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1.
Synthesis and Crystal Structure of the Holmium(III) Chloride Oxotellurate(IV) HoClTeO3 Orange coloured, rod—shaped single crystals of the holmium( III) chloride oxotellurate(IV) HoClTeO3 (orthorhombic, Pnma; a = 730.25(5), b = 696.54(5), c = 905.18(7) pm; Z = 4) are obtained during attempts to synthesize holmium(III) oxochlorotellurates(IV) by reaction of holmium oxychloride (HoOCl) and tellurium dioxide (TeO2; 1:1—2molar ratio, 800 °C, 40 d) in evacuated silica tubes. The crystal structure contains sevenfold coordinated Ho 3+ cations surrounded by five oxide and two chloride anions forming a pentagonal bipyramid. Interconnection of the [Ho(O1)(O2)4Cl2] polyhedra occurs via two edges made of four equatorial oxygen atoms (O2) under formation of {[Ho(O1)(O2)4/2Cl2/1]5‐} chains running parallel [010]. These arrange as hexagonal closest packing of rods and are linked to each other by Cl‐ anions to a three—dimensional {[Ho(O1)1/1(O2)4/2Cl2/2]4‐} network. All Te4+ cations are embedded therein and exhibit ψ1—tetrahedral coordination figures as discrete anionic [Te(O1)(O2)2]2‐ pyramids due to the stereochemical activity of the non—binding electron pairs („lone pairs”︁). They stabilize the {[HoO3Cl]4‐} network via covalent bonds to one axial (O1) and two equatorial oxygen atoms (O2) of each [HoO5Cl2] polyhedron. 相似文献
2.
Sc2Te5O13 and Sc2TeO6: The First Oxotellurates of Scandium Sc2Te5O13 and Sc2TeO6 are the first oxotellurates of scandium that could be structurally elucidated by X‐ray diffraction using single crystals. The scandium(III) oxotellurate(IV) Sc2Te5O13 was synthesized by reacting Sc2O3 with TeO2 at 850 °C and crystallizes in the triclinic system with space group (no. 2) and the lattice parameters a = 660.67(5), b = 855.28(7), c = 1041.10(9) pm, α = 86.732(8), β = 86.264(8), and γ = 74.021(8)° (Z = 2). The crystal structure contains chains respectively strands of alternatingly edge‐ and vertex‐sharing [ScO6]9? and [ScO7]11? polyhedra. These strands are connected by [TeO3+1](2+2)? oxotellurate(IV) anions. The coordination spheres of Sc3+ appear markedly smaller than those of M3+ cations in the other known compounds of the formula type M2Te5O13 (M = Y, Dy – Lu), therefore Sc2Te5O13 is not really isotypic, but only isopuntal with these compounds. Single crystals of the scandium(III) oxotellurate(VI) Sc2TeO6 were obtained through the fusion of a mixture of Sc2O3 and TeO3 at 850 °C. It crystallizes trigonally (a = 874.06(7), c = 479.85(4) pm and c/a = 0.549) with the Na2SiF6‐type structure in space group P321 (no. 150) and three formula units per unit cell. Its crystal structure is built up by a hexagonal closest packing (hcp) of oxide anions with the Sc3+ cations residing in 1/3 and the Te6+ cations in 1/6 of the octahedral interstices in a well‐ordered occupation pattern. Thus one can address the structural situation in Sc2[TeO6] as a stuffed β‐WCl6‐type arrangement. 相似文献
3.
