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1.
Uwe Kolitsch 《Acta Crystallographica. Section C, Structural Chemistry》2006,62(5):i35-i37
Sodium indium(III) chromate(VI) dihydrate, NaIn(CrO4)2·2H2O, synthesized from an aqueous solution at room temperature, is the first indium(III) member of the large family of compounds with kröhnkite [Na2CuII(SVIO4)2·2H2O]‐type chains. The crystal structure is based on infinite octahedral–tetrahedral [In(CrO4)2(H2O)2]− chains along [010], linked via charge‐balancing Na+ cations. The slightly distorted InO4(H2O)2 octahedra are characterized by a mean In—O distance of 2.125 Å. The CrO4 tetrahedra are strongly distorted (mean Cr—O = 1.641 Å). The Na atom shows an octahedral coordination, unprecedented among compounds with kröhnkite‐type chains. The NaO6 octahedra share opposite edges with the InO4(H2O)2 octahedra to form infinite [001] chains. The hydrogen bonds are of medium strength. NaIn(CrO4)2·2H2O belongs to the structural type F2 in the classification of Fleck, Kolitsch & Hertweck [Z. Kristallogr. (2002), 217 , 435–443], and is isotypic with KAl(CrO4)2·2H2O and MFe(CrO4)2·2H2O (M = K, Tl or NH4). All atoms are in special positions except one O atom. 相似文献
2.
Li2I(OH): A Compound with Onedimensional Infinite Edge Sharing [Li4/2(OH)+] Pyramids The pseudobinary system LiOH/LiI was investigated by X-ray methods. Two compounds, Li2I(OH) and Li5I(OH)4 exist. The structure of Li2I(OH) was solved by single-crystal data. For Li5I(OH)4 lattice constants and space group symmetry are given: Li2I(OH): Pnma, Z = 4, a = 10.339(4) Å, b = 5.567(1) Å, c = 6.643(2) Å, Z(Fo) mit (Fo)2 ≧ 3σ(Fo)2 = 439, Z (parameter) = 23, R/Rw = 0.030/0.040 Li5I(OH)4: Pmmn or P21mn(= Pmn21), Z = 2, a = 10.42 Å, b = 5.30 Å, c = 5.81 Å Li2I(OH) crystallizes in a new type of structure. The motif of a distorted hexagonal close-packed arrangement of iodide ions is penetrated by chains of [Li4/2(OH)+]. 相似文献
3.
Uwe Kolitsch Karolina Schwendtner 《Acta Crystallographica. Section C, Structural Chemistry》2004,60(9):i89-i90
Dicerium(IV) tetrachromate(VI) dihydrate, Ce(CrO4)4·2H2O, has been prepared from an acidic aqueous solution at room temperature. Its novel crystal structure, which was solved from single‐crystal X‐ray diffraction data, is built from isolated CrO4 tetrahedra and isolated Ce(O,H2O)n (n = 8 and 9) polyhedra. All atoms are in general positions. The mean Ce—O and Cr—O bond lengths are 2.358 and 1.651 Å, respectively. Comparisons are drawn with the structure of CeIV(CrO4)2·2H2O. 相似文献
4.
Li2Br(NH2): The First Ternary Alkali Metal Amide Halide The pseudobinary system LiNH2/LiBr was investigated by X-ray methods. The crystal structure of the compound Li2Br(NH2) was solved by single crystal data: Li2Br(NH2): Pnma, Z = 8, a = 12.484(2) Å, b = 7.959(1) Å, c = 6.385(1) Å, Z(Fo) with (Fo)2 ≧ 3σ(Fo)2 = 348, Z (parameter) = 51, R/Rw = 0.019/0.021 Li2Br(NH2) crystallizes in a new type of structure. To one another isolated chains of [Li2Li4/2(NH2)22+] show the motif of closest rod packing. They are connected via bromide ions in a distorted cubic primitive arrangement. 相似文献
5.
