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1.
Tetsuya Kawano 《Journal of solid state chemistry》2011,184(9):2466-2471
Single crystals of new oxyborates, Mg5NbO3(BO3)3 and Mg5TaO3(BO3)3, were prepared at 1370 °C in air using B2O3 as a flux. They were colorless and transparent with block shapes. X-ray diffraction analysis of the single crystals revealed Mg5NbO3(BO3)3 and Mg5TaO3(BO3)3 to be isostructural. The X-ray diffraction reflections were indexed to the orthorhombic Pnma (No. 62) system with a=9.3682(3) Å, b=9.4344(2) Å, c=9.3379(3) Å and Z=4 for Mg5NbO3(BO3)3 and a=9.3702(3) Å, b=9.4415(3) Å, c=9.3301(2) Å and Z=4 for Mg5TaO3(BO3)3. The crystal structures of Mg5NbO3(BO3)3 and Mg5TaO3(BO3)3 are novel warwickite-type superstructures having ordered arrangements of Mg and Nb/Ta atoms. Polycrystals of Mg5NbO3(BO3)3 prepared by solid state reaction at 1200 °C in air showed broad blue-to-green emission with a peak wavelength of 470 nm under 270 nm ultraviolet excitation at room temperature. 相似文献
2.
New uranyl vanadates A3(UO2)7(VO4)5O (M=Li (1), Na (2), Ag (3)) have been synthesized by solid-state reaction and their structures determined from single-crystal X-ray diffraction data for 1 and 3. The tetragonal structure results of an alternation of two types of sheets denoted S for ∞2[UO2(VO4)2]4− and D for ∞2[(UO2)2(VO4)3]5− built from UO6 square bipyramids and connected through VO4 tetrahedra to ∞1[U(3)O5-U(4)O5]8− infinite chains of edge-shared U(3)O7 and U(4)O7 pentagonal bipyramids alternatively parallel to a- and b-axis to construct a three-dimensional uranyl vanadate arrangement. It is noticeable that similar ∞[UO5]4− chains are connected only by S-type sheets in A2(UO2)3(VO4)2O and by D-type sheets in A(UO2)4(VO4)3, thus A3(UO2)7(VO4)5O appears as an intergrowth structure between the two previously reported series. The mobility of the monovalent ion in the mutually perpendicular channels created in the three-dimensional arrangement is correlated to the occupation rate of the sites and by the geometry of the different sites occupied by either Na, Ag or Li. Crystallographic data: 293 K, Bruker X8-APEX2 X-ray diffractometer equipped with a 4 K CCD detector, MoKα, λ=0.71073 Å, tetragonal symmetry, space group P4¯m2, Z=1, full-matrix least-squares refinement on the basis of F2; 1,a=7.2794(9) Å, c=14.514(4) Å, R1=0.021 and wR2=0.048 for 62 parameters with 782 independent reflections with I?2σ(I); 3, a=7.2373(3) Å, c=14.7973(15) Å, R1=0.041 and wR2=0.085 for 60 parameters with 1066 independent reflections with I?2σ(I). 相似文献
3.
Ytterbium(III) tetraaquatris(tetraoxorhenate(VII)), Yb(ReO4)3(H2O)4, was prepared by the reaction of Yb2O3 with concentrated HReO4 at room temperature. The colorless compound crystallizes in the monoclinic space group P21/n (No. 14) with four formula units per unit cell (a=730.5(1) pm, b=1484.1(5) pm, c=1311.7(2) pm, β=93.69(1)). The main feature of the crystal structure is the formation of chains ∞1[Yb(H2O)4(ReO4)2(ReO4)2/2] running along [100]. This arrangement shows distorted cubic antiprisms of [Yb(H2O)4(ReO4)2(ReO4)2/2] interconnected via the ReO4− ligands. The chains are held together in the solid by hydrogen bonding. The compound is paramagnetic and follows the Curie-Weiss law with a magnetic moment of 4.0 μB at room temperature and θ=−42 K. It loses hydration water in two steps at temperatures below 400 K; decomposition begins at 850 K, forming Yb2O3(Re2O7)2 and is complete at 1350 K leading to Yb2O3 as final product. 相似文献
4.
