Dataset for "Continuous flow for materials synthesis, assembly and crystallisation at Diamond: discovery and delivery of high value materials"

779 67 13089 2 39209 document 13089 CBZ form III post-nucleation seeded crystallisation KRAIC-D - CBZ form III habit separation (CBZKDB4) Chapter 4.MOV video/quicktime e47afe88eefcdb9069adf144a64b395e MD5 13547218 2020-03-27 10:11:46 https://researchdata.bath.ac.uk/779/1/CBZ%20form%20III%20post-nucleation%20seeded%20crystallisation%20KRAIC-D%20-%20CBZ%20form%20III%20habit%20separation%20%28CBZKDB4%29%20Chapter%204.MOV 779 1 1 video/quicktime other Carbamazepine (CBZ) is well known to typically present as needles for CBZ form II and as blocks for CBZ form III. However, in spite of only detecting CBZ III in the in situ Powder X-ray Diffraction data after post-nucleation seeding, aggregated needles were the main habit observed, in addition to a low proportion of small blocks. This is an unusual case of crystallising CBZ form III needles. The two habits are shown to separate as a result of their different interaction with the flow paths. en public cc_by

CBZ form III post-nucleation seeded crystallisation KRAIC-D - CBZ form III habit separation (CBZKDB4) Chapter 4.MOV

data 13090 2 39235 document 13090 Chapter 5 - KRAIC-S.zip application/zip f78ab0fc5f86621c0afb25b8e7325fba MD5 35399475 2020-03-31 11:09:05 https://researchdata.bath.ac.uk/779/2/Chapter%205%20-%20KRAIC-S.zip 779 2 2 application/zip other Videos of single crystals tracked by the slug triggering mechanism comprising an optical trigger and translation of the motorised stage to artificially suspend the single crystal in the X-ray beam during data collection. Videos are categorised into unseeded and seeded crystallisations of paracetamol (PCM). The unseeded cooling crystallisation are further segmented into 6.7 m and 8.7 m crystalliser length. N.B videos are rotated by 180° and thus is observed as residing in the top of solution slug en public cc_by

Chapter 5 - KRAIC-S.zip

data 13092 2 39250 document 13092 ESI Details of Videos for Chapter 5 - KRAIC-S.docx application/vnd.openxmlformats-officedocument.wordprocessingml.document 4c8af2a23979b3cfc59b87774e2378f5 MD5 21355 2020-03-31 12:39:27 https://researchdata.bath.ac.uk/779/3/ESI%20Details%20of%20Videos%20for%20Chapter%205%20-%20KRAIC-S.docx 779 3 3 application/vnd.openxmlformats-officedocument.wordprocessingml.document other Details of videos of single crystals tracked in solution slugs, including experiment type and run number. The Paracetamol (PCM) form II videos also state the polymorphic outcome as PCM form II was not produced in each case, in some instances the thermodynamically stable PCM form I polymorph was crystallised instead. en public cc_by

ESI Details of Videos for Chapter 5 - KRAIC-S.docx

documentation 13094 2 39266 document 13094 Data Management Plan.docx application/vnd.openxmlformats-officedocument.wordprocessingml.document bfff9c86ae7e4c23fceda2ae16ed5476 MD5 122864 2020-03-31 13:06:29 https://researchdata.bath.ac.uk/779/4/Data%20Management%20Plan.docx 779 4 4 application/vnd.openxmlformats-officedocument.wordprocessingml.document other en staffonly cc_by

Data Management Plan.docx

dmp 13095 1 39270 document 13095 indexcodes.txt text/plain e45c66e508e6c982258168d1d7d61643 MD5 733 2020-03-31 13:09:47 https://researchdata.bath.ac.uk/779/5/indexcodes.txt 779 5 5 text/plain other Generate index codes conversion from other to indexcodes en public

indexcodes.txt

http://eprints.org/relation/isVersionOf https://researchdata.bath.ac.uk/id/document/13092 http://eprints.org/relation/isVolatileVersionOf https://researchdata.bath.ac.uk/id/document/13092 http://eprints.org/relation/isIndexCodesVersionOf https://researchdata.bath.ac.uk/id/document/13092 13096 1 39271 document 13096 indexcodes.txt text/plain 7edf5dcddb949bc24c6f9fdde47313a2 MD5 3126 2020-03-31 13:09:48 https://researchdata.bath.ac.uk/779/6/indexcodes.txt 779 6 6 text/plain other Generate index codes conversion from other to indexcodes en staffonly

indexcodes.txt

http://eprints.org/relation/isVersionOf https://researchdata.bath.ac.uk/id/document/13094 http://eprints.org/relation/isVolatileVersionOf https://researchdata.bath.ac.uk/id/document/13094 http://eprints.org/relation/isIndexCodesVersionOf https://researchdata.bath.ac.uk/id/document/13094 13098 2 39283 document 13098 Context of Research.docx application/vnd.openxmlformats-officedocument.wordprocessingml.document 1a9f6a516ee49f34b1121f0ab088ba30 MD5 25578 2020-04-02 09:36:36 https://researchdata.bath.ac.uk/779/7/Context%20of%20Research.docx 779 7 7 application/vnd.openxmlformats-officedocument.wordprocessingml.document other Context of Research en public cc_by