Colorless platelets of Na2Lu3I3[TeO3]4 were obtained within five days at 775 °C by the reaction of Lu2O3 and TeO2 in a 3:8 molar ratio with NaI added in excess as both fluxing agent and reactant in evacuated silica ampoules. It crystallizes in the monoclinic space group P2/c with the lattice parameters a = 921.69(5), b = 552.71(3), c = 1664.37(9) pm, β = 90.218(4)° and Z = 2. The crystal structure of Na2Lu3I3[TeO3]4 exhibits two crystallographically different Lu3+ cations, both coordinated by eight O2– anions as square antiprisms. These polyhedra are interconnected through four common edges to build up {}^2_∞ {[LuO{}^e_8/2 ]5–} layers (e = edge‐linking) parallel to (100). Furthermore, the crystal structure includes a crystallographically unique Na+ cation surrounded by four O2– and four I– anions also in the shape of a square antiprism. These polyhedra connect via common (I2)–···(I2)– edges in generating {}^1_∞ {[Na2O8I{}^e_4 ]18–} double‐strands that are further linked by (I1)– vertices to result in the formation of {}^2_∞ {[Na2O8I3{}^e,v_3 ]17–} layers (v = vertex‐linking) spreading out parallel to (100) as well. Thus, the crystal structure contains two crystallographically distinct I– anions, of which (I1)– is coordinated nearly linear (? (Na–I1–Na) = 179.6°) by two Na+ cations, whereas (I2)– has contact to three of them displaying a distance of 114 pm from the triangular (Na+)3 plane. The crystal structure of Na2Lu3I3[TeO3]4 is completed by two crystallographically independent Te4+ cations that show stereochemically active non‐bonding electron pairs (“lone pairs”) and are located above and below the {}^2_∞ {[LuO{}^e_8/2 ]5–} layers forming isolated ψ1‐tetrahedral [TeO3]2– anions (d(Te–O) = 188–190 pm) with all oxygen atoms. 相似文献
4.
Novel Halogenochalcogeno(IV) Acids: [H3O(Benzo‐18‐Crown‐6)]2[Te2Br10] and [H5O2(Dibenzo‐24‐Crown‐8)]2[Te2Br10] Systematic studies on halogenochalcogeno(IV) acids containing tellurium and bromine led to the new crystalline phases [H3O(Benzo‐18‐Crown‐6)]2[Te2Br10] ( 1 ) and [H5O2(Dibenzo‐24‐Crown‐8)]2[Te2Br10] ( 2 ). The [Te2Br10]2‐ anions consists of two edge‐sharing distorted TeBr6 octahedra, the oxonium cations are stabilized by crownether. ( 1 ) crystallizes in the monoclinic space group P21/n with a = 14.520(5) Å, b = 22.259(6) Å, c = 16.053(5) Å, β = 97.76(3)° and Z = 4, whereas ( 2 ) crystallizes in the triclinic space group with a = 11.005(4) Å, b = 12.103(5) Å, c = 14.951(6) Å, α = 71.61(3)°, β = 69.17(3)°, γ = 68.40(3)° and Z = 1. 相似文献
5.
Single Crystals of the Cerium(III) Borosilicate Ce3[BSiO6][SiO4] Colorless, lath‐shaped single crystals of Ce3[BSiO6]‐ [SiO4] (orthorhombic, Pbca; a = 990.07(6), b = 720.36(4), c = 2329.2(2) pm, Z = 8) were obtained in attempts to synthesize fluoride borates with trivalent cerium in evacuated silica tubes by reaction of educt mixtures of elemental cerium, cerium dioxide, cerium trifluoride, and boron sesquioxide (Ce, CeO2, CeF3, B2O3; molar ratio 3 : 1 : 3 : 3) in fluxing CsCl (700 °C, 7 d) with the glass wall. The crystal structure contains eight‐ (Ce1) and ninefold coordinated Ce3+ cations (Ce2 and Ce3) surrounded by oxygen atoms. Charge balance is achieved by both discrete borosilicate ([BSiO6]5– ≡ [O2BOSiO3]5–) and ortho‐silicate anions ([SiO4]4–). The former consists of a [BO3] triangle linked to a [SiO4] tetrahedron by a single vertex. The anions form layers in [001] direction alternatingly built up from [BSiO6]5– and [SiO4]4– groups while Ce3+ cations are located in between. 相似文献
6.
Hydrates of Cerium(III) Chloride The thermal dehydration of CeCl3 · 7 H2O to CeCl3 gives four definite intermediates: CeCl3 · 6 H2O, CeCl3 · 3 H2O, CeCl3 · 2 H2O, CeCl3 · H2O. In the hexahydrate monomeric [CeCl2(H2O)6]+ units exist. A structure analysis of CeCl3 · 3 H2O gave an orthorhombic unit cell (S.G. Pnma; Z = 4) with a = 1 242.7(4) pm; b = 881.8(8) pm, c = 693.4(5) pm. The structure consists of [CeCl4/2Cl(H2O)3] chains, where two Ce3+ ions are connected via two chloride ions, forming bent chains in the [010] direction. The trihydrates LnCl3 · 3 H2O (Ln = Pr? Tb) are isotypic, also one modification of LaCl3 · 3 H2O. The structures of the di- and mono-hydrate are not yet known. Molar volumina and solution enthalpies in water vary linearly with the number of H2O molecules per formula unit. 相似文献
7.
