Synthesis,Crystal Structure and Thermal Decomposition of a New Energetic Dipotassium 3,3'-Dinitro-5,5'-bis-1,2,4-triazole-1,1'-diolate

A new energetic dipotassium 3,3?-dinitro-5,5?-bis-1,2,4-triazole-1,1?-diolate [K_2(DNOBT)] was synthesized, and structurally characterized by elemental analysis, IR spectra, 13 C NMR and single-crystal X-ray diffraction. K_2(DNOBT)·2H_2O crystallizes in monoclinic system, space group P21/n with a=6.0446(10), b=15.999(3), c=6.4169(11) ?, β=99.421(2)°, V=612.21(18) ?~3, Z=4, Dc=2.009 g·cm~(-3), F(000)=372, μ=0.838 mm~(-1), S=1.012, the final R=0.0248 and w R(I 2σ(I))=0.0604. Thermal decomposition of the title compound was studied by using DSC and TG-DTG, and there is primarily one exothermic decomposition process at 371.5 ℃.     

Two Cd(Ⅱ)-biphenyl-3,3’-disulfonyl-4,4’-dicarboxylate-2,2’-bipyridine Compounds: Structures and Luminescence

Two coordination polymers based on the mixed ligands of biphenyl-3,3?-disul-fonyl-4,4?-dicarboxylate(BPDSDC4–)and 2,2?-bipyridine(2,2?-bpy),{[Cd(BPDSDC)0.5(2,2?-bpy)(H2O)]·(H2O)}n(1)and{[Cd(BPDSDC)0.5(2,2?-bpy)2]·(H2O)}n(2)were synthesized.Both compounds crystallize in the monoclinic system,space group P21/n.For 1,a=7.5737(2),b=17.4284(5),c=13.5982(5)?,β=90.788(3)°,V=1794.76(10)?^3,Z=4,C17H15N2O7SCd,Mr=503.77,Dc=1.864 g/cm^3,μ=1.378 mm^?1,F(000)=1004,the final R=0.0299 and wR=0.0644 for 3137 observed reflections with I>2s(I).For 2,a=13.3097(2),b=10.66240(10),c=17.6583(3)?,β=91.779(2)°,V=2504.74(6)?^3,Z=4,C27H21N4O6SCd,Mr=641.94,Dc=1.702 g/cm^3,μ=1.008 mm^?1,F(000)=1292,the final R=0.0244 and wR=0.0583 for 4594 observed reflections with I>2s(I).The Cd(II)atoms in both compounds are six-coordinated.In 1,the Cd(2,2?-bpy)units are connected by BPDSDC4–ligands to generate a one-dimensional(1D)ribbon structure.The 1D ribbons are linked by the hydrogen bonds and π···π interactions to give a three-dimensional(3D)structure.In compound 2,the Cd(2,2?-bpy)2 units are linked by the BPDSDC^4–ligands to form a 1D chain.Compounds 1 and 2 show luminescent emissions.     

Synthesis,Crystal Structure and Thermal Decomposition of a New Energetic Potassium Salt of Bis（dinitromethyl）difurazanyl Ether

A new energetic organic potassium salt bis(dinitromethyl)difurazanyl ether potassium salt [K2(BDFE)] was synthesized, and structurally characterized by elemental analysis, IR spectra, 13 C NMR and single-crystal X-ray diffraction. K2(BDFE) crystallizes in monoclinic system, space group C2/c with a = 17.342(3), b = 12.6943(17), c = 8.0972(11), β = 110.630(2)°, V = 1668.3(4)3, Z = 4, Dc = 2.000 g/cm3, F(000) = 1000, μ = 0.675 mm-1, S = 1.058, the final R = 0.0499 and wR = 0.1452. The K ion is eight-coordinated with eight O atoms from one water molecule and four bis(dinitromethyl)difurazanyl ethers(BDFE), forming a distorted dodecahedral structure. Thermal decomposition of the title complex was studied by using DSC and TG-DTG. There are primarily two exothermic decomposition processes between 200 and 370 ℃.     

