Li5B7S13 und Li9B19S33: Zwei Lithiumthioborate mit neuen hochpolymeren Anionengerüsten

Li₅B₇S₁₃ and Li₉B₁₉S₃₃: Two Lithium Thioborates with Novel Highly Polymeric Anion Networks Li₅B₇S₁₃ (C2/c; a = 17.304(2) Å, b = 21.922(3) Å, c = 12.233(2) Å, β = 134.91(1)°; Z = 8) and Li₉B₁₉S₃₃ (C2/c; a = 23.669(9) Å, b = 14.361(3) Å, c = 12.237(3) Å, β = 103.77(2)°; Z = 4) were prepared by reaction of stoichiometric amounts of lithium sulfide, boron, and sulfur at 750°C (Li₅B₇S₁₃) and 700°C (Li₉B₁₉S₃₃) with subsequent annealing. The crystal structures consist of interpenetrating, polymeric boron sulfur anion networks which are formed by corner-sharing of B₄S₁₀ and B₁₀S₂₀ units (Li₅B₇S₁₃), or B₁₉S₃₆ units (Li₉B₁₉S₃₃). The lithium cations are situated in between with a strong disorder in Li₉B₁₉S₃₃.     

Synthesis, Crystal Structure, Fluorescent and Thermal Properties of Sodium Tridecafluorodizirconate Na5Zr2F13 Compound

1 INTRODUCTION Considerable research effort on the heavy metal fluoride glasses like barium, zirconium fluoride and a series of rare-earth fluorozirconate compounds du- ring the last two decades was initiated by the broad optical transmission window of these glasses and thereby the potential for ultralow-loss optical fi- bers[1~10]. The fluorozirconate of alkali metals was first reported in 1938[11], and most of the sodium and potassium fluorozirconates were reported amongthe 1940s and 19…     

Darstellung und Kristallstruktur von [Li(DME)2I]

Synthesis and Crystal Structure of [Li(DME)₂I] . LiI can be dissolved at 50°C in toluene/DME (2:1). At - 20°C [Li(DME)₂I] ( 1 ) was isolated in 75% yield. 1 was characterized by NMR techniques as well as an X-Ray structure determination. 1 crystallizes in the space group C2/c with a = 1 356.9(2), b = 813.2(1), c = 1 259.1(2) pm, and β = 99.74(1)°.     

Ein neues Lithiumhydrogensulfat,Li2(HSO4)2(H2SO4) – Synthese und Kristallstruktur

A New Lithium Hydrogen Sulfate, Li₂(HSO₄)₂(H₂SO₄) – Synthesis and Crystal Structure The title compound crystallizes in good shaped single crystals from the system lithium sulfate/sulfuric acid in the orthorhombic space group Pccn, unit cell parameters a = 17.645(4), b = 5.378(1), c = 10.667(3) Å. V = 1 012.2 ų, Z = 4, D_x = 2.009 g cm^?3. There are two types of SO₄ tetrahedra, SO₃(OH) and SO₂(OH)₂, connected via hydrogen bonds forming layers parallel to the xy-plane. The layers are linked by Li atoms, which are tetrahedral coordinated by O atoms coming two by two from neighboured layers.     

Lithiumtriamidostannat(II), Li[Sn(NH2)3] – Synthese und Kristallstruktur

Lithium Triamidostannate(II), Li[Sn(NH₂)₃] – Synthesis and Crystal Structure Rusty-red glistening, transparent crystals of Li[Sn(NH₂)₃] were obtained by reaction of metallic lithium with tetraphenyl tin in liquid ammonia at 110 °C. The structure was determined from X-ray single-crystal diffractometer data: Space group P 2₁/n, Z = 4, a = 8.0419(9) Å, b = 7.1718(8) Å, c = 8.5085(7) Å, β = 90.763(8)°, R₁ (F _o ≥ 4σ(F _o)) = 2.8%, wR₂ (F ≥ 2σ(F )) = 5.3%, N(F ≥ 2σ(F )) = 1932, N(Var.) = 65. The crystal structure contains trigonal pyramidal complex anions [Sn(NH₂)₃]^– with tin at the apex, which are connected to layers of sequence A B A B … by lithium in tetrahedra-double units [Li(NH₂)_2/2(NH₂)₂]₂.     

