO2(NO3)2] and [MoO2(NO3)2], in which V and Mo atoms form, respectively, trigonal- and pentagonal-bipyramidal polyhedra. Each of these polyhedrons also contains one terminal and two bridge O atoms and two terminal NO3 groups which are monodentate and bidentate in complexes I and II, respectively. Complex III has an island structure and consists of Cs+ cations and [MoO2(NO3)3] anions, in which the Mo atom is surrounded by one bidentate NO3 group and two monodentate NO3 groups and two terminal O atoms in the cis-positions; oxygen atoms form a polyhedron in the form of distorted octahedron. According to the ab initio calculation of isolated MoO2(NO3)2 molecules in the gas phase and solution, the coordination environment of the Mo atom, similarly to the Cr(VI) atom in CrO2(NO3)2, is formed by two bidentate nitrate groups and two terminal O atoms (polyhedron- twisted trigonal prism).  相似文献   

11.
Two new Cr(III) complexes, [Cr(bpb)(H2O)(OH)]·3H2O (1) and [Cr(bpb)(H2O)(N3)]·H2O (2) have been synthesized and structurally characterized. Both complexes were unexpectedly obtained as single crystals during the reactions of [Cr(bpb)(CN)2] or [Cr(bpb)(N3)2] with [Ni(L)](ClO4)2 (L = 3,10-dimethyl-1,3,6,8,10,12-hexaazacyclotetradecane) or MX2·nH2O (M = Cu, Ni and Mn, X = Cl and ClO4 ). Complex 1 crystallizes in the triclinic system, space group P-1, formula CrC18H21N4O7 with a = 7.1543(17) ?, b = 12.420(3) ?, c = 12.955(3) ?, α = 115.021(5)°, β = 95.544(5)°, and γ = 101.575(5)°. Complex 2 crystallizes in the monoclinic system, space group P21/c, formula CrC18H16N7O4 with a = 11.7171(9) ?, b = 9.4999(7) ?, c = 16.8799(13) ?, and β = 97.449(2)°. Both complexes exhibit distorted octahedral coordination environment with four nitrogen atoms of bpb2− situated at the equatorial plane (Cr–N bond distances range from 1.961(3) to 2.1088(15) ?), and the remaining two trans-positions occupied by terminal ligands H2O/HO and H2O/N3 in 1 and 2, respectively. It is noteworthy that a hydrogen-bonded folded ladder-like structure involving twelve O atoms in 1 and a chair-like hexagonal hydrogen-bonded cluster containing six O atoms are formed.  相似文献   

12.

Synthesis and structural characterization of two heterodinuclear ZnII-LnIII complexes with the formula [ZnLn(HL)(µ-OAc)(NO3)2(H2O)x(MeOH)1-x]NO3 · n H2O · n MeOH [Ln?=?Pr (1), Nd (2)] and the crystal and molecular structure of [ZnNd(HL)(µ-OAc)(NO3)2(H2O)] [ZnNd(HL)(OAc)(NO3)2(H2O)](NO3)2 · n H2O · n MeOH (3) are reported. The asymmetrical compartmental ligand (E)-2-(1-(2-((2-hydroxy-3-methoxybenzylidene)amino)-ethyl)imidazolidin-2-yl)-6-methoxyphenol (H2L) is formed from N1,N3-bis(3-methoxysalicylidene)diethylenetriamine (H2valdien) through intramolecular aminal formation, resulting in a peripheral imidazoline ring. The structures of 13 were revealed by X-ray crystallography. The smaller ZnII ion occupies the inner N2O2 compartment of the ligand, whereas the larger and more oxophilic LnIII ions are found in the outer O2O2’ site.

Graphic Abstract

Synthesis and structural characterization of two heterodinuclear ZnII-LnIII complexes (Ln?=?Pr, Nd) bearing an asymmetrical compartmental ligand formed in situ from N1,N3-bis(3-methoxysalicylidene)diethylenetriamine (H2valdien) through intramolecular aminal formation are reported.

