Li4Ca3Si2N6 and Li4Sr3Si2N6 – Quaternary Lithium Nitridosilicates with Isolated [Si2N6]10– Ions

The isotypic nitridosilicates Li₄Ca₃Si₂N₆ and Li₄Sr₃Si₂N₆ were synthesized by reaction of strontium or calcium with Si(NH)₂ and additional excess of Li₃N in weld shut tantalum ampoules. The crystal structure, which has been solved by single‐crystal X‐ray diffraction (Li₄Sr₃Si₂N₆: C2/m, Z = 2, a = 6.1268(12), b = 9.6866(19), c = 6.2200(12) Å, β = 90.24(3)°, wR₂ = 0.0903) is made up from isolated [Si₂N₆]^10– ions and is isotypic to Li₄Sr₃Ge₂N₆. The bonding angels and distances within the edge‐sharing [Si₂N₆]^10– double‐tetrahedra are strongly dependent on the lewis acidity of the counterions. This finding is discussed in relation to the compounds Ca₅Si₂N₆ and Ba₅Si₂N₆, which also exhibit isolated [Si₂N₆]^10– ions.     

Sr2(OLi2Sr4)[CrN4]2, ein Nitridochromat(VI)‐Oxid mit Sauerstoff in tetragonal‐bipyramidaler Koordination durch Lithium und Strontium

Sr₂(OLi₂Sr₄)[CrN₄]₂, a Nitridochromate(VI)‐Oxide with Oxygen in Tetragonal‐Bipyramidal Coordination by Lithium and Strontium Green gleaming crystals of Sr₂(OLi₂Sr₄)[CrN₄]₂ were prepared by reaction of Li, Sr and CrN/Cr₂N (approximate 1 : 1 mixture) with flowing nitrogen at 900 °C (molar overall composition Li : Sr : Cr = 6 : 1 : ∼3). The oxygen content results from a leak in the gas supply. The crystal structure was determined by single crystal methods (triclinic; P1; a = 615.87(9) pm, b = 682.50(10) pm, c = 754.30(8) pm, α = 82.302(14)°, β = 75.197(10)°, γ = 70.133(13)°; Z = 1) and contains distorted tetragonal bipyramids (OLi₂Sr₄)⁸⁺ and [Cr^VIN₄]^6–‐tetrahedra besides Sr²⁺.     

Diversity of Strontium Nitridogermanates(IV): Novel Sr4[GeN4], Sr8Ge2[GeN4], and Sr17Ge2[GeN3]2[GeN4]2

Single crystals of three new strontium nitridogermanates(IV) were grown in sealed niobium ampules from sodium flux. Dark red Sr₄[GeN₄] crystallizes in space group P2₁/c with a = 9.7923(2) Å, b = 6.3990(1) Å, c = 11.6924(3) Å and β = 115.966(1)°. Black Sr₈Ge₂[GeN₄] contains Ge^4– anions coexisting with [Ge^IVN₄]^8– tetrahedra and adopts space group Cc with a = 10.1117(4) Å, b = 17.1073(7) Å, c = 10.0473(4) Å and β = 115.966(1)°. Black Sr₁₇Ge₆N₁₄ features the same anions alongside trigonal planar [Ge^IVN₃]^5– units. It crystallizes in P1 with a = 7.5392(1) Å, b = 9.7502(2) Å, c = 11.6761(2) Å, α = 103.308(1)°, β = 94.651(1)° and γ = 110.248(1)°.     

Synthese und Kristallstruktur des ersten Oxonitridoborates — Sr3[B3O3N3]

Synthesis and Crystal Structure of the First Oxonitridoborate — Sr₃[B₃O₃N₃] The cyclotri(oxonitridoborate) Sr₃[B₃O₃N₃] was synthesized at 1450 °C as coarsely crystalline colourless crystals by the reaction of SrCO₃ with poly(boron amide imide) using a radiofrequency furnace. The structure was solved by single‐crystal X‐ray diffractometry (Sr₃[B₃O₃N₃], Z = 4, P2₁/n, a = 663.16(2), b = 786.06(2), c = 1175.90(3) pm, η = 92.393(1)°, R1= 0.0441, wR2 = 0.1075, 1081 independent reflections, 110 refined parameters). Besides Sr²⁺ there are hitherto unknown cyclic [B₃O₃N₃]^6— ions (B—N 143.7(10) — 149.1(9) pm, B—O 140.5(8) — 141.4(8) pm).     

