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1.
[Eu(ABA)(phen) 2(H 2O) 3](ClO 4) 3·3phen·4.5H 2O (1) and [Eu(Val)(phen) 2(H 2O) 3](ClO 4) 3·3phen·2H 2O (2) are two new europium complexes with amino acids and 1,10-phenanthroline (phen=1,10-phenanthroline, ABA=-amino butyl acid, Val=
-valine). Their crystal structures were measured by X-ray crystallography. Europium atoms in both complexes are nine-coordinated with bidentate 1,10-phenanthroline and carboxylate anion of amino acids, and water molecules. In the solid state, 1 and 2 have a structure involving aromatic stacking of the coordinated and non-coordinated 1,10-phenanthroline and the oxygen atoms of non-coordinated perchlorate anions being H-bond acceptors connect [Eu(ABA)(phen) 2(H 2O) 3] 3+·3phen·4.5H 2O or [Eu(Val)(phen) 2(H 2O) 3] 3+·3phen·2H 2O in their structures. In their interactions, several C–HO bonds play an important role. Owing to their different amino acid ligands and the number of lattice water molecules, there is some difference in their hydrogen bond patterns in 1 and 2. The side chain of
-valine is involved in the formation of C–HO bonds. Hydrogen bond and π–π interactions determine the supramolecular formation of three-dimensional net works of both complexes. 相似文献
2.
A series of chromium(III) complexes [Cr(bipy)(HC 2O 4) 2]Cl·3H 2O (1), [Cr(phen)(HC 2O 4) 2]Cl·3H 2O (2), [Cr(phen) 2(C 2O 4)]ClO 4 (3), [Cr 2(bipy) 4(C 2O 4)](SO 4)·(bipy) 0.5·H 2O (4) and [Mn(phen) 2(H 2O) 2] 2[Cr(phen)(C 2O 4) 2] 3ClO 4·14H 2O (5) were synthesized (bipy=4,4′-bipyridine, phen=1,10-phenanthroline), while the crystal structures of 1 and 3–5 have been determined by X-ray analysis. 1 and 3 are mononuclear complexes, 4 contains binuclear chromium(III) ions and 5 is a 3D supromolecule formed by complicated hydrogen bonding. 1–3 are potential molecular bricks of chromium(III) building blocks for synthesis heterometallic complexes. When we use these molecular bricks as ligands to react with other metal salts, unexpected complexes 4 and 5 are isolated in water solution. The synthesis conditions and reaction results are also discussed. 相似文献
3.
The potassium salt of o-aminophenol-N,N,O-triacetic acid (APTA) and KMnL·H 2O, KCoL·3H 2O, KNiL·3H 2O, KZnL·3ZH 2O, Co(CoL) 2·7H 2O and Ni(NiL) 2·8H 2O(L 3−:anion of APTA) have been synthesized and characterized by elementary analysis, thermogravimetric analysis, molar conductance, IR spectra, magnetic measurements and electronic spectra. The coordination environments of these metal ions have been discussed on the basis of these studies. The single crystal structure of cobalt(II)-APTA has been determined as CoL·0.5Co(H 2O) 6·4H 2O, which contains two types of cobalt(II). One type of cobalt(II) is coordinated with six water molecules to form Co(H 2O) 62+, the other is chelated by APTA to form a distorted octahedron and linked into an infinite chain anion [COC 6H 4(OCH 2COO)N(CH 2COO) 2−] n, in which each cobalt(II) atom is linked with neighbouring cobalt(II) atoms through two carboxylate oxygen atoms of the phenoxyacetate group. Water molecules occupy interstices in the structure. 相似文献
4.
3,6,9-trioxaundecanedioic acid (3,6,9-tddaH 2) reacts with Mn(CH 3CO 2) 2·4H 2O in ethanol to give [Mn(3,6,9-tdda)]·H 2O (1). Recrystallization of 1 from methanol gives crystals of [Mn(3,6,9-tdda) (H 2O) 2]·2H 2O (2). Complex 1 reacts with an ethanolic solution of 1,10-phenanthroline (phen) to give {[Mn(3,6,9-tdda)(phen) 2]·3H 2O·EtOH} n (3). All of the complexes are extremely water soluble. Complexes 2 and 3 were structurally characterised. The manganese(II) ion in 2 is seven coordinate, with an approximately pentagonal bipyramidal O 7 coordination sphere. The axial donors are water molecules and the pentagonal plane is occupied by the diacid, acting as a pentadentate ligand through the three ethereal oxygens and one oxygen atom from each of the carboxylate functions. In complex 3 the manganese(II) ion is six-coordinate, being bound to two bidentate phenanthroline ligands and to the carboxylate oxygen atoms from two symmetry related diacids which are coordinated in a cis fashion. The structure consists of polymeric chains, with diacid ligands bridging the manganese ions. There is π-π stacking of pairs of phenanthroline ligands on adjacent chains, running along both the z and y directions. 相似文献
5.
