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1.
The title compound (disodium dipotassium copper(II) tris-[molybdate (VI)]) is prepared by form melt and characterized by single crystal X-ray diffraction and UV-vis spectroscopy. It crystallizes in the triclinic space group P-1 with a = 7.4946(8) Å, b = 9.3428(9) Å, c = 9.3619(9) Å, α = 92.591(7)°, β = 105.247(9)°, γ = 105.496(9)°, V = 604.7 Å3, and Z = 2. Its structure is isotypic with that of Na4Mn(MoO4)3. It is formed by Cu2O10 distorted bi-octahedral dimers linked by two bridging bidentate Mo2O4 tetrahedra and, additionally, two monodentate Mo1O4 tetrahedra to form Cu2Mo4O20 units. These units are linked by the insertion of Mo3O4 tetrahedra to build infinite ribbons disposed along the c axis. All of these ribbons form a one-dimensional framework. Both K1 and K3 cations are located in the inversion center, and all the other atoms are at general positions. The structure model is supported by the bond valence sum (BVS) and charge distribution CHARDI methods. The Cu2+ cations adopt the [4+2] CuO6 Jahn-Teller distortion giving rise to an intense dd transition in the UV-vis absorption spectra.  相似文献   

2.
CsCu3O2 was prepared via the azide route. Stoichiometric mixtures of the precursors (CsN3, Cu2O and CuO) were heated in a special regime up to 450 °C and annealed at this temperature for 50 h in silver crucibles. Single crystals have been grown by subsequent annealing of as prepared powders at 450 °C for 2000 h in silver crucibles, which were sealed in glass ampoules under dried Ar. According to the X‐ray analysis of the crystal structure (P3¯m1, Z = 1, a = 5.250(1), c = 5.442(1)Å, γ = 120°) copper is linearly coordinated by oxygen atoms. The CuO2‐dumb‐bells are connected to an infinite two‐dimensional Cu3O2‐network. CsCu3O2 is isostructural with CsCu3S2, CsAu3S2, CsAu3Se2 and RbAu3Se2.  相似文献   

3.
Synthesis and Crystal-Structure of Na2Mn3O7 Single crystals of Na2Mn3O7 have been grown hydrothermally applying high oxygen pressure (p = 2 kbar). The new compound cystallizes triclinic; space group P1 ; a = 6.636(6) Å, b = 6.854(6) Å, c = 7.548(6) Å, α = 105.76(6)°, β = 106.86(6)°, γ = 111.60(6)°; Z = 2. The crystal structure has been solved and refined to R = 7.9% and Rw = 6.2% (diffractometer data, 1044 independent reflexions). The crystal structure consists of Mn3O72? anions with manganese coordinated octahedrally by oxygen. These layered anions are hold together by Na+ ions (coordination numbers 5 and 6).  相似文献   

4.
The system CuO/In2O3/P2O5 has been investigated using solid state reaction between CuO, In2O3 and (NH4)2HPO4 in silica glass crucibles at 900 °C. The powder samples were characterized by X‐ray diffraction, thermal analysis and FT‐IR spectroscopy. Orange single crystals of the new quaternary phase were achieved by the process of crystallization with mineralizers in sealed silica glass ampoules. They were then analyzed with EDX and single‐crystal X‐ray analysis in which the composition Cu8In8P4O30 with the triclinic space group P$\bar{1}$ (No 2) with a = 7,2429(14) Å, b = 8,8002(18) Å, c = 10,069(2) Å, α = 103,62(3)°, β = 106,31(3)°, γ = 101,55(3)° and Z = 1 was found. The three‐dimensional framework consists of [InO6] octahedra and distorted [CuO6] octahedra, overcaped [InO7] prisms and [PO4] tetrahedra, also trigonal [(CuIn)O5] bipyramids and distorted [(CuIn)O6] octahedra, where copper and indium are partly exchanged against each other. Cu8In8P4O30 exhibits an incongruent melting point at 1023 °C.  相似文献   

5.
Na2BaCuV2O8: A New Structure Type of the Alkaline-Alkaline Earth Copper Oxovanadates Single crystals of Na2BaCuV2O8 were prepared by a high temperature flux. It crystallizes with monoclinic symmetry space group C–C2/c, a = 9.4329 Å, b = 5.6858 Å, c = 14.0488 Å, β = 92.344° Z = 4 and represents a new structure type. The crystal structure show VO4 tetrahedra, stretched CuO6 octahedra, trigonal bipyramids around Na+ and a BaO10+2 polyedron.  相似文献   