Preparation and Crystal Structure of CrSO4 · 3 H2O Evaporating a solution of Cr2+ in dilute sulphuric acid at 70°C light blue crystals of CrSO4 · 3 H2O were grown. Its x-ray powder diffraction pattern is quite similar to that of CuSO4 · 3 H2O. The crystal structure refinement of CrSO4 · 3 H2O (space group Ce, a = 5.7056(8) Å, b = 13.211(2) Å, c = 7.485(1) Å, β = 96.73(1)°, Z = 4) from single crystal data, using the parameters of the copper compound as starting values, results in a final R-value of R = 3.8%. The surrounding of the Cr2+ ion can be described as a strongly elongated octahedron. The basal plane of the CrO6-octahedron consists of three hydrate oxygen atoms and one sulphate oxygen atom. The two more distant axial oxygen atoms also belong to sulphate groups. Thus they are forming chains of alterning CrO6-octahedra and SO4-tetrahedra along [110] and [1–10] linked via common corners. These chains are connected via sulphate groups and by bridging hydrogen bonds to a 3-dimensional network. 相似文献
6.
Unusual Coordination Polyhedra around Oxygen in Li4Cl(OH)3 The pseudobinary system LiOH/LiCl was investigated by X-ray methods. Two compounds, Li4Cl(OH)3 and Li2Cl(OH), were obtained. The crystal structure of Li4Cl(OH)3 solved by single-crystal methods is delt with. For Li2Cl(OH) powder diffraction data are given: Li4Cl(OH)3: P21/m, Z = 2, a = 5.4096(8) Å, b = 7.382(2) Å, c = 6.2076(8) Å, β = 94.40(1)°, Z(Fo) with (Fo)2 ≧ 3σ(Fo)2 = 483, Z (parameter) = 50, R/Rw = 0.022/0.025 Li2Cl(OH): Pmma, Z = 2, a = 7.680(8) Å, b = 4.001(7) Å, c = 3.899(6) Å The hydroxide rich compound crystallizes in a new type of structure which contains puckered layers [Li4(OH)3+] connected via chloride ions. 相似文献
7.
K2[CrF5·H2O] is monoclinic: a = 9.6835(3) Å, b = 7.7359(2) Å, c = 7.9564(3) Å, β = 95.94(1)°, Z = 4, space group C2/c (no 15). Its crystal structure was solved from its X‐ray powder pattern recorded on a powder diffractometer, using for the refinement the Rietveld method. It is built up from isolated octahedral [CrF5·OH2]2? anions separated by potassium cations. The dehydration of K2[CrF5·H2O] leads to anhydrous orthorhombic K2CrF5: a = 7.334(2) Å, b = 12.804(4) Å, c = 20.151(5) Å, Z = 16, space group Pbcn (no 60), isostructural with K2FeF5. 相似文献
8.
Reaction of a fresh Cu(OH)2x(CO3)1—x · yH2O precipitate with adipic acid (H2L) and 2, 2'—bipyridine (bpy) in ethanolic aqueous solution at room temperature afforded the hydrogen adipato bridged CuII coordination polymer [Cu(bpy)(HL)]2L · 6H2O consisting of double chains according to {[Cu(bpy)(HL)2/2]2L} and hydrogen bonded H2O molecules. The chains result from [Cu(bpy)]2+ units bridged by bis—monodentate hydrogen adipato ligands and further crosslinked by bis—monodentate adipato ligands. Through the interchain π—π stacking interactions and interchain C(bpy)—H···O(adipato) hydrogen bonding interactions, the double chains are assembled into layers, between which the crystal H2O molecules are located. The Cu atoms are square pyramidally coordinated by two N atoms of one bpy ligand and three O atoms of one adipato ligand and two hydrogen adipato ligands. The doubly bonded oxygen atom of the protonated carboxyl group occupies the apical position (Cu—N: 1.997, 2.005 Å; equatorial Cu—O: 1.925, 1.942 Å; apical Cu—O: 2.354 Å). Furthermore, the thermal behavior of the compound will be discussed. Crystal data: triclinic, P1¯ (no. 2), a = 9.618(1) Å, b = 9.933(1) Å, c = 12.782(2) Å, α = 70.88(1)°, β = 73.70(1)°, γ = 75.60(1)°, V = 1090.7(2) Å3, Z = 1, R = 0.0453 and wR2 = 0.1265 for 4643 observed reflections (Fo2 > 2σ(Fo2)) out of 4985 unique reflections. 相似文献
9.
(N2H5)2GeF6 and (N2H6)2(GeF6)F2 have been prepared by reactions of N2H4·H2O and N2H6F2 with fluorogermanic acid. The solids have been characterized by chemical analysis and vibrational spectra. X-ray diffraction study has shown that crystals of (N2H5)2GeF6 are monoclinic, space group P 21/n, with unit-cell dimensions a = 6.015 (2), b = 5.249 (1), c = 11.181 (2) Å, β = 100.15 (2)o, and Z = 2. There are N2H5+ cations and GeF62? anions in the crystals interconnected by hydrogen bonds of the type NH····F and NH····N. 相似文献
10.