Syntheses,Crystal Structures,and Biological Activities of Two 5-Pyrimidinyl-1,2,4-oxadiazoles

Two 5-pyrimidinyl-1,2,4-oxadiazoles were synthesized through two different routes and their structures were characterized by single-crystal X-ray diffraction, NMR and MS. Compound 3, 5-(2-chloro-4-methyl-6-phenylpyrimidin-5-yl)-3-phenyl-1,2,4-oxadiazole, crystallizes in orthorhombic, space group Pbca with a = 19.1575(11), b = 8.2115(5), c = 21.2035(12), V = 3335.6(3)3 and Z = 4. Compound 6, 5-(2,6-dichloropyrimidin-4-yl)-3-phenyl-1,2,4-oxadiazole, crystallizes in monoclinic space group Pn with a = 8.4275(13), b = 5.4088(8), c = 13.493(2), β = 99.768(3)o, V = 4658.6(6)3 and Z = 8. Preliminary bioassay indicated that the two title compounds had good herbicidal activities.     

Synthesis and Crystal Structure of a Novel Heptanuclear Ruthenium- and Sodium-containing Polyoxomolybdate [{Na(H_2O)_3}_2{Ru(dmso)_3}_2(MoO_4)_3]·_3H_2O

1 INTRODUCTION Polyoxomolybdates have been of great interest due to their unique structural varieties, associated multitude of properties and applications as catalysis, medicine and material[1, 2]. One of the most impor- tant aspects is the synthesis and investigation of the materials on polyoxomolybdates containing organo- metallic groups[3～5]. Such materials can provide molecular models for heterogeneous catalysis and display cooperative effects or bifunctional catalytic activity[6]. O…     

One-pot Synthesis and Crystal Structure of （1S,2R,3S,4R,5S）-1-Phenyl-2,4-dibenzoyl-3,5-difurylhexanol

(1S,2R,3S,4R,5S)-1-Phenyl-2,4-dibenzoyl-3,5-difurylhexanol 1 was synthesized by one-pot reaction of hypnone and furfurol in alkali H2O/EtOH solution and structurally defined to contain a chair-formed aliphatic carbocycle, on which the bulky substituents occupy the equatorial positions.     

Na2B2Se7, K2B2S7 und K2B2Se7: Drei Perchalkogenoborate mit neuem polymeren Anionengerüst

Na₂B₂Se₇, K₂B₂S₇, and K₂B₂Se₇: Three Perchalcogenoborates with a Novel Polymeric Anion Network Na₂B₂Se₇ (I 2/a; a = 11.863(4) Å, b = 6.703(2) Å, c = 13.811(6) Å, β = 109.41(2)°; Z = 4), K₂B₂S₇ (I 2/a; a = 11.660(2) Å, β = 6.827(1) Å, c = 12.992(3) Å, β = 106.78(3)°; Z = 4), and K₂B₂Se₇ (I 2/a; a = 12.092(4) Å, b = 7.054(2) Å, c = 13.991(5) Å, β = 107.79(3)°; Z = 4) were prepared by reaction of stoichiometric amounts of sodium selenide (potassium sulfide) with boron and sulfur or of potassium selenide and boron diselenide, respectively, at 600°C with subsequent annealing. The crystal structures consist of polymeric anion chains of composition ([B₂S₇]^2?)_n or ([B₂Se₇]^2?)_n formed by spirocyclically connected five-membered B₂S₃ (B₂Se₃) rings and six-membered B₂S₄ (B₂Se₄) rings. The nine-coordinate alkaline metal cations are situated in between.     