6.
In the title compound, Na+·H+·2C8H7O3, the anion contains a short Speakman-type hydrogen bond [O⃛O = 2.413 (2) Å]. The anions and the Na atoms lie across twofold axes.  相似文献   

7.
The blue copper complex compounds [Cu(phen)2(C6H8O4)] · 4.5 H2O ( 1 ) and [(Cu2(phen)2Cl2)(C6H8O4)] · 4 H2O ( 2 ) were synthesized from CuCl2, 1,10‐phenanthroline (phen) and adipic acid in CH3OH/H2O solutions. [Cu(phen)2‐ (C6H8O4)] complexes and hydrogen bonded H2O molecules form the crystal structure of ( 1 ) (P1 (no. 2), a = 10.086(2) Å, b = 11.470(2) Å, c = 16.523(3) Å, α = 99.80(1)°, β = 115.13(1)°, γ = 115.13(1)°, V = 1617.5(5) Å3, Z = 2). The Cu atoms are square‐pyramidally coordinated by four N atoms of the phen ligands and one O atom of the adipate anion (d(Cu–O) = 1.989 Å, d(Cu–N) = 2.032–2.040 Å, axial d(Cu–N) = 2.235 Å). π‐π stacking interactions between phen ligands are responsible for the formation of supramolecular assemblies of [Cu(phen)2(C6H8O4)] complex molecules into 1 D chains along [111]. The crystal structure of ( 2 ) shows polymeric [(Cu2(phen)2Cl2)(C6H8O4)2/2] chains (P1 (no. 2), a = 7.013(1) Å, b = 10.376(1) Å, c = 11.372(3) Å, α = 73.64(1)°, β = 78.15(2)°, γ = 81.44(1)°, V = 773.5(2) Å3, Z = 1). The Cu atoms are fivefold coordinated by two Cl atoms, two N atoms of phen ligands and one O atom of the adipate anion, forming [CuCl2N2O] square pyramids with an axial Cl atom (d(Cu–O) = 1.958 Å, d(Cu–N) = 2.017–2.033 Å, d(Cu–Cl) = 2.281 Å; axial d(Cu–Cl) = 2.724 Å). Two square pyramids are condensed via the common Cl–Cl edge to centrosymmetric [Cu2Cl2N4O2] dimers, which are connected via the adipate anions to form the [(Cu2(phen)2Cl2)(C6H8O4)2/2] chains. The supramolecular 3 D network results from π‐π stacking interactions between the chains. H2O molecules are located in tunnels.  相似文献   

8.
Na3Cu2O4 and Na8Cu5O10 were prepared via the azide/nitrate route from stoichiometric mixtures of the precursors CuO, NaN3 and NaNO3. Single crystals have been grown by subsequent annealing of the as prepared powders at 500 °C for 2000 h in silver crucibles, which were sealed in glass ampoules under dried Ar. According to the X-ray analysis of the crystal structures (Na3Cu2O4: P21/n, Z=4, a=5.7046(2), b=11.0591(4), c=8.0261(3) Å, β=108.389(1)°, 2516 independent reflections, R1(all)=0.0813, wR2 (all)=0.1223; Na8Cu5O10: Cm, Z=2, a=8.228(1), b=13.929(2), , β=111.718(2)°, 2949 independent reflections, R1(all)=0.0349, wR2 (all)=0.0850), the main feature of both crystal structures are CuO2 chains built up from planar, edge-sharing CuO4 squares. From the analysis of the Cu-O bond lengths, the valence states of either +2 or +3 can be unambiguously assigned to each copper atom. In Na3Cu2O4 these ions alternate in the chains, in Na8Cu5O10 the periodically repeated part consists of five atoms according to CuII-CuII-CuIII-CuII-CuIII. The magnetic susceptibilities show the dominance of antiferromagnetic interactions. At high temperatures the compounds exhibit Curie-Weiss behaviour (Na3Cu2O4: , , Na8Cu5O10: , , magnetic moments per divalent copper ion). Antiferromagmetic ordering is observed to occur in these compounds below 13 K (Na3Cu2O4) and 24 K (Na8Cu5O10).  相似文献   