Kristallstruktur von Natrium‐Dihydrogencyamelurat‐Tetrahydrat Na[H2(C6N7)O3] · 4 H2O

Crystal Structure of Sodium Dihydrogencyamelurate Tetrahydrate Na[H₂(C₆N₇)O₃] · 4 H₂O Sodium dihydrogencyamelurate‐tetrahydrate Na[H₂(C₆N₇)O₃]·4 H₂O was obtained by neutralisation of an aqueous solution, previously prepared by hydrolysis of the polymer melon with sodium hydroxide. The crystal structure was solved by single‐crystal X‐ray diffraction ( a = 6.6345(13), b = 8.7107(17), c = 11.632(2) Å, α = 68.96(3), β = 87.57(3), γ = 68.24(3)°, V = 579.5(2) ų, Z = 2, R1 = 0.0535, 2095 observed reflections, 230 parameters). Both hydrogen atoms of the dihydrogencyamelurate anion are directly bound to nitrogen atoms of the cyameluric nucleus, thus proving the preference of the keto‐tautomere in salts of cyameluric acid in the solid‐state. The compound forms a layer‐like structure with an extensive hydrogen bonding network.     

6‐Aza‐2′‐deoxy­uridine and N3‐anisoyl‐6‐aza‐2′‐deoxy­uridine

In 2‐(2‐deoxy‐β‐d ‐erythro‐pentofuranosyl)‐1,2,4‐triazine‐3,5(2H,4H)‐dione (6‐aza‐2′‐deoxy­uridine), C₈H₁₁N₃O₅, (I), the conformation of the glycosylic bond is between anti and high‐anti [χ = −94.0 (3)°], whereas the derivative 2‐(2‐deoxy‐β‐d ‐erythro‐pentofuranosyl)‐N⁴‐(2‐methoxy­benzoyl)‐1,2,4‐triazine‐3,5(2H,4H)‐dione (N³‐anisoyl‐6‐aza‐2′‐deoxy­uridine), C₁₆H₁₇N₃O₇, (II), displays a high‐anti conformation [χ = −86.4 (3)°]. The furanosyl moiety in (I) adopts the S‐type sugar pucker (²T₃), with P = 188.1 (2)° and τ_m = 40.3 (2)°, while the sugar pucker in (II) is N (³T₄), with P = 36.1 (3)° and τ_m = 33.5 (2)°. The crystal structures of (I) and (II) are stabilized by inter­molecular N—H⋯O and O—H⋯O inter­actions.     

Ca2Ga3MgN5 – A Highly Condensed Nitridogallate

The nitridogallate Ca₂Ga₃MgN₅ was obtained from reaction of the elements in sodium flux with Na‐azide at 760 °C in weld shut niobium ampoules. Crystal structure solution and refinement was carried out on the basis of single‐crystal X‐ray diffraction data. Ca₂Ga₃MgN₅ [space group C2/m (no. 12), a = 11.160(2), b = 3.2965(7), c = 8.006(2) Å, and β = 109.93(3)°, Z = 2] shows an anionic substructure made up of mixed (Mg/Ga)N₄ tetrahedra, which are sharing both common vertices and edges building a three‐dimensional network. The crystal structure of Ca₂Ga₃MgN₅ is related to known alkaline earth nitridosilicates (M^II₂Si₅N₈, M^II = Sr, Ba), but is significantly higher condensed due to additional edge‐sharing in the anionic substructure.     

