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1.
The title complexes, K[GaIII(Cydta)] · 2H2O(Cydta = trans-1,2-cyclohexanediaminetetraacetic acid) and K[GaIII(Pdta)] · 3H2O (Pdta = propylenediaminetetraacetic acid), were prepared, and their structures were studied by IR spectra, elemental analyses, NMR spectra, and single-crystal X-ray diffraction techniques. In the K[GaIII(Cydta)] · 2H2O complex, the Ga3+ is six-coordinated by the Cydta ligand yielding an octahedral conformation, and the complex crystallizes in the monoclinic system with the P21/c space group. The crystal data are as follows: a = 16.5039(19), b = 13.1499(16), c = 8.5204(10) Å, β = 101.650(2)°, V = 1811.0(4) Å3, Z = 4, ρ = 1.757 g/cm3, μ = 1.805 mm?1, F(000) = 984, R = 0.0291, and wR = 0.0698 for 3713 observed reflections with I ≥ 2σ(I). In the K[GaIII(Pdta)] · 3H2O complex, the Ga3+ is also six-coordinated by the Pdta ligand yielding an almost standard octahedral conformation, and the complex crystallizes in the orthorhombic system with P212121 space group. The crystal data are as follows: a = 8.8913(10), b = 11.6181(13), c = 17.0227(19) Å, V = 1758.4(3) Å3, Z = 4, ρ = 1.757 g/cm3, μ = 1.862 mm?1, F(000) = 952, R = 0.0288, and wR = 0.0724 for 3556 observed reflections with I ≥ 2σ(I).  相似文献   

2.
Single crystals of Li(H3O)[UO2(C2O4)2(H2O)] · H2O (I) have been synthesized and studied by X-ray diffraction. Compound I crystallizes in the monoclinic crystal system with the unit cell parameters: a = 7.1682(10) Å, b = 29.639(6) Å, c = 6.6770(12) Å, β= 112.3(7)°, space group P 21/c, Z = 4, R = 4.36%. Structure I contains discrete mononuclear groups [UO2(C2O4)2(H2O)]2? ascribed to the crystal-chemical group AB 2 01 M1 (A = UO2 2+, B01 =C2O 4 2? , M1 = H2O), which are “cross-linked” by the lithium ions into infinite layers {Li(UO2)(C2O4)2(H2O)2}? perpendicular to [010]. The hydroxonium ions are located between adjacent uranium-containing layers. A hydrogen bond system involving water molecules, oxalate ions, and hydroxonium combines the anionic layers into a three-dimensional framework.  相似文献   

3.
The 3-amino-1,2,4-triazole (atz)-based manganese complex was prepared and characterized through single-crystal X-ray diffraction, IR, EPR, and UV–visible spectroscopy. In the crystal structure, individual complex are interconnected through N(O)–H…Cl hydrogen bonds into 1D undulating chains running parallel to the [110] direction of the unit cell. Chains further grow into 2D supramolecular layers by way of the lattice water molecules of coordination and the chloride anions (O–H…Cl). Layers pack along the b-axis of the unit cell mediated by O–H…Cl(N) and N–H…O(Cl) hydrogen bonds forming a 3D supramolecular architecture. The theoretical calculations were also performed to optimize the structure of the complexes in the gas phase to confirm the structures proposed by X-ray crystallography. In addition, IR and UV–visible spectra of complex were calculated and compared with the corresponding experimental spectra to complete the experimental structural identification. The three-dimensional Hirshfeld surface (3D-HS) and their relative two-dimensional fingerprint plots (2D-FP) reveal that the structure is dominated by H…Cl/Cl…H (50.5%), H…O/O…H (11.3%) and N…O/O…N (10.2%) contacts.  相似文献   