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13.
A new complex compound. [Cu2Br3(C7H6N2)5]Br·4H2O, has been synthesized and its crystal structure investigated by single-crystal X-ray methods. The crystals are isostructural with those of the [Cu2Cl3(C7H6N2)5]Cl·4H2O salt. They are orthorombic, space group Pnma with 4 formula units in a cell of dimensions:a+19.923(1),b+17.555(2),c+12.0523(4)Å. The structure was refined by full-matrix least-squares to giveR+0.047 andR w+0.053 for 3569 intensities above 3σ(I). As in the chloride compound, the complex cation consists of pairs of distorted trigonal bipyramidal Cu(II) centers which share an edge by two equatorial bromide ions. The Cu...Cu nonbonding distance in the complex in 3.4894(7)Å. The two Cu?Br?Cu bridges are not equivalent and their geometry is slightly different from that in the chloride complex. Comparison of the investigated structure to other binulear bis(μ-halide) bridged copper(II) complexes of similar structure has been made.  相似文献   

14.
Abstract  The title compound 2-(2,3,4-trimethoxy-6-methylbenzylideneamino)phenol (C17H19NO4, M r = 301.33) was synthesised and characterized by elemental analysis, IR spectra and single crystal X-ray diffraction. The crystal belongs to monoclinic, space group P21/c, with a = 10.4458(14), b = 8.3870(10), c = 17.780(2) ?, β = 91.102(2)°, V = 1557.4(3) ?3, Z = 4, D c = 1.285 g/cm3, λ = 0.71073 ?, μ(Mo ) = 0.092 mm−1, F(000) = 640. The final refinement gave R = 0.0452, wR(F 2) = 0.1065 for 2,743 observed reflections with I > 2σ(I). X-ray diffraction analysis reveals that the molecule adopts an E configuration at the C=N functional bond. The dihedral angle between the two phenyl rings is 38.3(3)°. The crystal structure is stabilized by C–H···O, O–H···O and O–H···N hydrogen bonds and π–π stacking interactions. Graphical Abstract  The title compound 2-(2,3,4-trimethoxy-6-methylbenzylideneamino)phenol (C17H19NO4, M r = 301.33) was synthesised and characterized by elemental analysis, IR spectra and single crystal X-ray diffraction. The crystal belongs to monoclinic, space group P21/c, with a = 10.4458(14), b = 8.387(1), c = 17.780(2) ?, β = 91.102(2)°, V = 1557.4(3) ?3, Z = 4, D c = 1.285 g/cm3, λ = 0.71073 ?, μ(Mo ) = 0.092 mm−1, F(000) = 640. The final refinement gave R = 0.0452, wR(F 2) = 0.1065 for 2,743 observed reflections with I > 2σ(I). X-ray diffraction analysis reveals that the molecule adopts an E configuration at the C=N functional bond. The dihedral angle between the two phenyl rings is 38.3(3)°. The crystal structure is stabilized by C–H···O and O–H···O hydrogen bonds and π–π stacking interactions.   相似文献   

15.
A new manganese(II) pyrophosphate, Mn4(P2O7)2·10H2O, has been synthesized and characterized by single-crystal X-ray diffraction [orthorhombic space group Pnma, with unit cell parameters of a=9.3288(3) ?, b=25.9532(9) ?, c=8.4783(3) ?; Z=4]. All the pyrophosphate anions show non-linear P–O–P bonds with an average angle of 128.60°. The framework of this new pyrophosphate is made up of packed layers of MnO6 octahedra connected by double-tetrahedra P2O7 groups and a layer of Mn(H2O)6 units. The [P2O7]4− anions adopt a bent, near-staggered conformation. The absence of coincidences for the majority of the IR and Raman bands is in accord with the centrosymmetric structure of the material. The vibrational spectra have been interpreted in part on the basis of factor group effects. The structural changes occurring during heating have been investigated by TG-ATD. When Mn4(P2O7)2 .10H2O is gradually heated, it decomposes into an intermediate hydrated salt at 96°C and then to anhydrous Mn2P2O7 at 325°C. This thermal behaviour is different from that of Zn4(P2O7)2·10H2O. The crystal structure of the new managenese(II) pyrophosphate is compared with the known structures of Zn4(P2O7)2·10H2O, Mn2P2O7·2H2O and anhydrous Mn2P2O7. The adsorption and desorption isotherms of Mn4(P2O7)2·10H2O, Zn4(P2O7)2·10H2O and MnKHP2O7·2H2O have been investigated by BET measurements and the results show that the capacity for N2 sorption of the Mn(II) salt is two times lower than is that of the Zn(II) isotype and two or three times higher than is that of MnKHP2O7·2H2O.  相似文献   

16.

