Synthesis, Crystal Structure, and Hydrogen Bonding of μ-Hydroxo-μ-peroxo-bis[bis(ethylenediamine)cobalt(III)] Squarate
Black‐brown needle‐shaped single crystals of [Co2(en)4(O2)(OH)][C4O4]1.5·4H2O (en = ethylenediamine) were prepared in aqueous solution at room temperature [space group P$\bar{1}$ (no.2) with a = 800.20(8), b = 1225.48(7), c = 1403.84(9) pm, α = 100.282(5), β = 94.515(7), and γ = 95.596(6)°]. The Co3...
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| Published in: | Zeitschrift für anorganische und allgemeine Chemie (1950) Vol. 642; no. 7; pp. 560 - 565 |
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| Main Authors: | , |
| Format: | Journal Article |
| Language: | English |
| Published: |
Weinheim
WILEY-VCH Verlag
01.04.2016
WILEY‐VCH Verlag Wiley Subscription Services, Inc |
| Subjects: | |
| ISSN: | 0044-2313, 1521-3749 |
| Online Access: | Get full text |
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| Summary: | Black‐brown needle‐shaped single crystals of [Co2(en)4(O2)(OH)][C4O4]1.5·4H2O (en = ethylenediamine) were prepared in aqueous solution at room temperature [space group P$\bar{1}$ (no.2) with a = 800.20(8), b = 1225.48(7), c = 1403.84(9) pm, α = 100.282(5), β = 94.515(7), and γ = 95.596(6)°]. The Co3+ cations [Co(1), Co(2)] are coordinated in an octahedral manner by four nitrogen atoms stemming from the ethylenediamine molecules and two oxygen atoms each from a hydroxo group and a peroxo group, respectively. Both Co3+ coordination polyhedra are connected by a common corner and by the peroxo group leading to the dinuclear [(en)2Co(O2)(OH)Co(en)2]3+ cation. The squarate dianions, not bonded to Co3+, and the [(en)2Co(O2)(OH)Co(en)2]3+ cations are linked by hydrogen bonds forming a three‐dimensional supramolecular network containing water molecules. Magnetic measurements revealed a diamagnetic behavior indicating a low‐spin electron configuration of Co3+. The UV/Vis spectra show two LMCT bands [π*(O22–) → dσ*(Co3+)] at 274 and 368 nm and the d–d transition (1A1g → 1T1g) at 542 nm. Thermoanalytical investigations in air show that the compound is stable up to 120 °C. Subsequent decomposition processes to cobalt oxide are finished at 460 °C. |
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| Bibliography: | Supporting Information for this article is available on the WWW under http://dx.doi.org/10.1002/zaac.201600080 or from the author. istex:F6C5E94E99487AC5EE3724E5E05A7D896CC1C37E ark:/67375/WNG-0R514L81-3 ArticleID:ZAAC201600080 or from the author. Supporting Information for this article is available on the WWW under http://dx.doi.org/10.1002/zaac.201600080 ObjectType-Article-1 SourceType-Scholarly Journals-1 ObjectType-Feature-2 content type line 14 |
| ISSN: | 0044-2313 1521-3749 |
| DOI: | 10.1002/zaac.201600080 |