Three new compounds Ca(HF2)2, Ba4F4(HF2)(PF6)3 and Pb2F2(HF2)(PF6) were obtained in the system metal(II) fluoride and anhydrous HF (aHF) acidified with excessive PF5. The obtained polymeric solids are slightly soluble in aHF and they crystallize out of their aHF solutions. Ca(HF2)2 was prepared by simply dissolving CaF2 in a neutral aHF. It represents the second known compound with homoleptic HF environment of the central atom besides Ba(H3F4)2. The compounds Ba4F4(HF2)(PF6)3 and Pb2F2(HF2)(PF6) represent two additional examples of the formation of a polymeric zigzag ladder or ribbon composed of metal cation and fluoride anion (MF+)n besides PbF(AsF6), the first isolated compound with such zigzag ladder. The obtained new compounds were characterized by X-ray single crystal diffraction method and partly by Raman spectroscopy. Ba4F4(HF2)(PF6)3 crystallizes in a triclinic space group P1¯ with a=4.5870(2) Å, b=8.8327(3) Å, c=11.2489(3) Å, α=67.758(9)°, β=84.722(12), γ=78.283(12)°, V=413.00(3) Å3 at 200 K, Z=1 and R=0.0588. Pb2F2(HF2)(PF6) at 200 K: space group P1¯, a=4.5722(19) Å, b=4.763(2) Å, c=8.818(4) Å, α=86.967(10)°, β=76.774(10)°, γ=83.230(12)°, V=185.55(14) Å3, Z=1 and R=0.0937. Pb2F2(HF2)(PF6) at 293 K: space group P1¯, a=4.586(2) Å, b=4.781(3) Å, c=8.831(5) Å, α=87.106(13)°, β=76.830(13)°, γ=83.531(11)°, V=187.27(18) Å3, Z=1 and R=0.072. Ca(HF2)2 crystallizes in an orthorhombic Fddd space group with a=5.5709(6) Å, b=10.1111(9) Å, c=10.5945(10) Å, V=596.77(10) Å3 at 200 K, Z=8 and R=0.028. 相似文献
5.
Richard E. Sykora Peter Khalifah Zerihun Assefa Richard G. Haire 《Journal of solid state chemistry》2008,181(8):1867-1875
Colorless single crystals of Gd(IO3)3 or pale pink single crystals of Er(IO3)3 have been formed from the reaction of Gd metal with H5IO6 or Er metal with H5IO6 under hydrothermal reaction conditions at 180 °C. The structures of both materials adopt the Bi(IO3)3 structure type. Crystallographic data are (MoKα, λ=0.71073 Å): Gd(IO3)3, monoclinic, space group P21/n, a=8.7615(3) Å, b=5.9081(2) Å, c=15.1232(6) Å, β=96.980(1)°, V=777.03(5) Z=4, R(F)=1.68% for 119 parameters with 1930 reflections with I>2σ(I); Er(IO3)3, monoclinic, space group P21/n, a=8.6885(7) Å, b=5.9538(5) Å, c=14.9664(12) Å, β=97.054(1)°, V=768.4(1) Z=4, R(F)=2.26% for 119 parameters with 1894 reflections with I>2σ(I). In addition to structural studies, Gd(IO3)3, Er(IO3)3, and the isostructural Yb(IO3)3 were also characterized by Raman spectroscopy and magnetic property measurements. The results of the Raman studies indicated that the vibrational profiles are adequately sensitive to distinguish between the structures of the iodates reported here and other lanthanide iodate systems. The magnetic measurements indicate that only in Gd(IO3)3 did the 3+ lanthanide ion exhibit its full 7.9 μB Hund's rule moment; Er3+ and Yb3+ exhibited ground state moments and gap energy scales of 8.3 μB/70 K and 3.8 μB/160 K, respectively. Er(IO3)3 exhibited extremely weak ferromagnetic correlations (+0.4 K), while the magnetic ions in Gd(IO3)3 and Yb(IO3)3 were fully non-interacting within the resolution of our measurements (∼0.2 K). 相似文献
6.
