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1.
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   

2.
Two hydrated uranyl arsenates and a uranyl phosphate were synthesized by hydrothermal methods in the presence of amine structure-directing agents and their structures determined: (N2C6H14)[(UO2)(AsO4)]2(H2O)3, DabcoUAs, {NH(C2H5)3}[(UO2)2(AsO4)(AsO3OH)], TriethUAs, and (N2C4H12)(UO2)[(UO2)(PO4)]4(H2O)2, PiperUP. Intensity data were collected at room temperature using MoKα X-radiation and a CCD-based area detector. The crystal structures were refined by full-matrix least-squares techniques on the basis of F2 to agreement indices (DabcoUAs, TriethUAs, PiperUP) wR2=5.6%, 8.3%, 7.2% for all data, and R1=2.9%, 3.3%, 4.0%, calculated for 1777, 5822, 9119 unique observed reflections (|Fo|?4σF), respectively. DabcoUAs is monoclinic, space group C2/m, Z=2, a=18.581(1), b=7.1897(4), c=7.1909(4) Å, β=102.886(1)°, V=936.43(9) Å3, Dcalc=3.50 g/cm3. TriethUAs is monoclinic, space group P21/n, Z=4, a=9.6359(4), b=18.4678(7), c=10.0708(4) Å, β=92.282(1)°, V=1790.7(1) Å3, Dcalc=3.41 g/cm3. PiperUP is monoclinic, space group Pn, Z=2, a=9.3278(4), b=15.5529(7), c=9.6474(5) Å, β=93.266(1)°, V=1397.3(1) Å3, Dcalc=4.41 g/cm3. The structure of DabcoUAs contains the autunite-type sheet formed by the sharing of vertices between uranyl square bipyramids and arsenate tetrahedra. The triethylenediammonium cations are located in the interlayer along with two H2O groups and are disordered. Both TriethUAs and PiperUP contain sheets formed of uranyl pentagonal bipyramids and tetrahedra (arsenate and phosphate, respectively) with the uranophane sheet-anion topology. In TriethUAs, triethlyammonium cations are located in the interlayer. In PiperUP, the sheets are connected by a uranyl pentagonal bipyramid that shares corners with phosphate tetrahedra of adjacent sheets, resulting in a framework with piperazinium cations and H2O groups in the cavities of the structure.  相似文献   

3.
Two homeotypic hydrated uranyl arsenates, (UO2)[(UO2)(AsO4)]2(H2O)4, UAs4, and (UO2)[(UO2)(AsO4)]2(H2O)5, UAs5 were synthesized by hydrothermal methods. Intensity data were collected at room temperature using MoKα X-radiation and a CCD-based area detector. Their crystal structures were solved by direct methods and refined by full-matrix least-squares techniques on the basis of F2 to agreement indices (UAs4, UAs5) wR2=0.116, 0.060, for all data, and R1=0.046, 0.033, calculated for 3176, 5306 unique observed reflections (|Fo|>4σF) respectively. UAs4 is monoclinic, space group P21/c, Z=4, a=11.238(1), b=7.152(1), c=21.941(2)Å, β=104.576(2)°, V=1706.8(1)Å3, Dcalc=4.51 g/cm3. UAs5 is orthorhombic, space group Pca21, Z=4, a=20.133(2), b=11.695(1), c=7.154(1)Å, V=1684.4(1)Å3, Dcalc=4.65 g/cm3. Both structures contain sheets of arsenate tetrahedra and uranyl pentagonal bipyramids, with composition [(UO2)(AsO4)]1− and the uranophane sheet anion-topology. The sheets are connected by a uranyl pentagonal bipyramid in the interlayer that shares corners with an arsenate tetrahedron on each of two adjacent sheets, resulting in open-frameworks with isolated H2O groups in the larger cavities of the structures. The uranyl arsenate sheet in UAs4 is relatively planar, and is topologically identical with the uranyl phosphate sheet in (UO2)[(UO2)(PO4)]2(H2O)4. The uranyl arsenate sheet in UAs5 is the same geometrical isomer as in UAs4, but is highly corrugated, exhibiting approximately right angle bends of the sheet after every second uranyl arsenate chain repeat.  相似文献   