4.
A novel lanthanide complex of [Nd(2-EOBA)3(phen)(H2O)]2 · H2O (2-EOBA = 2-ethoxylbenzoate, phen = 1,10-phenanthroline), has been synthesized and structurally characterized by single crystal X-ray diffraction. The complex crystallizes in monoclinic, space group P2(1)/n with a = 14.7453(18) Å, b = 12.3628(15) Å, c = 19.473(2) Å, α = 90°, β = 93.349(2)°, γ = 90°. Two Nd3+ ions are connected together by two bridging 2-EOBA ligands and each Nd3+ ion is further coordinated by two chelating 2-EOBA ligands, one chelating phen molecule and one water molecule. The coordination number of Nd3+ ion is nine. The coordination geometry of Nd3+ ion is a distorted monocapped square-antiprism.  相似文献   

5.
A new complex [Co(DH)2(Thio)2]2[FeF5(H2O)] · 2CH3OH (where DH? is dimethylglyoxime monoanion, Thio is thiourea molecule) was synthesized and its structure was determined. The coordination polyhedron of the Co(III) atoms in two centrosymmetric complex cations is an octahedron, formed by four N atoms of two dimethylglyoxime residues and two S atoms of coordinated Thio molecules. One of the Thio molecules is almost perpendicular to a metal cycle (the dihedral angle 87.8(1)°), which is responsible for realization of intermolecular hydrogen bond N-H···O (N···O 2.990(3) Å). The second Thio molecule is almost parallel to the equatorial CoN4 fragment (the dihedral angle 159.4(1)°) to give rise to intramolecular π-π interaction between practically planar Thio molecule and one of the π-delocalized metal cycle. The Fe(III) coordination polyhedron is an octahedron, formed by five F atoms and by the O atom of coordinated water molecule. The key role in the crystal structure organization is played by intermolecular hydrogen bonds N-H···F, N-H···O, N-H···S, the intramolecular bonds O-H···O, formed by the donor NH2 groups of a complex cation with the F atoms of the [FeF5(H2O)]2? and the donor-acceptor groups of the Thio fragments.  相似文献   

6.
Single crystals of Cs[(UO2)2(C2O4)2(OH)] · H2O were synthesized and structurally studied using X-ray diffraction. The compound crystallizes in monoclinic space group P21/m, Z = 2, with the unit cell parameters a = 5.5032(4) Å, b = 13.5577(8) Å, c = 9.5859(8) Å, β = 97.012(3)°, V = 709.86(9) Å3, R = 0.0444. The main building units of crystals are [(UO2)2(C2O4)2(OH)]? layers of the A2K 2 02 M2 (A = UO 2 2+ , K02 = C2O 4 2? , and M2 = OH?) crystal-chemical family. Uranium-containing layers are linked into a three-dimensional framework via electrostatic interactions with outer-sphere cations and hydrogen bonds with water molecules.  相似文献   

7.
A method for the synthesis of potassium pivalates (trimethylacetates) from potassium tert-butoxide and pivalic acid was proposed. The complexes of the formulas [K(H2O)(Piv)](I) and [K2(Phen)(H2O)2(Piv)2] (II) (Piv denotes the pivalate anion and Phen denotes 1,10-phenanthroline) were obtained and characterized by elemental analysis and IR and 1H NMR spectroscopy. The crystal structures of complexes I and II were determined using X-ray diffraction. Crystal structure I has a layered motif with two nonequivalent K atoms (C.N.s 5 + 2 and 6). The coordination of phenanthroline in II gives rise to a ribbon motif, the structure containing three nonequivalent K atoms (C.N.s 6, 6 + 1, and 8).  相似文献   

8.
A new neptunium(V) complex [(NpO2)2(CH3COO)2(H2O)] ? 2H2O was synthesized and its crystal structure was determined. The unit cell parameters are: a = 24.007(10) Å, b = 6.779(3) Å, c = 8.076(3) Å, space group Pnma, Z = 4, V = 1314.2(9) Å3, R = 0.049, wR(F2) = 0.105. The crystal structure of the compound is composed of neutral [(NpO2)2(CH3COO)2(H2O)] layers and molecules of the water of crystallization. Each of the crystallographically independent neptunoyl ions performs a bidentate function thus forming a composite system of cation-cation bonds.  相似文献   

