Synthesis,thermal analysis,IR spectra,and crystal structure of ammonium 9-molybdomanganate

Ammonium 9-molybdomanganate (NH₄)₆[MnMo₉O₃₂]·6H₂O was synthesized and studied by single-crystal and powder X-ray diffraction, thermogravimetric analysis and IR spectroscopy. The crystals are trigonal, space group R32, a = 15.926(2) Å, c = 12.398(2) Å, V = 2723.3(7) ų, M = 1646.75, Z = 3, ρ(calcd) = 2.98 g/cm³.     

Synthesis,crystal structure,infrared spectrum and thermal behaviourof α-BaHPO4

The phosphate α-BaHPO₄ was synthesised as a single-phase crystalline powder starting from an aqueous solution of barium hydroxide and phosphorus pentoxide at 373 K. α-BaHPO₄ crystallises in a new structure type in which the Ba²⁺ ions form a distorted body-centred arrangement with the HPO₄^? anions in the quasi-octahedral voids (BaHPO₄, Aem2, Z = 16, a = 459.96(9), b = 22.809(5), c = 14.081(3) pm, wR₂ = 0.077, R₁ = 0.069, 1995 reflections, 102 parameters). The crystal structures of α-BaHPO₄ and β-BaHPO₄ are compared. The infrared spectrum and a thermal and thermogravimetric analysis of α-BaHPO₄ are also reported.     

Yttrium tris-propionate monohydrate: Synthesis,crystal structure,and thermal stability

The complex [Y(Prop)₃(H₂O)]_∞ (I) was prepared by treating yttrium carbonate, acetate, or acetylacetonate hydrates with propionic acid and characterized by the data of elemental analysis, IR spectroscopy, X-ray diffraction, and thermal analysis in air. Complex I has a polymeric layered structure with clear-cut structure-forming dimeric groups bridged by bidentate ligands. Only van der Waals interactions occur between the adjacent polymeric layers. In air, yttrium propionate monohydrate I is completely converted to the oxide at 600°C.     

Crystal structure, thermal analysis and IR spectrometric investigation of L-tyrosine hydrazide sulfate

Chemical preparation, X-ray single crystal, thermal analysis and IR spectrometric investigation of (C₉H₁₅N₃O₂)SO₄ denoted LTHS are described. The LTHS crystallizes in the monoclinic system with P2₁ space group. Its unit cell dimensions are a=5.5386(1) Å, b=8.0467(4) Å, c=14.0780(6) Å, β=93.339(3)° with V=626.36(4) Å³ and Z=2. The structure has been solved using direct method and refined to a reliability R factor of 0.0212. The LTHS structure is built up from organic chains parallel to the b axis, linked via N---H…O hydrogen bonds and interconnected by inorganic groups so as to build a three-dimensional arrangement.     

Synthesis,crystal structure,and thermal behavior of dimethylgold(III) acetate

A dimethylgold(III) compound with an acetate fragment [(CH₃)₂AuOCOCH₃]₂ has been synthesized. The complex was identified from the melting point, IR, ¹H NMR, and mass spectrometry data. The temperature dependence of saturated vapor pressure over crystals has been measured and the thermodynamic parameters of sublimation have been determined by Knudsen’s effusion method with mass spectrometric measurements of the composition of the gas phase: ΔH _subl = 100.87 kJ·mol^?1, ΔS _subl = 216.67 J·mol^?1·K^?1. The thermal behavior of the solid compound was investigated by differential thermal analysis. The compound was studied by X-ray diffraction. Crystal data for C₈H₁₈Au₂O₄: a = 12.214(5) Å, b = 14.307(3) Å, c = 7.6635(15) Å; β = 103.39(3)°, Z = 4, d _calc = 2.917 g/cm³, space group P2(1)/c, R = 0.0261. The [(CH₃)₂AuOCOCH₃]₂ dimer complex with an Au...Au distance of 2.989 Å is the structural unit. The gold atom has a square plane environment of two carbon and two oxygen atoms; the Au-O distances vary from 2.118 Å to 2.139 Å. The molecules are arranged in chains linked by van der Waals interactions.     