4.
Two hydrated uranyl arsenates, Cs2(UO2)[(UO2)(AsO4)]4(H2O)2 (CsUAs) and Rb2(UO2)[(UO2)(AsO4)]4(H2O)4.5 (RbUAs), were synthesized by hydrothermal methods. Intensity data were collected at room temperature using MoKα radiation and a CCD-based area detector. The crystal structure of RbUAs was solved by direct methods, whereas the structure model of the phosphate Cs2(UO2)[(UO2)(PO4)]4(H2O)2 was used for CsUAs; both were refined by full-matrix least-squares techniques on the basis of F2 to agreement indices (CsUAs, RbUAs) wR2=0.061,0.041, for all data, and R1=0.032,0.021, calculated for 5098, 4991 unique observed reflections (|Fo|>4σF), respectively. The compound CsUAs is orthorhombic, space group Cmc21, Z=4, a=15.157(2), b=14.079(2), c=13.439(2) Å, V=2867.9(1) Å3. RbUAs is monoclinic, space group C2/m, Z=4, a=13.4619(4), b=15.8463(5), c=14.0068(4) Å, β=92.311(1)°, V=2985.52(2) Å3. The structures consist of sheets of arsenate tetrahedra and uranyl pentagonal bipyramids, with composition [(UO2)(AsO4)], that are topologically identical to the uranyl silicate sheets in uranophane-beta. These sheets are connected by a uranyl pentagonal bipyramid in the interlayer that shares corners with two arsenate tetrahedra on each of two adjacent sheets and whose fifth equatorial vertex is an H2O group, resulting in an open framework with alkali metal cations in the larger cavities of the structures. CsUAs is isostructural with its phosphate analogue, and has two Cs atoms and a H2O group in its structural cavities. RbUAs is not isostructural with its phosphate analogue, although it has a homeotypic framework. Its structural cavities are occupied by three Rb atoms and four H2O groups; one Rb position and three of the interstitial H2O groups are half-occupied. The partial occupancies of these positions probably result from the accommodation of the larger As atoms (relative to P) in the framework and resultant larger cavities.  相似文献   

5.
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   

6.
Two new tellurites, NH4RbTe4O9·2H2O and NH4CsTe4O9·2H2O have been synthesized and characterized. The compounds were synthesized hydrothermally, in near quantitative yields, using the alkali metal halide, TeO2, and NH4OH as reagents. The iso-structural materials exhibit layered, two-dimensional structural topologies consisting of TeOx (x=3, 4, or 5) polyhedra separated by NH4+, H2O, Rb+ or Cs+ cations. Unique to these materials is the presence of TeO3, TeO4, and TeO5 polyhedra. Thermogravimetric and infrared spectroscopic data are also presented. Crystal data: NH4RbTe4O9·2H2O: Monoclinic I2/a (no. 15), a=18.917(3) Å, b=6.7002(11) Å, c=21.106(5) Å, β=101.813(2)°, V=2618.5(9) Å3, Z=8; NH4CsTe4O9·2H2O: Monoclinic I2/a (no. 15), a=18.9880(12) Å, b=6.7633(4) Å, c=21.476(2) Å, β=102.3460(10)°, V=2694.2(3) Å3, Z=8.  相似文献   

7.
The hydrothermal syntheses, single crystal structures, and some properties of Ba2MnIIMn2III(SeO3)6 and PbFe2(SeO3)4 are reported. These related phases contain three-dimensional frameworks of vertex (FeO6) and vertex/edge linked (MnO6) octahedra and SeO3 pyramids. In each case, the MO6/SeO3 framework encloses two types of 8 ring channels, one of which encapsulates the extra-framework cations and one of which provides space for the SeIV lone pairs. Crystal data: Ba2Mn3(SeO3)6, Mr=1201.22, monoclinic, P21/c (No. 14), a=5.4717 (3) Å, b=9.0636 (4) Å, c=17.6586 (9) Å, β=94.519 (1)°, V=873.03 (8) Å3, Z=2, R(F)=0.031, wR(F2)=0.070; PbFe2(SeO3)4, Mr=826.73, triclinic, (No. 2), a=5.2318 (5) Å, b=6.7925 (6) Å, c=7.6445 (7) Å, α=94.300 (2)°, β=90.613 (2)°, γ=95.224 (2)°, V=269.73 (4) Å3, Z=1, R(F)=0.051, wR(F2)=0.131.  相似文献   

