CAJ | 학술논문

在石油醚和丙酮溶液中,配合物 Ni[S2P(OCH2CH2PH)2]2 与1,10-邻菲啰啉(phen)反应得到了绿色的氮碱加合物1,10-林菲啰啉·双(O,O'-(二2-苯乙基)二硫代磷酸)合镍(Ⅱ),用元素分析、紫外-可见光谱、红外光谱、热分析和 X-射线单晶衍射进行了表征.加合物属单斜晶系,P21/c空间群.晶胞参数为 a=1.0987(9)nm,b=2.1432(9)nm,c=1.9025(5)nm,β=98.68(1)°,V=4.429(4)nm3,Z=4,Dc=1.370 Mg/m3,F(000)=1904,μ=0.743mm-1,可观测衍射点为 3498,R=0.057,wR=0.1492(I(2σ(I)).加合物为畸变八面体构型,配位原子来自于两个O,O'-二(2-苯乙基)二硫代磷酸根的 4 个硫原子和配体 phen 的2个氮原子.Ni-S 键的键长在0.2474(2)-0.2505(17)nm 范围内,Ni-N 键的键长分别为0.2081(4)nm 和 0.2090(5)nm.因分子间存在π-π堆积、C-H…O 和 C-H…S 氢键作用,加合物的晶体结构形成了一维链对和一维双链螺旋链.一维链对和一维双链螺旋链通过 C-H…O 氢键作用进一步延展为三维结构.
재석유미화병동용액중,배합물 Ni[S2P(OCH2CH2PH)2]2 여1,10-린비라람(phen)반응득도료록색적담감가합물1,10-림비라람·쌍(O,O'-(이2-분을기)이류대린산)합얼(Ⅱ),용원소분석、자외-가견광보、홍외광보、열분석화 X-사선단정연사진행료표정.가합물속단사정계,P21/c공간군.정포삼수위 a=1.0987(9)nm,b=2.1432(9)nm,c=1.9025(5)nm,β=98.68(1)°,V=4.429(4)nm3,Z=4,Dc=1.370 Mg/m3,F(000)=1904,μ=0.743mm-1,가관측연사점위 3498,R=0.057,wR=0.1492(I(2σ(I)).가합물위기변팔면체구형,배위원자래자우량개O,O'-이(2-분을기)이류대린산근적 4 개류원자화배체 phen 적2개담원자.Ni-S 건적건장재0.2474(2)-0.2505(17)nm 범위내,Ni-N 건적건장분별위0.2081(4)nm 화 0.2090(5)nm.인분자간존재π-π퇴적、C-H…O 화 C-H…S 경건작용,가합물적정체결구형성료일유련대화일유쌍련라선련.일유련대화일유쌍련라선련통과 C-H…O 경건작용진일보연전위삼유결구.
Reaction of complex Ni [S2P(OCH2CH2PH)2] 2 with nitrogen base donor 1,10-phenanthroline (phen) was carried out in petroleum ether and acetone solution to give green nitrogen base adduct 1,10-phenanthroline bis ( O, O'-di ( 2 -phenylethyl) dithiophosphato ) nickel ( II ), Ni [ S2P ( OCH2 CH2Ph )2]2. phen. The adduct was characterized by elemental analysis, UV-visible and IR spectra, thermal analysis and single-crystal X-ray diffraction. The crystal belongs to the monoclinic system, space group P2,/c with a = 1. 0987(9) nm, b = 2. 1432(9) nm, c =1.9025(5) nm,β = 98.68(1)°, V = 4.429(4) nm3, Z = 4, Dc = 1.370 Mg/m3,F(000) = 1904,μ= 0.743mm-1, the final R = 0.057 and wR = 0. 1492 for 3498 observed reflections (I(2σ(I)). The Ni(II) atom adopts a distorted octahedral geometry with four sulfur atoms from two O,O'-di(2-phenylethyl)dithiophosphate ligands and two nitrogen atoms from a phen ligand. The Ni-S distances rang from 0. 2474(2) to 0. 2505 (17) nm, and the Ni-N distances are 0. 2081 (4) and 0. 2090 (5) nm. The overall structure of adduct consists of 1 D chain-pair and 1 D double-stranded helical chain, which formed from intermolecular π-π stacking, C-H…O and C-H…S hydrogen-bonding interactions. They are further extended to 3D supramolecular network via C-H…O hydrogen-bonding interactions.