Selenostannates from Aqueous Solutions: Preparation and Structure of Na4SnSe4 · 16 H20 Pure selenostannates(IV) are prepared from aqueous solutions by reaction of SnSe2, with alkali selenides, strictly excluding oxygen. Na4SnSe4 · 16 H2O, being obtained from stoicheo-metric 1:2 quantities, is characterized by a complete X-ray structure analysis and by vibrational spectra. The compound is monoclinic (P21/m) with a = 8.673(3), b = 16.563(4), c = 8.647(2) Å, β = 92.10(2)°, Z = 2; it contains isolated tetrahedral SnSe44? ions [Sn? Se 2.504(2)?2.527(2) Å, Se? Sn? Se 106.6(1)?111.1(1)°] which are in contact to the hydrated octahedral [Na(OH2)6]+ ions through Se…?H? O bridges within an extensive hydrogen bridge system. The stretching vibrations of the SnSe44? ion are observed at 195 (n?1) and 252 cm?1 (n?3). The stretching force constant is approximately 1.59 mdyn/Å. 相似文献
11.
The first selenite chloride hydrates, Co(HSeO3)Cl · 3 H2O and Cu(HSeO3)Cl · 2 H2O, have been prepared from solution and characterised by single‐crystal X‐ray diffraction. The cobalt phase adopts an unusual “one‐dimensional” structure built up from vertex‐sharing pyramidal [HSeO3]2–, and octahedral [CoO2(H2O)4]2– and [CoO2(H2O)2Cl2]4– units. Inter‐chain bonding is by way of hydrogen bonds or van der Waals' interactions. The atomic arrangement of the copper phase involves [HSeO3]2– pyramids and Jahn‐Teller distorted [CuCl2(H2O)4] and [CuO4Cl2]8– octahedra, sharing vertices by way of Cu–O–Se and Cu–Cl–Cu bonds. Crystal data: Co(HSeO3)Cl · 3 H2O, Mr = 276.40, triclinic, space group P 1 (No. 2), a = 7.1657(5) Å, b = 7.3714(5) Å, c = 7.7064(5) Å, α = 64.934(1)°, β = 68.894(1)°, γ = 71.795(1)°, V = 337.78(7) Å3, Z = 2, R(F) = 0.036, wR(F) = 0.049. Cu(HSeO3)Cl · 2 H2O, Mr = 263.00, orthorhombic, space group Pnma (No. 62), a = 9.1488(3) Å, b = 17.8351(7) Å, c = 7.2293(3) Å, V = 1179.6(2) Å3, Z = 8, R(F) = 0.021, wR(F) = 0.024. 相似文献
12.
Crystal Structure of SrZn(OH)4 · H2O Colorless crystals of SrZn(OH)4 · H2O are obtained by electrochemical oxidation of Zn in a zinc/iron pair in an aqueous ammonia solution saturated with strontium hydroxide. The X-ray crystal structure determination was now successful including all hydrogen positions: P1 , Z = 2, a = 6.244(1) Å, b = 6.3000(8) Å, c = 7.701(1) Å, α = 90.59(1)°, β = 112.56(2)°, γ = 108.66(2)°, N(F ≥ 3σF) = 1967, N(Var.) = 84, R/Rw = 0.020/0.024. In SrZn(OH)4 · H2O Zn2+ is tetrahedrally coordinated by four OH? -ions while Sr2+ has 6 OH? and one H2O as neighbours. The polyhedra around Sr2+ are connected to chains which are linked three-dimensionally by isolated tetrahedra [Zn(OH)4]. Hydrogen bonds between H2O as donor and OH? are characterized by raman spectroscopy. 相似文献
13.