9.
Evidence for the existence of primitive life forms such as lichens and fungi can be based upon the formation of oxalates. These oxalates form as a film like deposit on rocks and other host matrices. The anhydrous oxalate mineral moolooite CuC2O4 as the natural copper(II) oxalate mineral is a classic example. Another example of a natural oxalate is the mineral wheatleyite Na2Cu2+(C2O4)2·2H2O. High resolution thermogravimetry coupled to evolved gas mass spectrometry shows decomposition of wheatleyite at 255°C. Two higher temperature mass losses are observed at 324 and 349°C. Higher temperature mass losses are observed at 819, 833 and 857°C. These mass losses as confirmed by mass spectrometry are attributed to the decomposition of tennerite CuO. In comparison the thermal decomposition of moolooite takes place at 260°C. Evolved gas mass spectrometry for moolooite shows the gas lost at this temperature is carbon dioxide. No water evolution was observed, thus indicating the moolooite is the anhydrous copper(II) oxalate as compared to the synthetic compound which is the dihydrate.  相似文献   

10.
Single crystals of Ba3[UO2(C2O4)2(NCS)]2 · 9H2O are synthesized and studied by X-ray diffraction. The crystals are orthorhombic, space group Fddd, Z = 16, and the unit cell parameters are a = 16.253(3) Å, b = 22.245(3) Å, c = 39.031(6) Å. The main crystal structural units are mononuclear complex groups [UO2(C2O4)2NCS]3? of the crystal-chemical family (AB 2 01 M1 (A = UO 2 2+ , B01 = C2O 4 2? , M1 = NCS?) of the uranyl complexes linked into a three-dimensional framework by electrostatic interactions and hydrogen bonds involving oxalate ions and water molecules.  相似文献   

11.
The crystal structure of complex [Mg(H2O)6][VO(edta)] · 3.5H2O (I) was determined by X-ray diffraction study. The crystals are monoclinic, a = 6.779 Å, b = 13.373(6) Å, c = 25.054 Å, β = 96.55°, Z = 4, space group P21. The unit cell contains two independent [VO(edta)]2? anions, two independent [Mg(H2O)6]2+ cations, and seven crystal-water molecules. The coordination polyhedron of each vanadium atom is formed by five donor atoms of the edta ligand (2N + 3O) (V(1)-N(1), 2.278 Å; V(1)-N(2), 2.149 Å; V(2)-N(3), 2.301 Å; V(2)-N(4), 2.165 Å; V-O(acet), 2.00 ± 0.02 Å) and the oxygen atom of the oxo group (V-O, 1.60 ± 0.01 Å). The edta ligands and the vanadium atom form three glycinate rings: two R-type rings and one G-type ring (one acetate branch remains free), as well as an E-type ring with an asymmetric gauche configuration. The [Mg(H2O)6] cations are slightly distorted octahedra (Mg-O, 2.013–2.132 Å, the OMgO angles are 86.6°–94.2°). The H2O molecules form a bifurcate system of H-bonds. The crystals of compound I belong to OD-type structures with an incomplete ordering of layers.  相似文献   

12.
The interaction of the [B10H10]2– and [B12H12]2– anions with aliphatic and aromatic nitro compounds (RNO2, where R = Et, n-Pr, i-Pr, tert-Bu, Ph) has been studied under irradiation with visible and UV light. It has been shown that, depending on the reaction conditions, both mono- and disubstituted nitro-closo-decaborates can be selectively obtained in yields up to 50%.  相似文献   

13.
The reaction of the trinuclear oxo-centered mixed-valence complex [Mn3O(O2CPh)6(Py)2(H2O)] with 2,2′-bipyridyl (Bipy) and another potential tripodal ligand affords the title compound [Mn3(PhCO2)6(Bipy)2] · H2O in good yield. The X-ray crystallographic diffraction study reveals that three mangenese ions are arranged in a linear mode with Mncenter-Mnterminal and Mnterminal-Mnterminal diatances of 3.588 and 7.176 Å, respectively. Molar magnetic susceptibility of the compound gradually decreases from 12.23 (300 K) to 4.45 cm3 K mol?1 (2 K). Taking into account the structure of this compound, the data in the 2.0–300 K range were fit to the appropriate theoretical expression to give J = ?2.73 cm?1, ρ = 2.07%, N a = ?0.0004 cm3 mol?1, g = 1.992, and R 2 = 0.99996. The magnetization versus external magnetic field measurements at 2 K shows that the ground state is S T = 5/2.  相似文献   