8.
Three new compounds, a one-dimensional (1D) zinc phosphite, (C4H8N2H4)[Zn(HPO3)2] (I), two three-dimensional (3D) metal phosphites (C4H8N2H4)[Zn3(HPO3)4] (II) and (C4H8N2H4)[Zn(3−x)Cox(HPO3)4(H2O)2] (x≈0.83) (III) have been synthesized under hydrothermal conditions templated by piperazine and characterized by single-crystal X-ray diffraction, XRD, IR, UV-vis spectra and SQUID magnetometer. Compound I displays 1D chain-like structure, containing corner-shared (cs) four-membered rings. Interestingly, the structures of II and III show 1D chains similar to those observed in I. It is noteworthy that III represents the first cobalt-substituted zinc-phosphite. Crystal data: I, monoclinic, C2/c, a=17.748(2) Å, b=7.428(9) Å, c=8.8071(11) Å, β=105.345(3)°, V=1091.9 Å3, Z=4. II, Monoclinic P21/c, a=9.9435(4) Å, b=10.1438(3) Å, c=17.8164(5) Å, β=95.665(2)°, V=1788.27 Å3, Z=4, and III, Monoclinic P21/c, a=7.2338(2) Å, b=15.0238(5) Å, c=9.2153(3) Å, β=107.741(2)°, V=953.88(5) Å3, Z=2.  相似文献   

9.
The reaction between PuO2 and SeO2 under mild hydrothermal conditions results in the formation of Pu(SeO3)2 as brick-red prisms. This compound adopts the Ce(SeO3)2 structure type, and consists of one-dimensional chains of edge-sharing [PuO8] distorted bicapped trigonal prisms linked by [SeO3] units into a three-dimensional network. Crystallographic data: Pu(SeO3)2, monoclinic, space group P21/n, a=6.960(1) Å, b=10.547(2) Å, c=7.245(1) Å, β=106.880(9)°, V=508.98(17) Å3, Z=4 (T=193 K), R(F)=2.92% for 83 parameters with 1140 reflections with I>2σ(I). Magnetic susceptibility data for Pu(SeO3)2 are linear from 35 to 320 K and yield an effective moment of 2.71(5) μB and a Weiss constant of −500(5) K.  相似文献   

10.
Single crystals of [H3dien]·(FeF6)·H2O (I) and [H3dien]·(CrF6)·H2O (II) are obtained by solvothermal synthesis under microwave heating. I is orthorhombic (Pna21) with a=11.530(2) Å, b=6.6446(8) Å, c=13.787(3) Å, V=1056.3(2) Å3 and Z=4. II is monoclinic (P21/c) with a=13.706(1) Å, b=6.7606(6) Å, c=11.3181(9) Å, β=99.38(1)°, V=1034.7(1) Å3 and Z=4. The structure determinations, performed from single crystal X-ray diffraction data, lead to the R1/wR2 reliability factors 0.028/0.066 for I and 0.035/0.102 for II. The structures of I and II are built up from isolated FeF6 or CrF6 octahedra, water molecules and triprotonated amines. In both structures, each octahedron is connected by hydrogen bonds to six organic cations and two water molecules. The iron-based compound is also characterized by 57Fe Mössbauer spectrometry: the hyperfine structure confirms the presence of Fe3+ in octahedral coordination and reveals the existence of paramagnetic spin fluctuations.  相似文献   

11.
A new open-framework compound, [C6H14N2][(UO2)4(HPO4)2(PO4)2(H2O)]·H2O, (DUP-1) has been synthesized under mild hydrothermal conditions. The resulting structure consists of diprotonated DABCOH22+ (C6H14N22+) cations and occluded water molecules occupying the channels of a complex uranyl phosphate three-dimensional framework. The anionic lattice contains uranophane-like sheets connected by hydrated pentagonal bipyramidal UO7 units. [C6H14N2][(UO2)4(HPO4)2(PO4)2(H2O)]·H2O possesses five crystallographically unique U centers. U(VI) is present here in both six- and seven-coordinate environments. The DABCOH22+ cations are held within the channels by hydrogen bonds to both two uranyl oxygen atoms and a μ2-O atom. Crystallographic data (193 K, Mo Kα, λ=0.71073 Å): DUP-1, monoclinic, P21/n, a=7.017(1) Å, b=21.966(4) Å, c=17.619(3) Å, β=90.198(3)°, Z=4, R(F)=4.76% for 382 parameters with 6615 reflections with I>2σ(I).  相似文献   