HoClTe2O5: A Telluriumdioxide‐rich Holmium(III) Chloride Oxotellurate(IV) While attempting to synthesize anionically derivatized holmium oxotellurates by reacting holmium chloride (HoCl3) with tellurium oxide (TeO3; molar ratio 1 : 3, 800°C 10 d) in evacuated silica ampoules, transparent, greenish yellow and coarse single crystals of holmium(III) chloride oxotellurate(IV) HoClTe2O5 (triclinic, P1; a = 762.07(6), b = 796.79(6), c = 1010.36(8) pm, α = 100.987(4), ß = 99.358(4), γ = 91.719(4)°; Z = 4) were obtained. The crystal structure contains eightfold coordinated (Ho1)3+ (only surrounded by oxygen atoms) and sevenfold coordinated (Ho2)3+ cations (surrounded by one chloride and six oxide anions). Each sort of holmium polyhedra convenes independently to chains along [100] by edge‐sharing which again combine alternately via O6 and O9 to form 2{[Ho2O10(Cl1)]15—} layers parallel (001). Each of the four crystallographically different Te4+ cations are surrounded by three close oxygen atoms (d(Te—O) = 188 — 195 pm) and always one more situated further away. The stereochemical activity of the non‐bonding electron pairs (“lone pairs”) leads to ψ1‐trigonal bipyramidal coordination figures. The ψ1‐tetrahedral [TeO3]2— basic units form discrete [Te2O5]2— doubles with ecliptic conformation which are arranged in a fish‐bone pattern parallel to (001) on both sides of the 2{[Ho2O10Cl]15—} layers. The coherence of the 2{[Ho2(Cl1)Te4O10]+} layers is exclusively maintained via Cl2—Te1 contacts with an extraordinary long distance of 335 pm. As (Cl1)— belongs to the coordination sphere of (Ho2)3+ and (Cl2)— is only surrounded by Te4+, the compound should be correctly named holmium(III) chloride oxochlorotellurate(IV) Ho2Cl[Te4O10Cl] (Z = 2). 相似文献
8.
Incorporation of Sulfate or Selenate Groups into Oxotellurates(IV): I. Calcium,Cadmium, and Strontium Compounds
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Seven new mixed oxochalcogenate compounds in the systems MII/XVI/TeIV/O/(H), (MII = Ca, Cd, Sr; XVI = S, Se) were obtained under hydrothermal conditions (210 °C, one week). Crystal structure determinations based on single‐crystal X‐ray diffraction data revealed the compositions Ca3(SeO4)(TeO3)2, Ca3(SeO4)(Te3O8), Cd3(SeO4)(Te3O8), Cd3(H2O)(SO4)(Te3O8), Cd4(SO4)(TeO3)3, Cd5(SO4)2(TeO3)2(OH)2, and Sr3(H2O)2(SeO4)(TeO3)2 for these phases. Peculiar features of the crystal structures of Ca3(SeO4)(TeO3)2, Ca3(SeO4)(Te3O8), Cd3(SeO4)(Te3O8), Cd3(H2O)(SO4)(Te3O8), and Sr3(H2O)2(SeO4)(TeO3)2 are metal‐oxotellurate(IV) layers connected by bridging XO4 tetrahedra and/or by hydrogen‐bonding interactions involving hydroxyl or water groups, whereas Cd4(SO4)(TeO3)3 and Cd5(SO4)2(TeO3)2(OH)2 crystallize as framework structures. Common to all crystal structures is the stereoactivity of the TeIV electron lone pair for each oxotellurate(IV) unit, pointing either into the inter‐layer space, or into channels and cavities in the crystal structures. 相似文献
9.