Cs5[Na{W4N10}]: The first framework nitridotungstate(VI)

Cs₅[Na{W₄N₁₀}] was prepared from a mixture of NaNH₂, CsNH₂ and tungsten powder (molar ration 1 : 10 : 4) at 700°C in autoclaves. After the reaction is finished the nitride is embedded in an alkali metal matrix. Dark red crystals were isolated by washing out the alkali metal with liquid ammonia at room temperature. The structure of Cs₅[Na{W₄N₁₀}] was solved by X-ray single crystal data: I4₁ (No. 80), Z = 4, a = 13.926(3) Å, c = 8.723(3) Å, Z(F) ≥ 3σ(F) = 1535, Z(Variables) = 63, R/R_w = 0.040/0.052. The compound is highly sensitive against moisture giving oxotungstates and ammonia. It contains a framework of tetrahedra [WNN_3/2^1.5?]. Sodium shares four terminal nitrogen ligands. Including sodium a distorted, β-cristobalite type arrangement [Na{W₄N₁₀}^5?] results. It contains caesium in all interstices formed by twelve nitrogen ligands in so-called Friauf polyhedra.     

Synthesis and Structural Characterization of [(η~5-C_5Me_5)_2Mo_2Fe_2S_4Br_2]

1 INTRODUCTION We once reported a CS bond cleavage reaction of (h5-C5Me5)Mo(StBu)3, which led to a Mo(IV) thio/thiolate complex (h5-C5Me5)MoS2(StBu)[1]. This reaction was facilitated by oxidants such as S8, gray selenium, and FeCl3[2]. The reaction with FeCl3 gave rise to a cubane cluster [(h5-C5Me5)2Mo2Fe2S4Cl2], which served as an excellent building block to construct various Mo/Fe/S clusters[2]. In this paper, we report the crystal structure of [(h5-C5Me5)2Mo2Fe…     

Synthesis and Crystal Structure of a Novel Manganese Coordination Polymer Constructed by 3,5-Dimethylbenzoic Acid with 4,4'-Bipyridine

1 INTRODUCTION There has been extensive interest in manganese complexes containing carboxylate ligands due to the richness in structural chemistry and potential appli- cations in catalysis[1～6], for example, some highly efficient manganese catalysis mimics[7, 8]. Further- more, 4,4?-bipy is an excellent bridging ligand, and so far a number of one-, two- and three-dimensional infinite metal-4,4?-bipy frameworks have already been generated[9, 10]. However, of the above-mentio- ned framework…     

Na7I2(OH)5: Ein Hydroxidiodid im System NaOH/NaI

Na₇I₂(OH)₅: A Hydroxide Iodide in the System NaOH/NaI The pseudobinary system NaOH/NaI is investigated by X-ray methods. The crystal structure of the compound Na₇I₂(OH)₅ was solved by single crystal data: Na₇I₂(OH)₅: P4/nmm, Z = 2, a = 7.748(2) Å, c = 10.260(3) Å, Z(F_o) = 443 with (F_o)² ≥ 3σ(F_o)², Z(parameter) = 28, R/R_w = 0.044/0.059 Na₇I₂(OH)₅ crystallizes in a new type of structure which contains puckered layers of ∞²[Na₇(OH)₅²⁺] connected via iodide ions.     

Darstellung und Kristallstrukturen von Li4−2xSr2+xB10S19 (x ≈ 0,27) und Na6B10S18. Zwei neue Thioborate mit hochpolymeren Makrotetraeder-Netzwerken

Synthesis and Crystal Structures of Li_4?2xSr_2+xB₁₀S₁₉ (x ≈ 0.27) and Na₆B₁₀S₁₈. Two Novel Thioborates with Highly Polymeric Macro-tetrahedral Networks Li_4?2xSr_2+xB₁₀S₁₉ (x ≈ 0.27) and Na₆B₁₀S₁₈ were prepared from the reaction of strontium sulfide and lithium sulfide (sodium sulfide) with boron and sulfur at 700°C in graphitized silica tubes. Li_4?2xSr_2+xB₁₀S₁₉ (x ≈ 0.27) crystallizes in the monoclinic space group P2₁/c with a = 10.919(2) Å, b = 13.590(3) Å, c = 16.423(4) Å, and β = 90.48(2)°, Na₆B₁₀S₁₈ in the tetragonal space group I4₁/acd with a = 14.415(3) Å, c = 26.137(4) Å. Both structures contain supertetrahedral B₁₀S₂₀ units which are linked through tetrahedral corners to form a three-dimensional polymeric network in the case of Na₆B₁₀S₁₈ and one-dimensional chains in the case of Li_4?2xSr_2+xB₁₀S₁₉ (x ≈ 0.27). All boron atoms are in tetrahedral BS₄ coordination (B? S bond lengths vary from 1.879(5) to 1.951(5) Å (1.875(10) to 1.987(9) Å)). The strontium and lithium (sodium) cations are located within large channels formed by the anions.     