9.
CoSm(SeO3)2Cl, CuGd(SeO3)2Cl, MnSm(SeO3)2Cl, CuGd2(SeO3)4 and CuSm2(SeO3)4: Transition Metal containing Selenites of Samarium and Gadolinum The reaction of CoCl2, Sm2O3, and SeO2 in evacuated silica ampoules lead to blue single crystals of CoSm(SeO3)2Cl (triclinic, , Z = 4, a = 712.3(1), b = 889.5(2), c = 1216.2(2) pm, α = 72.25(1)°, β = 71.27(1)°, γ = 72.08(1)°, Rall = 0.0586). If MnCl2 is used in the reaction light pink single crystals of MnSm(SeO3)2Cl (triclinic, , Z = 2, a = 700.8(2), b = 724.1(2), c = 803.4(2) pm, α = 86.90(3)°, β = 71.57(3)°, γ = 64.33(3)°, Rall = 0.0875) are obtained. Green single crystals of CuGd2(SeO3)2Cl (triclinic, , Z = 4, a = 704.3(4), b = 909.6(4), c = 1201.0(7) pm, α = 70.84(4)°, β = 73.01(4)°, γ = 70.69(4)°, Rall = 0.0450) form analogously in the reaction of CuCl2 and Gd2O3 with SeO2. CoSm(SeO3)2Cl contains [CoO4Cl2] octahedra, which are connected via one edge and one vertex to infinite chains. The Mn2+ ions in MnSm(SeO3)2Cl are also octahedrally coordinated by four oxygen and two chlorine ligands. The linkage of the polyhedra to chains occurs exclusively via edges. Both, the cobalt and the manganese compound show the Sm3+ ions in eight and ninefold coordination of oxygen atoms and chloride ions. In CuGd(SeO3)2Cl the Cu2+ ions are coordinated by three oxygen atoms and one Cl ion in a distorted square planar manner. One further Cl and one further oxygen ligand complete the [CuO3Cl] units yielding significantly elongated octahedra. The latter are again connected to chains via two common edges. For the Gd3+ ions coordination numbers of ?8 + 1”? and nine were found. Single crystals of the deep blue selenites CuM2(SeO3)4 (M = Sm/Gd, monoclinic, P21/c, a = 1050.4(3)/1051.0(2), b = 696.6(2)/693.5(1), c = 822.5(2)/818.5(2) pm, β = 110.48(2)°/110.53(2)°, Rall = 0.0341/0.0531) can be obtained from reactions of the oxides Sm2O3 and Gd2O3, respectively, with CuO and SeO2. The crystal structure contains square planar [CuO4] groups and irregular [MO9] polyhedra.  相似文献   

10.
Na2Sb5F9O3(NCS)2, a new complex, has been synthesized from NaSCN and SbF3 aqueous solutions and studied by chemical, X-ray diffraction, and thermal analyses and IR, 121,123Sb NQR, and 19F NMR spectroscopy. Its layered structure (triclinic symmetry system, a = 6.9998(1) Å, b = 9.4180(1) Å, c = 13.1094(2) Å, α = 74.815(1)°, β = 78.188(1)°, γ = 82.779(1)°, Z = 2, space group P $\bar 1$ ) is built of Na+ cations and [Sb10F18O6(NCS)4]4? decanuclear complex anions that consist of two [Sb5F9O3(NCS)2]2? pentanuclear complex anions linked by two weak Sb-F ionic bonds (2.529(2) Å). Decanuclear complex anions are linked into layers by secondary Sb…F bonds and Na-F bonds. Van der Waals interactions link these layers into a framework. The complex is stable up to 200°C.  相似文献   

11.
The first Alkaline Alkaline-Earth Oxocuprate (II, III): NaBa2Cu22+Cu3+O6 The compound NaBa2Cu3O6 was prepared by heating of Na2O2, BaO2, Cu2O in closed Ag-tubes. X-ray single crystal investigations led to orthorhombic symmetry, space group D-Fmmm; a = 8.4229; b = 11.4418; c = 14.4063 Å; Z = 8. Cu2+ and Cu3+ show square planar polygones of four and Na+ trigonal prisms of six O2?. The two barium point positions show coordination numbers C.N. = 8 and 6 + 4. The crystal structure is discussed.  相似文献   

12.
An organic–inorganic hybrid material based on paradodecatungstate anions and imidazolium cations, Na2(HIm)8(H2W12O42)·10H2O (HIm: imidazolium), has been synthesized under mildly acidic conditions. This compound was characterized by single-crystal X-ray diffraction, IR and UV–visible spectroscopies, and thermogravimetric and differential thermal analyses. The compound crystallizes in the triclinic P-1 space group with a = 11.6945(8) Å, b = 12.4782(6) Å, c = 14.0952(9) Å, α = 106.041(3)°, β = 109.338(2)°, γ = 100.249(3)°, V = 1781.0(3) Å3, and Z = 2. The crystal structure exhibits an infinite 1D inorganic structure built from [H2W12O42]10? clusters and sodium cations; adjacent chains are further joined up by hydrogen-bonding interactions between protonated imidazole cations, water molecules, and polyoxoanions, to form a 3D supramolecular architecture.  相似文献   