Context of Research.docx

documentation 13099 1 39288 document 13099 indexcodes.txt text/plain 7765df176880f28da2ca0c3a57980327 MD5 1852 2020-04-02 09:46:57 https://researchdata.bath.ac.uk/779/8/indexcodes.txt 779 8 8 text/plain other Generate index codes conversion from other to indexcodes en public

indexcodes.txt

http://eprints.org/relation/isVersionOf https://researchdata.bath.ac.uk/id/document/13098 http://eprints.org/relation/isVolatileVersionOf https://researchdata.bath.ac.uk/id/document/13098 http://eprints.org/relation/isIndexCodesVersionOf https://researchdata.bath.ac.uk/id/document/13098 13120 2 39368 document 13120 Slug Triggering Mechanism.3gp video/3gpp be3c6cdc1d215d48f910e496a782c05e MD5 145374136 2020-04-06 09:25:35 https://researchdata.bath.ac.uk/779/9/Slug%20Triggering%20Mechanism.3gp 779 9 9 video/3gpp other Slug Triggering Mechanism comprising the optical trigger and motorised stage translation to artificially suspend the solution slugs in the X-ray beam. en public cc_by

Slug Triggering Mechanism.3gp

data archive 7673 disk0/00/00/07/79 2020-10-15 13:23:39 2024-07-22 09:34:15 2020-10-15 13:23:39 data_collection show Wayment Lois L.E.Wayment@bath.ac.uk University of Bath; Diamond Light Source TRUE Supervisor Wilson Chick C.C.Wilson@bath.ac.uk 0000-0002-1039-132X University of Bath Supervisor Robertson Karen Karen.Robertson@nottingham.ac.uk 0000-0002-0719-5854 University of Nottingham Supervisor Warren Mark R mark.warren@diamond.ac.uk 0000-0003-1326-0744 Diamond Light Source Supervisor Allan David R. david.allan@diamond.ac.uk Diamond Light Source Supervisor Tang Chiu chiu.tang@diamond.ac.uk Diamond Light Source Other Scott Daniel C.D.Scott@bath.ac.uk 0000-0003-3051-0514 University of Bath Other Levenstein Mark markl@illinois.edu University of Illinois Urbana-Champaign Other Payne Pollyanna P.Payne@bath.ac.uk University of Bath Other Lunt Ruth R.A.Lunt@bath.ac.uk University of Bath Other Flandrin Pierre-Baptiste P.Flandrin@bath.ac.uk University of Bath Dataset for "Continuous flow for materials synthesis, assembly and crystallisation at Diamond: discovery and delivery of high value materials" CG0010 CG0020 CG0030 GE0030 GE0040 JK0100 JK0200 JK0500 KS0160 dept_chem Continuous crystallisation of the model system Carbamazepine (CBZ) in ethanol in the KRAIC-D (Kinetically Regulated Automated Input Crystalliser - Diffraction) platform on beamline I11 (high resolution powder diffraction) is presented. The effect of introducing a controlled solid interface into the crystallisation process is investigated, where CBZ form III seeds are introduced in polymorphic purity at different seeding positions (pre- and post-nucleation) throughout the length of the KRAIC-D. The video associated with Chapter 4 corresponds with a post-nucleation CBZ form III experiment where a separation of crystal habit is observed as a result of the different interaction with the flow paths in the solution slugs with the segmented flow. The second device is the KRAIC-S (Kinetically Regulated Automated Input Crystalliser - Single Crystal) platform installed at I19 (small molecule single crystal beamline) employed to investigate the continuous crystallisation of paracetamol (PCM) in 60:40 water:isopropanol via a range of experiments including unseeded and seeded cooling crystallisations. The unseeded experiments also looked at the crystallisation at different set points along the KRAIC-S (6.7 m and 8.7 m) to investigate crystal growth and crystal rotation at different length scales. The videos associated with Chapter 5 include single crystals produced from the range of experiments investigated. Each video tracks a different single crystal in a solution slug, where through use of the slug triggering mechanism, whereby an optical trigger prompts translation of the motorised stage to artificially suspend the single crystal in the X-ray beam during data collection. These videos complement the diffraction data and can provide explanation for data collections, which do not achieve cell indexation as the single crystal is shown to move in and out of the X-ray beam in these videos. 2020-06-01 University of Bath public RightsHolder University of Bath RightsHolder Diamond Light Source Engineering and Physical Sciences Research Council https://doi.org/10.13039/501100000266 EP/P006965/1 Future Continuous Manufacturing and Advanced Crystallisation Research Hub Diamond Light Source https://doi.org/10.13039/100011889 Diamond Light Source studentship Videos obtained using Camera positioned by X-ray beam on beamline I19, the small molecule single crystal beamline at Diamond Light Source. en 1 10.15125/BATH-00779 https://doi.org/10.1021/acs.analchem.0c00860 pub https://researchportal.bath.ac.uk/en/studentTheses/9b7f12d1-5f21-4bce-aa77-968da4033b35 thesis open