Pierre R. Ndong, M. Signé, Patrice T. Kenfack, Y. Mbiangué, Gouet Bebga, E. Wenger
{"title":"反式双(草酸-κ2O1,O2)铬酸盐(III)-哌啶配合阴离子有机-无机杂化盐的合成、表征和热分析","authors":"Pierre R. Ndong, M. Signé, Patrice T. Kenfack, Y. Mbiangué, Gouet Bebga, E. Wenger","doi":"10.4236/csta.2020.92004","DOIUrl":null,"url":null,"abstract":"A new organic-inorganic hybrid salt piperidinium trans-diaquabis(oxalato)- chromate(III) \ntetrahydrate, (C5H10NH2)[Cr(C2O4)2(H2O)2]·4H2O \n(1), has been synthesized in water and characterized by FTIR and UV-Vis \nspectroscopies, elemental and thermal analyses and by single-crystal X-ray \ndiffraction. 1 crystallizes in the \northorhombic non-centrosymmetric space group Cmc21 with the unit cell parameters a = \n7.4329(3), b = 9.9356(5), c = 23.6756(11) A, α = β = γ = 90°, V = 1748.45(14) A3 and Z = 4. The structure of 1 consists of [Cr(C2O4)2(H2O)2]- mononuclear anions, piperidinium cations and uncoordinated water molecules. The \nCrIII ion in the complex [Cr(C2O4)2(H2O)2]- is coordinated in a slightly distorted octahedral environment by four O atoms \nfrom two chelating oxalate dianions in the equatorial plane, and two O atoms \nfrom trans-coordinated water \nmolecules occupying the apical positions. In the crystal, N-H···O and O-H···O hydrogen bond \ninteractions connect the components into a 3-D framework. The IR spectrum of 1 is consistent with the presence of the various molecular building \nconstituents, namely oxalato and aqua ligands, piperidinium cations and solvent \nwater molecules. The UV-Vis spectrum shows two absorption bands around 564 and \n416 nm which are compatible with an anionic chromium(III) complex in an \noctahedral environment. Thermal analysis shows a three-step decomposition of 1, \nleading to formation of a metal oxide residue.","PeriodicalId":67661,"journal":{"name":"晶体结构理论与应用(英文)","volume":" ","pages":""},"PeriodicalIF":0.0000,"publicationDate":"2020-03-25","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":"2","resultStr":"{\"title\":\"Synthesis, Characterization and Thermal Analysis of an Organic-Inorganic Hybrid Salt Involving Trans-Diaquabis(oxalato-κ2O1,O2)chromate(III) Complex Anion with Piperidinium as Counter Cation\",\"authors\":\"Pierre R. Ndong, M. Signé, Patrice T. Kenfack, Y. Mbiangué, Gouet Bebga, E. Wenger\",\"doi\":\"10.4236/csta.2020.92004\",\"DOIUrl\":null,\"url\":null,\"abstract\":\"A new organic-inorganic hybrid salt piperidinium trans-diaquabis(oxalato)- chromate(III) \\ntetrahydrate, (C5H10NH2)[Cr(C2O4)2(H2O)2]·4H2O \\n(1), has been synthesized in water and characterized by FTIR and UV-Vis \\nspectroscopies, elemental and thermal analyses and by single-crystal X-ray \\ndiffraction. 1 crystallizes in the \\northorhombic non-centrosymmetric space group Cmc21 with the unit cell parameters a = \\n7.4329(3), b = 9.9356(5), c = 23.6756(11) A, α = β = γ = 90°, V = 1748.45(14) A3 and Z = 4. The structure of 1 consists of [Cr(C2O4)2(H2O)2]- mononuclear anions, piperidinium cations and uncoordinated water molecules. The \\nCrIII ion in the complex [Cr(C2O4)2(H2O)2]- is coordinated in a slightly distorted octahedral environment by four O atoms \\nfrom two chelating oxalate dianions in the equatorial plane, and two O atoms \\nfrom trans-coordinated water \\nmolecules occupying the apical positions. In the crystal, N-H···O and O-H···O hydrogen bond \\ninteractions connect the components into a 3-D framework. The IR spectrum of 1 is consistent with the presence of the various molecular building \\nconstituents, namely oxalato and aqua ligands, piperidinium cations and solvent \\nwater molecules. The UV-Vis spectrum shows two absorption bands around 564 and \\n416 nm which are compatible with an anionic chromium(III) complex in an \\noctahedral environment. Thermal analysis shows a three-step decomposition of 1, \\nleading to formation of a metal oxide residue.