12.
Hydrothermal reactions of lead(II) acetate with 5-sulfoisophthalic acid monosodium salt (NaH2BTS) and N-(phosphonomethyl)-N-methylglycine, MeN(CH2CO2H)(CH2PO3H2) (H3L1), or a new aminodiphosphonic acid, 3-Pyridyl-CH2N(CH2PO3H2)2 (H4L2), afforded two novel lead(II) phosphonate-sulfonate hybrids, namely, Pb3[L1][BTS][H2O]·H2O 1 and Pb2[HL3][BTS]·H2O 2 (H2L3=3-Pyridyl-CH2(Me)N(CH2PO3H2)). H2L3 was formed as a result of the decomposition of one phosphonate group in H4L2 during the reaction. Compound 1 crystallizes in the triclinic space group with a=9.9148(4) Å, b=10.4382(4) Å, c=10.6926(2) Å, α=96.495(2)°, β=110.599(2)°, γ=98.433(2)°, V=1008.31(6) Å3, and Z=2. The structure of compound 1 features a 3D network built from the interconnection of hexanuclear Pb6(L1)2 units and 1D double chains of lead(II) carboxylate-sulfonate. Compound 2 crystallizes in the monoclinic space group P21/c with a=9.5403(7) Å, b=11.6170(8) Å, c=19.7351(15) Å, β=97.918(2)°, V=2166.4(3) Å3, and Z=4. Compound 2 has a 3D network structure built by the cross-linkage of 1D double chains of lead(II) phosphonates and 2D layers of lead(II) carboxylate-sulfonate.  相似文献   

13.
The new selenite-chlorides with composition Sr3(SeO3)2Cl2 (I) and Sr2M(SeO3)2Cl2 (M=Co, Ni (II and III)) were obtained. They crystallize in monoclinic system I: space group C2/m, a=13.203(2) Å, b=5.5355(8) Å, c=6.6170(10) Å, β=95.89(1)°, Z=2; II Space group P21/n, a=5.3400(10) Å, b =6.4279(6) Å, c=12.322(1) Å, β=92.44(1)°, Z=2; III: space group P21/n, a=5.3254(11) Å, b=6.4363(13) Å, c=12.197(2), β=92.53(3)°, Z=2. All three compounds are constructed in the same manner. Sr polyhedra form infinite layers, which are interconnected into a 3D framework by means of Sr polyhedra in the case of I or Co and Ni polyhedra in the case of II and III. Se atoms are situated inside the channels of the 3D framework. The topological analysis of ELF for I confirmed that the lone electron pairs of SeO3 groups are located inside these channels.  相似文献   

14.
Two new lanthanum sulfates DySO4(OH) 1 and Eu2(SO4)3(H2O)82 have been hydrothermally synthesized. The colorless crystals were characterized by IR, TGA, ICP and XRD. The structure was determined by single-crystal X-ray diffraction. 1 crystallizes with monoclinic symmetry, space group P2(1)/n [a=7.995(4) Å, b=10.945(5) Å, c=8.164(4) Å, α=90°, β=93.619(6)°, γ=90°, V=713.0(5) Å3, Z=8]. It displays a three-dimensional framework, based on the novel Dy-O chains connected by the sulfate groups through helical chains. 2 crystallizes with monoclinic symmetry, space group C2/c, [a=13.5605(17) Å, b=6.7676(8) Å, c=18.318(2) Å, α=90°, β=102.265(2)°, γ=90°, V=1642.7 (4) Å3, Z=4]. Its layered framework is attained by the europium atoms connected by the sulfate groups arranged in a helical manner.  相似文献   