Cis-[Cr(en)2F2]ClO4 · NaClO4 · H2O (en = 1,2-diaminoethane) was obtained as the red crystalline product from the saturated solutions of both NaClO4 and cis-[Cr(en)2F2]ClO4 in water. The compound crystallizes in the monoclinic P21/n (No.14) space group with a = 9.540(2), b = 11.840(2); c = 14.659(3) Å, β = 95.02(1)°, Z = 4. The unit cell of the racemic crystal contains cis-[Cr(en)2F2]+ in the Λλλ and Δδδ enantiometric forms, Na+, ClO4?, and lattice H2O. Cr has octahedral coordination. Cr? F and Cr? N bonds are 1.868(4), 1.887(5) and from 2.067(2) to 2.100(8) Å. Mean Cl? O bond is 1.38 Å. Na+ ions are in the distorted octahedral environment. Infrared spectrum confirms the presence of the lattice H2O and proves the cis structure of [Cr(en)2F2]+. 相似文献
14.
K2Br(OH) and Rb2Br(OH): Two New Ternary Alkali Metal Halide Hydroxides with a Pronounced Structural Relationship to KOH resp. RbOH Two isotypic compounds K2Br(OH) and Rb2Br(OH) were prepared in the systems KOH/KBr and RbOH/RbBr. Their structures were determined by single crystal X-ray methods: K2Br(OH): P21/m, Z = 2, a = 6.724(1) Å, b = 4.272(4) Å, c = 8.442(2) Å, β = 108.14(2)°, Z(Fo) = 651 with (Fo)2 ≥ 3σ(Fo)2, Z(parameter) = 28, R/Rw = 0.041/0.047 Rb2Br(OH): P21/m, Z = 2, a = 6.918(3) Å, b = 4.483(2) Å, c = 8.850(5) Å, β = 108.08(6)°, Z(Fo) = 326 mit (Fo)2 ≥ 3σ(Fo)2, Z(parameter) = 27, R/Rw = 0.074/0.082. The compounds are built up by chains of [M2(OH)+] connected via Br?. The structure of the chains as well as their orientation to one another show a pronounced relationship to the structures of the room temperature modifications of the isotypic binary hydroxides KOH and RbOH. 相似文献
15.
(NH4)2PO3H, H2O crystallizes in the monoclinic system, space group P21/c, with a = 6.322(1) Å, b = 8.323(1) Å, c = 12.676(1) Å, β = 98.84(1) and Z = 4. The structure was refined to R = 0.022 based on 853 independent X-Rays intensities. Improved dimensions of the tetrahedral PO3H2? ion have been obtained: P?H = 1.34(2) and P?O = 1.514(2) Å. The geometry of this ion is compared with that of PO3F2? and SO32? ions and we find a decrease of the volume: VF? > VH+ > Vlone pair. 相似文献
16.
Two novel isopropylamine‐templated uranyl chromates, [(CH3)2CHNH3]3[(UO2)3(CrO4)2O(OH)3] ( 1 ) and [(CH3)2CHNH3]2[(UO2)2(CrO4)3(H2O)] ( 2 ) were prepared by hydrothermal method at 100 °C. The compounds were characterized by electron microprobe analysis and X‐ray diffraction crystal structure analysis [ 1 : trigonal, P31m, a = 9.646(4), c = 8.469(4) Å, V = 682.4(5) Å3; 2 : monoclinic, P21/c, a = 11.309(3), b = 11.465(3), c = 17.055(5) Å, β = 99.150(6)°, V = 2183.2(11) Å3]. The structure of 1 is based upon trimers of uranyl bipyramids interlinked by CrO4 tetrahedra to form [(UO2)3(CrO4)2O(OH)3]3– layers, whereas, in the structure of 2 , UO7 and UO6(H2O) pentagonal bipyramids are linked through CrO4 tetrahedra into the [(UO2)2(CrO4)3(H2O)]2– layers. The structures show many similarities to related uranyl selenate compounds, thus providing additional data on similarities and differences between uranyl sulfates, chromates, selenates, and molybdates. 相似文献
17.
Crystal Structure of CaZn2(OH)6 · 2 H2O The electrochemical oxidation of zinc in a zinc/iron-pair leads in an aqueous NH3 solution of calciumhydroxide at room temperature to colourless crystals of CaZn2(OH)6 · 2 H2O. The X-ray structure determination was now successful including all hydrogen positions. P21/c, Z = 2, a = 6.372(1) Å, b = 10.940(2) Å, c = 5.749(2) Å, β = 101.94(2)° N(F ≥ 3σF) = 809, N(Var.) = 69, R/RW = 0.011/0.012 The compound CaZn2(OH)6 · 2H2O contains Zn2+ in tetrahedral coordination by OH? and Ca2+ in octahedral coordination by four OH? and two H2O. The tetrahedra around Zn2+ form corner sharing chains, three-dimensionally linked by isolated polyhedra around Ca2+. Weak hydrogen bridge bonds result between H2O as donor and OH?. 相似文献
18.