The solid–liquid equilibria of the ternary system H 2O–Fe(NO 3) 3–Co(NO 3) 2 were studied by using a synthetic method based on conductivity measurements. Two isotherms were established at 0 and 15 °C, and the stable solid phases which appear are the iron nitrate nonahydrate (Fe(NO3)3·9H2O), the iron nitrate hexahydrate (Fe(NO3)3·6H2O), the cobalt nitrate hexahydrate (Co(NO3)2·6H2O) and the cobalt nitrate trihydrate (Co(NO3)2·3H2O). 相似文献
6.
Two new compounds, [Ni(en) 2]{[Ni(en) 2] 2[Mo VI6Mo V2V IV8O 40(SiO 4)]}[(NH 2) 2(C 2H 4) 2NH]·2H 2O(1) and [Ni(en) 2]{[Ni(en) 2] 2[Mo VI5Mo V3V IV8O 40(VO 4)]}(en)·H 2O(2)(en=ethylenediamine), have been hydrothermally synthesized and characterized by elemental analysis, infrared(IR), X-ray photoelectron spectroscopy(XPS), electron spin-resonance(ESR) and thermogravimetric(TG) analysis and single-crystal X-ray diffraction(XRD) analysis. Both the compounds exhibit a 1D chain composed of bi-supporting tetra-capped Keggin clusters and nickle coordination fragments. The 1D chains are further assembled into a 3D supramolecular network with different packing modes via hydrogen bonds. The magnetic susceptibility of compound 1 demonstrates the presence of antiferromagnetic interactions. 相似文献
7.
A novel manganese complex, [Mn(phen) 2(H 2O) 2](sac) 2·H 2O, was synthesized by the reaction of [Mn(sac) 2(H 2O) 4]·2H 2O with 1,10-phenantroline in aqueous solution and characterized by elemental analysis, IR spectral evidence, magnetic measurements, thermal analysis and single crystal X-ray diffraction. The compound crystallizes in triclinic system, space group P-1, with Z=2. The saccharinate ions do not coordinate the central metal, instead are present as the complementary anions. In the complex cation, Mn(II) is coordinated by two phen and two aqua ligands, and exhibits a distorted octahedral coordination with a high-spin configuration. The presence of lattice and coordinate water molecules are also confirmed by thermal analysis and IR spectroscopy. 相似文献
8.
The infrared spectra of isotopically dilute (matrix-isolated HDO molecules) isostructural compounds M(HCOO) 2·2H 2O (M=Mn,Fe,Co,Ni,Zn,Cu) are presented and discussed in the region of the OD stretching modes. According to the structural data the compounds under study are divided into two groups: in M(HCOO) 2·2H 2O (M=Mn,Ni,Zn) the H 2O(1) molecules form stronger hydrogen bonds as compared to H 2O(2); in M(HCOO) 2·2H 2O (M=Fe,Co,Cu) the H 2O(2) molecules form stronger hydrogen bonds as compared to the H 2O(1) molecules. The influence of the metal–water interactions (synergetic effect) and the unit-cell volumes (repulsion potential of the lattice) on the hydrogen bond strength within the isostructural series is discussed. The wavenumbers of the uncoupled OD stretching modes of the HDO molecules influenced by guest ions (Cu 2+ ions matrix-isolated in M(HCOO) 2·2H 2O and M 2+ ions matrix-isolated in Cu(HCOO) 2·2H 2O) are presented and commented. For example, the analysis of the spectra reveals that when Cu 2+ ions are included in the structure of M(HCOO) 2·2H 2O the hydrogen bonds of the type M–OH 2OCHO–Cu are considerably weaker as compared to those of the same type formed when M 2+ ions are included in the structure of Cu(HCOO) 2·2H 2O if the cations remain unchanged. 相似文献
9.
