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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| Vydané v: | Zeitschrift für anorganische und allgemeine Chemie (1950) Ročník 642; číslo 7; s. 560 - 565 |
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| Hlavní autori: | , |
| Médium: | Journal Article |
| Jazyk: | English |
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Weinheim
WILEY-VCH Verlag
01.04.2016
WILEY‐VCH Verlag Wiley Subscription Services, Inc |
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| ISSN: | 0044-2313, 1521-3749 |
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| Abstract | 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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| AbstractList | 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, [alpha] = 100.282(5), [beta] = 94.515(7), and [gamma] = 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-) [arrow right] dσ*(Co3+)] at 274 and 368 nm and the d-d transition (1A1g [arrow right] 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. 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. Black‐brown needle‐shaped single crystals of [Co 2 (en) 4 (O 2 )(OH)][C 4 O 4 ] 1.5 · 4H 2 O (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 Co 3+ 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 Co 3+ coordination polyhedra are connected by a common corner and by the peroxo group leading to the dinuclear [(en) 2 Co(O 2 )(OH)Co(en) 2 ] 3+ cation. The squarate dianions, not bonded to Co 3+ , and the [(en) 2 Co(O 2 )(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 Co 3+ . The UV/Vis spectra show two LMCT bands [π*(O 2 2– ) → d σ *(Co 3+ )] at 274 and 368 nm and the d–d transition ( 1 A 1g → 1 T 1g ) 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. |
| Author | Robl, Christian Köferstein, Roberto |
| Author_xml | – sequence: 1 givenname: Roberto surname: Köferstein fullname: Köferstein, Roberto organization: Institute of Inorganic and Analytical Chemistry, Friedrich-Schiller-University Jena, Humboldtstrasse 8, 07743 Jena, Germany – sequence: 2 givenname: Christian surname: Robl fullname: Robl, Christian email: crr@uni-jena.de organization: Institute of Inorganic and Analytical Chemistry, Friedrich-Schiller-University Jena, Humboldtstrasse 8, 07743 Jena, Germany |
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| Snippet | 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... Black‐brown needle‐shaped single crystals of [Co 2 (en) 4 (O 2 )(OH)][C 4 O 4 ] 1.5 · 4H 2 O (en = ethylenediamine) were prepared in aqueous solution at room... 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... |
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| SubjectTerms | Aqueous solutions Cobalt Crystal structure Ethylenediamine Peroxo Squarate Supramolecular network |
| Title | Synthesis, Crystal Structure, and Hydrogen Bonding of μ-Hydroxo-μ-peroxo-bis[bis(ethylenediamine)cobalt(III)] Squarate |
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