13.
A Contribution on the Crystal Structure of CuYW2O8, CuHoW2O8, and CuYW2O8 Single crystals of (I) CuY2O8, (II), CuHoW2O8, and (III) CuYbW2O8 were prepared and investigated by X-ray technique. (I) crystallizes with triclinic symmetry, space group C? P1 (a = 5.939 Å, b = 6.042 Å, c = 5.025 Å; α = 112.30°, β = 111.77°; Z = 1). (II) and (III) belong to monoclinic symmetry, space group C? P2/n (II) (a = 10.045 Å, b = 5.808 Å, c = 5.021 Å; β = 94.38°; z = 2 (III) a = 9.948 Å, b = 5.824 Å, c = 5.008 Å; β = 93.36°; Z = 2). The crystal structures will be discussed with respect to other to copper rare earth tungstates.  相似文献   

14.
A novel compound, KBi(C6H4O7) · 3.5H2O (I), has been synthesized in the Bi(NO3)2-K3(HCit) system (HCit3? is an anion of citric acid C6H8O7) at a component ratio (n) of 8 in a water-glycerol mixture, and its crystal structure has been determined. The crystals are unstable in air. The crystals are triclinic: a = 7.462 Å, b = 10.064 Å, c = 17.582 Å, α = 100.27°, β = 99.31°, γ = 105.48°, V = 1221.2 Å3, Z = 2, space group $P\bar 1$ . In the structure of I, asymmetric binuclear fragments [Bi2(Cit4?)2(H2O)2]2? are linked through inversion centers into polymeric chain anions. Ions K+ and crystal water molecules are arranged in channels between the chains. The Bi(1)...Bi(2) distances in the binuclear fragment are 4.62 Å, and the Bi(1)...Bi(1) and Bi(2)...Bi(2) distances between bismuth atoms in the chain are 5.83 and 5.95 Å, respectively. The chains are linked through bridging oxygen atoms of the ligands Cit to form layers. In the centrosymmetric four-membered chelate ring Bi2O2 formed through Bi-O(Cit) bonds, the distances Bi(1)-Bi(1) are equal to 4.55 Å, and Bi(1)-O are 2.66 and 2.84 Å. The Bi-O bond lengths in I are in the range 2.12–3.16 Å. The Cit ligands act as hexadentate chelating/bridging ligands.  相似文献   

15.
Synthesis and Structure of the First Ternary Lead(II) Copper(I) Oxide: PbCu2O2 PbCu2O2 can be prepared by solid state reaction or by precipitation from a basic aqueous solution. Single crystals of the new compound were prepared by recrystallisation from a molten mixture (PbO? Cu2O) and investigated by X-ray diffractometer technique. PbCu2O2 crystallizes isotypically with the homologue silver compound PbAg2O2 (monoclinic with a = 8.223 Å, b = 8.289 Å, c = 6.015 Å, β = 132.62°, Z = 4, space group C? C 1 2/c 1). The crystallographic data from the X-ray investigation are reported. The structure is built by endless [PbO4/4]- and [CuO2/4]-chains. Pb2+ has a one-sided asymmetric coordination with four next oxygen neighbours and Cu+ forms a stretched dumbbell with two oxygen atoms.  相似文献   

16.
The system CuO‐Fe2O3‐P2O5 has been investigated by means of the solid state reaction between CuO, Fe2O3 and (NH4)2HPO4 in quartz crucibles at 900 °C. The powder samples were characterized by X‐ray diffraction, IR spectroscopy and TG/DTA. Single crystals of a new quaternary phase Cu8Fe2P4O21 were achieved by cooling from the melt of the compound in a sealed, evacuated quartz ampoule. Cu8Fe2O5(PO4)4 crystallizes in the monoclinic space group C2/m (No 12) with a = 15.9733(8) Å, b = 5.9438(3) Å, c = 9.5530(5) Å, β = 113.76(1)°, Z = 2. The three‐dimensional framework consists of [FeO6] octahedra, three different [CuO5] polyhedra and [PO4] tetrahedra. Cu8Fe2P4O21 exhibits an incongruently melting point at 945 °C.  相似文献   