Synthesis, crystal structure and thermal decomposition of a novel praseodymium supermolecular complex

A novel complex, [Pr(5-nip)(phen)(NO3)(DMF)] (5-nip: 5-nitroisophthalic acid; phen: 1,10-phenanthroline, DMF: N,N-dimethylformamide), was prepared and characterized by single crystal X-ray diffraction, elemental analysis, IR spectrum and DTG-DSC techniques. The results show that the crystal is monoclinic, space group P2(1)/n with a=11.0876(6) Å, b=12.8739(7) Å, c=16.9994(8) Å; β=91.193(4)°, Z=4, D _c=1.822 Mg m^–3, F(000)=1320. Each Pr(III) ion is nine-coordinated by one chelating bidentate and two monodentate bridging carboxylate groups, one chelating bidentate nitryl group, one DMF molecule and one 1,10-phenanthroline molecule. The complex is constructed with one-dimensional ribbons featuring dinuclear units and the one-dimensional ribbons are further assembled into two-dimensional networks by strong π–π stacking interactions. The complex has high stability up to 500°C. The enthalpy change of formation of the compound in DMF was measured using an RD496-III type microcalorimeter with the value of –9.214±0.173 kJ mol^–1.     

Synthesis, crystal structure and thermal analysis of tetraiodo-4, 4’-bi-1, 2, 4-triazole

Tetraiodo-4,4’-bi-1,2,4-triazole(1)was synthesized from a reaction of iodine monochloride with 4,4’-bi-1,2,4-triazole(2),which was prepared by a transamination reaction between 4-amine-1,2,4-triazole and N,N-dimethylformamide azine dihydrochloride(3)obtained via a Vilsmeier reaction.The title compound was extensively characterized by melting point,elemental analysis,IR,HRMS and single crystal X-ray diffraction.The single crystal X-ray structural analysis reveals that compound 1 exhibits a stable conformation with the two triazole rings being perpendicular to minimize three-dimensional steric hindrance and stacking through aromatic π...π packing interactions between molecules.The thermal analysis from TGA and DSC indicates that compound 1 decomposes at 275.40℃ and 338.35℃,respectively.     

Synthesis, crystal structure and thermal decomposition study of a new barium acetato-propionate complex

The present study reports on a novel barium acetato-propionate complex, obtained by the reaction of barium acetate with propionic acid, used as an oxide precursor with applications in superconducting thin films deposition. The molecular structure has been determined by X-ray diffraction on single crystals and demonstrated to be [Ba₇(CH₃CH₂COO)₁₀(CH₃COO)₄·5H₂O]. The barium acetato-propionate is a three-dimensional channel-type polymer. The thermal decomposition of the barium precursor has been studied by simultaneous differential thermal analysis-thermogravimetry-mass spectrometry (DTA-TG-MS) in air at a heating rate of 10 °C/min. Based on these analyses, infrared spectroscopy was further used to characterize the precursor solution by the step-wise addition of the reagents. The X-ray diffraction on the precursor powder at different temperatures was performed.     

Synthesis, structure and VUV luminescent properties of rubidium rare-earth fluorides

RbF-LnF₃ (Ln=rare earth) systems were synthesized by hydrothermal technique. Under the hydrothermal condition, the light rare-earth elements form LnF₃ (Ln=La-Nd), while the heavy ones form RbLn₂F₇ (Ln=Y, Er, Yb and Lu) with the RbEr₂F₇ structure type. RbLn₃F₁₀ compounds were found for the in-between rare-earth cations (Ln=Eu-Tm and Y), which crystallize exclusively in the cubic γ-KYb₃F₁₀-type structure. The luminescent properties under vacuum ultraviolet light were studied for the Eu³⁺-doped RbLn₃F₁₀ (Ln=Y, Gd) and a high quantum efficiency of about 150% was observed for RbGd₃F₁₀:Eu³⁺.     

Synthesis,crystal structure and thermal behavior of 4-amino-3,5-dinitropyrazole copper salt

A novel energetic combustion catalyst, 4-amino-3,S-dinitropyrazole copper salt （[Cu（adnp）2（H2O）2]）, was synthesized in a yield of 93.6% for the first time. The single crystal of [Cu（adnp）2（H2O）2] was determined by single crystal X-ray diffraction. It crystallizes in a triclinic system, space group p^-1 with crystal parameters a = 5.541（3） A, b = 7.926（4） A, c = 10.231（5） A,β = 101.372（8）°, V = 398.3（3） A3, Z = 1, μ = 1.467 mm^-1, F（0 0 0） = 243, and Dc = 2.000 g cm^-3. The thermal behavior and non-isothermal decomposition reaction kinetics of [Cu（adnp）2（H2O）2] were studied by means of different heating rate differential scanning calorimetry （DSC）. The kinetic equation of major exothermic decomposition reaction for [Cu（adnp）2（H2O）2] was obtained. The entropy of activation （△S≠）, enthalpy of activation （△H≠）, free energy of activation （△G≠）, the self-accelerating decomposition temperature （TSADT） and the critical temperature of thermal explosion （Tb） are 59.42 j mol^-1 K^-1, 169.5 kJ mol^-1, 1141.26 kJ mol ^-1 457.3 K and 468.1 K, respectively.     