Zerihun Assefa Jie Ling Thomas E. Albrecht-Schmitt 《Journal of solid state chemistry》2006,179(12):3653-3663
The reaction of Lu3+ or Yb3+ and H5IO6 in aqueous media at 180 °C leads to the formation of Yb(IO3)3(H2O) or Lu(IO3)3(H2O), respectively, while the reaction of Yb metal with H5IO6 under similar reaction conditions gives rise to the anhydrous iodate, Yb(IO3)3. Under supercritical conditions Lu3+ reacts with HIO3 and KIO4 to yield the isostructural Lu(IO3)3. The structures have been determined by single-crystal X-ray diffraction. Crystallographic data are (MoKα, λ=0.71073 Å): Yb(IO3)3, monoclinic, space group P21/n, a=8.6664(9) Å, b=5.9904(6) Å, c=14.8826(15) Å, β=96.931(2)°, V=766.99(13), Z=4, R(F)=4.23% for 114 parameters with 1880 reflections with I>2σ(I); Lu(IO3)3, monoclinic, space group P21/n, a=8.6410(9), b=5.9961(6), c=14.8782(16) Å, β=97.028(2)°, V=765.08(14), Z=4, R(F)=2.65% for 119 parameters with 1756 reflections with I>2σ(I); Yb(IO3)3(H2O), monoclinic, space group C2/c, a=27.2476(15), b=5.6296(3), c=12.0157(7) Å, β=98.636(1)°, V=1822.2(2), Z=8, R(F)=1.51% for 128 parameters with 2250 reflections with I>2σ(I); Lu(IO3)3(H2O), monoclinic, space group C2/c, a=27.258(4), b=5.6251(7), c=12.0006(16) Å, β=98.704(2)°, V=1818.8(4), Z=8, R(F)=1.98% for 128 parameters with 2242 reflections with I>2σ(I). The f elements in all of the compounds are found in seven-coordinate environments and bridged with monodentate, bidentate, or tridentate iodate anions. Both Lu(IO3)3(H2O) and Yb(IO3)3(H2O) display distinctively different vibrational profiles from their respective anhydrous analogs. Hence, the Raman profile can be used as a complementary diagnostic tool to discern the different structural motifs of the compounds. 相似文献
7.
Pavel Kopel Jiří Kameníček Václav Petříček Aleš Kurečka Božena Kalinska Jerzy Mrozinski 《Polyhedron》2007
Nickel and copper complexes containing 1,3,5-benzenetricarboxylic acid, with a combination of selected N-donor ligands and Schiff bases, of the composition Ni3(bimz)6(btc)2 · 12H2O (1), Ni3(btz)9(btc)2 · 12H2O (2), Ni2(L1)(btc) · 7H2O (3), Ni3(L2)2(Hbtc) · 9H2O (4), Ni2(L3)(btc) · 4H2O (5), Cu2(L4)(btc) · 7H2O (6), [Cu3(pmdien)3(btc)](ClO4)3 · 6H2O (7) and [Cu3(mdpta)3(btc)](ClO4)3 · 4H2O (8); H3btc = 1,3,5-benzenetricarboxylic acid, bimz = benzimidazole, btz = 1,2,3-benztriazole, L1 = 2-[(phenylimino)methyl]phenol, L2 = N,N′-bis-(salicylidene)propylenediamine, L3 = 2-{[(2-nitrophenyl)methylene]amino}phenol, L4 = 2-[(4-methoxy-phenylimino)methyl]phenol, pmdien = N,N,N′,N″,N″-pentamethyldiethylenetriamine, mdpta = N,N-bis-(3-aminopropyl)methylamine, have been synthesized. The complexes have been studied by elemental analysis, IR, UV–Vis spectroscopies, magnetochemical and conductivity measurements and selected compounds also by thermal analysis. The crystal and molecular structure of complex 8 was solved. The complex is trinuclear with btc3−-bridge. The coordination polyhedron around each copper atom can be described as a distorted square with a CuON3 chromophore formed by one oxygen atom of carboxylate and three nitrogen atoms of mdpta. The magnetic properties of 8 have been studied in the 1.8–300 K temperature range revealing a very weak antiferromagnetic exchange interaction with J = −0.56 cm−1 for g = 2.13(9). The antimicrobial activities against selected strains of bacteria were evaluated. It was found that only complex 5 is able to inhibit the growth of Staphylococcus strains. 相似文献
8.
