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1.
A new vanadium(III) oxalatophosphate has been synthesized hydrothermally and characterized by single-crystal X-ray diffraction and thermogravimetric analysis. It crystallizes in the triclinic space group with a=11.604(2) Å, b=12.391(2) Å, c=15.220(3) Å, α=71.090(3)°, β=82.630(3)°, γ=62.979(3)°, V=1843.8(5) Å3 and Z=2. The structure consists of V6(HPO4)6 double 6-ring (D6R) units connected by coordinating C2O42− and PO43− anions to form anionic sheets in the ab plane with charge-compensating quadruply protonated 1,4-bis(3-aminopropyl)piperazinium cations and water molecules between the sheets. It is one of the few compounds with 2D layer structures and the second example containing D6R units in the system of metal oxalatophosphates. The iron analogue was also synthesized.  相似文献   

2.
Two new vanadium squarates have been synthesized, characterized by infrared and thermal behavior and their structures determined by single crystal X-ray diffraction. Both structures are made of discrete, binuclear vanadium entity but in 1, [V(OH)(H2O)2(C4O4)]2·2H2O the vanadium atom is trivalent and the entity is neutral while in 2, (NH4)[(VO)2(OH)(C4O4)2(H2O)3]·3H2O, the vanadium atom is tetravalent and the entity is negatively charged, balanced by the presence of one ammonium ion. Both molecular anions are bridged by two terminal μ2 squarate ligands. 1 crystallizes in the triclinic system, space group P-1, with lattice constants a=7.5112(10) Å, b=7.5603(8) Å, c=8.2185(8) Å, α=106.904(8)°, β=94.510(10)°, γ=113.984(9)° while 2 crystallizes in the monoclinic system, space group C2/c, with a=14.9340(15) Å, b=6.4900(9) Å, c=17.9590(19) Å and β=97.927(12)°. From the magnetic point of view, V(III) binuclear species show ferromagnetic interactions at low temperatures. However, no anomalies pointing to magnetic ordering are observed down to 2 K.  相似文献   

3.
Three manganese oxalates have been hydrothermally synthesized, and their structures determined by single-crystal X-ray diffraction. MnC2O4·2H2O (I) is orthorhombic, P212121, , , , , Z=4, final R, Rw=0.0832, 0.1017 for 561 observed data (I>3σ(I)). The one-dimensional structure consists of chains of oxalate-bridged manganese centers. [C4H8(NH2)2][Mn2(C2O4)3] (II) is triclinic, , , , , α=81.489(2)°, β=81.045(2)°, γ=86.076(2)°, , Z=1, final R, Rw=0.0467, 0.0596 for 1773 observed data (I > 3σ (I)). The three-dimensional framework is constructed from seven coordinate manganese and oxalate anions. The material contains extra-framework diprotonated piperazine cations. Mn2(C2O4)(OH)2 (III) is monoclinic, P21/c, , , , β=91.10(3)°, , Z=1, final R1, wR2=0.0710, 0.1378 for 268 observed data (I>2σ (I)). The structure is also three dimensional, with layers of MnO6 octahedra pillared by oxalate anions. The hydroxide group is found bonded to three manganese centers resulting in a four coordinate oxygen.  相似文献   

4.
By hydrothermal reaction of In2O3 with H2C2O4·2H2O in the presence of H3BO3 at 155 °C, an open-framework three-dimensional indium oxalate of formula [In(OH)(C2O4)(H2O)]3·H2O (1) has been obtained. The compound crystallizes in the trigonal system, space group R3c with , , , Z=6, R1=0.0352 at 298 K. The small pores in 1 are filled with water molecules. It loses its filled water at about 180 °C without the change of structure, then the bounded water at 260 °C, and completely decompounds at 324 °C. The residue is confirmed to be In2O3.  相似文献   

5.
A new layered inorganic-organic hybrid aluminum phosphate-oxalate [H3N(CH2)4NH3]2[Al4(C2O4)(H2PO4)2(PO4)4]·4[H2O](AlPO-CJ25) has been synthesized hydrothermally, by using 1,4-diaminobutane (DAB) as structure-directing agent. The structure has been solved by single-crystal X-ray diffraction analysis and further characterized by IR, 31P MAS NMR, TG-DTA as well as compositional analyses. Crystal data: the triclinic space group P-1, a=8.0484(7) Å, b=8.8608(8) Å, c=13.2224(11) Å, α=80.830(6)°, β=74.965(5)°, γ=78.782(6)°, Z=2, R1[I>2σ(I)]=0.0511 and wR2(all data)=0.1423. The alternation of AlO4 tetrahedra and PO4 tetrahedra gives rise to the four-membered corner-sharing chains, which are interconnected through AlO6 octahedra to form the layered structure with 4,6-net sheet. Interestingly, oxalate ions are bis-bidentately bonded by participating in the coordination of AlO6, and bridging the adjacent AlO6 octahedra. The layers are held with each other through strong H-bondings between the terminal oxygens. The organic ammonium cations and water molecules are located in the large cavities between the interlayer regions.  相似文献   