Synthesis,crystal structure,thermal stability,and luminescent properties of lithium trimesate coordination polymer

Russian Chemical Bulletin - A metal-organic coordination polymer of the formula [Li3(btc)(H2O)] (1a) (H3btc is the trimesic acid, C6H3(COOH)3) was obtained upon heating a mixture of LiBH4 and H3btc...     

Crystal structure and IR spectrum of dipropargyl phthalate

A. N. Nesmeyanov Institute of Organometallic Compounds, Academy of Sciences of the USSR. Translated from Zhurnal Strukturnoi Khimii, Vol. 32, No. 3, pp. 144–146, May–June, 1991.     

Synthesis,crystal structure,and thermal behavior of a diiron toluenethiolate complex with triphenylphosphine coligand

Transition Metal Chemistry - A bis(p-toluenethiolato) dinuclear-carbonyl complex with triphenylphosphine coligand, [μ-(SC6H4CH3-p)2Fe2(CO)5(PPh3)], has been synthesized from...     

四面体异核金属羰基簇合物的合成、表征及单晶结构分析

利用金属交换反应, 使金属羰基配合物PhCCo~3(CO)~9和过渡金属配合物NaMo(CO)~3(RCp)在THF中回流反应, 制备出三个新的异核三金属羰基簇合物PhCCo~2Mo(CO)~8(RCp)(R=HCO, CH~3CO, C~2H~5O~2C)。结果表明, 与金属交换剂NaMo(CO)~3Cp相比较, 环戊二烯上吸电子基团C=O的存在减弱了金属交换剂NaMo(CO)~3(RCp)的交换活性。同时发现加热可加速该反应向产物的转化以及进一步证明了该金属交换反应的普遍性。对合成的簇合物进行了元素分析, 红外和氢的核磁谱的结构表征。对簇合物PhCCo~2(CO)~8(C~2H~5O~2CCp)的单晶进行了X射线结构测定, 该晶体属于单斜晶系, 空间群为P2~1/c, 晶胞参数: α=1.1356(2)nm,b=1.4030(2)nm, c=1.6076(3)nm, β=107.19(1)°, Z=4。D~c=1.80g/cm^3,R=0.048, Rw=0.057。     

N-咔唑-二硫代甲酸-4-苯乙烯基甲酯的合成、晶体结构及热稳定性

近年来,可逆加成-断裂链转移聚合(Reversible addition-fragmentation chain transfer polymerization) :RAFT聚合这一"活性"/可控自由基聚合方式成为高分子化学研究的热点之一[1-2],并被应用于纳米材料[3]、生物医药[4]等领域.研究RAFT聚合的首要问题是合成高活性的RAFT试剂,最常用的RAFT试剂是具有二硫代酯结构的化合物[Z-C(S)-S-R].     

Synthesis,crystal structure and thermal stability of new copper(II) trichloroacetate complexes

We have synthesized two novel complexes of copper(II) trichloro acetate, Cu₂(CCl₃COO)₃(OH)(H₂O)₄·H₂O and Cu(CCl₃COO)₂(MeCN), and determined their crystal structures and thermal stability. While the complex with acetonitrile has a discrete binuclear paddle-wheel structure, typical of copper carboxylates, the aqua-hydroxo complex belongs to a novel unique chain–molecular type of basic copper complexes.     

The syntheses,crystal structure,thermal analysis,and anticancer activities of novel dipicolinate complexes

[Cu(pydc)(eim)₃]?H₂O (1), [Cu(pydc)(4hp)(H₂O)] (2), and [Ni(pydc)(3hp)(H₂O)₂][Cu(pydc)(3hp)(H₂O)₂]?3H₂O (3) (H₂pydc = 2,6-pyridinedicarboxylic acid or dipicolinic acid, eim = 2-ethylimidazole, 4hp = 4-hydroxypyridine, 3hp = 3-hydroxypyridine) were synthesized and characterized by elemental analysis, spectroscopic measurements (UV–vis and IR spectra), and single-crystal X-ray diffraction. Crystal analysis revealed that the complexes extended to 3-D supramolecular networks through intermolecular H-bonding and molecular interactions between the ligand moieties and water molecules. The thermal stabilities of complexes are investigated by thermogravimetry, differential thermogravimetry, and differential thermal analysis techniques. The effects of complexes on the proliferation of HT-1080 fibrosarcoma cells were investigated using the quick cell proliferation assay. The cell viability changes were found to depend on the concentrations and type of complex.