Cis-dioxidomolybdenum(VI) complexes [MoO2L1(DMSO)] (1), [MoO2L2(H2O)]·DMF (2) and [MoO2L3(DMF)] (3) were synthesized by solution based reactions of aroylhydrazones (H2L1 = 5-chloro-2-hydroxybenzaldehyde nicotinoylhydrazone, H2L2 = 2-hydroxy-5-iodobenzaldehyde nicotinoylhydrazone and H2L3 = 3,5-dichloro-2-hydroxybenzaldehyde nicotinoylhydrazone) with bis(acetylacetonato)dioxidomolybdenum(VI) complex, [MoO2(acac)2] in presence of DMSO or DMF. The synthesized aroylhydrazones and their molybdenum complexes were characterized by elemental analysis, spectroscopic techniques (FT-IR, UV–Vis, 1H NMR) and conductivity measurements. Finally the three dimensional structures of the complexes were confirmed by single crystal X-ray diffraction studies. Crystal structures of 1, 2 and 3 were solved by direct methods and refined with full-matrix least-squares calculations using the SHELXS97 and SHELXL2014 software programs respectively. Complex 1 got crystallized in monoclinic space group, P21/c with Z = 4, whereas complexes 2 and 3 in triclinic space group, P$$\overline {1}$$1¯ with Z = 2. The ligands, H2L1−3 showed coordination to the metal ion in a dibasic tridentate manner through deprotonated phenolate oxygen, azomethine nitrogen and enolate oxygen.Graphical AbstractAll the three dioxidomolybdenum(VI) complexes exhibit a distorted octahedral geometry around molybdenum atom. ORTEP plot of [MoO2L2(H2O)]·DMF. (Displacement ellipsoids are drawn at 50% probability)

中文翻译：

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烟酰腙衍生的二氧化钼 (VI) 配合物的合成、光谱表征和晶体结构

顺式二氧化钼 (VI) 配合物 [MoO2L1(DMSO)] (1)、[MoO2L2(H2O)]·DMF (2) 和 [MoO2L3(DMF)] (3) 通过基于溶液的芳酰腙 (H2L1 = 5) 反应合成-氯-2-羟基苯甲醛烟酰腙，H2L2 = 2-羟基-5-碘苯甲醛烟酰腙和 H2L3 = 3,5-二氯-2-羟基苯甲醛烟酰腙）与双（乙酰丙酮）二氧化钼（VI）络合物，[Mo]ac）在 DMSO 或 DMF 存在下。合成的芳酰腙及其钼配合物通过元素分析、光谱技术（FT-IR、UV-Vis、1H NMR）和电导率测量进行表征。最后通过单晶X射线衍射研究证实了配合物的三维结构。1的晶体结构，2 和 3 分别通过直接方法求解，并分别使用 SHELXS97 和 SHELXL2014 软件程序通过全矩阵最小二乘法计算进行细化。配合物 1 在单斜空间群 P21/c 中结晶，Z = 4，而配合物 2 和 3 在三斜空间群中结晶，P$$\overline {1}$$1¯，Z = 2。配体 H2L1−3 显示通过去质子化的苯酚氧、偶氮甲碱氮和烯醇氧以二元三齿方式与金属离子配位。图形摘要所有三种二氧化钼（VI）配合物都表现出围绕钼原子的扭曲八面体几何形状。[MoO2L2(H2O)]·DMF的ORTEP图。（位移椭球以 50% 的概率绘制）而配合物 2 和 3 在三斜空间群中，P$$\overline {1}$$1¯ 且 Z = 2。配体 H2L1−3 通过去质子化酚氧、偶氮甲碱氮以二元三齿方式与金属离子配位和烯化氧。图形摘要所有三种二氧化钼（VI）配合物都表现出围绕钼原子的扭曲八面体几何形状。[MoO2L2(H2O)]·DMF的ORTEP图。（位移椭球以 50% 的概率绘制）而配合物 2 和 3 在三斜空间群中，P$$\overline {1}$$1¯ 且 Z = 2。配体 H2L1−3 通过去质子化酚氧、偶氮甲碱氮以二元三齿方式与金属离子配位和烯化氧。图形摘要所有三种二氧化钼（VI）配合物都表现出围绕钼原子的扭曲八面体几何形状。[MoO2L2(H2O)]·DMF的ORTEP图。（位移椭球以 50% 的概率绘制）[MoO2L2(H2O)]·DMF的ORTEP图。（位移椭球以 50% 的概率绘制）[MoO2L2(H2O)]·DMF的ORTEP图。（位移椭球以 50% 的概率绘制）