A new family of heteropolytungstate complexes (NH 4) 21[Ln(H 2O) 5{Ni(H 2O)} 2As 4W 40O 140]· xH 2O(Ln=Y, Ce, Pr, Nd, Sm, Eu, Gd) were prepared by the reaction of Na 27[NaAs 4W 40O 140]·60H 2O with NiCl 2·6H 2O and Ln(NO 3) 3· xH 2O at pH≈4.5. The crystal structures of (NH 4) 21[Gd(H 2O) 5{Ni(H 2O)} 2As 4W 40O 140]·51H 2O was determined by X-ray diffraction analysis and element analysis. The compound crystallizes in the monoclinic space group P2 1/ n with a=19.754(3), b=24.298(4), c=39.350(6) Å, β=100.612(3)°, V=18564(5) Å 3, Z=2, R1( wR2)=0.0544(0.0691). The central site S1 and two opposite sites S2 of the big cyclic ligand [As 4W 40O 140] 28− are occupied by one Ln 3+and two Ni 2+, respectively, each site supply four O d coordinating to metal ion, another one water molecule and other five water molecules coordinate, respectively, to Ni 2+and Ln 3+. Polyanion [Ln(H 2O) 5{Ni(H 2O)} 2As 4W 40O 140] 21− has C2v symmetry. IR and UV–vis spectra of [NaAs 4W 40O 140] 27− of the title compounds are discussed. 相似文献
10.
A new sodium cobalt carbonate hydroxide hydrate, Na 2Co 8(CO 3) 6(OH) 6·6H 2O, has been prepared at room temperature by treatment of Co(OH)NO 3·H 2O with a concentrated aqueous solution of NaHCO 3. X-Ray powder diffractometry and the results of the chemical analyses show that the compound is isotypical to Na 2Ni 8(CO 3) 6(OH) 6·6H 2O —kambaldaite, a unique mineral with no known synthetic or natural analogues. 相似文献
11.
Five new complexes of composition [Cu(dpt)Ni(CN) 4] (1) (dpt=dipropylenetriamine), [Cu(dien)Ni(CN) 4]·2H 2O (2) (dien=diethylenetriamine), [Cu( N, N′-dimeen)Ni(CN) 4]·H 2O (3) ( N, N′-dimeen= N, N′-dimethylethylenediamine), [Cu( N, N-dimeen)Ni(CN) 4]·H 2O (4) ( N, N-dimeen= N, N-dimethylethylenediamine) and [Cu(trimeen)Ni(CN) 4] (5) (trimeen= N, N, N′-trimethylethylenediamine) have been obtained by the reactions of the mixture of Cu(ClO 4) 2·6H 2O, appropriate amine and K 2[Ni(CN) 4] in water and have been characterized by IR and UV–Vis spectroscopies and magnetic measurements. The crystal structure of [Cu(dpt)Ni(CN) 4] (1) has been determined by single-crystal X-ray analysis. The structure of 1 consists of a one-dimensional polymeric chain ---Cu(dpt)---NC---Ni(CN) 2---CN---Cu(dpt)--- in which the Cu(II) and Ni(II) atoms are linked by CN groups. The nickel atom is four coordinate with four cyanide-carbon atoms (two cyano groups are terminal and two cyano groups (in cis fashion) are bridged) in a square-planar arrangement and the copper atom is five coordinate with two cyanide-nitrogen and three dpt-nitrogen atoms, in a distorted square-pyramidal arrangement. The temperature dependence of magnetic susceptibility (2–300 K) was measured for compound 1. The magnetic investigation showed the presence of a very weak antiferromagnetic interaction ( J=−0.16 cm −1) between the copper atoms within each chain through the diamagnetic Ni(CN) 4 2− ions. 相似文献
12.
Hydrated strontium borate, SrB 4O 7·3H 2O, has been synthesized and characterized by XRD, FT-IR, DTA-TG and chemical analysis. The molar enthalpy of solution of SrB 4O 7·3H 2O in 1 mol dm −3 HCl(aq) was measured to be (21.15 ± 0.29) kJ mol −1. With incorporation of the previously determined enthalpies of solution of Sr(OH) 2·8H 2O(s) in [HCl(aq) + H 3BO 3(aq)] and H 3BO 3 in HCl(aq), and the enthalpies of formation of H 2O(l), Sr(OH) 2·8H 2O(s) and H 3BO 3(s), the enthalpy of formation of SrB 4O 7·3H 2O was found to be −(4286.7 ± 3.3) kJ mol −1. 相似文献
13.
