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Oxidopolyborate anions templated by transition-metal complex cations: Self-assembled syntheses and structural studies (XRD) of [Co(NH3)6]2[B4O5(OH)4]3·11H2O, [Ni(phen)3][B7O9(OH)5]·9.5H2O and [Zn(dac)2(H2O)2][B7O9(OH)5]·H2O

Oxidopolyborate anions templated by transition-metal complex cations: Self-assembled syntheses and structural studies (XRD) of [Co(NH3)6]2[B4O5(OH)4]3·11H2O, [Ni(phen)3][B7O9(OH)5]·9.5H2O and [Zn(dac)2(H2O)2][B7O9(OH)5]·H2O
Oxidopolyborate anions templated by transition-metal complex cations: Self-assembled syntheses and structural studies (XRD) of [Co(NH3)6]2[B4O5(OH)4]3·11H2O, [Ni(phen)3][B7O9(OH)5]·9.5H2O and [Zn(dac)2(H2O)2][B7O9(OH)5]·H2O

The new oxidopolyborate salts [Co(NH3) 6] 2[B4O5(OH)4] 3·11H2O (1), [Ni(phen)3][B7O9(OH)5]·9.5H2O (2), and [Zn(dac)2(H2O)2][B7O9(OH)5]·H2O (3), were crystallized, in moderate yields, from aqueous solutions containing B(OH)3 and the hydroxide salt of the corresponding cationic metal complex (prepared in situ) in moderate yields. Complexes 1–3, characterized by spectroscopic (NMR, IR) and thermal (TGA) methods and by single-crystal XRD studies, were obtained through cation-templated self-assembly reactions. Compound 1 contains insular tetraborate2- anions (4-1:2Δ + 2T) and 2 and 3 both contain insular heptaborate2- anions (‘O+’ isomer, 6:(3Δ + 3T) + Δ). The X-ray structures show that in all three compounds the polyborate anions are H-bonded together into extended networks, and there are multiple cation-anion H-bond interactions present in 1 and 3. Compound 2 has cation-cation π-stacking interactions. These interactions are likely to be responsible for templating the observed structures. Thermal decomposition of 1–3 in air yielded amorphous anhydrous borates of composition CoB6O10.5, NiB7O11.5 and ZnB7O11.5, respectively.

Heptaborate(2-), Oxidoborate, Tetraborate(2-), Transition-metal complex, XRD study
0022-2860
Altahan, Mohammed A.
a333d79b-2ef3-4c3f-86a2-519740d08a72
Beckett, Michael A.
5b021ef6-fa5c-4f6d-9998-3313558f0dc1
Coles, Simon J.
3116f58b-c30c-48cf-bdd5-397d1c1fecf8
Horton, Peter
154c8930-bfc3-495b-ad4a-8a278d5da3a5
Altahan, Mohammed A.
a333d79b-2ef3-4c3f-86a2-519740d08a72
Beckett, Michael A.
5b021ef6-fa5c-4f6d-9998-3313558f0dc1
Coles, Simon J.
3116f58b-c30c-48cf-bdd5-397d1c1fecf8
Horton, Peter
154c8930-bfc3-495b-ad4a-8a278d5da3a5

Altahan, Mohammed A., Beckett, Michael A., Coles, Simon J. and Horton, Peter (2020) Oxidopolyborate anions templated by transition-metal complex cations: Self-assembled syntheses and structural studies (XRD) of [Co(NH3)6]2[B4O5(OH)4]3·11H2O, [Ni(phen)3][B7O9(OH)5]·9.5H2O and [Zn(dac)2(H2O)2][B7O9(OH)5]·H2O. Journal of Molecular Structure, 1200, [127071]. (doi:10.1016/j.molstruc.2019.127071).

Record type: Article

Abstract

The new oxidopolyborate salts [Co(NH3) 6] 2[B4O5(OH)4] 3·11H2O (1), [Ni(phen)3][B7O9(OH)5]·9.5H2O (2), and [Zn(dac)2(H2O)2][B7O9(OH)5]·H2O (3), were crystallized, in moderate yields, from aqueous solutions containing B(OH)3 and the hydroxide salt of the corresponding cationic metal complex (prepared in situ) in moderate yields. Complexes 1–3, characterized by spectroscopic (NMR, IR) and thermal (TGA) methods and by single-crystal XRD studies, were obtained through cation-templated self-assembly reactions. Compound 1 contains insular tetraborate2- anions (4-1:2Δ + 2T) and 2 and 3 both contain insular heptaborate2- anions (‘O+’ isomer, 6:(3Δ + 3T) + Δ). The X-ray structures show that in all three compounds the polyborate anions are H-bonded together into extended networks, and there are multiple cation-anion H-bond interactions present in 1 and 3. Compound 2 has cation-cation π-stacking interactions. These interactions are likely to be responsible for templating the observed structures. Thermal decomposition of 1–3 in air yielded amorphous anhydrous borates of composition CoB6O10.5, NiB7O11.5 and ZnB7O11.5, respectively.

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Accepted/In Press date: 11 September 2019
e-pub ahead of print date: 13 September 2019
Published date: 15 January 2020
Keywords: Heptaborate(2-), Oxidoborate, Tetraborate(2-), Transition-metal complex, XRD study
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Identifiers

Local EPrints ID: 434789
URI: http://eprints.soton.ac.uk/id/eprint/434789
DOI: doi:10.1016/j.molstruc.2019.127071
ISSN: 0022-2860
PURE UUID: 67729387-05b8-42e1-a19b-12796cefe5e1
ORCID for Simon J. Coles: ORCID iD orcid.org/0000-0001-8414-9272
ORCID for Peter Horton: ORCID iD orcid.org/0000-0001-8886-2016

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Date deposited: 09 Oct 2019 16:30
Last modified: 17 Mar 2024 02:50

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Contributors

Author: Mohammed A. Altahan
Author: Michael A. Beckett
Author: Simon J. Coles ORCID iD
Author: Peter Horton ORCID iD

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