Thermal Decomposition of Ammonium 3-Nitro-1,2,4-triazol-5-onate Monohydrate

The thermal decomposition of ammonium 3-nitro-1,2,4-triazol-5-onate monohydrate[NH4（NTO）·H2O] was studied by means of thermal analysis-MS coupling and the combination technique of in situ thermolysis cell with rapid-scan Fourier transform infrared spectroscopy. The results show that there are two endothermic steps and one exothermic step in the decomposition process of NH4（NTO）·H2O. The detected gas products consist of NH3, H2O, N2, CO2, CO, and NO2.     

Cobalt(II) coordination polymers built on isomeric dipyridyl triazole ligands with pyromellitic acid: Synthesis, characterization and their effects on the thermal decomposition of ammonium perchlorate

Three new cobalt(Ⅱ) coordination compounds,[Co(3,3’-Hbpt)2(H2pm)(H2O)2]·2H2O(1),[Co(4,4’-Hbpt)(pm)0.5(H2O)]·3H2O (2) and [Co(3,4’-Hbpt)(pm) 0.5 (H2O)3]·2H2O(3)(3,3’-Hbpt=3,5-bis(3-pyridyl)-1H-1,2,4-triazole;4,4’-bpt=3,5-bis(4-pyridyl)1H-1,2,4-triazole,3,4’-Hbpt=3-(3-pyridyl)-5-(4’-pyridyl)-1H-1,2,4-triazole and H4pm=pyromellitic acid) have been synthesized by hydrothermal reactions.Single-crystal X-ray diffraction reveals that compound 1 has a one-dimensional (1D) chain network,2 exhibits a four-connected three-dimensional (3D) structure with 1D open channels encapsulated by water molecules,while 3 displays a regular two-dimensional (2D) architecture connected through 1D metal helical chains.In addition,the efficacy of compounds 1-3 as additives to promote the thermal decomposition of ammonium perchlorate (AP) is explored by differential scanning calorimetry (DSC).     

Preparation,Crystal Structure,Thermal Decomposition and Explosive Properties of K2（tza）2（H2O） （tza=Tetrazole-1-acetic Acid）

A new energetic compound based on the tetrazole-1-acetic acid (tza) and potassium(I) salt, K2(tza)2(H2O), was synthesized and characterized by elemental analysis and FT-IR spectrum. Its crystal structure was determined by single-crystal X-ray diffraction analysis. The results show that the crystal belongs to the orthorhombic system, space group Pna21 with a = 1.11972(17) nm, b = 0.46647(7) nm, c = 2.5158(4) nm, V = 1.3140(3) nm3, K2C6H8N8O5, Mr = 350.40 g·mol-1, Dc = 1.771 g·cm-3, μ(MoKα) = 0.759 mm-1, F(000) = 712, Z = 4, R = 0.023 and wR = 0.0527 for 2961 observed reflections (I > 2σ(I)). The K(I) cation is six-coordinated with four O atoms from three carboxylate groups, one O atom from one H2O molecule and one N atom from tetrazolyl ring, in which each tza is coordinated in a tridentate chelating bridging coordination mode. The thermal decomposition mechanism of the title complex was studied by DSC and TG-DTG techniques. Under nitrogen atmosphere at a heating rate of 10 K·min-1, the thermal decomposition of the complex contains one main exothermic process between 191.7 and 243.8 ℃ in the DSC curve. Its combustion heat was mensurated by oxygen bomb calorimetry. The non-isothermal kinetics parameters were calculated by the Kissinger's method and Ozawa-Doyle's method, respectively. The sensitivity properties of K2(tza)2(H2O) were also determined with standard methods, which was very sensitive to flame.     