Ho2Te4O11 and Ho2Te5O13: Two Telluriumdioxide‐rich Oxotellurates(IV) of Trivalent Holmium Ho2Te4O11 (monoclinic, C2/c; a = 1240.73(8), b = 511.21(3), c = 1605.84(9) pm, β = 106.142(7)°; Z = 4) and Ho2Te5O13 (triclinic, P1; a = 695.67(5), b = 862.64(6), c = 1057.52(7) pm, α = 89.057(6), β = 86.825(6), γ = 75.056(6)°; Z = 2) are obtained by the reaction of holmium sesquioxide with tellurium dioxide in appropriate molar ratios (Ho2O3 : TeO2 = 1 : 4 and 1 : 5, respectively) in evacuated silica tubes within eight days at 800 °C. The application of cesium chloride (CsCl) as flux in about five times molar excess secures fast and complete reactions to the single‐crystalline products aimed at. In the crystal structure of Ho2Te4O11 [HoO8] polyhedra are connected via oxygen edges thereby building up a network {[Ho2O10]14–} (001). On the other hand, the crystal structure of Ho2Te5O13 exhibits oxygen‐linked [(Ho1)O8] and [(Ho2)O7] polyhedra, which form ribbons {[(Ho1)2(Ho2)2O20]28–} running along [100]. Common to both structures, however, is the stereochemical activity of the non‐bonding electron pairs (“lone pairs”) of all the of the Te4+ cations (Te1 and Te2 in Ho2Te4O11, Te1–Te5 in Ho2Te5O13) causing ψ1‐polyhedral figures of coordination with 3 + 1, 4 and 3 + 2 oxygen atoms, respectively, around the central atoms. 相似文献
10.
Na6Sn4Se11 · 22 H2O can be crystallised at –8 °C as yellow‐orange needles from the 1 : 2 H2O/CH3OH mother liquor of a superheated reaction mixture of NaOH(s), Sn and Se. The bicyclic [Sn4Se11]6– anion exhibits crystallographic C2 symmetry and is composed of corner‐bridged SnSe4 tetrahedra. Two opposite tin atoms of an Sn4Se4 8‐membered ring are linked by a common Se atom, thereby affording two 6‐membered boat‐shaped Sn3Se3 rings with a shared Sn–Se–Sn bridging unit. [Sn4Se11]6– thus represents the immediate precursor of the well‐known adamantane‐like [Sn4Se10]4– anion. 相似文献
11.
Incorporation of Sulfate or Selenate Groups into Oxotellurates(IV): II. Compounds with Divalent Lead
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Four mixed oxochalcogenate compounds in the systems PbII/XVI/TeIV/O/(C), (XVI = S and Se) were obtained as minority phases under hydrothermal conditions (210 °C, one week). Their compositions as determined on the basis of single‐crystal X‐ray diffraction data are Pb3(SeO4)(TeO3)2, Pb7O4(SeO4)2(TeO3), Pb5(SeO4)2(TeO4)(CO3), and Pb2(SO4)(TeO3). All crystal structures are centrosymmetric, and in each case the oxochalcogenate anions are isolated from each other. The Pb2+ cations exhibit distorted coordination polyhedra with coordination numbers ranging from six to ten, in the majority of cases with a “one‐sided” coordination by oxygen atoms. The presence of the very rare square‐pyramidal TeIVO44– anion distinguishes the structure of Pb5(SeO4)2(TeO4)(CO3) from the other structures, where the oxotellurate(IV) anions exist in the TeO32– trigonal‐pyramidal configuration. 相似文献
12.
Syntheses and X‐Ray Crystal Structures of [Li(thf)4][SnCl5(thf)] and {[Li(Et2O)2]2‐(μ‐Cl2)2‐SnIVCl2}
The syntheses and single crystal X‐ray structure determinations are reported for [Li(thf)4][SnCl5(thf)] ( 1 ) and {[Li(Et2O)2]2‐(μ‐Cl2)2‐SnIVCl2} ( 2 ). Compound 1 is ionic with a tetrahedral coordinated lithium cation and distorted octahedral tin (IV) atom in the anion, while compound ( 2 ) is a centrosymmetric heteronuclear double salt of LiCl and SnCl4. [Li(thf)4][SnCl5(thf)] is monoclinic, P21/n, a = 11.204(1), b = 15.599(1), c = 17.720(2) Å; β = 96.734(2)°, Z = 4, R 0.0418; {[Li(Et2O)2]2‐(μ‐Cl2)2‐SnIVCl2} is monoclinic, P21/n, a = 10.848(2), b = 12.764(2), c = 11.748(2) Å; β = 90.388(3)°, Z = 4, R = 0.0851. 相似文献
13.
