Larisa A Kovbasyuk , Olga Yu Vassilyeva , Vladimir N Kokozay , Hyungphil Chun , Ivan Bernal , Jan Reedijk , Gerard Van Albada , Brian W Skelton
{"title":"由零价金属制备的三乙醇胺氯化铜:已知Cu(II)化合物的另一种多晶型或与全三角双锥体铜的混合价配合物?","authors":"Larisa A Kovbasyuk , Olga Yu Vassilyeva , Vladimir N Kokozay , Hyungphil Chun , Ivan Bernal , Jan Reedijk , Gerard Van Albada , Brian W Skelton","doi":"10.1016/S1463-0184(01)00010-7","DOIUrl":null,"url":null,"abstract":"<div><p><span>Two new copper complexes with triethanolamine (H</span><sub>3</sub>L) have been prepared using copper powder and characterized by X-ray crystallography, IR and EPR spectroscopy. These are [Cu<sup>I</sup>(H<sub>3</sub>L)Cl]<sub>x</sub>⋅[Cu<sup>II</sup>(H<sub>2</sub>L)Cl]<sub>1−x</sub> (<em>X</em>=0; 2/3) (<strong>1</strong>) and [Cu<sup>II</sup>(H<sub>2</sub>L)SCN] (<strong>2</strong>). Both complexes are neutral species and contain copper atoms in trigonal bipyramidal environments. The important dimensions in <strong>1</strong> are Cu-N 2.011(5), 3Cu-O 2.073(3), Cu-Cl 2.239(2) Å and N-Cu-Cl=180.0°; in <strong>2</strong> Cu-N<sub>NCS</sub> 1.918(3), Cu-N<sub>H2Tea</sub> 1.983(3), Cu-O 2.004(2), 2Cu-O 2.13(1) Å and N<sub>H2Tea</sub>-Cu-N<sub>NCS</sub>=174.6(1)°. <strong>2</strong> has all the copper atoms in the oxidation state II, while the three-fold symmetry in <strong>1</strong> would suggest that the metal atoms are formally in the oxidation state I. Results of magnetic measurements of several samples of <strong>1</strong> are rationalized by assuming that a continuous range of composition for [Cu<sup>I</sup>(H<sub>3</sub>L)Cl]<sub>x</sub>⋅[Cu<sup>II</sup>(H<sub>2</sub>L)Cl]<sub>1−x</sub> can occur. In the case of <em>x</em>=0, <strong>1</strong> becomes a polymorph of the reported compound [Cu<sup>II</sup>(H<sub>2</sub>L)Cl].</p></div>","PeriodicalId":10766,"journal":{"name":"Crystal Engineering","volume":"4 2","pages":"Pages 201-213"},"PeriodicalIF":0.0000,"publicationDate":"2001-06-09","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"https://sci-hub-pdf.com/10.1016/S1463-0184(01)00010-7","citationCount":"5","resultStr":"{\"title\":\"Triethanolamine copper chloride prepared from zerovalent metal: another polymorph of a known Cu(II) compound or a mixed-valence complex with all-trigonal bipyramidal copper?\",\"authors\":\"Larisa A Kovbasyuk , Olga Yu Vassilyeva , Vladimir N Kokozay , Hyungphil Chun , Ivan Bernal , Jan Reedijk , Gerard Van Albada , Brian W Skelton\",\"doi\":\"10.1016/S1463-0184(01)00010-7\",\"DOIUrl\":null,\"url\":null,\"abstract\":\"<div><p><span>Two new copper complexes with triethanolamine (H</span><sub>3</sub>L) have been prepared using copper powder and characterized by X-ray crystallography, IR and EPR spectroscopy. These are [Cu<sup>I</sup>(H<sub>3</sub>L)Cl]<sub>x</sub>⋅[Cu<sup>II</sup>(H<sub>2</sub>L)Cl]<sub>1−x</sub> (<em>X</em>=0; 2/3) (<strong>1</strong>) and [Cu<sup>II</sup>(H<sub>2</sub>L)SCN] (<strong>2</strong>). Both complexes are neutral species and contain copper atoms in trigonal bipyramidal environments. The important dimensions in <strong>1</strong> are Cu-N 2.011(5), 3Cu-O 2.073(3), Cu-Cl 