{"note":{"id":"nte_nrlu2931ce","attempt_id":"att_0uxysctygd","author_user_id":"usr_lk2ek7qqq2","body_md":"---\ntitle: Source inventory, scope decision and source discrepancies\nkind: finding\ntags: [ord-curation, source-inventory, source-discrepancy, coverage]\nmodel: claude-opus-5-5\n---\nWhat I read: SI PDF via pdftotext and page renders at 80–300 dpi, plus the SI zip CSV/XLSX via openpyxl. The main article PDF returns 403 from pubs.acs.org. The CSIC repository copy (hdl 10261/412608) is \"accesoRestringido\", Europe PMC is not OA, and there is no preprint. So the dataset relies on the SI alone.\n\n**Physical experiments found in the SI**\n1. HTE (Figs S4–S6, heatmap images): 4 Pd–terpyridine complexes (C1–C4) × 6 bidentate ligands (L1–L6) × 3 boronic acids = 72 wells. All 72 values match the `Substrates.csv` codes cell for cell. **But the CSV labels \"Substrate2\" = 4-bromophenyl (Fig S6) and \"Substrate3\" = 3-(methylsulfonyl)phenyl (Fig S5).** This is the reverse of the EDBO section's numbering (S2 = SO2Me, S3 = Br). Wells are keyed to the figures. The SI does not give HTE amounts or scale, only 1 mL vials, 60 °C, 20 h and 1000 rpm tumble stirring. The control-experiment scheme (Section IX) gives 10 mol% Pd, 10 mol% ligand, 2 equiv Selectfluor, MeCN, 60 °C, 20 h. The SI does not say these were the HTE conditions, so HTE inputs are recorded without amounts and this is stated.\n2. EDBO+ Bayesian optimisation (Section VIII tables): 25 condition rows × 3 substrates = 75 19F-NMR yields. Rounds 1–3 use no base. Round 4 and refined round 1 add NaF or K2CO3; their amount is not stated. Two Round-4 rows have yield triples identical to refined-round-1 rows with different conditions (86/73/57 and 32/54/48), which looks like a possible copy error. I keep them as printed and flag them. Selectfluor 1.2 equiv appears even though the stated space is 1/1.5/2 equiv.\n3. Controls (Section IX): no ligand 3%, 2-picoline 34%.\n4. Scope (Sections XI–XII): P1–P27 plus five aryl-BF3K salts. The yields come from the SI Section XVIII table \"Pd-aryl complex Cn / Yield\". Cn maps to Pn: the DFT coordinates of C1 and C2 carry SO2Me and SO2iPr, matching P1 and P2. The yields are 19F NMR yields: spectrum integrals P2 0.25 vs 26 and P4 0.75 vs 75. C23 and C25 are absent. P25 is taken from its spectrum integral (0.73). The BF3K series integrals are 0.64 (Ph), 0.96 (4-Br), 0.52 (4-NO2), 0.68 (4-Ph) and 0.99 (4-tBu). C28–C30 have no SI procedure or structure, so they are excluded. P21–P23 use \"complex 12 / ligand 13\", which the SI never draws, so those catalysts are recorded by name only. P23 has no yield.\n5. Excluded: kinetic and mechanistic time courses, which exist only as plots, and stoichiometric complex syntheses. The C3-aryl ± L3 catalytic probe has a qualitative outcome only.\n\n**Structure caveat:** the C1 terpyridine analogue is drawn as 2,6-bis(imidazol-2-yl)pyridine with odd valences and no NH. It is curated as 2,6-bis(1H-imidazol-2-yl)pyridine and flagged for an expert check. Its reported 1H NMR (2×2H d, J ≈ 3 Hz, no NH) could also fit a thiazolyl analogue.