Supplementary Material for Chemical Communications
This journal is © The Royal Society of Chemistry 2003
The first organically templated 1-D lithioberyllofluoride chain, [LiBe2F7][C4N2H12][H2O]1.5
Lee A. Gerrard,* Mark T. Weller
Supplementary data.
TGA
3.00E+05
1.20E+01
2.50E+05
1.00E+01
2.00E+05
8.00E+00
1.00E+05
6.00E+00
5.00E+04
0.00E+00
Weight mg
MCals/s
1.50E+05
mCal/s
mg
4.00E+00
0
50
100
150
200
250
300
350
400
450
500
-5.00E+04
2.00E+00
-1.00E+05
-1.50E+05
0.00E+00
Temp C
TGA curve for title compound. Carried out in static air in the range 25 to 500 ºC (heating rate 10 ºC/min). Mass loss between 100-150 ºC is 10 %
and is due to the solvent water and HF molecules. Second and third mass loss is due to each of the piperazine molecules at roughly 20 %.
Supplementary Material for Chemical Communications
This journal is © The Royal Society of Chemistry 2003
IR of [LiBe2F7][C4N2H12][H2O]1.5
80
70
% Transmittance
60
50
40
30
20
10
0
3850
3350
2850
2350
1850
1350
850
Wavenumber (cm-1)
IR showing the main stretches at 3587, 3443, 3247, 3022, 3005, 2872, 2820 and 2576 cm-1 for (O-H), (N-H) and (C-H).
350
Supplementary Material for Chemical Communications
This journal is © The Royal Society of Chemistry 2003
Metal-Metal distances
BE(1)
BE(1)
BE(2)
BE(2)
LI(1)
LI(1)
- LI(1)
- LI(1)a
- LI(1)
- LI(1)b
- LI(1)a
- LI(1)b
2.972(3)
3.093(3)
3.022(3)
3.058(3)
3.994(3)
4.085(4)
a = 1-x,1-y,1-z, b = -x,1-y,1-z
Hydrogen bonding distances
Table S9 - Hydrogen Bonds (Angstrom, Deg)
for: s92 in P-1
D
N1
N1
N2
N2
-----
H
H1
H2
H7
H8
..
..
..
..
A
F7
F1
F2
F4
D-H
0.90(2)
0.90(2)
0.86(2)
0.89(2)
H…A
1.76(2)
1.90(2)
1.79(2)
1.94(2)
D…A
2.622(2)
2.766(3)
2.630(2)
2.774(2)
Translation of Symmetry Code to Equiv.Pos
[2666.00]
[2656.00]
[1654.00]
= 1-x,1-y,1-z
= 1-x,-y,1-z
= 1+x,y,-1+z
D-H…A
160(2)
162(2)
165(2)
155(2)
Symmop-A
2_656
2_666
2_666
1_654
Supplementary Material for Chemical Communications
This journal is © The Royal Society of Chemistry 2003
Synthetic details and analytical data
The title compound was synthesised by a two-step hydrothermal process followed by a slow evaporation. BeF2 (0.1 g), HF (0.17 ml) and
C4N2H10 (0.18 g) were added to H2O (1 ml) in a 23 ml Teflon lined autoclave and heated to 150 C for 2 hr. The mix was then cooled for 3 hr
and one equivalent of Li2CO3 (0.035 g) was added then reheated at 150 C for 1 day. After the resulting solution was left to cool and slowly
evaporate colourless rod like single crystals were formed. Anal. Calc. for Li2Be4F14C8N4H30O3; C 16.97; H 5.50; N 9.66 %; Found C 16.70; H
5.93; N 9.68 %. IR (cm–1): 3587w, 3443wb, 3247m, 3022m, 3005m, 2872w, 2820w, 2575w (O-H), (N-H) and (C-H) stretches.