15.
The reaction of Os3(CO)12 with an excess of 1-hydroxypyridine-2-thione and Me3NO gives three mononuclear osmium complexes Os(CO)22-SC5H4N(O))2 (1), Os(CO)22-SC5H4N(O))(η2-SC5H4N) (2), and Os(CO)22-SC5H4N)2 (3). The results of single-crystal X-ray analyses reveal that complex 1 contains two O,S-chelate pyridine-2-thione N-oxide (PyOS) ligands, whereas complex 2 contains one O,S-chelate PyOS and one N,S-chelate pyridine-2-thiolate group. The unique structure of 2 provides evidence of the pathway for this transformation. When this reaction was monitored by 1H NMR spectroscopy the triosmium complexes Os3(CO)10(μ-H)(μ-η1-S-C5H4N(O)) (4) and Os3(CO)9(μ-H)(μ-η12-SC5H4N(O)) (5) were identified as intermediates in the formation of the mononuclear final products 1-3. The proposed pathway is further supported by the observation of several dinuclear osmium intermediates by electrospray ionization mass spectrometry. In addition, the reaction of Os3(CO)12 with 1-hydroxypyridine-2-thione in the absence of Me3NO at 90 °C generated mononuclear complex 2 as the major product along with smaller amounts of complexes 1 and 3. These results suggest that the N-oxide facilitates the decarbonylation reaction. Crystal data for 1: monoclinic, space group C2/c, a = 26.9990(5) Å, b = 7.6230(7) Å, c = 14.2980(13) Å, β = 101.620(2)°, V = 2882.4(4) Å3, Z = 8. Crystal data for 2: monoclinic, space group C2/c, a = 5.7884(3) Å, b = 13.9667(7) Å, c = 17.2575(9) Å, β = 96.686(1)°, V = 1385.69(12) Å3, Z = 4.  相似文献   

16.
Two new alkali uranyl oxychloro vanadates M7(UO2)8(VO4)2O8Cl with M=Rb, Cs, have been synthesized by solid-state reactions and their structures determined from single-crystal X-ray diffraction data. They crystallize in the orthorhombic system with space groups Pmcn and Pmmn, respectively. The a and b unit cell parameters are almost identical in both compounds while the c parameter in the Rb compound is doubled: Rb—a=21.427(5) Å, b=11.814(3) Å, c=14.203(3) Å, V=3595.1(1) Å3, Z=4, ρmes=5.93(2) g/cm3, ρcal=5.82(1) g/cm3; Cs—a=21.458(3) Å, b=11.773(2) Å, c=7.495(1) Å, V=1893.6(5) Å3, Z=2, ρmes=6.09(2) g/cm3, ρcal=6.11(1) g/cm3. A full-matrix least-squares refinement yielded R1=0.0221, wR2=0.0562 for 2675 independent reflections and R1=0.0386, wR2=0.1042 for 2446 independent reflections, for the Rb and Cs compounds, respectively. Data were collected with Mo(Kα) radiation and a charge coupled device (CCD) detector of a Bruker diffractometer. Both structures are characterized by [(UO2)8(VO4)2O8Cl]n7n layers parallel to the (001) plane. The layers are built up from VO4 tetrahedra, UO7 and UO6Cl pentagonal bipyramids, and UO6 distorded octahedra. The UO7 and UO6Cl pentagonal bipyramids are associated by sharing opposite equatorial edges to form infinite chains (UO5-UO4Cl-UO5)n parallel to the a axis. These chains are linked together by VO4 tetrahedra, UO6 octahedra, UO7 corner sharing and UO6Cl, Cl sharing. Both structures differ simply by the symmetry of the layers. The unit cell contains one centrosymmetric layer in the Cs compound, whereas in the two-layer unit cell of the Rb compound, two non-centrosymmetric consecutive layers are related by an inversion center. The layers appear to be held together by the alkali ions. The mobility of the M+ ions within the interlayer space in M7(UO2)8(VO4)2O8Cl and carnotite analog compounds is compared.  相似文献   

