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Details van artikel 3 van 73 gevonden artikelen
| Titel: |
ANIONIC COORDINATION COMPLEXES OF Mo AND W WHICH CRYSTALLIZE FROM LIQUID CLATHRATE MEDIA WITH OXONIUM ION-CROWN ETHER CATIONS |
| Auteur: |
Atwood, Jerry L. Bott, Simon G. Junk, Peter C. May, Michael T. |
| Verschenen in: |
Journal of coordination chemistry |
| Paginering: | Jaargang 37 (1996) nr. 1-4 pagina's 89-105 |
| Jaar: |
1996-02-01 |
| Inhoud: |
The complexes [H3O+·18-crown-6][MoOCl4(H2O)-], 1, and [H2O·aza-18-crown-6·(H+)] [MoOCl4(H2O)-], 3, were synthesized from a mixture of Mo(CO)6, HCl(g), H2O and either 18-crown-6 for 1 or mono-aza-18-crown-6 for 3, in toluene. For complex 4, [H2O·aza-18-crown-6·(H+)]2[WOCl4(H2O)-][Cl-], reaction conditions were as for 3 except W(CO)6 was used in place of Mo(CO)6. Similarly, for complex 2, [H3O+·18-crown-6][WOBr4(H2O)-], W(CO)6 and HBr were used in the reaction mixture. These reactions were promoted by UV radiation and formed liquid clathrates almost immediately upon reaction. X-ray crystal structures were performed on each compound. Complex 1 crystallizes in the triclinic space group P/i with a = 10.206(1), b = 10.486(1), c = 11.701(1) Å, α = 71.11(1), β = 74.60(1), γ = 75.08(1)°, and Dc = 1.649 g cm-3 for Z = 2. Refinement based on 3925 observed reflections led to a final R value of 0.078. Complex 2 crystallizes in the monoclinic space group P21/c with a = 9.710(1), b = 19.824(1), c = 12.399(1) Å, β = 104.58(1)°, and Dc = 2.369 g cm-3 for Z = 4. Refinement based on 2008 observed reflections led to a final R value of 0.090. Complex 3 crystallizes in the orthorhombic space group Pnmn with a = 16.927(1), b = 12.226(1), c = 11.167(1) Å, and Dc = 1.598 g cm-3 for Z = 4. Refinement based on 1486 observed reflections led to a final R value of 0.040. Complex 4 crystallizes in the monoclinic space group C2/m with a = 11.761(2), b = 12.096(2), c = 14.966(1) Å, β = 132.91(1)°, and Dc = 1.502 g cm-3 for Z = 4. Refinement based on 2021 observed reflections led to a final R value of 0.051. In all cases the metal coordination sphere was essentially octahedral with the water ligand trans to the oxo species. |
| Uitgever: |
Taylor & Francis |
| Bronbestand: |
Elektronische Wetenschappelijke Tijdschriften |
Details van artikel 3 van 73 gevonden artikelen
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