14.
Four new low melting salts, “Ionic Liquids” consisting of the [CrIII(NCS)4(Phen)]? complex monoanion and imidazolium based cations A, with A = 1-ethyl-3-methylimidazolium (EMIm), 1-butyl-3-methylimidazolium (BMIm), 1,3-dimethyl-2,4,5-triphenylimidazolium (DML), and 1,2,3,4,5-pentamethyl-imidazolium (PMIm), were investigated. Single-crystal X-ray investigations established the structures of the four compounds. (EMIm)[Cr(NCS)4(Phen)] (I): triclinic, \(P\bar 1\), a = 8.1382(6), b = 10.4760(8), c = 16.003(1) Å, α = 90.330(4)°, β = 94.759(4)°, γ = 107.305(4)°, Z = 2, R 1(F)/wR 2(F 2) = 0.0650/0.1770; (BMIm)[Cr(NCS)4(Phen)] (II): triclinic, \(P\bar 1\), a = 8.5545(4), b = 9.8620(4), c = 16.6762(6) Å, α = 92.503(2)°, β = 97.517(2)°, γ = 91.249(2)°, Z = 2, R 1(F)/wR 2(F 2) = 0.0393/0.0848; (DML)[Cr(NCS)4(Phen)] · C3H6O (III): triclinic, \(P\bar 1\), a = 11.0475(9), b = 13.589(1), c = 14.582(1) Å, α = 83.013(4)°, β = 87.116(4)°, γ = 70.333(5)°, Z = 2, R 1(F)/wR 2(F 2) = 0.0407/0.1023; (PMIm)[Cr(NCS)4(Phen)] · C3H6O (IV): orthorhombic, Pbca, a = 17.379(1), b = 16.514(1), c = 22.304(1) Å, Z = 8, R 1(F)/wR 2(F 2) = 0.0460/0.1107 (in addition III and IV contain co-crystallized acetone molecules). Each compound was characterized by elemental analysis, NMR, IR, und UV-Vis spectroscopy. Magnetic properties were derived from NMR investigations (EVANS method). All four compounds are paramagnetic with effective magnetic moments of spin-only CrIII. Melting points were obtained from DSC measurements. All melting points are higher than required for “Ionic Liquids”, but nevertheless “low” for molten salts.  相似文献   

15.
Single crystals of Mg pivalate hydrate, Mg(H2O)6(Piv)2 · 3H2O (HPiv = (CH3)3CCOOH) are synthesized and their structure is determined by X-ray diffraction method. The crystals are rhombic: a = 10.917(2) Å, b = 12.625(2) Å, c = 31.394(8) Å, Z = 8, space group Pbca, R 1 = 0.0525. The Mg atom has octahedral surrounding of the O atoms of water molecules (Mg-O 2.044–2.137 Å). The cationic chains of [Mg(H2O)6] 2+ lie in the voids of doubled network anionic layers of [(H2O)3(Piv)2] ∞∞ 2? . Inside the layer, the pivalate anions alternate with water molecules in the xy plane, being bonded to them by hydrogen bonds. The cationic chains and the anionic layers are united into layered packs by hydrogen bonds between coordinated water molecules and pivalate anions and between coordinated and crystal hydrate water molecules.  相似文献   

16.
Synthesis and X-ray diffraction study of [UO2CrO4(C5NH5COO)] · H2O crystals were performed. The compound crystallizes in the monoclinic system with the unit cell parameters a = 7.5025(3) Å, b = 11.5188(6) Å, c = 13.0518(6) Å, β = 97.877(4)°, V = 1117.29(9) Å3, space group P21/n, Z = 4, R = 0.0263. The structure is formed by three [UO2CrO4(C5NH5COO)] layers parallel to (10\(\bar 1\)). The coordination polyhedron of uranium atoms is a pentagonal bipyramid, whose apices are occupied by oxygen atoms of uranyl, three chromate groups, and two molecules of isonicotinic acid. Crystal chemical formula of the [UO2CrO4(C5NH5COO)] layer can be represented as AT3B2, where A = UO 2 2+ , T3 = CrO 4 2? , and B2 = C5NH5COO molecules. The isonicotinic acid molecules are in the form of zwitterions.  相似文献   