A New Oxophosphate (IV/III) Anion – Preparation and Crystal Structure of Na6P4O10 · 2 H2O A new oxophosphate anion, P4O106?, was obtained by cleavage and simultaneous oxidation of the cyclo-hexaphosphate(III) anion in a solution of aqueous ammonia and ethanol. With sodium it forms a salt with the composition Na6P4O10 · 2 H2O. The crystal structure has been determined by single crystal X-ray diffraction (3 745 diffractometer data), the cell constants were obtained from X-ray powder data, space group P1 ; a = 6.004(1), b = 6.173(2), c = 11.496(2) Å, α = 99.26(2)°, β = 95.92(2)°, γ = 117.63(2)°, Z = 1, R = 0.044. The backbone of the anion is formed by phosphorus atoms directly bonded to each other. The coordination of each phosphorus atom is completed to four by oxygene. The resulting oxidation numbers are +III for the inner phosphorus atoms and +IV for the terminal phosphorus atoms. The site symmetry of the anion is approximately C2h. Based on a 31P-NMR spectra of a solution the coupling constants of the AA ‘BB’ system were determined. 相似文献
14.
The crystal structures of Ce2[SeO3]3 and Pr2[SeO3]3 have been refined from X‐ray single‐crystal diffraction data. The compounds were obtained using stoichiometric mixtures of CeO2, SeO2, Ce, and CeCl3 (molar ratio 3:3:1:1) or Pr6O11, SeO2, Pr, and PrCl3 (molar ratio 3:27:1:2) heated in evacuated sealed silica tubes at 830 °C for one week. Ce2[SeO3]3 crystallizes orthorhombically (space group: Pnma), with four formula units per unit cell of the dimensions a = 839.23(5) pm, b = 1421.12(9) pm, and c = 704.58(4) pm. Its structure contains only a single crystallographically unique Ce3+ cation in tenfold coordination with oxygen atoms arranged as single‐face bicapped square antiprism and two different trigonal pyramidal [SeO3]2? groups. The connectivity among the [CeO10] polyhedra results in infinite sheets of face‐ and edge‐sharing units propagating normal to [001]. Pr2[SeO3]3 is monoclinic (space group: P21/n) with twelve formula units per unit cell of the dimensions a = 1683.76(9) pm, b = 705.38(4) pm, c = 2167.19(12) pm, and β = 102.063(7)°. Its structure exhibits six crystallographically distinct Pr3+ cations in nine‐ and tenfold coordination with oxygen atoms forming distorted capped square antiprisms or prisms (CN = 9), bicapped square antiprisms and tetracapped trigonal prisms (CN = 10), respectively. The [PrO9] and [PrO10] polyhedra form double layers parallel to (111) by edge‐ or face‐sharing, which are linked by nine different [SeO3]2? groups to build up a three‐dimensional framework. In both compounds, the discrete [SeO3]2? anions (d(Se4+–O2?) = 166–174 pm) show the typical Ψ1‐tetrahedral shape owing to the non‐bonding “lone‐pair” electrons at the central selenium(IV) particles. Moreover, their stereochemical “lone‐pair” activity seems to flock together in large empty channels running along [010] in the orthorhombic Ce2[SeO3]3 and along [101] in the monoclinic Pr2[SeO3]3 structure, respectively. 相似文献
15.
Barbara Schüpp‐Niewa Larysa Shlyk Yurii Prots Rainer Niewa Gernot Krabbes 《无机化学与普通化学杂志》2006,632(4):572-576
Single crystals of the new 6H‐perovskite Ba3ZrRu2O9 have been grown from BaCO3 and RuO2 in presence of BaCl2 on ZrO2 bars. Ba3ZrRu2O9 crystallizes in the space group P63/mmc (No. 194) with a = 5.7827(2) Å and c = 14.2509(5) Å (Z = 2, R1 = 0.037, wR2 = 0.078). The structure consists of pairs of face‐shared RuO6 octahedra forming [Ru2O9] units, which are interconnected by corner‐sharing ZrO6 octahedra. The structural relationships of the title compound and of the already known barium‐zirconium‐ruthenate Ba4ZrRu3O12, 4H‐ and 9R‐BaRuO3 and BaZrO3 are discussed. 相似文献
16.