Neue Sr‐Verbindungen mit planaren Al‐Si/Ge‐Anionen und eine Korrektur zu SrSi‐II und SrGe0.76

New Sr Compounds with Planar Al‐Si/Ge Anions and a Correction of SrSi‐II and SrGe_0.76 Planar anions with considerable p_π‐p_π interactions between heavier group 13 and 14 elements are observed in several alkaline earth trielides and tetrelides. In the intermetallics of the series SrAlxGe_2?x (border phases: x = 1: , a = 429.4(3), c = 474.4(3) pm, Z = 1, R1 = 0.0305, SrPtSb type and x = 1.6: P6/mmm, a = 440.4(2), c = 478.2(2) pm, Z = 1, R1 = 0.0125, AlB₂ type) graphite analogue planar Al/Ge nets with short Al‐Ge bonds are stacked in identical orientation, showing inter‐layer distances of approx. 475 pm. Starting from the related planar ribbons of condensed six‐membered rings in the known intermetallics (M^IV = Si, Ge) a series of new metal‐rich oxides with chain pieces consisting of three, two and finally only one six‐membered ring have been prepared and characterized on the basis of single crystal X‐ray data. The formal fragmentation of the ribbons is achieved by the incorporation of [OSr₆] octahedra, chains of which (connected via common corners) exactly fit the distance between the planar anions. The structures of the two compounds (M^IV = Si, Ge; formerly erroneously reported as SrSi and SrGe_0.76, space group Immm, a = 482.48(5)/484.55(8), b = 1306.5(2)/1342.2(2), c = 1814.0(2)/1857.4(3) pm, Z = 2, R1 = 0.0369/0.0316) contain isolated planar anions [M₂Al₂M₂Al₂M₂]^18? with only one six‐membered ring. In the monoclinic structures of the silicide Sr₁₃[Al₆Si₈][O] (C2/m, a = 2245.1(4), b = 482.76(5), c = 1720.6(5) pm, β=125.21(2)°, Z = 2, R1 = 0.0579) and the germanide Sr₁₆[Al₈Ge₁₀][O] (C2/m, a = 2287.23(14), b = 484.94(3), c = 2065.70(13) pm, β=120.150(4)°, Z = 2, R1 = 0.0730) anions [Si₂Al₂Si₂Al₂Si₂Al₂Si₂] and [Ge₂M₂Ge₂M₂Ge₂M₂Ge₂M₂Ge₂] with two and three six‐membered rings are left as fragments of the ribbons in Sr₃Al₂M₂. The puzzling bonding situation in these type of polar intermetallics at the Zintl border is calculated (using the DFT FP‐LAPW approach) for the structures with manageably small unit cells and discussed for the series SrAlM – Sr₃Al₂M₂ – Sr₁₆[Al₈M₁₀][O] – Sr₁₃[Al₆M₈][O] – Sr₁₀[Al₄M₆][O].     

2,5,8‐Trihydrazino‐s‐heptazine: A Precursor for Heptazine‐based Iminophosphoranes

The title compound  C₆N₇(NHNH₂)₃ ( 1 ) was obtained from melem C₆N₇(NH₂)₃ or melon [C₆N₇(NH₂)NH]_n and hydrazine by an autoclave synthesis. Upon treatment with a 10 % HCl solution it is transformed into the trihydrochloride  [C₆N₇(NHNH₃)₃]Cl₃ ( 2 ). Compounds 1 and 2 were analysed with ¹³C NMR, ¹⁵N NMR, FTIR and Raman spectroscopy. Furthermore, the single‐crystal X‐ray structure of the pentahydrate of 2 is reported (P\bar{1} , a = 674.96(3), b = 1214.17(6), c = 1272.15(6) pm, α = 66.288(2)°, β = 75.153(2)°, γ = 80.420(2)°, V = 920.30(8)·10⁶ pm³, Z = 2, T = 90(2) K). The thermal decomposition of 1 and 2 was investigated with TG/DTA. Reaction of 1 with NaNO₂/HCl yields triazido‐s‐heptazine, C₆N₇(N₃)₃ ( 3 ). Tris(tri‐n‐butylphosphinimino)‐s‐heptazine ( 4 ) was synthesised from 3 and characterised by means of ¹³C, ³¹P, ¹H NMR, FTIR and MALDI‐TOF spectroscopy. Similar to s‐heptazine derivative 3 , compounds 1 and 4 are precursors for graphitic carbon nitrides, which have attracted considerable attention recently, and to various potential applications, such as flame retardants and (photo) catalysis.     

