Synthesis and Spectroscopic and Structural Characterization of Racemic Ammonium Dimeric(malato)dioxomolybdenum

Abstract

Abstract: The complex (NH₄)4[Mo∧O₂(S,SHmal)₂]·[MoΔO₂(R,RHmal)₂] was prepared from the reaction of ammonium molybdate and R,Smalic acid at pH=2——3. It was characterized by elementary analysis, conductivity measurement, optical rotation, IRand Xray diffraction. The complex crystallizes in monoclinic space group P2₁/a with unit cell parameters: a=0.8061(2) nm, b=1.3286(2) nm, c=1.3232(2) nm, β=91.82(2)°, V=1.4164(9) nm3, Z=2, D_c=2.008 g·cm^-3, F(000)=864, μ=9.700 cm^-1 for 1902 reflections with I≥3σ(I). The molybdenum atom is coordinated by two bidentate homochiral malic acid in distorted octahedron, while the βcarboxyl groups remain uncomplexed. The crystal contains two isolated monomeric malatomolybdates(Ⅵ) anions in the configurations of ∧S,S and ΔR,R. The two enantiomeric anions result in the formation of racemic compound. There is no evidence for the other diastereoisomers like (NH₄)₂[Mo∧O₂(R,SHmal)₂], (NH₄)₂[MoΔO₂(R,SHmal)₂], (NH₄)₂[Mo∧O₂(R,RHmal)₂] and (NH₄)₂[MoΔO₂(S,SHmal)₂] in this experiment.

Key words: Malic acid, Malate, Oxomolybdenum(Ⅵ) complex, Nitrogenase, Crystal structure

CLC Number:

O614.61

TrendMD:

YAN WenBin ZHOU ZhaoHui, ZHANG Hui, WAN HuiLin, Cai QiRui . Synthesis and Spectroscopic and Structural Characterization of Racemic Ammonium Dimeric(malato)dioxomolybdenum[J]. Chem. J. Chinese Universities, 2001, 22(12): 1967.

References

Related Articles 15

[1]	LIU Qingqing, WANG Pu, WANG Yongshuai, ZHAO Man, DONG Huanli. Synthesis and Topochemical Polymerization Study of Naphthalene/perylene Imides Substituted Diacetylene Derivatives [J]. Chem. J. Chinese Universities, 2022, 43(6): 20220091.
[2]	SHI Naike, ZHANG Ya, SANSON Andrea, WANG Lei, CHEN Jun. Uniaxial Negative Thermal Expansion and Mechanism in Zn（NCN） [J]. Chem. J. Chinese Universities, 2022, 43(6): 20220124.
[3]	ZHAO Ying, QIAO Ling, ZHAO Guofeng, CHEN Li. Synthesis and Biological Activity of Lycorine Derivatives Containing Malate Ester [J]. Chem. J. Chinese Universities, 2021, 42(9): 2789.
[4]	YUE Shengli, WU Guangbao, LI Xing, LI Kang, HUANG Gaosheng, TANG Yi, ZHOU Huiqiong. Research Progress of Quasi-two-dimensional Perovskite Solar Cells [J]. Chem. J. Chinese Universities, 2021, 42(6): 1648.
[5]	TIAN Xia,YANG Fuqun,YUAN Wei,ZHAO Lei,YAO Lei,ZHEN Xiaoli,HAN Jianrong,LIU Shouxin. Synthesis, Structure and Recognition Properties of Macrocyclic Crown Ethers with Oxadiazole ^† [J]. Chem. J. Chinese Universities, 2020, 41(3): 490.
[6]	LIU Dongmei,SU Yajing,LI Shanshan,XU Qiwei,LI Xia. Transition Metal Coordination Polymers Constructed by 4-(4-Carboxyphenoxy)isophthalic Acid: Synthesis, Crystal Structure, Fluorescence Sensing and Photocatalysis ^† [J]. Chem. J. Chinese Universities, 2020, 41(2): 253.
[7]	QIN Liulei,LIU Yang,GUAN Xiaoqin,ZHENG Xiaoyuan,ZHANG Ziyu,LIU Zunqi. Synthesis and Switchable Dielectric Properties of an Inorganic-organic Hybrid Complex [H₂(DABCO)CuCl₄]·H₂O ^† [J]. Chem. J. Chinese Universities, 2020, 41(1): 70.
[8]	LI Bing,WANG Xuemin,BAI Fengying,LIU Shuqing. Synthesises, Structures and Antibacterial Activities of a Series of Rare Earth Nitrogen Heterocyclic Complexes^† [J]. Chem. J. Chinese Universities, 2019, 40(4): 632.
[9]	WANG Dongmei,LIU Zihua,LI Guanghua,LIU Yunling,LI Chunxia. Synthesis, Structure and Fluorescent Property of Indium-based Bimetallic Metal-organic Frameworks^† [J]. Chem. J. Chinese Universities, 2018, 39(9): 1886.
[10]	TIAN Huan, ZHANG Menglong, WANG Lisha, TONG Bihai, ZHAO Zhuo. Synthesis of 4,13-Dithio Benzene and-18-Crown-6 and Its Selective Extractability on A $g + †$ [J]. Chem. J. Chinese Universities, 2018, 39(6): 1191.
[11]	ZHU Lei,HAN Junyan,CHANG Haizhen,QIU Yuyuan,ZHANG Yanan,PENG Danni,HU Wei,MIAO Shaobin. Different Pathways for the Cyclocondensation Reactions of 1,2-Diamine and 1,2-Diketone^† [J]. Chem. J. Chinese Universities, 2018, 39(12): 2686.
[12]	CHEN Qidan, TANG Junjie, FANG Qianrong. Highly Stable Fluorine Containing Hierarchical Porous Covalent Organic Framework^† [J]. Chem. J. Chinese Universities, 2018, 39(11): 2357.
[13]	LI Zheng, LI Rui, LI Xia. Synthesis, Crystal Structure and Fluorescent Properties of Transition Metal Complexes Constructed with 2-(3'-Carboxyphenoxy)benzoic Acid and N-Donor Ligands^† [J]. Chem. J. Chinese Universities, 2018, 39(11): 2363.
[14]	YUN Jixing,HU Zhili,LI Yumeng,JIN Jing,CHEN Chong,YAN Xin,LIU Yonghua,DING Yu,CHI Yuxian,NIU Shuyun. Synthesis, Structure and Photoelectric Property of A Series of Ni(Ⅱ) Complexes Constructed Through Aromatic Carboxylic Ligands^† [J]. Chem. J. Chinese Universities, 2018, 39(10): 2161.
[15]	TAN Ying, XIAO Mengwu, YE Jiao, HU Aixi, ZENG Ziqing, OU Xiaoming. Synthesis, Crystal Structure and Fungicidal Activity of (Z)-3,3-Dimethyl-1-(1H-1,2,4-triazol-1-yl)butan-2-one O-[(5-Aryl-1,3,4-oxadiazol-2-yl)methyl] oxime [J]. Chem. J. Chinese Universities, 2017, 38(8): 1375.