Dark brown crystals of [NnPr4]2[TeBr6(SeBr2)2] ( 1 ) were obtained when selenium and bromine (1:1) were allowed to react in acetonitrile solution in the presence of tellurium(IV) bromide and tetrapropylammonium bromide. The salt 1 crystallizes in the monoclinic space group P21/n with the cell dimensions a = 14.7870(3) Å, b = 9.5523(3) Å, c = 16.7325(3) Å, β = 110.56(10)° (at 123(2) K). In the solid state the [TeBr6(SeBr2)2]2– anion contains a nearly regular [TeBr6] octahedron in which the four equatorial bromo ligands have developed bonds to SeII atoms of the SeBr2 molecules. The contacts between the bridging bromo and the SeII atoms of the SeBr2 molecules are 3.0000(4) and 3.0561(4) Å, and can be interpreted as bonds of the donor‐acceptor type with the bridging bromo ligands as donors and the SeBr2 molecules as acceptors. The TeIV–Br distances are in the range 2.6816(3)–2.7131(3) Å and the SeII–Br bond lengths in the coordinated SeBr2 molecules are 2.3548(4) and 2.3725(4) Å. 相似文献
17.
Azido Complexes of Vanadium(IV) and Vanadium(V): (Ph4P)2[VOCl2(μ‐N3)]2 and (Ph4P)2[VOCl(μ‐N3)(N3)2]2 (Ph4P)2[VOCl2(μ‐N3)]2 ( 1 ) was prepared by reaction of (Ph4P)[VO2Cl2] with trimethylsilylazide in the molar ratio 1:2 in dichloromethane solution to give dark green, moisture sensitive, non‐explosive single crystals. The reaction is accompanied by the formation of the dark blue side‐product (Ph4P)2[VOCl(μ‐N3)(N3)2]2 ( 2a ), which can be obtained as the main product by application of a large excess of Me3SiN3. Dark blue needles of 2a crystallize spontaneously from the CH2Cl2 solution within one hour at 4 °C. After standing at 4 °C under its mother liquid within 24 hours a first‐order phase transition of 2a occurs forming dark blue prismatic single crystals of 2b . According to single crystal X‐ray structure determinations, 2a and 2b crystallize in the same type of space group , however, with different lattice dimensions. The vanadium(IV) complex 1 is characterized by X‐ray structure determination and by vibrational spectroscopy (IR, Raman) as well as by EPR spectroscopy, whereas 2b is characterized by IR spectroscopy. 1 : Space group P21/n, Z = 2, a = 1009.5(1), b = 1226.6(2), c = 1943.0(2) pm, β = 98.42(1)°, R1 = 0.0672. The complex anion forms centrosymmetric units with V2N2‐four‐membered rings with a V···V distance of 335.6(1) pm and coordination number five on the vanadium(IV) atoms. 2a : Space group , Z = 1, a = 1089.0(2), b = 1097.1(2), c = 1310.1(2) pm, α = 92.99(1)°, β = 106.12(2)°, γ = 117.05(2)°, V = 1309.8(4) Å3, dcalc. = 1.440 g·cm?3, R1 = 0.0384. The complex anion forms centrosymmetric units of symmetry Ci with V2N2 four‐membered rings and VN bond lengths of 200.4(3) and 234.4(2) pm, respectively. The non‐bonding V···V distance amounts to 356.2(1) pm. 2b : Space group , Z = 1, a = 1037.3(2), b = 1157.6(2), c = 1177.2(2) pm, α = 98.48(2)°, ° = 103.82(2)°, γ = 106.33(2)°, V = 1281.8(4) Å3, dcalc. = 1.471 g·cm?3, R1 = 0.0724. The structure of the complex anion is similar to the anion of 2a with VN bond lengths of the four‐membered V2N2 ring of 203.3(4) and 235.2(4) pm, respectively, and a non‐bonding V···V distance of 357.5(1) pm. 相似文献
18.