Li2Sr4Al2Ta2N8O,a Nitridoalumotantalate with BCT‐Zeolite Type Structure

Li₂Sr₄Al₂Ta₂N₈O was synthesized from Li₃AlN₂, Sr(NH₂)₂, LiN₃, and lithium metal as fluxing agent in weld shut tantalum crucibles. Single crystals were obtained as byproduct from reaction with the ampoule material. The crystal structure (P2₁/n (no. 14), a = 9.4081(19), b = 10.012(2), c = 5.9832(12) Å, β = 93.44(3)°, Z = 2) was solved on the basis of single‐crystal X‐ray diffraction data. Li₂Sr₄Al₂Ta₂N₈O is built up of vertex sharing AlN₄ and TaN₄ tetrahedra, forming a BCT‐zeolite type structure with Sr²⁺ ions and molecular Li₂O units incorporated into the voids. Lattice energy calculations (MAPLE) confirmed the electrostatic bonding interactions and the chemical composition.     

The Crystal Structures of Two No–Metal Tricyanomelaminates: Diammonium Tricyanomelaminate Dihydrate [NH4]2[C6N9H] · 2 H2O and Dimelaminium Tricyanomelaminate Melamine Dihydrate [C3N6H7]2[C6N9H] · C3N6H6 · 2 H2O

Diammonium tricyanomelaminate dihydrate [NH₄]₂[C₆N₉H] · 2 H₂O ( 1 ) and dimelaminium tricyanomelaminate melamine dihydrate [C₃N₆H₇]₂[C₆N₉H] · C₃N₆H₆ · 2 H₂O ( 2 ) were obtained by metathesis reactions from Na₃[C₆N₉] in aqueous solution and characterized by single‐crystal X‐ray diffraction and ¹⁵N solid‐state NMR spectroscopy ( 1 ). Both salts contain mono‐protonated tricyanomelaminate (TCM) anions and crystallize as dihydrates. Considering charge balance requirements, the crystal structure of 1 (C2/c, a = 3181.8(6) pm, b = 360.01(7) pm, c = 2190.4(4) pm, β = 112.39(3)°, V = 2319.9(8) 10⁶ · pm³) can best be described by assuming a random distribution of an ammonium ion – crystal water pair over two energetically similar sites. Apart from two melaminium cations, 2 (P2₁/c, a = 674.7(5) pm, b = 1123.6(5) pm, c = 3400.2(5) pm, β = 95.398(5), V = 2566(2) 10⁶ · pm³) contains one neutral melamine per formula unit acting as an additional “solvent” molecule and yielding a donor‐acceptor type of π–stacking interaction.     

1H, 13C and 15N NMR spectroscopic,x‐ray structural and ab initio/HF studies on nitramino and N‐alkylamino‐4‐nitro derivatives of pyridine N‐oxides and pyridines

The ¹H, ¹³C and ¹⁵N NMR spectra in DMSO‐d₆ were measured for eight nitraminopyridine N‐oxides, ten 4‐nitropyridine N‐oxides, four 2‐nitraminopyridines and five 4‐nitropyridines. Their chemical shift assignments are based on PFG ¹H,X (X = ¹³C and ¹⁵N) HMQC and HMBC experiments. The relative energies for the tautomers of two nitraminopyridine N‐oxides were determined by ab initio HF/6–311G** calculations. A single‐crystal x‐ray structural analysis was made for 4‐methyl‐2‐nitraminopyridine: C₆H₇O₂N₃, M = 153.15, triclinic, space group P‐1 (No. 2), a = 7.0275(4), b = 6.8034(3), c = 8.6086(5) Å, α = 103.620(2), β = 90.309(2), γ = 122.215(3)°, V = 334.11(3) ų, Z = 2. Copyright © 2003 John Wiley & Sons, Ltd.     

