Electronic Supplementary Material (ESI) for Dalton Transactions
This journal is © The Royal Society of Chemistry 2012
Electronic Supplementary Information
For
Multifunctional Lanthanum Tetraphosphonates:
Flexible, Ultramicroporous and Proton-Conducting
Hybrid Frameworks
Rosario M.P. Colodrero,a Pascual Olivera-Pastor,a Enrique R. Losilla,a Miguel A.G.
Aranda,a Laura Leon-Reina,b Maria Papadaki,c Alistair C. McKinlay,d Russell E.
Morris,d Konstantinos D. Demadis*c and Aurelio Cabeza.*a
a
Departamento de Química Inorgánica, Universidad de Málaga, Campus Teatinos s/n, Málaga29071, Spain. Fax: 34 952131870; Tel: +34 952131877; E-mail: [email protected]
b
Servicios Centrales de Apoyo a la Investigación, Universidad de Málaga, Campus Teatinos s/n,
Málaga-29071, Spain.
c
Crystal Engineering, Growth and Design Laboratory, Department of Chemistry, University of Crete,
Voutes Campus, Crete, GR-71003, Greece. Fax: +30 2810 545001; Tel: +30 2810 545051; E-mail:
[email protected]
d
School of Chemistry, University of St Andrews, Purdie Building, St Andrews, KY16 9ST, UK.
Table of contents:
Figures: XRPD Rietveld plots for:
S1 La(H5DTMP)·7H2O (phase 1)
S2 La(H5DTMP) (phase 2)
S3 La(H5DTMP).2H2O (phase 3)
S4 Comparative X-ray diffraction patterns for Ln(H5DTMP)·7H2O, Ln=La and Sm
S5 View of the 3D framework for La(H5DTMP)·7H2O (1) showing the 1D channels
S6 1D chain of hydrogen-bonded lattice water molecules within the channel of (1).
Tables: Bond lengths & H-bond distances for:
S1 Selected bond lengths for La(H5DTMP)·nH2O, n=0, 2 and 7 (phases 1-3)
S2 Selected H-bond distances for La(H5DTMP)·7H2O (phase 1)
S3 Selected H-bond distances for La(H5DTMP).2H2O (phase 3)
1
Electronic Supplementary Material (ESI) for Dalton Transactions
This journal is © The Royal Society of Chemistry 2012
Figure S1. XRPD Rietveld plot for La(H5DTMP)·7H2O (phase 1)
Figure S2. XRPD Rietveld plot for La(H5DTMP) (phase 2).
2
Electronic Supplementary Material (ESI) for Dalton Transactions
This journal is © The Royal Society of Chemistry 2012
Figure S3. XRPD Rietveld plot for La(H5DTMP).2H2O (phase 3).
Figure S4. Comparison of the powder patterns for Ln(H5DTMP)·7H2O, Ln=La and Sm.*
* The high background observed for Sm(H5DTMP).7H2O is due to the sample holder.
3
Electronic Supplementary Material (ESI) for Dalton Transactions
This journal is © The Royal Society of Chemistry 2012
Figure S5. Ball and stick view of the 3D framework for La(H5DTMP)·7H2O (1) showing the 1D
channels running along the c-axis and defined by 30-membered rings. Colour codes, La: purple; P:
shy-blue; O: red; C: small yellow spheres; N: small blue spheres.
Figure S6. One-dimensional chain of hydrogen-bonded lattice water molecules within the channel
along the c axis. H-bonding distances in the 5-water cluster are shown in the inset.
a
2.908 Å
2.912 Å
b
2.413 Å
4
2.861 Å
Electronic Supplementary Material (ESI) for Dalton Transactions
This journal is © The Royal Society of Chemistry 2012
Table S1. Selected bond lengths for La(H5DTMP)·nH2O (phases 1-3)
LENGTH (Å)
Bond
Phase 1 (n = 7)
Phase 2 (n = 0)
Phase 3 (n = 2)
La_O2
2.768(35)
2.802(30)
2.568(16)
La_O5
2.461(32)
2.36(4)
2.474(16)
La_O6
2.602(31)
2.439(24)
2.623(17)
La_O2b
2.310(24)
2.37(4)
2.640 (17)
La_O5b
2.782(29)
2.75(4)
2.556(16)
La_O6b
2.271(22)
2.694(23)
2.599(17)
Table S2. Selected H-Bond distances for La La(H5DTMP)·7H2O (phase 1)
Vector
LENGTH (Å)
Vector
LENGTH (Å)
Vector
LENGTH (Å)
Vector
LENGTH (Å)
Ow1_O1
3.11(6)
Ow2_Ow3
2.41(6)
Ow3_Ow6
2.24(6)
Ow5_O4
2.88(5)
Ow1_O2
2.75(5)
Ow2_Ow4
2.909(12)
Ow4_Ow5
2.86(5)
Ow5_O6
3.06(6)
Ow1_O5
2.44(6)
Ow2_Ow5
3.03(6)
Ow4_Ow6
3.02(6)
Ow6_Ow7
2.77(7)
Ow1_O6
3.44(6)
Ow2_Ow6
2.86(5)
Ow4_O4b
2.85(5)
Ow2_Ow7
2.912(12)
Ow4_Ow7
2.902(12)
Table S3. Selected H-Bonds distances for La(H5DTMP)·2H2O (phase 3)
Vector
LENGTH (Å)
Ow1_O4b
2.67(8)
Ow2_O1b
3.13(5)
5