Herein, we present a new method for preparing homoligand 3D coordination polymers. First, a layered metal-organic framework Zn
3(BDC)
3(H
2O)
2·4DMF
1 (BDC is terephthalate, DMF is
N,
N-dimethylformamide) was fabricatedfrom a H
2BDC by liquid-liquid diffusion. Second, the layered product,
1, was used as a precursor to solvothermallyreact with further H
2BDC at 140-180
![](/images/entities/deg.gif)
C, resulting in two products of BDC insertion into the layered structure.These are [Zn
3(
p-BDC)
4]·2HPIP,
2 (HPIP is partly protonated piperazine), and [Zn
3(
p-BDC)
3(H
2BDC)]·(C
6H
15NO)·H
2O·3DMF,
3 (C
6H
15NO is triethylamine
N-oxide). Single-crystal X-ray diffraction shows that
2 possesses a layer-pillared structure of
4-BDC, with 1D channels, while
3 has a layer-pillared structure of
2-BDC, with 2D channels.N
2-sorption experiments show
3 has a relatively high BET surface area of 750 m
2/g. It is proposed that
2 followsthe crystal growth mechanism of Ostwald ripening, whereas the crystal structure of
3 might be formed by aninsertion mechanism.