Lei Yang 《Journal of solid state chemistry》2005,178(4):1197-1202
A new three-dimensional open-framework gallophosphate: [H3N(CH2)2NH3]1/2·[Ga5 (PO4)4(OH)4] has been prepared by hydro(solvo)thermal synthesis in presence of ethylenediamine (en) as structure-directing agent. Its structure was determined by means of single-crystal X-ray diffraction analysis with the following crystal data: monoclinic space group C2/m, a=10.1604(9) Å, b=12.0085(15) Å, c=7.1892(7) Å, β=90.797(6)°, V=877.08(16) Å3, Z=2, R1=0.0264, wR2=0.0764. The total numbers of measured reflections and unique reflections were 3508 and 1300, respectively. It is built up from a new secondary building unit (SBU) Ga4P4O20(OH)4, in which Ga atoms exhibit distorted trigonal bipyramidal coordination and P atoms are in tetrahedral coordination. The SBU Ga4P4O20(OH)4 are linked into a layer by bridge oxygen atoms. The GaO4(OH)2 octahedra link the layers into a three-dimentional framework. Diprotonated ethylenediamine was found in the channel of the framework. The material was characterized by IR spectroscopy, 1H NMR spectra, thermogravimetric and differential thermal analyses and elemental analysis. 相似文献
9.
Two new potassium uranyl molybdates K2(UO2)2(MoO4)O2 and K8(UO2)8(MoO5)3O6 have been obtained by solid state chemistry . The crystal structures were determined by single crystal X-ray diffraction data, collected with MoKα radiation and a charge coupled device (CCD) detector. Their structures were solved using direct methods and Fourier difference techniques and refined by a least square method on the basis of F2 for all unique reflections, with R1=0.046 for 136 parameters and 1412 reflections with I?2σ(I) for K2(UO2)2(MoO4)O2 and R1=0.055 for 257 parameters and 2585 reflections with I?2σ(I) for K8(UO2)8(MoO5)3O6. The first compound crystallizes in the monoclinic symmetry, space group P21/c with a=8.250(1) Å, b=15.337(2) Å, c=8.351(1) Å, β=104.75(1)°, ρmes=5.22(2) g/cm3, ρcal=5.27(2) g/cm3 and Z=4. The second material adopts a tetragonal unit cell with a=b=23.488(3) Å, c=6.7857(11) Å, ρmes=5.44(3) g/cm3, ρcal=5.49(2) g/cm3, Z=4 and space group P4/n.In both structures, the uranium atoms adopt a UO7 pentagonal bipyramid environment, molybdenum atoms are in a MoO4 tetrahedral environment for K2(UO2)2(MoO4)O2 and MoO5 square pyramid coordination in K8(UO2)8(MoO5)3O6. These compounds are characterized by layered structures. The association of uranyl ions (UO7) and molybdate oxoanions MoO4 or MoO5, give infinite layers [(UO2)2(MoO4)O2]2− and [(UO2)8(MoO5)3O6]8− in K2(UO2)2(MoO4)O2 and K8(UO2)8(MoO5)3O6, respectively. Conductivity properties of alkali metal within the interlayer spaces have been measured and show an Arrhenius type evolution. 相似文献
10.