2.239(2) Å and N-Cu-Cl=180.0°; in <strong>2</strong> Cu-N<sub>NCS</sub> 1.918(3), Cu-N<sub>H2Tea</sub> 1.983(3), Cu-O 2.004(2), 2Cu-O 2.13(1) Å and N<sub>H2Tea</sub>-Cu-N<sub>NCS</sub>=174.6(1)°. <strong>2</strong> has all the copper atoms in the oxidation state II, while the three-fold symmetry in <strong>1</strong> would suggest that the metal atoms are formally in the oxidation state I. Results of magnetic measurements of several samples of <strong>1</strong> are rationalized by assuming that a continuous range of composition for [Cu<sup>I</sup>(H<sub>3</sub>L)Cl]<sub>x</sub>⋅[Cu<sup>II</sup>(H<sub>2</sub>L)Cl]<sub>1−x</sub> can occur. In the case of <em>x</em>=0, <strong>1</strong> becomes a polymorph of the reported compound [Cu<sup>II</sup>(H<sub>2</sub>L)Cl].</p></div>\",\"PeriodicalId\":10766,\"journal\":{\"name\":\"Crystal Engineering\",\"volume\":\"4 2\",\"pages\":\"Pages 201-213\"},\"PeriodicalIF\":0.0000,\"publicationDate\":\"2001-06-09\",\"publicationTypes\":\"Journal Article\",\"fieldsOfStudy\":null,\"isOpenAccess\":false,\"openAccessPdf\":\"https://sci-hub-pdf.com/10.1016/S1463-0184(01)00010-7\",\"citationCount\":\"5\",\"resultStr\":null,\"platform\":\"Semanticscholar\",\"paperid\":null,\"PeriodicalName\":\"Crystal Engineering\",\"FirstCategoryId\":\"1085\",\"ListUrlMain\":\"https://www.sciencedirect.com/science/article/pii/S1463018401000107\",\"RegionNum\":0,\"RegionCategory\":null,\"ArticlePicture\":[],\"TitleCN\":null,\"AbstractTextCN\":null,\"PMCID\":null,\"EPubDate\":\"\",\"PubModel\":\"\",\"JCR\":\"\",\"JCRName\":\"\",\"Score\":null,\"Total\":0}","platform":"Semanticscholar","paperid":null,"PeriodicalName":"Crystal Engineering","FirstCategoryId":"1085","ListUrlMain":"https://www.sciencedirect.com/science/article/pii/S1463018401000107","RegionNum":0,"RegionCategory":null,"ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":null,"EPubDate":"","PubModel":"","JCR":"","JCRName":"","Score":null,"Total":0}
Triethanolamine copper chloride prepared from zerovalent metal: another polymorph of a known Cu(II) compound or a mixed-valence complex with all-trigonal bipyramidal copper?
Two new copper complexes with triethanolamine (H3L) have been prepared using copper powder and characterized by X-ray crystallography, IR and EPR spectroscopy. These are [CuI(H3L)Cl]x⋅[CuII(H2L)Cl]1−x (X=0; 2/3) (1) and [CuII(H2L)SCN] (2). Both complexes are neutral species and contain copper atoms in trigonal bipyramidal environments. The important dimensions in 1 are Cu-N 2.011(5), 3Cu-O 2.073(3), Cu-Cl 2.239(2) Å and N-Cu-Cl=180.0°; in 2 Cu-NNCS 1.918(3), Cu-NH2Tea 1.983(3), Cu-O 2.004(2), 2Cu-O 2.13(1) Å and NH2Tea-Cu-NNCS=174.6(1)°. 2 has all the copper atoms in the oxidation state II, while the three-fold symmetry in 1 would suggest that the metal atoms are formally in the oxidation state I. Results of magnetic measurements of several samples of 1 are rationalized by assuming that a continuous range of composition for [CuI(H3L)Cl]x⋅[CuII(H2L)Cl]1−x can occur. In the case of x=0, 1 becomes a polymorph of the reported compound [CuII(H2L)Cl].
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