Fluorides and Fluoro Acids. V. Crystal Structure of the 1:4 Phase in the System Water-Hydrogen Fluoride and a New Investigation of One of the 1:2 Phases In the quasi binary system H2O? HF the 1:2 phase of known crystal structure was recognized as the stable high-temperature phase. A more accurate redetermination of its structure (monoclinic, space group P21/c, Z = 4, a = 3.477, b = 6.024, c = 11.358 Å, β = 96.70° at ?100°C, R = 0.032 for 1356 observed MoKα data) confirmed the previous results of a layer structure formed by strong hydrogen bonds. H3OF · HF appears besides H3OHF2 as a possible structural formula. — The crystal structure of the 1:4 phase of the system was also determined (triclinic, P1 , Z = 2, a = 5.574, b = 6.429, c = 6.874 Å, α = 115.79, β = 96.63, γ = 108.79° at ?113°C, R = 0.049 for 1942 observed MoKα data). By strong hydrogen bonds the atoms form rings, which are condensed to parallel ribbons. Possible structural formulae, based on the distribution of interatomic distances, are H3OH3F4, H3OH2F3 · HF and H3OF · 3 HF. — Interatomic distances in the hydrogen bonds F? H…?F and O? H…?F of both structures and the known one of the 1:1 phase are discussed in comparison. 相似文献
19.
Synthesis, Crystal Structure and Thermal Behaviour of Fluoroaluminates of the Composition (NH4)[M(H2O)6](AlF6) (M = Zn, Ni), [Zn(H2O)6][AlF5(H2O)], and (PyH)4[Al2F10] · 4 H2O Four new fluoroaluminates were obtained from fluoroacidic solutions of respective metal salts. The compounds of zinc ( I a : P21/c, a = 12.688(3), b = 6.554(1), c = 12.697(3) Å, β = 95.21(3)°, V = 1051.5(4) Å3, Z = 4) and nickel ( I b : P21/c, a = 12.685(3), b = 6.517(1), c = 12.664(2)Å, β = 94.55(2)°, V = 1043.6(4) Å3, Z = 4) are isotypic and represent a new structure type consisting of two different cations, NH4+ and [M(H2O)6]2+ and [AlF6]3–‐anions. [Zn(H2O)6][AlF5(H2O)] ( II : C2/m, a = 10.769(2), b = 13.747(3), c = 6.487(1)Å, β = 100.02(3)°, V = 945.7(3) Å3, Z = 4) is characterized by a H2O/F‐disorder in the [AlF5(H2O)]‐octahedra in two trans positions. In (PyH)4[Al2F10] · 4 H2O ( III : Cmc21, a = 15.035(3), b = 20.098(4), c = 12.750(4) Å, V = 5364(2) Å3, Z = 8), bioctahedral [Al2F10]4– anions have been found for the first time. The structures are described and discussed in comparison. The new compounds were used as precursors in order to obtain new AlF3‐phases. However, the thermal decomposition did not result in the formation of any new metastable AlF3‐phase. Instead, phase mixtures of either α‐AlF3 and β‐AlF3 or AlF3 and MF2 were obtained. 相似文献
20.
(Phenacetin)4·2I4·2H2O is triclinic, a = 13.641 (7), b = 12.807 (6), c = 7.201 (3) Å, α = 99.8 (4), b? = 86.5 (4), γ = 104.0 (5)°, P1 , Z = 1. The ordered crystal structure has been refined to RF = 0.050, using 4173 independent reflections measured on a four-circle diffractometer with MoKa (graphite monochromator) radiation. The crystals are composed of alternating positively and negatively charged slices; each positive slice contains a double layer of stacks of hemi-protonated phenacetin molecules which are H-bonded through their carbonyl groups (d(O - - - O) = 2.432 (4) Å) while each negative slice contains a single layer of I2?4-ions linked in chains along [100] through H-bonds to pairs of water molecules. The axes of the phenacetin stacks are parallel to the planes of the (I2?4·2H2O)-layers. The I2?4-ion is centro-symmetric and can be approximately represented as I?- - - I–I- - - I? (d(I? - - - I) = 3.404 (1) Å; d(I–I) = 2.774 (1) Å). The compound is a pseudo-type A basic salt. 相似文献