Jin-Xiao Mi Cheng-Xin Wang Rong Li Yuanming Pan 《Journal of solid state chemistry》2010,183(12):2763-2769
A new iron phosphate (NH4)4Fe3(OH)2F2[H3(PO4)4] has been synthesized hydrothermally at HF concentrations from 0.5 to 1.2 mL. Single-crystal X-ray diffraction analysis reveals its three-dimensional open-framework structure (monoclinic, space group P21/n (No. 14), a=6.2614(13) Å, b=9.844(2) Å, c=14.271(3) Å, β=92.11(1)°, V=879.0(3) Å3). This structure is built from isolated linear trimers of corner-sharing Fe(III) octahedra, which are linked by (PO4) groups to form ten-membered-ring channels along [1 0 0]. This isolated, linear trimer of corner-sharing Fe(III) octahedra, [(FeO4)3(OH)2F2], is new and adds to the diverse linkages of Fe polyhedra as secondary building units in iron phosphates. The trivalent iron at octahedral sites for the title compound has been confirmed by synchrotron Fe K-edge XANES spectra and magnetic measurements. Magnetic measurements also show that this compound exhibit a strong antiferromagnetic exchange below TN=17 K, consistent with superexchange interactions expected for the linear trimer of ferric octahedra with the Fe-F-Fe angle of 132.5°. 相似文献
11.
Jie Ling 《Journal of solid state chemistry》2007,180(5):1601-1607
Ag4(Mo2O5)(SeO4)2(SeO3) has been synthesized by reacting AgNO3, MoO3, and selenic acid under mild hydrothermal conditions. The structure of this compound consists of cis-MoO22+ molybdenyl units that are bridged to neighboring molybdenyl moieties by selenate anions and by a bridging oxo anion. These dimeric units are joined by selenite anions to yield zigzag one-dimensional chains that extended down the c-axis. Individual chains are polar with the C2 distortion of the Mo(VI) octahedra aligning on one side of each chain. However, the overall structure is centrosymmetric because neighboring chains have opposite alignment of the C2 distortion. Upon heating Ag4(Mo2O5)(SeO4)2(SeO3) looses SeO2 in two distinct steps to yield Ag2MoO4. Crystallographic data: (193 K; MoKα, λ=0.71073 Å): orthorhombic, space group Pbcm, a=5.6557(3), b=15.8904(7), c=15.7938(7) Å, V=1419.41(12), Z=4, R(F)=2.72% for 121 parameters with 1829 reflections with I>2σ(I). Ag2(MoO3)3SeO3 was synthesized by reacting AgNO3 with MoO3, SeO2, and HF under hydrothermal conditions. The structure of Ag2(MoO3)3SeO3 consists of three crystallographically unique Mo(VI) centers that are in 2+2+2 coordination environments with two long, two intermediate, and two short bonds. These MoO6 units are connected to form a molybdenyl ribbon that extends along the c-axis. These ribbons are further connected together through tridentate selenite anions to form two-dimensional layers in the [bc] plane. Crystallographic data: (193 K; MoKα, λ=0.71073 Å): monoclinic, space group P21/n, a=7.7034(5), b=11.1485(8), c=12.7500(9) Å, β=105.018(1) V=1002.7(2), Z=4, R(F)=3.45% for 164 parameters with 2454 reflections with I>2σ(I). Ag2(MoO3)3SeO3 decomposes to Ag2Mo3O10 on heating above 550 °C. 相似文献
12.
Karolina Kazmierczak 《Journal of solid state chemistry》2011,184(5):1221-1226
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
13.
