Whole-mol­ecule disorder of the heterometallic complex di­aqua-1κ2O-di­chlorido-2κ2Cl-(μ-2-formyl-6-meth­oxy­phenolato-1κ2O1,O2:2κO6){μ-2-meth­oxy-6-[(methyl­imino)­meth­yl]phenolato-1κ2N,O1:2κO6}lead(II)nickel(II)

IF 0.6 Q4 CRYSTALLOGRAPHY
Olga Yu. Vassilyeva , Vladimir N. Kokozay , Evgeny Goreshnik
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引用次数: 0

Abstract

In the crystal the title compound exhibits full-mol­ecule disorder [occupancy ratio 0.711 (6): 0.289 (6)], generated by a false twofold rotation about the shorter, Ni–Pb, axis of the mol­ecule.
The new mol­ecular complex [NiPb(C9H10NO2)(C8H7NO3)Cl2(H2O)2] with the Schiff base 2-meth­oxy-6-[(methyl­imino)­meth­yl]phenol and ortho-vanillin ligands, both deprotonated, crystallizes in the monoclinic space group P21/c with one mol­ecule per asymmetric unit. The heterometallic mol­ecule exhibits a whole-mol­ecule orientational disorder [occupancy ratio 0.711 (6): 0.289 (6)] about a pseudo-twofold rotation axis that roughly bis­ects the mol­ecule along the Ni–Pb axis. The Ni centre coordination is distorted octa­hedral [Ni—N/Oeq = 1.996 (8)–2.021 (7) Å, major component] with two water mol­ecules in the apexes [2.088 (6) and 2.090 (5) Å]. The Pb atom is six-coordinate in a highly distorted tetra­gonal–bipyramidal geometry. Two phenolato and two methoxo O atoms from the deprotonated ligand moieties are nearly coplanar with the metal centre [Pb–O 2.301 (8)–2.740 (10) Å, major component], while the two chlorides are located on opposite sides of the plane [Pb—Cl = 2.821 (5) and 2.868 (5) Å]. The Ni–Pb pair of metals is bridged by two phenolato O atoms enabling a metal–metal separation of 3.441 (3)/3.477 (7) Å. Two intra­molecular O–H⋯Cl hydrogen bonds between coordinated aqua and chloride ligands appear to be a reason for the Cl–Pb–Cl and O–Ni–O angles being far from 180°. In the solid state, the well-separated heterometallic mol­ecules are inter­linked by π–π stacking and weak O—H⋯Cl and C—H⋯Cl/O hydrogen bonds. The mol­ecules show no significant inter­molecular inter­actions: the minimal MM distance in the crystal is about 7.65 Å (Ni⋯Pb).

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异金属配合物二水-1 - κ2 - O-二氯-2- κ2 Cl-(μ-2-甲酰基-6-甲基-氧-苯酚-1 - κ2 - O,O:2 - κO 6){μ-2-甲基-氧-6-[(甲基亚氨基)-甲基]苯酚-1 - κ2 N,O:2 - κO 6}铅(II)镍(II)的全分子无序性。
新分子配合物[NiPb(C9H10NO2)(C8H7NO3)Cl2(H2O)2]与希夫碱2-甲基氧-6-[(甲基亚氨基)-甲基基]苯酚和邻香兰素配体均去质子化,在单斜空间群P21/c中结晶,每个不对称单元有一个分子。异质金属分子在沿Ni-Pb轴大致平行的伪双重旋转轴上表现出全分子取向紊乱[占比0.711(6):0.289(6)]。Ni中心配位为扭曲的八面体[Ni- n /Oeq = 1.996 (8)-2.021 (7) Å,主要成分],两个水分子位于顶端[2.088(6)和2.090 (5)Å]。铅原子是高度扭曲的四边形-双锥体六坐标结构。去质子化配体上的两个酚O原子和两个甲氧基O原子几乎与金属中心共面[Pb-Cl = 2.301 (8)-2.740 (10) Å,主要成分],而两个氯化物则位于平面的两侧[Pb-Cl = 2.821(5)和2.868 (5)Å]。Ni-Pb金属对由两个酚O原子桥接,使得金属-金属分离为3.441 (3)/3.477 (7)Å。在配位的水和氯配体之间的两个分子内O-H⋯Cl氢键似乎是Cl- pb -Cl和O-Ni-O角远未达到180°的原因。在固态中,分离良好的异金属分子通过π-π堆叠和弱的O- h⋯Cl和C-H⋯Cl/O氢键相互连接。分子之间没有显着的分子间相互作用:晶体中的最小M⋯M距离约为7.65 Å (Ni⋯Pb)。
本文章由计算机程序翻译,如有差异,请以英文原文为准。
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来源期刊
CiteScore
1.90
自引率
0.00%
发文量
351
审稿时长
3 weeks
期刊介绍: Acta Crystallographica Section E: Crystallographic Communications is the IUCr''s open-access structural communications journal. It provides a fast, simple and easily accessible publication mechanism for crystal structure determinations of inorganic, metal-organic and organic compounds. The electronic submission, validation, refereeing and publication facilities of the journal ensure rapid and high-quality publication of fully validated structures. The primary article category is Research Communications; these are peer-reviewed articles describing one or more structure determinations with appropriate discussion of the science.
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