Neue Germanide mit geordneter Ce3Pt4Ge6‐Struktur – Die Verbindungen Ln3Pt4Ge6 (Ln: Pr–Dy)

New Germanides with an Ordered Variant of the Ce₃Pt₄Ge₆ Type of Structure – The Compounds Ln₃Pt₄Ge₆ (Ln: Pr–Dy) Six new germanides Ln₃Pt₄Ge₆ with Ln = Pr–Dy were synthesized by heating mixtures of the elements at 900 °C, annealing the inhomogeneous powders at 1050‐1100 °C for six days and then cooling down from 700 °C in the course of two months. The crystal structures of Pr₃Pt₄Ge₆ (a = 26.131(5), b = 4.399(1), c = 8.820(2) Å), Sm₃Pt₄Ge₆ (a = 25.974(3), b = 4.356(1), c = 8.748(1) Å), and Dy₃Pt₄Ge₆ (a = 26.079(5), b = 4.311(1), c = 8.729(2) Å) were determined by single crystal X‐ray methods. The compounds are isotypic (Pnma, Z = 4) and crystallize with an ordered variant of the Ce₃Pt₄Ge₆ type of structure (Cmcm, Z = 2) consisting of CaBe₂Ge₂‐ and YIrGe₂‐analogous units. The platinum atoms are located in distorted square pyramids of germanium atoms and build up with them a three‐dimensional network. The coordination polyhedra of the platinum and germanium atoms around the rare‐earth metal atoms are pentagonal and hexagonal prisms. These are completed by some additional atoms resulting in coordination numbers of 14 and 15 respectively. The other germanides were investigated by powder methods resulting in the following lattice constants: a = 26.067(6), b = 4.388(1), c = 8.800(2) Å for Ln = Nd; a = 25.955(7), b = 4.337(1), c = 8.728(2) Å for Ln = Gd; a = 25.944(5), b = 4.322(1), c = 8.698(2) Å for Ln = Tb. The atomic arrangement of Ln₃Pt₄Ge₆ is compared with the well‐known monoclinic structure of Y₃Pt₄Ge₆.     

K3[C3N3(COO)3]·2H2O – Crystal Structure of a New Alkali Derivative of the Multidentate Ligand Triazine Tricarboxylate

Potassium‐1,3,5‐triazine‐2,4,6‐tricarboxylate dihydrate K₃[C₃N₃(COO)₃] · 2H₂O was obtained by saponification of the respective ethyl ester in aqueous solution under mild conditions and subsequent crystallization at 4 °C. The crystal structure of the molecular salt was elucidated by single‐crystal X‐ray diffraction [P , a = 696.63(14), b = 1748.5(3), c = 1756.0(3) pm, α = 119.73(3), β = 91.96(3), γ = 93.84(3)°, V = 1847.6(6) · 10⁶ pm³, Z = 6, T = 200 K]. Perpendicular to [100] the triazine tricarboxylate and potassium ions are arranged in layers alternating with layers of crystal water molecules. Two thirds of the triazine tricarboxylate units form hexagonal channels being filled with the remaining triazine tricarboxylate molecules. K₃[C₃N₃(COO)₃] · 2H₂O was additionally investigated by means of FTIR spectroscopy, TG and DTA measurements.     

Crystal Chemistry of the M11+,2+–M22+,3+–(H)‐Arsenites: the First Cadmium(II) Arsenite,Na4Cd7(AsO3)6