17.
Benzene 1,2,4,5‐tetrasulfonic acid (H4B4S) was prepared in two steps starting from 1,2,4,5‐Tetrachlorobenzene. Slow evaporation of an aqueous reaction mixture of H4B4S and Cu2(OH)2(CO3) led to light green single crystals of [Cu2(B4S)(H2O)8] · 0.5H2O. X‐ray single crystal investigations revealed the compound to be triclinic [P , Z = 1, a = 710.0(1), b = 713.7(1), c = 1077.1(2) pm, α = 98.41(2)°, β = 102.91(2)°, γ = 100.69(2)°]. In the crystal structure the Cu2+ ions are coordinated by four water molecules and two monodentate sulfonate anions yielding a tetragonally distorted [CuO6] octahedron. The anions are connected to further copper ions leading to ladder shaped chains running along the [100] direction. According to DTA/TG investigations the dehydration of the compound is finished at 240 °C and the decomposition of the anhydrous sulfonate starts at 340 °C.  相似文献   

18.
The reaction of CuCl with WOCl3 at 400 °C leads to a mixture of Cu1?x[W2O2Cl6] ( 1 ) and Cu1?x[W4O4Cl10] ( 2 ) in form of black lustrous needles. Both compounds crystallize in space group C2/m with a = 12.7832(5) Å, b = 3.7656(2) Å, c = 10.7362(3) Å, β = 119.169(2)° for 1 and a = 12.8367(19) Å, b = 3.7715(7) Å, c = 15.955(3) Å, β = 102.736(5)° for 2 . The structures are made up of WO2Cl4 octahedra. In the case of 1 two octahedra are edge‐sharing via chlorine atoms to form pairs which are linked via the trans‐positioned oxygen atoms to form infinite double strands . In the structure of 2 two of these double strands are condensed via terminal chlorine atoms to form quadruple strands . Like for all members of the Mx[W2O2X6] structure family (X = Cl, Br) nonstochiometry with respect to the cations M was observed. The copper content of 1 and 2 was derived from the site occupation factors of the respective structure refinements. For several crystals examined the copper content varied between x = 0.27 and 0.17 for 1 and x = 0.04 for 2 . In both structures the oxochlorotungstate strands are negatively charged and connected to layers by the monovalent copper ions, which are tetrahedrally coordinated by the non‐bridging chlorine atoms of the strands. The structure models imply disorder of the Cu+ ions over closely neighboured sites.  相似文献   

19.
Synthesis and X-ray investigation of a (GunH)2[Fe(Cit)2] single crystal are described [a = 10.327(2) Å, b = 10.414(2) Å, c = 11.267(2) Å; β = 117.25(3)°, V = 1077.2(4) Å3, P21/n, Z = 2, R(F) = 0,0239, 1196 reflections with I > 2σ(I )], where GunH is the guanidine cation (C(NH2)3)+, and Cit is the citric acid anion (C6H6O7)2?. The structure is composed of guanidinium cations and centrosymmetrical sym-cis-octahedral complex anions [Fe(Cit)2]2?. The Cit2? anion acts as a cyclic tridentate ligand and forms condensed fiveand six-membered metal-containing cycles.  相似文献   

20.
Ammonium decamolybdodimetallates (NH4)n[M2Mo10O34(OH)4] · 7H2O, where M = Cr3+ (n = 6), Cu2+ (n = 8), or Ni2+ (n = 8), were synthesized for the first time and studied by X-ray diffraction, thermogravimetry, and IR spectroscopy. The compounds crystallize in the triclinic system with the following unit cell parameters: a = 10.68(2) Å, b = 9.46(2) Å, c = 7.97(2) Å, α = 75.12(3)°, β = 96.82(3)°, γ = 102.21(3)°, V = 754.4(3) Å3, ρcalcd = 4.05 g/cm3, Z = 1 for the chromium compound; and a = 10.57(2) Å, b = 9.29(2) Å, c = 8.47(2) Å, α = 73.91(3)°, β = 96.05(3)°, γ = 104.71(3)°, V = 854.3(3) Å3, ρcalcd = 3.68 g/cm3, Z = 1 (for the copper compound); and a = 10.96(2) Å, b = 8.95(2) Å, c = 7.40(2) Å, α = 71.76(3)°, β = 97.04(3)°, γ = 102.91(3)°, V = 875.3(3)Å3, ρcalcd = 3.65 g/cm3, Z = 1 for the nickel compound.  相似文献   

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