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Supporting Information

Ligand Flexibility and Framework Rearrangement in a New Family of Porous

Metal-Organic Frameworks

Samuel M. Hawxwell,

Guillermo Mínguez Espallargas,

Darren Bradshaw,

Matthew J.

Rosseinsky,

Timothy J. Prior,

Alastair J. Florence,

Jacco van de Streek

and Lee

Brammer*

Department of Chemistry, University of Sheffield, Brook Hill, Sheffield, S3 7HF, UK.

Department of Chemistry, University of Liverpool, Crown Street, Liverpool, L69 7ZD, UK

Synchrotron Radiation Source, CCLRC Daresbury Laboratory, Daresbury, Warrington WA4

4AD, UK

Solid-State Research Group, Strathclyde Institute of Pharmacy and Biomedical Sciences,

University of Strathclyde, 27 Taylor Street, Glasgow G4 0NR, Scotland

Cambridge Crystallographic Data Centre, 12 Union Road, Cambridge CB2 1EZ, UK

Experimental

1. General

All chemicals were purchased from Aldrich or Lancaster and used as received. Infra-red spectra

were recorded on a Perkin-Elmer Spectrum RX I FT-IR spectrometer equipped with a SensIR

diamond attenuated total reflectance fitting.

H NMR spectra were recorded on a Bruker AC-250

(250 MHz) or AMX-400 (400 MHz) supported by an Aspect 3000 data system. Chemical shifts

are reported in ppm with the solvent resonance as the internal standard (CHCl

: δ 7.27 ppm and

DMSO: δ 2.50 ppm). Data are reported as follows: chemical shift; multiplicity (s = singlet, d =

doublet, t = triplet, br = broad, m = multiplet); integration.

C NMR spectra were recorded on a

Bruker AC-250 (62.9 MHz) or AMX-400 (100.6 MHz) with complete proton decoupling.

Chemical shifts are reported in ppm with the solvent resonance as the internal standard (CHCl

: δ

77.00 ppm and DMSO: δ 39.50 ppm). The electron ionisation mass spectra were obtained on a

VG Auto Spec Magnetic Sector machine working positive or negative ion mode. The elemental

analyses were conducted by the Elemental Analysis service, Department of Chemistry,

University of Sheffield. Powder diffraction data were obtained on a Bruker-AXS D8 Advance

powder diffractometer at the Strathclyde Institute of Pharmacy and Biomedical Science,

University of Strathclyde, using Cu K

α1

radiation (λ = 1.54056 Å).

2. Synthesis

2.1 Butane Tetraester (Me

L1)

1 2 3 4 5 6 ... 10 11

Inhaltsverzeichnis

Seite 1 - Supporting Information

S1Supporting Information Ligand Flexibility and Framework Rearrangement in a New Family of Porous Metal-Organic Frameworks Samuel M. Hawxwell,a Guill

Seite 2

S10 Figure S6. TGA trace for 1 (heating under N2 at 5 ºC min-1 from room temperature to 600 ºC) Figure S7. TGA trace for 2 (heating under N2 at

Seite 3

S11 [2] SHELXTL 5.1, Bruker Analytical X-Ray Instruments, Inc., 1998. [3] (a) Shankland, K.; David, W. I. F.; Sivia, D. S. J. Mater. Chem. 1997, 7,

Seite 4

S2A mixture of dimethyl 5-hydroxyisophthalate (2.43 g, 11.6 mmol), 1,4-dibromobutane (1.08 g, 5.00 mmol) and K2CO3 (2.50 g, 18.1 mmol) were stirred i

Seite 5

S3 A mixture of dimethyl 5-hydroxyisophthalate (2.10 g, 10.0 mmol), trans-1,4-dibromobut-2-ene (1.05 g, 4.90 mmol), K2CO3 (2.21 g, 16.0 mmol) and di

Seite 6

S4Elemental Analysis: calcd for C20H18O11 (H42·H2O) C 55.30 % H 4.18 %, found C 55.49 % H 3.91 % 2.5 [Zn2(L1)(H2O)4]·2H2O (1) Zn(ClO4)2·6H2O (0.112

Seite 7

S5b (Å) 8.5113(17) 14.1157(7) c (Å) 9.827(2) 16.6631(8) α (°) 68.56(3) 66.602(1) β (°) 79.47(3) 87.138(1) γ (°) 86.62(3) 89.757(1) V (Å3) 5

Seite 8

S6 Figure S2. Alternative view of two-fold interpenetrated diamondoid network exhibited by 2. Colours as in Figure S1. Hydrogen atom, water molecule

Seite 9 - Sorption for 1

S7structure was then refined against the data in the range 4 - 65 o 2θ using a restrained Rietveld method as implemented in TOPAS v3.1 [10], where on

Seite 10

S8 Figure S4. Crystal structure of 3 shown without water molecules in channels. Hydrogen atoms on coordinated water molecules are omitted (and were n

Seite 11

S9made phases, and by immersion of the reaction chamber into solid carbon dioxide contained in a cryogenic vessel (at 198 K) during isotherm measurem

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