Abstract  

A novel 3,4,7,8-tetrachloro-1,10-phenanthroline (Cl4phen) Zn(II) complex has been synthesized. The complex, [Zn(Cl4phen)2(H2O)2](NO3)2·CH3CH2OH (1), has been identified and characterized by single crystal X-ray diffraction, elemental analysis, FT-IR, thermogravimetric analysis and photoluminescence studies. Single crystal X-ray diffraction analysis reveals that complex (1) belongs to the monoclinic system, space group P2(1)/c, a = 10.061(2) Å, b = 18.924(4) Å, c = 18.189(4) Å, β = 100.94(3)°, and Z = 4. Complex (1) consists of cationic species [Zn(Cl4phen)2(H2O)2]2+, NO3 and CH3CH2OH. The zinc atom displays a distorted cis-N4O2 octahedral geometry. Via extended Zn–O–H···O–N–O···H–O–Zn bridge, every mononuclear unit is linked with other ones to form one-dimensional (1D) infinite chain of hydrogen bond system. Three-dimensional (3D) polymeric network arrangement was built via weak C–H···O and π-stacking interactions between Cl4phen moieties. A solvent-dependency effect of complex (1) was observed in spectroscopic properties.  相似文献   

17.
The compound [UO2(NO3)2(H2O)2] · 2C12H18O was synthesized and studied by IR spectroscopy and X-ray diffraction. The structure consists of the neutral island groups [UO2(NO3)2(H2O)2], which belong to the crystal-chemical group AB 01 2 M 1 2 (A = UO2 2+, B 01 = NO3, M 1 = H2O) of uranyl complexes, and 1-adamantyl methyl ketone molecules. The characteristic features of the association of the complexes [UO2(NO3)2(H2O)2] and 1-adamantyl methyl ketone molecules in the crystal structure via hydrogen bonds are considered with the use of Voronoi-Dirichlet polyhedra.  相似文献   

18.
Two transition metal(II) complexes of betaine (Me3N+CH2COO, designated as BET) and pyridine betaine (C5H5N+CH2COO, pyBET) have been prepared and investigated by X-ray crystallography and infrared spectroscopy. [Ni(BET)2(H2O)4] (NO3)2 (1), (R F=0.054 for 2518 observed MoK data) comprises slightly distorted octahedral [Ni(BET)2(H2O)4]2+ cations in which the Ni(II) atom is centrosymmetrically coordinated by four aqua ligands and twotrans-related unidentate BET ligands, and the uncoordinated carboxy oxygens form intramolecular hydrogen bonds with the aqua ligands. [Co(pyBET)4(H2O)2]·2[Co(pyBET)Cl3] (2) (R F=0.029 for 4696 observed data) consists of discrete octahedral [Co(pyBET)4(H2O)2]2+ cations and tetrahedral [Co(pyBET)Cl3] anions. In the centrosymmetric cation each of the twotrans-related aqua ligands form a pair of intramolecular hydrogen bonds with the uncoordinated oxygen atoms of two unidentate pyBET ligands. In the anion the cobalt atom is coordinated by one unidentate pyBET ligand and three chloro ligands.  相似文献   

19.
The crystal structure of the [La(DMSO)6(H2O)PW12O40] · C2H5OH complex (I) (where DMSO is dimethyl sulfoxide) is determined by X-ray diffraction analysis. The coordination polyhedron of the La atom is a distorted tricapped trigonal prism in which two cap sites are occupied by oxygen atoms of the heteropolyanions. For these atoms, the La-O distances [2.760(9) and 2.801(9) Å] are considerably longer than the other distances [ranging from 2.441(10) to 2.569(10) Å] in the environment of the La atom. __________ Translated from Kristallografiya, Vol. 47, No. 6, 2002, pp. 1039–1041. Original Russian Text Copyright ? 2002 by Grigoriev, Shirokova, Fedoseev, Den Auwer.  相似文献   

20.
The crystal structure of new complexes of praseodymium(III) and ytterbium(III) (elements from the initial and final parts of the lanthanide series), namely, [Pr(NO3)3 (Terpy)((CH3)2CO)] (I) and [Yb(NO3)2(Terpy)(H2O)2]NO3 · 2H2O (II), is investigated. The structure of compound I consists of [Pr(NO3)3(Terpy)((CH3)2CO)] neutral complexes. The coordination number of the praseodymium atom is 10. The coordination polyhedron of the praseodymium atom can be described as a distorted bicapped tetragonal antiprism. The structure of compound II is composed of [Yb(NO3)2(Terpy)(H2O)2]+ cationic complexes, nitrate anions, and molecules of crystallization water. The structural components are joined together via a three-dimensional system of hydrogen bonds. The coordination polyhedron of the ytterbium atom can be represented as a distorted tricapped trigonal prism. The coordination number of the ytterbium atom is 9.  相似文献   

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