Paramagnetic species formed during the vacuum thermal decomposition of Mg- and K-sulfites and -thiosulfates are identified by EPR. During the thermal decomposition of the magnesium compounds, SO−2 is observed as a radical stabilized at the surface of the solid residue. In the case of K2SO3, another SO−2 radical species is observed; this SO−2 is formed inside the crystalline lattice of K2SO3 as a result of dislocations during the thermal treatment. If K2SO3 results from the “in suit” decomposition of K2S2O3 1/3H2O, we observe moreover that the decomposition of the thiosulfate is accompanied with the intermediary formation of SO−2 and S−??? radicals. The combined thermal analysis techniques of thermogravimetry and EPR show that K2Mg(S2O3)2. 6H2O decompose in the same manner as an equimolar mixture of K2S2O3·1/3H2O and MgS2O3·6H2O. 相似文献
14.
Three new aminodiphosphonates, namely M(phen)(AEDPH 3) 2·4H 2O (M = Zn, (1); Ni, (2)) and Cu(phen)(AEDPH 3) 2·H 2O (4), in addition to the previously reported Co(phen)(AEDPH 3) 2·4H 2O (3), Cu(2,2′-bipy)(H 2O)(HEDPH 2)·2H 2O (5), and Cu(phen)(H 2O)(HEDPH 2)·2H 2O (6) (AEDPH 4 = 1-aminoethylidenediphosphonic acid, HEDPH 4 = 1-hydroxyethylidenediphosphonic acid, phen = 1,10-phenanthroline and 2,2′-bipy = 2,2′-bipyridyl), have been synthesized and characterized. These compounds are all synthesized at the similar condition (80 °C), whereas they illustrate different frameworks. Compounds 1, 2 and 3 are isomorphous, which contain two same chelate and one six-coordinated metal ion, and display a three-dimensional (3D) supramolecular structure through hydrogen bonds and π–π stacking interactions. Compound 4 contains a chelate and a monodentate , while the Cu ion is five-coordinated. The coordination model of Cu 2+ in 4 is similar to that of 5 and 6. Comparing with four aminoethylidenediphosphonates, the difference of their structures is directed to the coordination model of the metal ions, while the three copper(II) diphosphonates illustrate different structures based on the deprotonized degree of the corresponding diphosphonic acids. 相似文献
15.
Two polymeric complexes, [Cu 2(btec)(phen) 2] n·(H 2O) n (1) and [Cd 4(btec) 2(phen) 4(H 2O) 4] n (2) (H 4btec=1,2,4,5-benzenetetracarboxylic acid; PHEN=1,10-phenanthroline), were synthesized by solvothermal reactions at 140 °C. Both complex 1 and 2 possess infinite double-chain structures, in which each Cu(II) center has a tetrahedral configuration and the Cd(II) centers adopt triangular prismatic and square-based pyramidal configurations simultaneously. The inter-chain face to face π–π interactions among the aromatic rings of phen and the hydrogen bond interactions between aqua molecules and carboxyl O atoms result in 3-D networks in the two complexes. The ESR spectra study of complex 1 shows that there is negligibly small long-range super-exchange interactions between the Cu(II) atoms via benzenecarboxylate bridging. 相似文献
16.
[Co(η 2-CO 3)(NH 3) 4](NO 3)·0.5H 2O and [(NH 3) 3Co(μ-OH) 2(μ-CO 3)Co(NH 3) 3][NO 3] 2·H 2O were prepared by prolonged aerial oxidation of a solution of Co(NO 3) 2·6H 2O and ammonium carbonate in aqueous ammonia. The formation of these side products highlights the richness of the chemistry of these systems and the possibility of by products if methods are not strictly adhered to. The X-ray crystal structures of [Co(η 2-CO 3)(NH 3) 4][NO 3]·0.5H 2O and [(NH 3) 3Co(μ-OH) 2(μ-CO 3)Co(NH 3) 3][NO 3] 2·H 2O reveal a monomeric octahedral cobalt center with η 2-bound CO 32− in the former, while the latter consists of a dimeric array where the two cobalt centers are bridged by two OH − and one μ 2-CO 32− groups with three terminal NH 3 ligands for each Co center. In both complexes extensive hydrogen bonding interactions are evident. 相似文献
17.
