Readme file for dataset relating to paper "Stable and Ordered Amide Frameworks Synthesised Under Reversible Conditions which Facilitate Error Checking"

All file names in the data set refer to sample names in paper

Dataset contains text/ascii data files for powder Xray diffraction, FT-IR spectroscopy and synchrotron pdf.

Samples preparation:
Synthesis of PATnC
A solution of trimesoyl chloride (6.40 g, 24.11 mmol) in dry DMF (30 mL) was added drop wise to a solution of trans-1,4-cyclohexanediamine (4.50 g, 39.42 mmol) and triethyl amine (12 mL, 79.06 mmol) in dry DMF (500 mL) at 0 °C with strong stirring over the course of 1 hour under N2. The suspension was allowed to warm to room temperature and stirred overnight followed by quenching with water (500 mL). The solids were filtered, dried in vacuo, ground into a coarse powder and then ball milled (15 min forward, 10 min rest, 15 min reverse, 350 rpm, 2 repetitions) into a fine powder. This powder was suspended in water (250 mL) and stirred overnight. The solid was filtered and the filtrate found to be pH neutral. The solid was dried by filtration and then activated at 110 °C under vacuum (10-1 mbar) overnight to yield PATnC as a fine very pale yellow powder (7.36 g, 22.5 mmol, 93.2 %). 
Synthesis of CAF-1 via PATnC
A Pyrex tube (OD 9.7 mm, ID 5.3 mm) was charged with dry PATnC (100 mg, 0.31 mmol, dried under 10-3 mbar at 120 °C overnight) and water (50 µL, 2.78 mmol). The water was frozen by submerging the bottom of the tube in liquid N2 and the tube was evacuated to 10-4 mbar and sealed with an approximate length of 10 cm. The tube was placed in a 300 mL Parr pressure reactor with 30 mL of water which was then sealed. The reactor was placed in an oven heating to 250 °C at 10 °Cmin-1 where it was held for 3 days followed by cooling at the same rate back to room temperature. The reactor and tube were opened and the solid was washed with DMF (3 x 10 mL), water (3 x 10 mL) and MeOH (3 x 10 mL) then dried by filtration yielding CAF-1 as a very pale yellow powder (99.1 mg, 0.30 mmol, 99.1 %).
Synthesis of PATCnC
4,4',4'',4'''-methanetetrayltetrabenzoic acid  (4.00 g, 8.06 mmol) was refluxed in thionyl chloride (30 mL, 0.41 mol) at 70 °C for 3 hours under N2 until the suspension had become a dark red/brown solution. The excess thionyl chloride was removed in vacuo yielding 4,4’,4’’,4’’’-methanetetraaryltetrabenzoyl chloride which was used without further purification. 4,4’,4’’,4’’’-methanetetraaryltetrabenzoyl chloride was dissolved in dry DMF (60 mL) and added drop wise with strong stirring to a solution of trans-1,4-cyclohexanediamine (2.00 g, 17.5 mmol) and triethyl amine (5.00 mL, 32.9 mmol) in dry DMF (750mL) over 1 hour at 0 °C under N2. The suspension was allowed to warm to room temperature and was stirred overnight followed by quenching with water (500 mL). The solids were filtered and washed with DMF (3 x 250 mL). The solids were dried overnight in vacuo, ground into a fine powder, suspended in water (250 mL) and stirred for 1 hour. The solid was filtered and washed with water until the pH of the filtrate was neutral (3 x 250 mL) followed by MeOH (250 mL) and dried by filtration. The solid was activated at 120 °C under vacuum (10-1 mabr) overnight to yield PATCnC as a pale yellow powder (3.51 g, 5.37 mmol, 66.7 % over two steps).
Synthesis of CAF-2
A Pyrex tube (OD 9.7 mm, ID 5.3 mm)  was charged with dry PATCnC (100 mg, 0.15 mmol, dried under 10-3 mbar at 120 °C overnight) and water (40 µL, 2.22 mmol). The water was frozen by submerging the bottom of the tube in liquid N2 and the tube was evacuated to 10-4 mbar and sealed with an approximate length of 10 cm. The tube was placed in a 300 mL Parr pressure reactor with 30 mL of water which was then sealed. The reactor was placed in an oven heating to 240 °C at 10 °Cmin-1 where it was held for 7 days followed by cooling at 0.1 °Cmin-1 back to room temperature. The reactor and tube were opened and the solid was washed with DMF (10 x 10 mL), water (10 x 10 mL) and MeOH (10 x 10 mL) then dried by filtration yielding CAF-2 as a grey powder (90.55 mg, 0.14 mmol, 92.5 %).

Samples characterization:
Lab PXRD. Lab X-ray powder diffraction data were collected on a Bruker D8 Advance powder X-ray diffractometer at 298 K in transmission geometry  with  Cu Ka1 radiation ( ? = 1.54060 Å). Samples were ground into fine powders and loaded into 0.7 mm internal diameter borosilicate capillaries. Typical scans were collected as step scans over 1 h between 3 and 50 °2?.
FT-IR spectroscopy. Infrared spectra were collected from finely ground powdered samples between 4000 and 650 cm-1 using a Perkin Elmer Spectrum 100 instrument in Attenuated Total Reflectance (ATR) mode with a resolution of 4 cm-1, 4 scans were collected per sample after the collection of  a background.
Synchrotron PDF. Room temperature pair distribution function (PDF) data were collected on the I15 beamline at Diamond Light Source, Oxfordshire, at a wavelength of 0.1620 Å. Samples were sealed inside 0.7 mm diameter borosilicate capillaries.