论文部分内容阅读
3-硝基-1,2,4-三唑-5-酮(NTO)作为一种高能低感度含能材料受到了有关工作者的极大重视.其金属盐在火炸药方面有重要的用途,因而引起了人们极大的关注,我们制备了NTO的钴配合物单晶,测定了其结构,并研究了它的热分解机理.1 晶体制备与组成将NTO分散于蒸馏水中(M:V=1:4),在60℃下,边搅拌边用氢氧化锂的水溶液中和至pH值7左右,然后将制得的溶液在60℃下逐渐滴加到硝酸钴水溶液中,得到棕黄色沉淀物,将沉淀物溶于蒸馏水中,在室温下培养得到适用于X射线衍射法结构测定的桔黄色单晶,元素分析结果,计算值(%):Co 12.78,C 10.42,N 24.30,H 3.92;实测值(%):Co 12.12,C9.85,N 24.78,H 4.01.IR:v_C=Ο=1644cm～(-1),v_(NO_2)~(as)=1509cm～(-1),v_(NO_2)~s=13llcm～(-1),v_(M-Ο)=327cm～(-1),v_(M-N)=261cm～(-1).2 晶体结构测定选用尺寸为0.20mm×0.25mm×0.35mm的单晶,在CAD4PDP11/44型四圆单晶衍射仪上,用MoKα射线、石墨单色器,以25个衍射点精确测定取向矩阵和晶胞参数,用θ/2θ方式扫描,在2°<θ<25°范围内共收集独立衍射1705个,其中I>3.0σ(I)者为1509个用于结构测定和修正,数据经L_p校正,但未经吸收校正,所得晶体属单斜晶系,空间群P2_1/c,其晶体学数据为:α=0.9284(l)nm,b=1.4239(1)nm,c=0.6506(1)nm,β
Nitro-1,2,4-triazol-5-one (NTO) has received great attention as a high-energy, low-energy and energetic material and its metal salts have important applications in explosives and explosives , Which attracted people’s attention. We prepared a single crystal of cobalt complex of NTO, determined its structure and studied its thermal decomposition mechanism.1 Preparation and Composition of Crystal NTO was dispersed in distilled water (M: V = 1: 4) was neutralized with an aqueous solution of lithium hydroxide to a pH of about 7 at 60 ° C with stirring, and then the obtained solution was gradually added dropwise to a cobalt nitrate aqueous solution at 60 ° C to obtain a tan yellow The precipitate was dissolved in distilled water and cultured at room temperature to obtain an orange single crystal suitable for X-ray diffractometry. Elemental analysis (%): Co 12.78, C 10.42, N 24.30, H 3.92; found (%): Co 12.12, C9.85, N 24.78, H 4.01.IR:v_C=Ο=1644cm~(-1),v_(NO_2)~(as)=1509cm~(-1), v_ (MN) = 261cm -1, v_ (NO_2) ~ s = 1311cm -1, v_ (M_O) = 327cm -1, and the size of the crystal structure is 0.20mm × 0.25mm × 0.35mm single crystal, in the CAD4PDP11 / 44 four-round single-crystal diffractometer, with MoKα ray, graphite monochromator , The orientation matrix and unit cell parameters were accurately measured by 25 diffraction spots and scanned by θ / 2θ. A total of 1705 independent diffraction spots were collected in the range of 2 ° <θ <25 °, where I> 3.0σ (I) was 1509 The data were corrected by L_p but corrected without absorption. The obtained crystals were monoclinic with space group P2_1 / c. The crystallographic data were as follows: α = 0.9284 (1) nm, b = 1.4239 (1) nm, c = 0.6506 (1) nm, β