Automated stopped-flow library synthesis for rapid optimisation and machine learning directed experimentation

Completed the deliverables within this attempt and submitted sub_848xlgrwq7 with dataset art_wslzjap52k and source archive art_5cti3kttwb. Verification vrn_ecbgir0e3u is running in formal curator review process rpr_4eolysgncm; no formal acceptance or ORD ingestion is claimed. This is the first internally reviewed submission of this five-paper goal, not one formally solved problem.

The dataset has 1,229 distinct experimental records: 1,070 exact chromatographic-area percentages, 59 additional source-figure area ranges, 11 explicitly crossed analytical-failure entries without fabricated numerical outcomes, and 89 quantified SNOBFIT experiments. Eighteen Figure 2 internal-standard/product ratios attach to matching screen entries rather than creating duplicates. Overlapping cross-validation tables were reconciled. S4.2 point 30 lacks both conditions and result and is transparently excluded.

Primary sources establish inputs/quantities, stopped-flow timing, workup/analysis, full chemical identities and HPLC-DAD area semantics. Twenty-nine numerical-table/figure-category disagreements are preserved and documented. Toluene is a pre-reaction standard in the actual method, so that input placement is retained despite the generic workup warning. Every reaction cites DOI10.1039/D2SC03016K and includes the established public organizational curator identity and accurate computational provenance. No ORD dataset/reaction IDs are assigned.

A separate Astra ultra agent independently audited all records and structures, all1,140 figure cells, source hashes, SI mappings, additional ratios and legitimate exclusions. It found zero must-fix or should-fix issues, reran ord-schema0.8.3 successfully, and rebuilt the exact delivered compressed dataset byte for byte. The sources archive includes the actual validator log, reconstruction scripts, licensed sources, hashes and coverage audit. Dataset SHA2567a1d7be049ce72bd3d4fdbc5d698280e28b9d8b8ddf324db8efdf64be2683a15; sources SHA25665170e5b0250d241e3b68d6a2ef7f6cf0158100bedb7f465a61f14f7218c3965. Independent internal review is not formal human curator approval.

Official toolkit preflight passed artifact requirements; the contract has only a human review stage, which is not executable locally. Signed PUT upload URLs returned401 with a sign-in requirement despite their documented no-auth instructions; the supported upload_artifact MCP tool succeeded using the toolkit's authenticated transport, and server hashes matched. No duplicate successful artifacts/submissions were created.

Continue from this attempt only if actionable formal feedback arrives, using the official continuation mechanism; do not resubmit while merely waiting for the external review. The durable goal checkpoint retains local/recoverable artifacts and the independent QA reports.

Draft dataset contains 1229 experimental records: 1070 exact area percentages, 59 additional figure-only area bins, 11 individually located crossed-cell no-analysis results, and 89 quantitative SNOBFIT points. Eighteen Figure 2 ratios are attached to matching existing experiments. All 54 source product graphs match independently constructed acid/amine amide connections, all compounds have parseable SMILES, correct roles and amounts, and no dataset/reaction IDs are assigned. Exact ORD 0.8.3 validation CLI exit 0 with no errors/warnings; complete output is saved. Extracting the sources ZIP and rerunning extraction/build reproduces dataset bytes exactly (SHA-256 7a1d7be049ce72bd3d4fdbc5d698280e28b9d8b8ddf324db8efdf64be2683a15); all raw source hashes match. Public curator identity uses the connected user's established organizational identity, Tokens for Progress <hello@tokensforprogress.org>. The draft remains unsubmitted pending independent internal QA; final campaign acceptance is a distinct independent human ORD-curator review.

Checked main Figures 3 and 6 against the 1070 numeric records. The 900-cell first screen omits 64 records from the machine-learning table, including the entire A3/B4 acid/amine combination; 59 omitted cells still have published area-percentage color bins and 5 are crossed white analytical failures. The 240-cell external screen omits 6 records, all explicitly crossed white. These 70 individually located primary-figure cells will be included without invented exact numbers: 59 categorical area ranges and 11 no-analysis-result observations. The s007 table and figure colors also disagree at 29 existing numeric records (including two exact threshold-boundary cases); the source reconciliation CSV preserves both. Numerical source values take precedence, with figure discrepancies described rather than silently overwritten. Figure 2's 18 ratios map uniquely to existing screening records and will be additional measurements, not duplicated reactions. Methods confirm toluene internal standard was premixed in the amine stock before reaction, so its actual pre-addition is preserved as input role INTERNAL_STANDARD despite the generic post-reaction warning in the Skill.

This exact goal has five active attempts, all live wishlist cards confirmed Available: Avila att_05j0abohe7, Angello att_g3zvu0yzl5, Basford att_9wgv0fyay0, Ramírez att_fwzkfjqh6e, McCorkindale att_3yi4b0t01a. Zero submissions or formal solves yet; source reconciliation and drafting remain in progress. Resume these attempts rather than creating duplicates. Workers use explicitly selected gpt-6-astra ultra; independent draft reviews will follow before submission.

Avila ESI s007 has 1,070 core experiments, including the 234 temporal test campaign. Other split tables overlap; s012 contains descriptors only. SI S4 reports additional SNOBFIT experiments, one injection-missed record without measurements. Main-method checking establishes that the tabular Success field is target chromatographic area percentage, not calibrated yield. Draft will preserve these distinctions and justify coverage.

The public organizational curator identity already used in the connected user's existing public ORD artifact art_d2d0utjmg9/current submission sub_6w8gn583pk was inspected for continuity: Tokens for Progress, hello@tokensforprogress.org. That older work is not counted among the requested five. New records will accurately document automated curation and actual creation time.

Resumed the existing attempt and read its pinned contract. The final ESI table s007 contains 1070 experiments (836 initial and 234 temporal-test), while SI S4.1/S4.2 add 89 quantified SNOBFIT experiments plus one injection-missed row without conditions. Main paper Figure 2 additionally reports 18 internal-standard/product ratios for DoE examples; these will be mapped to corresponding library records if identical conditions/structures, avoiding duplicate experiments. Main sections 2.3 and 4.4 establish that table Success is the target-product UV peak area divided by total chromatogram area at 254 nm, not calibrated yield or stoichiometric conversion. SI optimisation values are I.S./product area ratios, also not yields. Source structures are being checked against Scheme 1 and SI Figure S3. No output upload or submission yet.

Confirmed wishlist item 126570038 remains Available through the public GitHub project page filtered to stopped-flow (2026-10-13). Will compare every data-bearing supplementary table, preserve distinct experimental observations, reconcile train/test copies, and derive amounts/conditions/analytical interpretation from the original SI. Installed ord-schema 0.8.3 in an isolated Python environment. Deliverable will undergo independent agent review before submission; schema validity alone will not be treated as proof of faithful curation.