Synthesis via Precursor Method and Shape Evolution of Basic Magnesium Carbonate

Basic magnesium carbonate(4 MgCO3·Mg(OH)2·4 H2 O) with spherical-like structure was synthesized through precursors thermal decomposition. The precursor of magnesium carbonate trihydrates(MgCO3·3 H2 O) was synthesized by brine and ammonium bicarbonate, and the thermal decomposition conditions were investigated in detail. The obtained particulate was characterized using SEM, XRD and laser particle analyzer. The result showed that it was easy to obtain spherical-like 4 MgCO3·Mg(OH)2·4 H2 O by precursor thermal decomposition at 80~100 ℃ with thermal decomposition time 90 min, stirring time 15 min and the liquid initial concentration 0.1 mol/L, while rod-like 4 MgCO3·Mg(OH)2·4 H2 O with a surface of "house of card" structure was more likely to be obtained at low temperature(55 ℃), and rosette-like products were obtained at a little higher temperature(80 ℃) by direct synthesis.     

Synthesis and Molecular Structure of 1,5,1 ＇,5 ＇-Tetraphenyl- 1H, 1H ＇-3,3 ＇- dialkylthio-bi- 1,2,4-t riazole

The title compound 1,5,1',5'-tetraphenyl-1H,1H'-3,3'-dialkylthio-bi-1,2,4-tri- azole (2, C28H20N6S2, Mr = 504.62) was prepared by the reaction of 1-benzoyl-3-phenylamino- thiourea 1 and Mn(OAc)3·2H2O in acetic acid under microwave irradiation. The crystal is of monoclinic, space group P21/c with a = 11.3931(10), b = 16.5787(14), c = 26.470(2) , β = 98.274(2)o, Z = 8, V = 4947.8(8) 3, Dc = 1.355 g/cm3, μ(MoKα) = 0.245 mm-1, F(000) = 2096, the final R = 0.0583 and wR = 0.1502 for 8705 observed reflections (I > 2σ(I)). X-ray analysis reveals that the title compound is 1,5,1',5'-tetraphenyl-1H,1H'-3,3'-dialkylthio-bi-1,2,4-triazo- le, and its formation mechanism was proposed.     

Syntheses and Crystal Structures of Copper（Ⅱ） and Nickel Complexes with 1,2,3-Triazole-carboxylic Acid

Three novel complexes [Cu(L1)2(H2O)2] (1), [Ni(L1)2(H2O)2]·(H2O)4(2,HL1=5-methyl-1-(4-methylphenyl)-1,2,3-triazole-4-carboxylic acid) and [Ni2 (HL2)2(CH3OH)6]·(CH3OH)2(3,H3L2=1,2,3-triazole-4,5-dicarboxylic acid) were synthesized and characterized by elemental analysis, IR and X-ray diffraction. Complexes 1 and 2 are mononuclear structures, and are assembled into a two-dimensional sheet by C(7) H(7)···O(3) weak interactions or hydrogen-bonding interaction. Complex 3 is a centrosymmetric dinuclear structure, and is assembled into a three-dimensional supramolecular structure by hydrogen-bonding interaction.     

Synthesis,Crystal Structure and Biological Activity of 4-Amino-2,4-dihydro-5-((3,5-dimethyl-1H-pyrazol-1-yl)methyl)-3H-1,2,4-triazole-3-thione Schiff Base

The target compound 1,2,4-triazole Schiff base containing pyrazole ring was synthesized by 4-amino-2,4-dihydro-5-((3,5-dimethyl- lH-pyrazol-1-yl)methyl)-3H-1,2,4-triazole-3-thione and 3,4,5-trimethoxy benzaldehyde.The structure was confirmed by IR,~1H NMR,H RMS,elemental analysis and single-crystal X-ray diffraction.The crystal belongs to the triclinic system,space group P1 with a = 7.8772(17),b = 8.2986(18),c = 15.392(3) A,α= 93.360(4),β= 94.609(4),γ= 93.584(4)°,C_(18)H_(22)N_6O_3S,M_r= 402.47,V= 998.9(4) A~3,Z= 2,F(000) = 422,D_c =1.335 g/cm~3,μ= 0.194 mm~(-1),the final R = 0.0533 and wR = 0.1329 for 3517 observed reflections with I 2σ(I).The preliminary bioassay results indicate that the target compound has good fungicidal activity against Gibberlla nicotiancola in EC50 value and F.O.f.sp.niveum in EC_(95) value.