Richard E. Sykora Brian L. Scott Thomas E. Albrecht-Schmitt 《Journal of solid state chemistry》2004,177(3):725-730
The uranyl and neptunyl(VI) iodates, K3[(UO2)2(IO3)6](IO3)·H2O (1) and K[NpO2(IO3)3]·1.5H2O (2), have been prepared and crystallized under mild hydrothermal conditions. The structures of 1 and 2 both contain one-dimensional ∞1[AnO2(IO3)3]1−(An=U,Np) ribbons that consist of approximately linear actinyl(VI) cations bound by iodate anions to yield AnO7 pentagonal bipyramids. The AnO7 units are linked by bridging iodate anions to yield chains that are in turn coupled by additional iodate anions to yield ribbons. The edges of the ribbons are terminated by monodentate iodate anions. For 1 and 2, K+ cations and water molecules separate the ribbons from one another. In addition, isolated iodate anions are also found between ∞1[UO2(IO3)3]1− ribbons in 1. In order to aid in the assignment of oxidation states in neptunyl containing compounds, a bond-valence sum parameter of 2.018 Å for Np(VI) bound exclusively to oxygen has been developed with b=0.37 Å. Crystallographic data (193 K, MoKα, λ=0.71073): 1, triclinic, , a=7.0609(4) Å, b=14.5686(8) Å, c=14.7047(8) Å, α=119.547(1)°, β=95.256(1)°, γ=93.206(1)°, Z=2, R(F)=2.49% for 353 parameters with 6414 reflections with I>2σ(I); (203 K, MoKα, λ=0.71073): 2, monoclinic, P21/c, a=7.796(4) Å, b=7.151(3) Å, c=21.79(1) Å, β=97.399(7)°, Z=4, R(F)=6.33% for 183 parameters with 2451 reflections with I>2σ(I). 相似文献
14.
Edurne S. Larrea José L. Pizarro Teófilo Rojo 《Journal of solid state chemistry》2007,180(5):1686-1697
The Mn5−xCox(HPO4)2(PO4)2(H2O)4 (x=1.25, 2, 2.5, 3) finite solid solution has been synthesized by mild hydrothermal conditions under autogeneous pressure. The phases crystallize in the C2/c space group with Z=4, belonging to the monoclinic system. The unit-cell parameters obtained from single crystal X-ray diffraction are: a=17.525(1), b=9.0535(6), c=9.4517(7) Å, β=96.633(5) ° being R1=0.0436, wR2=0.0454 for Mn75Co25; a=17.444(2), b=9.0093(9), c=9.400(1) Å, β=96.76(1) ° being R1=0.0381, wR2=0.0490 for Mn60Co40; a=17.433(2), b=8.9989(9), c=9.405(1) Å, β=96.662(9) ° being R1=0.0438, wR2=0.0515 for Mn50Co50 and a=17.4257(9), b=8.9869(5), c=9.3935(5) Å, β=96.685(4) ° being R1=0.0296, wR2=0.0460 for Mn40Co60. The structure consists of a three dimensional network formed by octahedral pentameric entities (Mn,Co)5O16(H2O)6 sharing vertices with the (PO4)3− and (HPO4)2− tetrahedra. The limit of thermal stability of these compounds is, approximately, 165 °C, near to this mean temperature the phases loose their water content in two successive steps. IR spectra show the characteristic bands of the water molecules and the phosphate and hydrogen-phosphate oxoanions. The diffuse reflectance spectra are consistent with the presence of MO6 octahedra environments in slightly distorted octahedral geometry, except for the M(3)O6 octahedron which presents a remarkable distortion and so a higher Dq parameter. The mean value for the Dq and B-Racah parameter for the M(1),(2)O6 octahedra is 685 and 850 cm−1, respectively. These parameters for the most distorted M(3)O6 polyhedron are 825 and 880 cm−1, respectively. The four phases exhibit antiferromagnetic couplings as the major magnetic interactions. However, a small spin canting phenomenon is observed at low temperatures for the two phases with major content in the anisotropic-Co(II) cation. 相似文献
15.
The interaction of diethyl (pyridyn-2-ylmethyl)phosphonate (2-pmpe) with Cu(NO3)2 · 6H2O leads to a partial hydrolysis of the starting ligand and formation of the compound of the formula Cu2(2-mpmpe)2(H2O)2(NO3)2, where 2-mpmpe = monoethyl (pyridyn-2-ylmethyl)phosphonate. The crystal and molecular structure of a copper(II) compound was determined by single X-ray diffraction method. Its structure consists of five-coordinated in distorted square planar geometry (CuNO4 chromophore) copper(II) ions doubly bridged by OPO from phosphonate. The Cu?Cu distance is 4.69 Å. The crystal packing is determined by the interdinuclear hydrogen bond system, which leads to a three-dimensional (3D) H-bonds network. The compound was characterized by infrared, ligand field, EPR spectroscopy, and magnetic studies. The magnetic properties of the title compound investigated over the 1.8–300 K, revealed the occurrence of a weak ferromagnetic coupling through phosphonate bridge (J = 1.86 cm−1) and interdimer superexchange coupling through H-bond network (zJ′ = −0.17 cm−1). Spectroscopic and magnetic properties are presented in the light of crystal structure. 相似文献
16.