The crystal structures among M1–M2–(H)‐arsenites (M1 = Li⁺, Na⁺, K⁺, Rb⁺, Cs⁺, Ca²⁺, Sr²⁺, Ba²⁺, Cd²⁺, Pb²⁺; M2 = Mg²⁺, Mn^2+,3+, Fe^2+,3+, Co²⁺, Ni²⁺, Cu²⁺, Zn²⁺) are less investigated. Up to now, only the structure of Pb₃Mn(AsO₃)₂(AsO₂OH) was described. The crystal structure of hydrothermally synthesized Na₄Cd₇(AsO₃)₆ was solved from the single‐crystal X‐ray diffraction data. Its trigonal crystal structure [space group R$\bar{3}$ , a = 9.5229(13), c = 19.258(4) Å, γ = 120°, V = 1512.5(5) ų, Z = 3] represents a new structure type. The As atoms are arranged in monomeric (AsO₃)^3– units. The surroundings of the two crystallographically unique sodium atoms show trigonal antiprismatic coordination, and two mixed Cd/Na sites are remarkably unequal showing tetrahedral and octahedral coordinations. Despite the 3D connection of the AsO₃ pyramids, (Cd,Na)O_x polyhedra and NaO₆ antiprisms, a layer‐like arrangement of the Na atoms positioned in the hexagonal channels formed by CdO₄ deformed tetrahedra and AsO₃ pyramids in z = 0, 1/3, 2/3 is to be mentioned. These pseudo layers are interconnected to the 3D network by (Cd,Na)O₆ octahedra. Raman spectra confirmed the presence of isolated AsO₃ pyramids.     

[Na(DB18-C-6)(H2O)2][Na(DB18-C-6)(SCN)2]：Two-Di-mensional Network Complex Assembled by π-π Stacking Interactios,Hydrogen Bonds and Electrostatic Interactions

A novel two‐dimensional network dibenzo‐18‐crown‐6 (DB18‐C6) complex: [Na (DB18‐C‐6) (H₂O)₂] [Na (DB18‐C‐6) (SCN)₂] has been isolated and characterized by elemental, IR and X‐ray diffraction analysis. The crystal structure belongs to monoclinic, space group P2₁/c with cell dimensions a = 1.06178(7), b = 1.40243(8), c = 3.03496(19) nm, β = 90.4220(10)°, V = 4.5292(5) nm³, Z=4, D_calcd =1.351 g/ cm³, F(000) = 1936, R₁ = 0.0369, wR₂ = 0.0821. The most interesting feature in this structure is that complex cation and complex anion form a two‐dimensional network via τ‐τ stacking interactions, hydrogen bonds and electrostatic interactions.     

Synthesis and Characterization of a Two‐Dimensional Zinc Phosphite,Zn3(tren)(HPO3)3·xH2O (x ≈ 0.5; tren = tris(2‐aminoethyl)amine)

A new zinc phosphite with the formula Zn₃(tren)(HPO₃)₃·xH₂O (x≈0.5) has been synthesized under hydrothermal conditions and characterized by FTIR, elemental analysis, powder X‐ray diffraction, single‐crystal X‐ray diffraction, thermogravimetric analysis and its fluorescent spectrum. The compound crystallizes in the triclinic system, space group (No.2), a = 10.1188(9) Å, b = 10.4194(9) Å, c = 10.5176(9) Å, α = 60.763(2)°, β = 70.6150(10)°, γ = 80.725(2)°, V = 912.77(14) ų, Z = 2. The structure consists of double crankshaft chains, which are linked by Zn‐O‐P bonds to form 8‐ and 12‐membered channels along the [100] direction. The claw‐like Zn‐centered complexes of Zn(N₄C₆H₁₈) as the supported templates, hang into the 12‐MR channels through Zn‐O‐P linkages with framework.     

Hydrothermal Synthesis and X‐ray Crystal Structure of Four Inorganic‐Organic Hybrid Compounds in Vanadium /Copper Iodate Family