6.
A cobalt phosphonate (H3O)6·[Co4(H2O)4(HPMIDA)2(PMIDA)2)]·2H2O, 1, has been synthesized from a mild solvothermal reaction of Co(II) ion with N-(phosphonomethyl)iminodiacetic acid (H4PMIDA). Compound 1 crystallizes in the triclinic space group with cell parameters of , , , α=93.06(3)°, β=99.66(3)°, γ=90.34(3)° and Z=1. Compound 1 shows a novel tetra-nuclear molecular structure. In the crystal lattice, molecules of 1 hydrogen bond to each other to form two-dimensional (2D) layers, which are further linked together by the co-crystallized H2O molecules and H3O+ counter ions through hydrogen bonding to form the 3D supramolecular network. Thermogravimetric analysis, IR spectrum, magnetic susceptibility and luminescent spectra are given.  相似文献   

7.
A novel 3-D compound of (enH2)1.5[Bi3(C2O4)6(CO2CONHCH2CH2NH3)]·6.5H2O has been hydrothermally synthesized and characterized by IR, ultraviolet-visible diffuse reflection integral spectrum (UV-Vis DRIS), fluorescence spectra, TGA and single crystal X-ray diffraction. It crystallizes in the monoclinic system, space group C2/c with , , , β=112.419(3)°, , Z=8, R1=0.0463 and wR2=0.1393 for unique 7686 reflections I>2σ(I). In the title compound, the Bi atoms have eight-fold and nine-fold coordination with respect to the oxygen atoms, with the Bi atoms in distorted dodecahedron and monocapped square antiprism, respectively. The 3-D framework of the title compound contains channels and is composed of linkages between Bi atoms and oxalate units, forming honeycomb-like layers with two kinds of 6+6 membered aperture, and pillared by oxalate ligands and monamide groups. The channels have N-ethylamine oxalate monamide group CO2CONHCH2CH2NH3+, which is formed by the in situ reaction of en and oxalate acid. At room temperature, the complex exhibits intense blue luminescence with an emission peak at 445 nm.  相似文献   

8.
Single crystal susceptibilities of Er(C2O4) (C2O4H)·3H2O are reported over the 1.5–20 K interval, and EPR spectra at 4.2 K of Y (C2O4) (C2O4H·3H2O doped with Er3+ are also reported. The susceptibilities follow the CurieWeiss law, with g| = 12.97 ± 0.05, g = 2.98 ± 0.05, θ| = ?0.25 ± 0.05 K, and θ = ?0.12 ± 0.05 K.  相似文献   

9.
The crystal structure of a double salt of sodium and cesium with 2-diphenylacetyl-1,3-indandione of the composition [Cs2Na(H2O)2(C23H16O3)(C23H15O3)3] (I) was studied by X-ray crystallography. The crystals of I are monoclinic, Z = 2, space group P21/n, a = 10.212(2) ?, b = 23.479(5) ?, c = 15.638(3) ?, β = 98.30(03)°. The compound contains [Cs2NaO10] trimers, in which the central Na atom shares two edges with two Cs atoms through deprotonated bridging ligands. The trimers are connected to adjacent trimers by paired C-H...O contacts to form layers. The layers form an infinite open framework via hydrogen bonds between the oxygen atoms of keto groups of noncoordinated indandione moieties and water molecules that enter the cesium coordination sphere in trimers of the adjacent layers.  相似文献   

10.
An unprecedented hybrid solid obtained by self-assembly of octamolybdate clusters into a three-dimensional alkali metal modified neodymium-organic heterometallic framework is described. Crystal data: monoclinic, space group P21/n, , , , β=98.90(3)°; ; Z=2, R (final)=0.0474. The data were collected on a Rigaku R-AXIS RAPID IP diffractometer at 293 K using graphite-monochromated MoKα radiation () and oscillation scans technique in the range of 1.98°<θ<27.48°.  相似文献   