Li4Ge2B as a new derivative of the Mo2B5 and Li5Sn2 structure types

Binary and multicomponent intermetallic compounds based on lithium and p‐elements of Groups III–V of the Periodic Table are useful as modern electrode materials in lithium‐ion batteries. However, the interactions between the components in the Li–Ge–B ternary system have not been reported. The structure of tetralithium digermanium boride, Li₄Ge₂B, exhibits a new structure type, in the noncentrosymmetric space group R3m, in which all the Li, Ge and B atoms occupy sites with 3m symmetry. The title structure is closely related to the Mo₂B₅ and Li₅Sn₂ structure types, which crystallize in the centrosymmetric space group Rm. All the atoms in the title structure are coordinated by rhombic dodecahedra (coordination number = 14), similar to the atoms in related structures. According to electronic structure calculations using the tight‐binding–linear muffin‐tin orbital–atomic spheres approximation (TB–LMTO–ASA) method, strong covalent Ge—Ge and Ge—B interactions were established.     

Synthesis and Structural Characterization of Two Molybdenum~phosphate Cluster Compounds: (C_(14)N_(14)H_(63) )Na(H_2Mo_6P_4O_(31))_2·8H_2Oand(C_(14)N_(14)H_(63))Na(H_2Mo_6P_4O_(31) )_2·5H_2O

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Synthesis and Crystal Structure of 3,5-Dichloro-N-(2-methoxyphenyl)benzamide

<正>The title compound was synthesized by the direct reaction of 3,5-dichlorobenzoic acid with 2-methoxyaniline in the presence of DCC and HOBT. The structure was supported by the spectroscopic data and unambiguously confirmed by the single-crystal X-ray diffraction studies. It crystallizes from a methanol solution in the monoclinic space group P2_1/c with unit cell dimensions of a = 4.9369(16), b = 13.351(5), c = 20.168(7), β = 96.755(8)°, V = 1320.1(8)~3 and Z = 4.     

Synthesis and Crystal Structure of Na2TiO3

The crystal structure of a sodium titanium oxide Na2TiO3 obtained by high temperature solid state reaction method was determined from single-crystal X-ray diffraction study. The compound crystallizes in the monoclinic system, space group C2/c, Mr = 141.88, a = 9.885(1), b = 6.4133(8), c = 5.5048(7) , β = 115.50(3)o, V = 314.99(7) 3, Z = 4, Dc = 2.992 g/cm3, λ = 0.71073 , μ = 27.80 cm–1, F(000) = 272, T = 295 K, R = 0.0189 and wR = 0.0512 for 30 variables and 370 contributing unique reflections. The three-dimensional structure in Na2TiO3 is constructed by the TiO(1)4O(2) and NaO(1)3O(2)2 groups. The titanium atoms are grouped in the form of trigonal bipyramid and arranged along the c axis by sharing the edges. The structure is compared with other structures of related A2BO3 compounds.     

The Novel Benzo-15-Crown-5 with Palladium(II) Complex:[Na(B15C5)]2[Pd(SCN)4]

A novel Pd(II) Benzo-15-crown-5 complex [Na(B15C5)]2[Pd(SCN)4] has been isolated and characterized by IR and X-ray diffraction analysis.The crystal structure belongs to monoclinic,space group P21/n with cell dimensions,a=1.0164(6),b=1.3743(3),c=1.4987(7) nm,b=95.248(6)o ,V=2.0847nm3,Z=2,F(000)=944,R=0.053,Rw=0.072.The compound consists of two [Na(B15C5)]+ complex cations and a [Pd(SCN)4]2- complex anion.Each sodium ion is coordinated by five crown ether oxygen atoms and one N atom from the SCN group of [Pd(SCN)4]2- to form stable neutral complex.