Group 6 Oxyfluoro‐Anion Salts of [XeF<sub>5</sub>]<sup>+</sup> and [Xe<sub>2</sub>F<sub>11</sub>]<sup>+</sup>: Syntheses and Structures of [XeF<sub>5</sub>][M<sub>2</sub>O<sub>2</sub>F<sub>9</sub>] (M=Mo, W), [Xe<sub>2</sub>F<sub>11</sub>][M′OF<sub>5</sub>] (M′=Cr, Mo, W), [XeF<sub>5</sub>][HF<sub>2</sub>]⋅CrOF<sub>4</sub>, and [XeF<sub>5</sub>][WOF<sub>5</sub>]⋅XeOF<sub>4</sub>
Bibliographic record
Abstract
Abstract The reactions of the fluoride‐ion donor, XeF 6 , with the fluoride‐ion acceptors, M′OF 4 (M′=Cr, Mo, W), yield [XeF 5 ] + and [Xe 2 F 11 ] + salts of [M′OF 5 ] − and [M 2 O 2 F 9 ] − (M=Mo, W). Xenon hexafluoride and MOF 4 react in anhydrous hydrogen fluoride (aHF) to give equilibrium mixtures of [Xe 2 F 11 ] + , [XeF 5 ] + , [(HF) n F] − , [MOF 5 ] − , and [M 2 O 2 F 9 ] − from which the title salts were crystallized. The [XeF 5 ][CrOF 5 ] and [Xe 2 F 11 ][CrOF 5 ] salts could not be formed from mixtures of CrOF 4 and XeF 6 in aHF at low temperature (LT) owing to the low fluoride‐ion affinity of CrOF 4 , but yielded [XeF 5 ][HF 2 ]⋅CrOF 4 instead. In contrast, MoOF 4 and WOF 4 are sufficiently Lewis acidic to abstract F − ion from [(HF) n F] − in aHF to give the [MOF 5 ] − and [M 2 O 2 F 9 ] − salts of [XeF 5 ] + and [Xe 2 F 11 ] + . To circumvent [(HF) n F] − formation, [Xe 2 F 11 ][CrOF 5 ] was synthesized at LT in CF 2 ClCF 2 Cl solvent. The salts were characterized by LT Raman spectroscopy and LT single‐crystal X‐ray diffraction, which provided the first X‐ray crystal structure of the [CrOF 5 ] − anion and high‐precision geometric parameters for [MOF 5 ] − and [M 2 O 2 F 9 ] − . Hydrolysis of [Xe 2 F 11 ][WOF 5 ] by water contaminant in HF solvent yielded [XeF 5 ][WOF 5 ]⋅XeOF 4 . Quantum‐chemical calculations were carried out for M′OF 4 , [M′OF 5 ] − , [M′ 2 O 2 F 9 ] − , {[Xe 2 F 11 ][CrOF 5 ]} 2 , [Xe 2 F 11 ][MOF 5 ], and {[XeF 5 ][M 2 O 2 F 9 ]} 2 to obtain their gas‐phase geometries and vibrational frequencies to aid in their vibrational mode assignments and to assess chemical bonding.
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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 | 0.021 | 0.013 |
| Meta-epidemiology (narrow) | 0.036 | 0.040 |
| Meta-epidemiology (broad) | 0.032 | 0.018 |
| Bibliometrics | 0.013 | 0.023 |
| Science and technology studies | 0.016 | 0.020 |
| Scholarly communication | 0.012 | 0.015 |
| Open science | 0.024 | 0.018 |
| Research integrity | 0.021 | 0.042 |
| Insufficient payload (model declined to judge) | 0.000 | 0.004 |
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; both teacher heads agree on what is shown here.
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".