Synthesis and characterisation of <i>tris</i> (2,4-xylyl)phosphane oxide and the heavier chalcogen derivatives of <i>tris</i> (2,4-xylyl)- and <i>tris</i> (3,5-xylyl)phosphane
Bibliographic record
Abstract
The synthesis and characterisation of the novel sulfide and selenide adducts of both tris(2,4-xylyl)phosphane (i.e., 1; S adduct: 3; Se material: 4) and tris(3,5-xylyl)phosphane (5) are reported (S: 7; Se: 8) in addition to the previously unknown oxide of 1 (viz., 2). The heavier group 16 (Selenium) compounds 4 and 8 were produced by a rarely used photochemical protocol employing dialkyldiselenides as the Se source. Attempts to obtain the elusive selenide complex of trimesitylphosphane (9: i.e., tris(2,4,6-trimethylphenyl)phosphane) by this and other previously untried methods is also detailed but were ultimately unsuccessful. These observations further support the surmised instability and/or inaccessible nature of the selenide adduct of 9. Crystals of both 3 and 4 were obtained in the monoclinic P2 1 / c space group each with two unique molecules in the unit cell; the 3,5-congeners 7 and 8 are found in the trigonal R3 c space group. Compound 2 was found to crystallize in space group C2/c. The isolated and examined crystalline material obtained from bulk 8 is found to contain 81.0% of the phosphane-selenide with the residual lattice sites being occupied by selenide-free 5. The solid-state structural aspects of the examples reported herein are discussed and are placed into context with other (aryl) 3 P=E (E = O, S, or Se) materials.
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How this classification was reachedexpand
Full frame distilled prediction
Teacher imitationNot calibrated prevalence, not ground truth. Human validation pending. Learned from the 10,348 direct Codex labels and 10,348 direct Gemma labels. Candidate is the union of thresholded teacher heads; consensus is their intersection. These outputs are machine_predicted_unvalidated and are not human labels or direct frontier model labels.
Codex and Gemma teacher scores by category
| Category | Codex | Gemma |
|---|---|---|
| Metaresearch | 0.001 | 0.001 |
| Meta-epidemiology (narrow) | 0.000 | 0.000 |
| Meta-epidemiology (broad) | 0.001 | 0.000 |
| Bibliometrics | 0.000 | 0.000 |
| Science and technology studies | 0.000 | 0.001 |
| Scholarly communication | 0.000 | 0.000 |
| Open science | 0.000 | 0.000 |
| Research integrity | 0.000 | 0.000 |
| Insufficient payload (model declined to judge) | 0.000 | 0.000 |
Machine scores (provisional)
The two teacher heads of the student model, read on this work. A score orders the frame for review; it never asserts a category, and the validation status ships verbatim with every row.
Baseline scores from an immature model (maturity gate not passed, 7 training rounds). Scores rank; they never assert a category.
score_only:v0-immature-baseline · verbatim from the scoring run: score_only means the number may rank works, and no category label ships from itClassification
machine, unvalidatedMachine predicted; a candidate call from one teacher head, not a consensus.
How this classification was reached, model by model and score by score, is at the end of the page under "How this classification was reached".