17.
Under hydrothermal conditions, the complex [Mn(lmdc)2(H2O)2] · 2H2O (I) was synthesized and characterized by elemental analysis and IR spectrum (HImdc = 4,5-imidazofedicarboxylic acid). The crystal structure of I was determined by single-crystal X-ray diffraction (crystallizing in the monoclinic crystal system, P 2/c space group, a = 11.000(2), b = 7.1281(14), c = 12.696(3) Å, β = 122.45(3), Z = 2. In I, the Mn2+ ion was chelated by two Imdc with one of their nitrogen atoms and a carboxylic oxygen atom, while two water molecules occupy the axial position of the Mn atom forming a distorted octahedral geometry. Three-dimensional structure of I was formed by intermolecular hydrogen bonds. UV-Vis and fluorescence spectra of I interacting with DNA show that insertion is the main binding mode between I and fish sperm DNA. Gel electrophoresis shows that I cleaves both supercoiled and circular pBR322 DNA to form a small molecular fragment.  相似文献   

18.
A novel Salen-type bisoxime ligand, 6,6′-dimethoxy-2,2′-[(1,4-butylene)dioxybis(nitrilomethylidyne)]diphenol (H2L) and its tetranuclear Cu(II) complex, [Cu4L2(pic)4(H2O)2]·2H2O, have been synthesized and characterized by elemental analyses, IR, TG-DTA and 1H-NMR etc. The X-ray crystal structure of the complex reveals that formation of a tetranuclear structure, which consists of four copper(II) atoms, two pentadentate L2−units, four picratols, two coordinated water molecules and two crystallizing water molecules. Around four copper ions are all octahedral geometries. It was demonstrated that the picratols in the tetranuclear copper(II) complex show a novel tridentate coordination mode.  相似文献   

19.
The influence of specific features of the structure and nature of the cations (Ph4P+, H(Phen)+, Cs+, and (CH3)4N+) on the ERP spectra of the nickel ions in salts with the dicarbollylnickelate anion [Ni(B9C2H11)2] is studied. It is shown that the change in the cation type in these compounds results in the electron density redistribution, which affects the change in the main and average values of the g factor. The g av value increases over that observed in frozen solutions upon the localization of the positive charge of the cation on one atom and in the absence of the screening effect of the solvent and large functional groups of the cation. The exception is the compound (Ph4P+)NiCb2 (Cb is B9C2H11) with solvated CCl4 molecules. For all compounds studied, the temperature dependence of the linewidths in the EPR spectra is described by the equation ΔH = αT + βT7 with different α and β values and is defined by the temperature dependence of the relaxation process caused by the Raman interaction.  相似文献   

20.
A new coordination polymer [Ag3hmt3(3-btc)]·5H2O (1 )(hmt = hexamethylenetetramine, btc = 1,3,5-benzenetricarboxyl)has been successfully synthesized. Crystal data: P21/a , a = 11.9906(2) Å, b = 17.3689(2) Å, c = 16.96100(10) Å, = 101.9820(14)°, V = 3455.40(7) Å3, Z = 4, Dc = 2.002 mg/m3. In the hexagonal structure of the Ag-hmt unit, each Ag-hmt unit comprises three Ag atoms and three hmt ligands. The 3-btc ligands bridge the adjacent two-dimensional honeycomb-like Ag-hmt layers to form three-dimensional networks. Structural analysis shows that hydrogen bonds play a key role for the structural stability of the compounds.Original Russian Text Copyright © 2004 by Shoubo Qin, Sheming Lu, Yanxiong Ke, Jianmin Li, Shuxi Zhou, Xintao Wu, and Wenxin DuTranslated from Zhurnal Strukturnoi Khimii, Vol. 45, No. 3, pp. 566–571, May–June 2004.  相似文献   

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