The two new compounds, Sr4Cu3(AsO4)2(AsO3OH)4·3H2O (1) and Ba2Cu4(AsO4)2(AsO3OH)3(2), were synthesized under hydrothermal conditions. They represent previously unknown structure types and are the first compounds synthesized in the systems SrO/BaO-CuO-As2O5-H2O. Their crystal structures were determined by single-crystal X-ray diffraction [space group C2/c, a=18.536(4) Å, b=5.179(1) Å, c=24.898(5) Å, β=93.67(3)°, V=2344.0(8) Å3, Z=4 for 1; space group P42/n, a=7.775(1) Å, c=13.698(3) Å, V=828.1(2) Å3, Z=2 for 2]. The crystal structure of 1 is related to a group of compounds formed by Cu2+-(XO4)3− layers (X=P5+, As5+) linked by M cations (M=alkali, alkaline earth, Pb2+, or Ag+) and partly by hydrogen bonds. In 1, worth mentioning is the very short hydrogen bond length, D···A=2.477(3) Å. It is one of the examples of extremely short hydrogen bonds, where the donor and acceptor are crystallographically different. Compound 2 represents a layered structure consisting of Cu2O8 centrosymmetric dimers crosslinked by As1φ4 tetrahedra, where φ is O or OH, which are interconnected by Ba, As2 and hydrogen bonds to form a three-dimensional network. The layers are formed by Cu2O8 centrosymmetric dimers of CuO5 edge-sharing polyhedra, crosslinked by As1O4 tetrahedra. Vibrational spectra (FTIR and Raman) of both compounds are described. The spectroscopic manifestation of the very short hydrogen bond in 1, and ABC-like spectra in 2 were discussed. 相似文献
17.
Koichiro Fukuda Tomoyuki Iwata Akira Moriyama Shinobu Hashimoto 《Journal of solid state chemistry》2006,179(12):3870-3876
A complete series of solid solutions was prepared in the SrZr(PO4)2-BaZr(PO4)2 system and examined by conventional X-ray powder diffraction (XRPD). The crystals of SrxBa1−xZr(PO4)2 with x?0.1 were isomorphous with yavapaiite (KFe(SO4)2, space group C2/m). The solid solution with 0.2?x?0.7 has been composed of a new phase, showing a superstructure along the a-axis (c-axis of the yavapaiite substructure). The crystals with 0.8?x?0.9 were composed of both the new phase and the triclinic phase, the latter being isostructural with SrZr(PO4)2 (x=1). The crystal structure of the new phase has been determined using direct methods, and it has been further refined by the Rietveld method. The crystal of Sr0.7Ba0.3Zr(PO4)2 (x=0.7) is monoclinic (space group P2/c, Z=4 and Dx/Mg m−3=3.73) with a=1.53370(8) nm, b=0.52991(3) nm, c=0.84132(4) nm, β=92.278(1)° and V=0.68321(6) nm3. Final reliability indices are Rwp=7.32%, Rp=5.60% and RB=3.22%. The powder specimen was also examined by high-temperature XRPD and differential thermal analysis (DTA) to reveal the occurrence of two phase transitions during heating; the space group changed from P2/c to C2/m at ∼400 K, followed by the monoclinic-to-hexagonal (or trigonal) transition at 1060 K. The P2/c-to-C2/m transition has been, for the first time, described in the yavapaiite-type compounds. 相似文献
18.
