质子化N，N＇-双（吡啶基-2-亚甲基）-1，4-二氮环庚烷高氯酸盐的合成、表征和晶体结构研究

合成并表征了一个吡啶功能化1,4-二氮环庚烷(DACH)化合物[N,N'-双(吡啶基-2-亚甲基)-1,4-二氮环庚烷]的质子化高氯酸盐.用X-射线衍射技术测定了标题化合物H4BPDACH·(ClO4)4·1.5H2O (1)的晶体结构三斜晶系,P-1空间群,晶胞参数a=0.7911(5) nm, b=1.269 5(9) nm, c=1.517 8(11) nm, α=104.448(13)°, β=102.383(13) °, γ=92.159(12) °, V=1.435 2(17) nm3, Z=2. 化合物1的不对称单元中包含两个晶体学独立的[H4BPDACH]4+阳离子,其中DACH环均采取类似的船式构象,但两个侧臂吡啶环分别采取顺势和反式排列.质子化NH基团和溶剂及阴离子之间存在多重氢键相互作用,这进一步稳定了此结构.

Synthesis,Characterization and Crystal Structure of the ProtonatedN,N''''-Bis(pyridin-2-ylmethyl)-1,4-diazacycloheptane Perchlorate

The protonated perchlorate of a pyridyl-functionalized l,4-diazacycloheptane (DACH) compound [namely N,N'-bis(pyridin-2-ylmethyl)-1,4-diazacycloheptane (BPDACH)] was synthesized and characterized. The crystal structure of the title compound, H4BPDACH·(ClO4)4·1.5H2O (1) was determined by single-crystal X-ray diffraction analysis: crystallizing in triclinic crystal system, space group P-1 with a=0.791 1(5) nm, b=1.269 5(9) nm, c=1.517 8(11) nm, α=104.448(13)°, β=102.383(13)°, γ=92.159(12)°, V=1.435 2(17) nm3, Z=2. The asymmetric unit of compound 1 contains two crystallographically independent [H4BPDACH]4+ cations, in which the DACH rings are folded up into similar chair configuration, but two pendant arms are in different cis- and trans-arrangements, respectively. Multiple hydrogen bonds were observed between the protonated NH groups and the solvates/anions, which further stabilize this structure.