11.
The preparation, crystal structure and magnetic properties of a new oxalate-containing copper(II) chain of formula {[(CH3)4N]2[Cu(C2O4)2] · H2O}n (1) [(CH3)4N+ = tetramethylammonium cation] are reported. The structure of 1 consists of anionic oxalate-bridged copper(II) chains, tetramethylammoniun cations and crystallization water molecules. Each copper(II) ion in 1 is surrounded by three oxalate ligands, one being bidentate and the other two exhibiting bis-bidenate coordination modes. Although all the tris-chelated copper(II) units from a given chain exhibit the same helicity, adjacent chains have opposite helicities and then an achiral structure results. Variable-temperature magnetic susceptibility measurements of 1 show the occurrence of a weak ferromagnetic interaction through the oxalate bridge [J = +1.14(1) cm−1, the Hamiltonian being defined as H = –JnmSi · Sj]. This value is analyzed and discussed in the light of available magneto-structural data for oxalate-bridged copper(II) complexes with the same out-of-plane exchange pathway.  相似文献   

12.
A new sodium hydroxygallophosphate, Na3Ga4O(OH)(H2O)(PO4)4·H2O, has been prepared by hydrothermal synthesis. Its structure has been determined from a single-crystal X-ray diffraction study. It crystallizes in the P21/c space group with the cell parameters a=9.445(2) Å, b=9.028(1) Å, c=19.209(3) Å, β=102.08(2), V=1603.4(4) Å3. Its three-dimensional framework can be described from PO4 monophosphate groups sharing their apices with original Ga4O16(OH)(H2O) tetrameric building units, which result from the assembly of one GaO4 tetrahedron, one GaO5 trigonal bipyramid and two octahedra: GaO5(OH) and GaO4(OH)(H2O). The sodium cations and one water molecule are located in tunnels running along b.  相似文献   

13.
The lanthanide sulphate octahydrates Ln2(SO4)3·8H2O (Ln=Ho, Tm) and the respective tetrahydrate Pr2(SO4)3·4H2O were obtained by evaporation of aqueous reaction mixtures of trivalent rare earth oxides and sulphuric acid at 300 K. Ln2(SO4)3·8H2O (Ln=Ho, Tm) crystallise in space group C2/c (Z=4, aHo=13.4421(4) Å, bHo=6.6745(2) Å, cHo=18.1642(5) Å, βHo=102.006(1) Å3 and aTm=13.4118(14) Å, bTm=6.6402(6) Å, cTm=18.1040(16) Å, βTm=101.980(8) Å3), Pr2(SO4)3·4H2O adopts space group P21/n (a=13.051(3) Å, b=7.2047(14) Å, c=13.316(3) Å, β=92.55(3) Å3). The vibrational and optical spectra of Ho2(SO4)3·8H2O and Pr2(SO4)3·4H2O are also reported.  相似文献   

14.
A new 3D coordination polymer, [LaAg(Pydc)(HPydc)(C2O4)0.5(H2O)2] n (I) (H2Pydc = pyridine-3,5-dicarboxylic acid), has been hydrothermally synthesized and characterized by elemental analyses and single crystal X-ray diffraction. The X-ray diffraction analysis reveals that I (C15H11AgLaN2O12) crystallizes in triclinic space group P $ \bar 1 $ \bar 1 and features an interesting 3D framework constructed by 2D layers via strong Ag-Ag interactions. Unit cell parameters for I (n = 1): a = 7.749(2), b = 8.316(1), c = 14.239(3) ?, α = 97.64(2)°, β = 100.12(2)°, γ = 94.37(2)°, and Z = 2.  相似文献   

15.
Two solid-state coordination compounds of rare earth metals with glycin, [Gd4/3Y2/3(Gly)6(H2O)4](ClO4)6·5H2O and [ErY(Gly)6(H2O)4](ClO4)6·5H2O were synthesized. The low-temperature heat capacities of the two coordination compounds were measured with an adiabatic calorimeter over the temperature range from 78 to 376 K. [Gd4/3Y2/3(Gly)6(H2O)4](ClO4)6·5H2O melted at 342.90 K, while [ErY(Gly)6(H2O)4](ClO4)6·5H2O melted at 328.79 K. The molar enthalpy and entropy of fusion for the two coordination compounds were determined to be 18.48 kJ mol−1 and 53.9 J K−1 mol−1 for [Gd4/3Y2/3(Gly)6(H2O)4](ClO4)6·5H2O, 1.82 kJ mol−1 and 5.5 J K−1 mol−1 for [ErY(Gly)6(H2O)4](ClO4)6·5H2O, respectively. Thermal decompositions of the two coordination compounds were studied through the thermogravimetry (TG). Possible mechanisms of the decompositions are discussed.  相似文献   