Lei Wang 《Journal of solid state chemistry》2004,177(1):80-88
Two organically templated zincophosphites, (C6H14N2)·[Zn3(HPO3)4] and (C4H14N2)·[Zn3(HPO3)4] have been prepared under hydrothermal conditions and characterized by single-crystal X-ray diffraction. (C6H14N2)·[Zn3(HPO3)4] crystallizes in the triclinic space group , with cell parameters, a=9.363(4) Å, b=10.051(4) Å, c=10.051(4) Å, α=85.777(13)°, β=82.091(9)°, and γ=79.783(9)°. (C4H14N2)·[Zn3(HPO3)4] crystallizes in the monoclinic space group P21/c, with cell parameters, a=9.9512(3) Å, b=10.1508(3) Å, c=17.8105(5) Å, and β=95.6510(10)°. Although the two structures are different, they have the same anionic framework compositions of [Zn3(HPO3)4]2−. Their frameworks are built up from strictly alternating ZnO4 tetrahedra and HPO3 pseudo pyramids by sharing vertexes. There exist channels with an eight-membered ring window along the a- and c-axis. Powder X-ray diffraction, IR spectroscopy, 31P MAS solid-state NMR, thermogravimetric and differential thermal analyses were also carried out. 相似文献
19.
Koichiro Fukuda Tomoyuki Iwata Takahiro Niwa 《Journal of solid state chemistry》2006,179(11):3420-3428
Crystal structure and phase transformations of calcium yttrium orthophosphate Ca3Y(PO4)3 were investigated by X-ray powder diffraction, selected-area electron diffraction, transmission electron microscopy and optical microscopy. The high-temperature phase is isostructural with eulytite, cubic (space group ) with a=0.983320(5) nm, V=0.950790(8) nm3, Z=4 and Dx=3.45 Mg m−3. The crystal structure was refined with a split-atom model, in which the oxygen atoms are distributed over two partially occupied sites. Below the stable temperature range of eulytite, the crystal underwent a martensitic transformation, which is accompanied by the formation of platelike surface reliefs. The inverted crystal is triclinic (space group P1) with a=1.5726(1) nm, b=0.84267(9) nm, c=0.81244(8) nm, α=109.739(4)°, β=90.119(5)°, γ=89.908(7)°, V=1.0134(1) nm3, Z=4 and Dx=3.24 Mg m−3. The crystal grains were composed of pseudo-merohedral twins. The adjacent twin domains were related by the pseudo-symmetry mirror planes parallel to with the composition surface . When the eulytite was cooled relatively slowly from the stable temperature range, the decomposition reaction of Ca3Y(PO4)3→β-Ca3(PO4)2+YPO4 occurred. 相似文献
20.
S. Obbade C. Dion M. Rivenet M. Saadi F. Abraham 《Journal of solid state chemistry》2004,177(6):2058-2067
A new sodium uranyl vanadate Na(UO2)4(VO4)3 has been synthesized by solid-state reaction and its structure determined from single-crystal X-ray diffraction data. It crystallizes in the tetragonal symmetry with space group I41/amd and following cell parameters: a=7.2267(4) Å and c=34.079(4) Å, V=1779.8(2) Å3, Z=4 with ρmes=5.36(3) g/cm3 and ρcal=5.40(2) g/cm3. A full-matrix least-squares refinement on the basis of F2 yielded R1=0.028 and wR2=0.056 for 52 parameters with 474 independent reflections with I?2σ(I) collected on a BRUKER AXS diffractometer with MoKα radiation and a CCD detector. The crystal structure is characterized by ∞2[(UO2)2(VO4)] sheets parallel to (001) formed by corner-shared UO6 distorted octahedra and V(2)O4 tetrahedra, connected by V(1)O4 tetrahedra to ∞1[UO5]4− chains of edge-shared UO7 pentagonal bipyramids alternately parallel to the a- and b-axis. The resulting three-dimensional framework creates mono-dimensional channels running down the a- and b-axis formed by face-shared oxygen octahedra half occupied by Na. The powder of Li analog compound Li(UO2)4(VO4)3 has been synthesized by solid-state reaction. The two compounds exhibit high mobility of the alkaline ions within the two-dimensional network of non-intersecting channels. 相似文献