10.1021/ic0261326.s004
Hugh D. Selby
Hugh D.
Selby
Bryan K. Roland
Bryan K.
Roland
Michael D. Carducci
Michael D.
Carducci
Zhiping Zheng
Zhiping
Zheng
Hydrogen-Bonded Extended Arrays of the [Re<sub>6</sub>(μ<sub>3</sub>-Se)<sub>8</sub>]<sup>2+</sup>
Core-Containing Clusters
American Chemical Society
2003
Re
crystal engineering motif
31 P NMR
compound
tran
ligand substitution reaction
ci
PEt 3
Se
amide
isonicotinamide
cluster
stereochemistry
2003-02-08 00:00:00
Dataset
https://acs.figshare.com/articles/dataset/Hydrogen-Bonded_Extended_Arrays_of_the_Re_sub_6_sub_sub_3_sub_-Se_sub_8_sub_sup_2_sup_Core-Containing_Clusters/3610746
Site-differentiated solvated clusters of the general formula [Re<sub>6</sub>(μ<sub>3</sub>-Se)<sub>8</sub>(PEt<sub>3</sub>)<i><sub>n</sub></i>(MeCN)<sub>6</sub><sub>-</sub><i><sub>n</sub></i>](SbF<sub>6</sub>)<sub>2</sub> (<i>n</i> = 4, <i>cis</i> and
<i>trans</i>; <i>n</i> = 5) undergo ligand substitution reaction with isonicotinamide to afford the corresponding amide derivatives,
[Re<sub>6</sub>(μ<sub>3</sub>-Se)<sub>8</sub>(PEt<sub>3</sub>)<i><sub>n</sub></i>(isonicotinamide)<sub>6</sub><sub>-</sub><i><sub>n</sub></i>]<sup>2+</sup> [<b>1</b> (<i>n</i> = 5); <b>2</b> (<i>n</i> = 4, <i>trans</i>); <b>3</b> (<i>n</i> = 4, <i>cis</i>)]. Retention of stereochemistry
in each case was confirmed by <sup>1</sup>H and <sup>31</sup>P NMR. The solid-state structures of all three compounds were established
crystallographically, which revealed self-complementary hydrogen-bonding interactions between adjacent cluster
units. While complex <b>1</b> exists as hydrogen-bonded dimers in the solid state, compounds <b>2</b> and <b>3</b> form one-dimensional
chains of clusters bridged by paired hydrogen bonds. It is the rigid stereochemistry of the cluster, combined with
the classic crystal engineering motif of complementary N−H···O amide hydrogen bonding, that affords the predictable
solid-state structures and dimensionality.