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The NgF2 ⋅ MOF4 (Ng=Kr, Xe; M=Mo, W) and XeF2 ⋅ 2MOF4 complexes were synthesized in anhydrous HF (aHF) solvent and melts, respectively. Their single‐crystal X‐ray diffraction (SCXRD) structures show NgF2 ⋅ MOF4 and XeF2 ⋅ 2MOF4 have Ft−Ng−Fb‐ ‐ ‐M arrangements, in which the NgF2 ligands coordinate to MOF4 through Ng−Fb‐ ‐ ‐M bridges. The XeF2 ligands of XeF2 ⋅ 2MOF4 also coordinate to F3OM−Fb’‐ ‐...
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