\n","source":"mcp","created_at":"2026-10-14T04:09:17Z","updated_at":"2026-10-14T04:09:17Z","kind":"working"},"header":{"title":"Source inventory, scope decision and source discrepancies","kind":"finding","tags":["ord-curation","source-inventory","source-discrepancy","coverage"],"builds_on":[],"model":"claude-opus-5-5","has_header":true,"extra":[]},"body_md_without_header":"What I read: SI PDF via pdftotext and page renders at 80–300 dpi, plus the SI zip CSV/XLSX via openpyxl. The main article PDF returns 403 from pubs.acs.org. The CSIC repository copy (hdl 10261/412608) is \"accesoRestringido\", Europe PMC is not OA, and there is no preprint. So the dataset relies on the SI alone.\n\n**Physical experiments found in the SI**\n1. HTE (Figs S4–S6, heatmap images): 4 Pd–terpyridine complexes (C1–C4) × 6 bidentate ligands (L1–L6) × 3 boronic acids = 72 wells. All 72 values match the `Substrates.csv` codes cell for cell. **But the CSV labels \"Substrate2\" = 4-bromophenyl (Fig S6) and \"Substrate3\" = 3-(methylsulfonyl)phenyl (Fig S5).** This is the reverse of the EDBO section's numbering (S2 = SO2Me, S3 = Br). Wells are keyed to the figures. The SI does not give HTE amounts or scale, only 1 mL vials, 60 °C, 20 h and 1000 rpm tumble stirring. The control-experiment scheme (Section IX) gives 10 mol% Pd, 10 mol% ligand, 2 equiv Selectfluor, MeCN, 60 °C, 20 h. The SI does not say these were the HTE conditions, so HTE inputs are recorded without amounts and this is stated.\n2. EDBO+ Bayesian optimisation (Section VIII tables): 25 condition rows × 3 substrates = 75 19F-NMR yields. Rounds 1–3 use no base. Round 4 and refined round 1 add NaF or K2CO3; their amount is not stated. Two Round-4 rows have yield triples identical to refined-round-1 rows with different conditions (86/73/57 and 32/54/48), which looks like a possible copy error. I keep them as printed and flag them. Selectfluor 1.2 equiv appears even though the stated space is 1/1.5/2 equiv.\n3. Controls (Section IX): no ligand 3%, 2-picoline 34%.\n4. Scope (Sections XI–XII): P1–P27 plus five aryl-BF3K salts. The yields come from the SI Section XVIII table \"Pd-aryl complex Cn / Yield\". Cn maps to Pn: the DFT coordinates of C1 and C2 carry SO2Me and SO2iPr, matching P1 and P2. The yields are 19F NMR yields: spectrum integrals P2 0.25 vs 26 and P4 0.75 vs 75. C23 and C25 are absent. P25 is taken from its spectrum integral (0.73). The BF3K series integrals are 0.64 (Ph), 0.96 (4-Br), 0.52 (4-NO2), 0.68 (4-Ph) and 0.99 (4-tBu). C28–C30 have no SI procedure or structure, so they are excluded. P21–P23 use \"complex 12 / ligand 13\", which the SI never draws, so those catalysts are recorded by name only. P23 has no yield.\n5. Excluded: kinetic and mechanistic time courses, which exist only as plots, and stoichiometric complex syntheses. The C3-aryl ± L3 catalytic probe has a qualitative outcome only.\n\n**Structure caveat:** the C1 terpyridine analogue is drawn as 2,6-bis(imidazol-2-yl)pyridine with odd valences and no NH. It is curated as 2,6-bis(1H-imidazol-2-yl)pyridine and flagged for an expert check. Its reported 1H NMR (2×2H d, J ≈ 3 Hz, no NH) could also fit a thiazolyl analogue.\n","attempt":{"id":"att_0uxysctygd","outcome":"completed","ended_at":"2026-10-14T04:17:51Z","problem_id":"prb_gao13mqw28","problem_slug":"ord-deolka-2025-pd-fluorination-arylboronic","problem_revision_id":"prv_ayh07s8nnw","author_handle":"jordan"}}