Incorporation of Sulfate or Selenate Groups into Oxotellurates(IV): III. Compounds with Magnesium or Zinc
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The mixed oxochalcogenate compounds Mg2(SO4)(TeO3)(H2O), Mg3(SO4)(TeO3)(OH)2(H2O)2, Zn2(SeO4)(TeO3), and Zn4(SO4)(TeO3)3 were obtained under hydrothermal conditions (210 °C, autogenous pressure). Structure analyses using single‐crystal X‐ray data revealed tellurium in all four compounds to be present in oxidation state +IV, whereas sulfur or selenium atoms exhibit an oxidation state of +VI. In the crystal structures of the two magnesium compounds, [MgO5(H2O)] octahedra [Mg2(SO4)(TeO3)(H2O) structure, isotypic with the Co and Mn analogues] or [MgO4(OH)2] and [MgO4(OH)2(H2O)2] octahedra [Mg3(SO4)(TeO3)(OH)2(H2O)2 structure, novel structure type] as well as trigonal‐pyramidal TeO32– anions make up metal oxotellurate sheets, which are bridged by SO42– anions. The polar crystal structure of Zn2(SeO4)(TeO3) is isotypic with Zn2(MoO4)(TeO3) and consists of [ZnO4] tetrahedra, [ZnO6] octahedra, SeO42– and TeO32– anions as principal building units that are connected into a framework structure. Such a structural arrangement, with basically the same coordination polyhedra as in Zn2(SeO4)(TeO3) but with SO42– instead of SeO42– anions, is also found in the tellurium‐rich compound Zn4(SO4)(TeO3)3 that crystallizes in a novel structure type. 相似文献
19.
V. Brandel 《Journal of solid state chemistry》2005,178(4):1054-1063
A new uranium (IV) phosphate of proposed formula U2(PO4)2HPO4·H2O, i.e. uranium phosphate-hydrogenphosphate hydrate (UPHPH), was synthesized in autoclave and/or in polytetrafluoroethylene closed containers at 150 °C by three ways: from uranium (IV) hydrochloric solution and phosphoric acid, from uranium dioxide and phosphoric acid and by transformation of the uranium hydrogenphosphate hydrate U(HPO4)2·nH2O. The new product appears similar to the previously published thorium phosphate-hydrogenphosphate hydrate Th2(PO4)2HPO4·H2O (TPHPH). From preliminary studies, it was found that UPHPH crystallizes in monoclinic system (, , , β=91.67(3)° and ). Heated under inert atmosphere, this compound is decomposed above 400 °C into uranium phosphate-triphosphate U2(PO4)P3O10, uranium diphosphate α-UP2O7 and diuranium oxide phosphate U2O(PO4)2.Crystallized cerium (IV) phosphate-hydrogenphosphate hydrate Ce2(PO4)2HPO4·H2O (CePHPH) was also synthesized from (NH4)2Ce(NO3)6 and phosphoric acid solutions by the same method (monoclinic system: , , , β=91.98(1)° and ). When heating above 600 °C, cerium (IV) is reduced into Ce (III) and forms a mixture of CePO4 (monazite structure) and CeP3O9. 相似文献
20.
Pnictogenidostannates(IV) with Discrete Tetrahedral Anions: New Representatives (E1)4(E2)2[Sn(E15)4] (with E1 = Na, K; E2 = Ca, Sr, Ba; E15 = P, As, Sb, Bi) of the Na6[ZnO4] Type and the Superstructure Variant of K4Sr2[SnAs4] The silvery to dark metallic lustrous compounds (E1)4(E2)2[Sn(E15)4] (E1 = Na, K; E2 = Ca, Sr, Ba; E15 = P, As, Sb, Bi) were prepared from melts of stoichiometric mixtures of the elements. They crystallize in the Na6[ZnO4]‐type structure (hexagonal, space group: P63mc, Z = 2; Na4Ca2[SnP4]: a = 938.94(7), c = 710.09(8) pm; K4Sr2[SnAs4]: a = 1045.0(2), c = 767.0(1) pm; K4Ba2[SnP4]: a = 1029.1(6), c = 780.2(4) pm; K4Ba2[SnAs4]: a = 1051.3(1), c = 795.79(7) pm; K4Ba2[SnSb4]: a = 1116.9(2), c = 829.2(1) pm; K4Ba2[SnBi4]: a = 1139.5(2), c = 832.0(2) pm). The anionic partial structure consists of tetrahedra [Sn(E15)4]8– orientated all in the same direction along [001]. In the cationic partial structure one of the two cation positions is occupied statistically by alkali and alkaline earth metal atoms. Up to now only for K4Sr2[SnAs4] a second modification could be isolated, forming a superstructure type with three times the unit cell volume (hexagonal, space group: P63cm, Z = 6; a = 1801.3(2), c = 767.00(9) pm) and an ordered cationic partial structure. 相似文献