Synthesis, Solid-State NMR, and X-ray Powder Diffraction Characterization of Group 12 Coordination Polymers, Including the First Example of a C-Mercuriated Pyrazole Norberto Masciocchi Simona Galli Enrica Alberti Angelo Sironi Corrado Di Nicola Claudio Pettinari Luciano Pandolfo 10.1021/ic061349b.s004 https://acs.figshare.com/articles/dataset/Synthesis_Solid_State_NMR_and_X_ray_Powder_Diffraction_Characterization_of_Group_12_Coordination_Polymers_Including_the_First_Example_of_a_C_Mercuriated_Pyrazole/3051067 Cadmium and mercury acetates have been reacted with pyrazole (Hpz) and 3,5-dimethylpyrazole (Hdmpz), affording distinct mixed-ligand species, selectively prepared upon slightly modifying the reaction conditions. Two polymorphs of [{Cd(μ-ac)<sub>2</sub>(Hpz)<sub>2</sub>}<i><sub>n</sub></i>], as well as the [{Cd(μ-ac)<sub>2</sub>(Hdmpz)<sub>2</sub>}<i><sub>n</sub></i>] species (Hac = acetic acid), were obtained by solution chemistry, while the two-dimensional [{Cd<sub>3</sub>(μ<sub>3</sub>-ac)<sub>4</sub>(μ-pz)<sub>2</sub>(Hpz)<sub>2</sub>}<i><sub>n</sub></i>] and [{Cd(μ-ac)(μ-pz)}<i><sub>n</sub></i>] polymers were prepared upon controlled thermal treatment of one of the [{Cd(μ-ac)<sub>2</sub>(Hpz)<sub>2</sub>}<i><sub>n</sub></i>] forms. Two mercury derivatives, [{Hg<sub>3</sub>(μ-ac)<sub>3</sub>(μ-pz)<sub>3</sub>}<i><sub>n</sub></i>] and [{Hg(ac)(μ-dmpz)}<i><sub>n</sub></i>], were also prepared, the latter containing one-dimensional chains of Hg(II) ions bridged by C-mercuriated Hdmpz ligands. All their crystal structures (but one) were determined by powder diffraction methods using conventional X-ray laboratory equipment, supported by <sup>13</sup>C CPMAS NMR measurements. The latter method helped in assigning a C-metalated nature to an amorphous material of [Hg(ac)(pz)] formula, obtained by employing EtOH as a solvent. A few other Hdmpz-containing cadmium acetates were also prepared, but their polyphasic nature, evidenced by diffraction methods, hampered their complete structural characterization. 2006-10-30 00:00:00 solution chemistry diffraction methods 13 C CPMAS NMR measurements Hg First Example powder diffraction methods Hdmpz polyphasic nature mercury derivatives reaction conditions Group 12 Coordination Polymers species crystal structures mercury acetates latter method