\",\"PeriodicalId\":67661,\"journal\":{\"name\":\"晶体结构理论与应用(英文)\",\"volume\":\" \",\"pages\":\"\"},\"PeriodicalIF\":0.0000,\"publicationDate\":\"2020-03-25\",\"publicationTypes\":\"Journal Article\",\"fieldsOfStudy\":null,\"isOpenAccess\":false,\"openAccessPdf\":\"\",\"citationCount\":\"2\",\"resultStr\":null,\"platform\":\"Semanticscholar\",\"paperid\":null,\"PeriodicalName\":\"晶体结构理论与应用(英文)\",\"FirstCategoryId\":\"1089\",\"ListUrlMain\":\"https://doi.org/10.4236/csta.2020.92004\",\"RegionNum\":0,\"RegionCategory\":null,\"ArticlePicture\":[],\"TitleCN\":null,\"AbstractTextCN\":null,\"PMCID\":null,\"EPubDate\":\"\",\"PubModel\":\"\",\"JCR\":\"\",\"JCRName\":\"\",\"Score\":null,\"Total\":0}","platform":"Semanticscholar","paperid":null,"PeriodicalName":"晶体结构理论与应用(英文)","FirstCategoryId":"1089","ListUrlMain":"https://doi.org/10.4236/csta.2020.92004","RegionNum":0,"RegionCategory":null,"ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":null,"EPubDate":"","PubModel":"","JCR":"","JCRName":"","Score":null,"Total":0}
引用次数: 2
摘要
在水中合成了一种新型的有机-无机杂化盐,(C5H10NH2)[Cr(C2O4)2(H2O)2]·4H2O(1),并用红外光谱、紫外可见光谱、元素分析、热分析和单晶x射线衍射对其进行了表征。1在正交非中心对称空间群Cmc21中结晶,晶胞参数a = 7.4329(3), b = 9.9356(5), c = 23.6756(11) a, α = β = γ = 90°,V = 1748.45(14) A3, Z = 4。1的结构由[Cr(C2O4)2(H2O)2]-单核阴离子、胡椒离子和不配位水分子组成。配合物[Cr(C2O4)2(H2O)2]-中的CrIII离子在稍微扭曲的八面体环境中由两个螯合草酸根离子的四个O原子在赤道平面上配位,两个来自反配位的水分子的两个O原子占据顶端位置。在晶体中,N-H··O和O- h··O氢键相互作用将这些成分连接成一个三维框架。1的红外光谱与各种分子构建成分的存在一致,即草酸和水配体、哌替啶阳离子和溶剂水分子。紫外可见光谱在564和416 nm处显示出与阴离子铬(III)配合物在八面体环境下相容的两个吸收带。热分析表明,1分三步分解,导致形成金属氧化物残留物。
Synthesis, Characterization and Thermal Analysis of an Organic-Inorganic Hybrid Salt Involving Trans-Diaquabis(oxalato-κ2O1,O2)chromate(III) Complex Anion with Piperidinium as Counter Cation
A new organic-inorganic hybrid salt piperidinium trans-diaquabis(oxalato)- chromate(III)
tetrahydrate, (C5H10NH2)[Cr(C2O4)2(H2O)2]·4H2O
(1), has been synthesized in water and characterized by FTIR and UV-Vis
spectroscopies, elemental and thermal analyses and by single-crystal X-ray
diffraction. 1 crystallizes in the
orthorhombic non-centrosymmetric space group Cmc21 with the unit cell parameters a =
7.4329(3), b = 9.9356(5), c = 23.6756(11) A, α = β = γ = 90°, V = 1748.45(14) A3 and Z = 4. The structure of 1 consists of [Cr(C2O4)2(H2O)2]- mononuclear anions, piperidinium cations and uncoordinated water molecules. The
CrIII ion in the complex [Cr(C2O4)2(H2O)2]- is coordinated in a slightly distorted octahedral environment by four O atoms
from two chelating oxalate dianions in the equatorial plane, and two O atoms
from trans-coordinated water
molecules occupying the apical positions. In the crystal, N-H···O and O-H···O hydrogen bond
interactions connect the components into a 3-D framework. The IR spectrum of 1 is consistent with the presence of the various molecular building
constituents, namely oxalato and aqua ligands, piperidinium cations and solvent
water molecules. The UV-Vis spectrum shows two absorption bands around 564 and
416 nm which are compatible with an anionic chromium(III) complex in an
octahedral environment. Thermal analysis shows a three-step decomposition of 1,
leading to formation of a metal oxide residue.