17.
Seven new uranyl vanadates with mono-protonated amine or tetramethylammonium used as structure directing cations, (C2NH8)2{[(UO2)(H2O)][(UO2)(VO4)]4}·H2O (DMetU5V4) (C2NH8){[(UO2)(H2O)2][(UO2)(VO4)]3}·H2O (DMetU4V3), (C5NH6)2{[(UO2)(H2O)][(UO2)(VO4)]4}·H2O (PyrU5V4), (C3NH10){[(UO2)(H2O)2][(UO2)(VO4)]3}·H2O (isoPrU4V3), (N(CH3)4){[(UO2)(H2O)2][(UO2)(VO4)]3}·H2O (TMetU4V3), (C6NH14){[(UO2)(H2O)2][(UO2)(VO4)]3}·H2O (CHexU4V3), and (C4NH12){[(UO2)(H2O)][(UO2)(VO4)]3} (TButU4V3) were prepared from mild-hydrothermal reactions using dimethylamine, pyridine, isopropylamine, tetramethylammonium hydroxide, cyclohexylamine and tertiobutylamine, respectively, with uranyl nitrate and vanadium oxide in acidic medium. The structures were solved using single-crystal X-ray diffraction data. The compounds exhibit three-dimensional uranyl-vanadate inorganic frameworks built from uranophane-type uranyl-vanadate layers pillared by uranyl polyhedra with cavities in between occupied by protonated organic moieties. In the uranyl-vanadate layers the orientations of the vanadate tetrahedra give new geometrical isomers leading to unprecedented pillared systems and new inorganic frameworks with U/V=4/3. Crystallographic data: (DMetU5V4) orthorhombic, Cmc21 space group, a=15.6276(4), b=14.1341(4), c=13.6040(4) Å; (DMetU4V3) monoclinic, P21/n space group, a=10.2312(4), b=13.5661(7), c=17.5291(7) Å, β=96.966(2); (PyrU5V4), triclinic, P1 space group, a=9.6981(3), b=9.9966(2), c=10.5523(2) Å, α=117.194(1), β=113.551(1), γ=92.216(1)°; (isoPrU4V3) monoclinic, P21/n space group, a=10.3507(1), b=13.6500(2), c=17.3035(2) Å, β=97.551(1)°; (TMetU4V3) orthorhombic, Pbca space group, a=17.1819(2), b=13.6931(1), c=21.4826(2) Å; (CHexU4V3), triclinic P−1 space group, a=9.8273(6), b=11.0294(7), c=12.7506(8) Å, α=98.461(3), β=96.437(3), γ=105.955(3)°; (TButU4V3), monoclinic, P21/m space group, a=9.8048(4), b=17.4567(8), c=15.4820(6) Å, β=106.103(2).  相似文献   

18.
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   

19.
Two uranyl tellurates, AgUO2(HTeO5) (1) and Pb2UO2(TeO6) (2), were synthesized under hydrothermal conditions and were structurally, chemically, and spectroscopically characterized. 1 crystallizes in space group Pbca, a=7.085(2) Å, b=11.986(3) Å, c=13.913(4) Å, V=1181.5(5) Å3, Z=8; 2 is in P2(1)/c, a=5.742(1) Å, b=7.789(2) Å, c=7.928(2) Å, V=90.703(2) Å3, and Z=2. These are the first structures reported for uranyl compounds containing tellurate. The U6+ cations are present as (UO2)2+ uranyl ions that are coordinated by O atoms to give pentagonal and square bipyramids in compounds 1 and 2, respectively. The structural unit in 1 is a sheet consisting of chains of edge-sharing uranyl pentagonal bipyramids that are one bipyramid wide, linked through the dimers of TeO6 octahedra. In 2, uranyl square bipyramids share each of their equatorial vertices with different TeO6 octahedra, giving a sheet with the autunite-type topology. Sheets in 1 and 2 are connected through the low-valence cations that are located in the interlayer region. The structures of 1 and 2 are compared to those of uranyl compounds containing octahedrally coordinated cations.  相似文献   

20.
Two layered indium oxalates, In(C2O4)2.5(C3N2H12)(H2O)3, I, and In(C2O4)1.5(H2O)3, II, have been hydrothermally synthesized. In I, the linkage between indium and oxalate units gives rise to a sheet with a rectangular 12-membered aperture (six indium atoms and six oxalate units). Indium atom of II has an unusual pentagonal bipyramidal coordination arrangement. The connectivity between indium and oxalate units forms a neutral puckered layer with 12- (along a-axis) and eight-membered (along b-axis) apertures. Crystal data for these two indium oxalates are as follows: I, triclinic, space group: P-1 (No. 2), a=8.725(3) Å, b=9.170(3) Å, c=9.901(3) Å, α=98.101(4)°, β=97.068(4)°, γ=102.403(4)°, V=756.3(4) Å3, Z=2, M=463.0(5), ρcalc=2.042 g/cm3, R1=0.0377, wR2=0.0834. II, monoclinic, space group: P21/c (No. 14), a=10.203(5) Å, b=6.638(1) Å, c=11.152(7) Å, β=95.649(4)°, V=751.7(4)Å3, Z=4, M=300.9(0), ρcalc=2.659 g/cm3, R1=0.0229, wR2=0.0488. TG analyses indicate the water molecules of I can be removed at 150°C. The dehydrated product retains structural integrity.  相似文献   

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