Synthesis of two Ni(II) complexes with furfural S-methylthiosemicarbazone (HL) of the formula [Ni(HL) 2(H 2O) 2](ClO 4) 2 (A) and [Ni(HL) 2(ClO 4) 2] (B) are reported. Compound A was obtained from an ethanolic solution of Ni(ClO 4) 2·6H 2O and HL, whilst compound B was produced by heating compound A to 378 K. An X-ray analysis of the complex A showed that it has a trans(H 2O)- trans(HL) octahedral configuration in which HL behaves as a bidentate (NN) ligand. On the basis of the IR and electronic spectra as well as the magnetism, it was found that the compound B has also an octahedral configuration in which, HL and ClO 4 groups, are coordinated. 相似文献
18.
Two mononuclear Ru II complexes of polypyridyl ligands, cis-[Ru(bpy) 2(4,4′-bpy)Cl](PF 6)·H 2O (1) and cis-[Ru(phen) 2(CH 3CN) 2](PF 6) 2 (2) (bpy=2,2′-bipyridyl, 4,4′-bpy=4,4′-bipyridyl, and PHEN=1,10-phenanthroline), have been synthesized and characterized by elemental analyses, IR and UV–vis spectra. The crystal structures of both complexes have been determined by X-ray diffraction, indicating that each Ru II center is hexa-coordinated (RuN 5Cl for 1 and RuN 6 for 2) and takes a distorted octahedral geometry. The favored feature of both complexes is that they are quite useful complex precursors for further constructing new functional architectures. 相似文献
19.
Two novel hydrogen maleato (HL) bridged Cu(II) complexes ∞1[Cu(phen)Cl(HL) 2/2] 1 and ∞1[Cu(phen)(NO 3)(HL) 2/2] 2 were obtained from reactions of 1,10-phenanthroline, maleic acid with CuCl 2·2H 2O and Cu(NO 3) 2·3H 2O, respectively, in CH 3OH/H 2O (1:1 v/v) at pH=2.0 and the crystal structures were determined by single crystal X-ray diffraction methods. Both complexes crystallize isostructurally in the monoclinic space group P2 1/ n with cell dimensions: 1 a=8.639(2) Å, b=15.614(3) Å, c=11.326(2) Å, β=94.67(3)°, Z=4, Dcalc=1.720 g/cm 3 and 2 a=8.544(1) Å, b=15.517(2) Å, c=12.160(1) Å, β=90.84(8)°, Z=4, Dcalc=1.734 g/cm 3. In both complexes, the square pyramidally coordinated Cu atoms are bridged by hydrogen maleato ligands into 1D chains with the coordinating phen ligands parallel on one side. Interdigitation of the chelating phen ligands of two neighbouring chains via π–π stacking interactions forms supramolecular double chains, which are then arranged in the crystal structures according to pseudo 1D close packing patterns. Both complexes exhibit similar paramagnetic behavior obeying Curie–Weiss laws χ m( T−θ)=0.414 cm 3 mol −1 K with the Weiss constants θ=−1.45, −1.0 K for 1 and 2, respectively. 相似文献
20.
The reaction of an ethanolic solution of copper(II) pyridinecarboxylates CuX 2· nH 2O (where X is nicotinate (nic) ( n=0) or isonicotinate (isonic) ( n=4)) with ethylenediamine (en) in a molar ratio of 1:2 lead to the isolation of solid tetragonally distorted octahedral complexes of the type [Cu(en) 2(H 2O) 2]X 2· nH 2O ( n=1 for nic; n=0 for isonic). The analogous reaction of CuX 2· nH 2O with diethylenetriamine (dien) in a molar ratio of 1:1 leads to the formation of square-pyramidal pentacoordinated complexes of the type [CuX(dien)(H 2O)]X. On the other hand, the reaction of equimolar quantities of copper(II) nitrate and dien with nicotinate anions (equimolar quantities of pyridinecarboxylic acid and NaOH) in ethanolic solutions gives a solid monomeric complex [Cu(nic)(NO 3)dien)(H 2O)]·H 2O in which the coordination polyhedron around the Cu(II) atom is a (4+1+1) distorted tetragonal bipyramid. Based on the molecular structure the electronic and IR spectra are discussed. Moreover, the results of the quantitative determination of antimicrobial activity of the isonic complexes [Cu(isonic) 2(H 2O) 4], [Cu(en) 2(H 2O) 2](isonic) 2, [Cu(isonic)(dien)(H 2O)](isonic), as well as isonicotinic acid, ethylenediamine and diethylenetriamine alone are discussed. 相似文献
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