16.
17.
A new form of cobalt succinate has been discovered using high-throughput methods and its structure was solved by single crystal X-ray diffraction. Co7(C4H4O4)4(OH)6(H2O)37H2O crystallizes in the monoclinic space group P21/c with cell parameters: a=7.888(2) Å, b=19.082(6) Å, c=23.630(7) Å, β=91.700(5)°, V=3555(2) Å3, R1=0.0469. This complex structure, containing 55 crystallographically distinct non-hydrogen atoms, is compared to the previously reported nickel phase, characterized using ab initio structure solution from synchrotron powder diffraction data.  相似文献   

18.
Two novel vanadium selenites {[VO(OH)(H2O)](SeO3)}4·2H2O 1 and (H3NCH2CH2NH3)[(VO)(SeO3)2] 2 were synthesized by hydrothermal method and their crystal structures were determined by single-crystal X-ray diffraction. It is characterized by inductively coupled plasma (ICP), thermogravimetric (TG) and elemental analyses. Compound 1 crystallizes in the monoclinic system, space group C2/c, a=21.2250(11) Å, b=12.6309(6) Å, c=17.0249(10) Å, β=96.830(3)°, V=4531.8(4) Å3 and Z=8, R1 [I>2σ(I)]=0.0344, wR2 [I>2σ(I)]=0.119; Compound 2 crystallizes in the monoclinic system, space group P21/c, a=9.6389(4) Å, b=6.9922(3) Å, c=15.0324(5) Å, β=102.297(2)°, V=989.90(7) Å3 and Z=4, R1 [I>2σ(I)]=0.0452, wR2 [I>2σ(I)]=0.117. {[VO(OH)(H2O)](SeO3)}4·2H2O has a 1D structure constructed from the {[VO(OH)(H2O)](SeO3)} chains. (H3NCH2CH2NH3)[(VO)(SeO3)2] has a layered structure composed of alternating VO5 and SeO3 units with protonated ethylenediamine as interlayer guest.  相似文献   

19.
Two new salts of malonic acid have been prepared: the copper(II) malonate tetrahydrate and the copper(II)-ammonium double malonate. Their study by thermal analysis (TG and DTA) leads to the following results:Cu(C3H2O4)·4H2O: the dehydration is rather complex and it is only under careful conditions that an intermediate hydrate Cu(C3H2O4)·3H2O could be traced. At about 170°C the dehydration is not ended (the salt holds yet about 0.15H2O) and the anhydrous salt occurs only at about 240°C. It decomposes immediately leading to residues the composition of which depends upon the surrounding atmosphere; the part played by the gas given off is discussed.Cu(NH4)2(C3H2O4)2: this salt melts and decomposes simultaneously at about 190°C. During the decomposition the copper nitride Cu3N forms as intermediate compound (as well as copper metal). Concerning the final residues of the decomposition the results and the conclusions are the same as the ones of the previous case.  相似文献   

20.
The new U(VI) compound, [Ni(H2O)4]3[U(OH,H2O)(UO2)8O12(OH)3], was synthesized by mild hydrothermal reaction of uranyl and nickel nitrates. The crystal-structure was solved in the P-1 space group, a=8.627(2), b=10.566(2), c=12.091(4) Å and α=110.59(1), β=102.96(2), γ=105.50(1)°, R=0.0539 and wR=0.0464 from 3441 unique observed reflections and 151 parameters. The structure of the title compound is built from sheets of uranium polyhedra closely related to that in β-U3O8. Within the sheets [(UO2)(OH)O4] pentagonal bipyramids share equatorial edges to form chains, which are cross-linked by [(UO2)O4] and [UO4(H2O)(OH)] square bipyramids and through hydroxyl groups shared between [(UO2)(OH)O4] pentagonal bipyramids. The sheets are pillared by sharing the apical oxygen atoms of the [(UO2)(OH)O4] pentagonal bipyramids with the oxygen atoms of [NiO2(H2O)4] octahedral units. That builds a three-dimensional framework with water molecules pointing towards the channels. On heating [Ni(H2O)4]3[U(OH,H2O)(UO2)8O12(OH)3] decomposes into NiU3O10.  相似文献   

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