Four inorganic‐organic hybrid compounds with the formulae (1,10‐phen)(VO₂)(IO₃) ( 1 ), (2,2′‐bipy)(VO₂)(IO₃) ( 2 ), [Cu₃(2,2′‐bipy)₃Cl₃(IO₃)₂]·I_1.5 ( 3 ), and [Cu(2,2′‐bipy)(H₂O)(IO₃)₂]· (H₂O)₂ ( 4 ) are hydrothermally synthesized at 120 °C for 6 d and characterized by single‐crystal X‐ray diffraction. The use of two different bidentate organodiamine ligands 1,10‐phen and 2,2′‐bipy in the V/I/O system gives rise to compounds 1 and 2 , which crystallize in a monoclinic system with the space group C2/c, a = 17.8131(6) Å, b = 15.0470(7) Å, c = 12.9902(4) Å, β = 133.095(2)°, V = 2542.49(17) ų for 1 and space group P2₁/c, a = 13.3095(5) Å, b = 15.0993(8) Å, c = 13.0454(4) Å, β = 116.971(2)°, V = 2335.88(17) ų for 2 . The use of the bidentate organodiamine ligand 2,2′‐bipy in the Cu/I/O system gives rise to the variety in the structure of products 3 and 4 , which crystallize in a triclinic system with the same space group . a = 8.5143(2) Å, b = 10.4908(3) Å, c = 22.8420(6) Å, α = 93.769(10)°, β = 91.723(10)°, γ = 112.111(10)°, V = 1882.83(9) ų for 3 and a = 6.731(6) Å, b = 10.110(4) Å, c = 12.899(6) Å, α = 106.00(5)°, β = 95.45(4)°, γ = 107.69(6)°, V = 788.4(9) ų for 4 . The solid‐state structures of the compounds 1 and 2 have chains with repeat units of alternative corner sharing of [VO₄N₂] octahedra and [IO₃] pyramids. Compound 3 is a chain containing [IO₃] pyramids and [VO₄N] square pyramids and compound 4 consists of Cu(2,2′‐bipy)²⁺ linked by one water molecule and two [IO₃] pyramids. The thermal stabilities of the compounds are investigated.     

Synthesis, Structure and Biological Activities of S-[α-（ 4-Methoxyphenylcarbonyl ）-2-（1,2,4-triazole-l-yl） ethyl-N, N-dime-thyldithiocarbamate

The title compound was prepared by reaction of N, N‐dimethyldithiocarbamate sodium with l‐bromo‐l‐(4‐methoxyphenylcarbonyl)‐2‐(1, 2, 4‐triazole‐l‐yl) ethane. Its crystal structure has been determined by X‐ray diffraction analysis. The crystal belongs to triclinic with space group Pī, a = 0.7339(2) nm, b = 1.1032(2) nm, c = 1.1203(2) nm, a = 90.27(3)°, β = 102.03(3)°, γ = 104.91(3)°, Z=2, V = 0.8556(3) nm³, D_c = 1.360 g/cm³, μ =0.325 mm^?1, F(000)=368, final R₁ =0.0475. The planes of 4‐methoxybenzyl group and triazole ring are nearly perpendicular to each other. The dihedral angle is 83.97°. There is an obvious π‐π stacking interaction between the molecules in the crystal lattice. The results of biological test show that the title compound has fungicidal and plant growth regulating activities.     

Struktur und magnetische Eigenschaften von Bis{3‐amino‐1,2,4‐triazolium(1+)}pentafluoromanganat(III): (3‐atriazH)2[MnF5]

Structure and Magnetic Properties of Bis{3‐amino‐1,2,4‐triazolium(1+)}pentafluoromanganate(III): (3‐atriazH)₂[MnF₅] The crystal structure of (3‐atriazH)₂[MnF₅], space group P1, Z = 4, a = 8.007(1) Å, b = 11.390(1) Å, c = 12.788(1) Å, α = 85.19(1)°, β = 71.81(1)°, γ = 73.87(1)°, R = 0.034, is built by octahedral trans‐chain anions [MnF₅]^2–_∞ separated by the mono‐protonated organic amine cations. The [MnF₆] octahedra are strongly elongated along the chain axis (<Mn–F_ax> 2.135 Å, <Mn–F_eq> 1.842 Å), mainly due to the Jahn‐Teller effect, the chains are kinked with an average bridge angle Mn–F–Mn = 139.3°. Below 66 K the compound shows 1D‐antiferromagnetism with an exchange energy of J/k = –10.8 K. 3D ordering is observed at T_N = 9.0 K. In spite of the large inter‐chain separation of 8.2 Å a remarkable inter‐chain interaction with |J′/J| = 1.3 · 10^–5 is observed, mediated probably by H‐bonds. That as well as the less favourable D/J ratio of 0.25 excludes the existence of a Haldene phase possible for Mn³⁺ (S = 2).