10.1021/ic100724r.s002 Guo-Hong Ning Guo-Hong Ning Liao-Yuan Yao Liao-Yuan Yao Li-Xia Liu Li-Xia Liu Ting-Zheng Xie Ting-Zheng Xie Yi-Zhi Li Yi-Zhi Li Yu Qin Yu Qin Yuan-Jiang Pan Yuan-Jiang Pan Shu-Yan Yu Shu-Yan Yu Self-Assembly and Host−Guest Interaction of Metallomacrocycles Using Fluorescent Dipyrazole Linker with Dimetallic Clips American Chemical Society 2010 bpy PF phen macrocycle Fluorescent Dipyrazole Linker 1 H UV Dimetallic ClipsBy 13 C NMR diimine ligands M 8L 4L electrospray ionization mass spectrometry analysis 2010-09-06 00:00:00 Dataset https://acs.figshare.com/articles/dataset/Self_Assembly_and_Host_Guest_Interaction_of_Metallomacrocycles_Using_Fluorescent_Dipyrazole_Linker_with_Dimetallic_Clips/2734564 By employing diimine ligands coordinated dimetallic clips ([(bpy)<sub>2</sub>Pd<sub>2</sub>(NO<sub>3</sub>)<sub>2</sub>](NO<sub>3</sub>)<sub>2</sub> or [(phen)<sub>2</sub>Pd<sub>2</sub>(NO<sub>3</sub>)<sub>2</sub>](NO<sub>3</sub>)<sub>2</sub>, where bpy = 2,2′-bipyridine, phen = 1,10-phenanthroline) as the corner and anthracene-, naphthalene-, and benzene-based dipyrazolate dianions as the linker, a series of positively charged metallomacrocycles ([M<sub>4</sub>L<sub>2</sub>]<sup>4+</sup> or [M<sub>8</sub>L<sub>4</sub>]<sup>8+</sup>) have been synthesized through a directed self-assembly method in aqueous solution. Every macrocycle has a cavity to bind solvent molecules or anions. The structures were characterized by elemental analysis, <sup>1</sup>H and <sup>13</sup>C NMR, electrospray ionization mass spectrometry, and single crystal X-ray diffraction analysis for compound <b>1</b>·4PF<sub>6</sub>¯ (<b>1</b> = {[(bpy)Pd]<sub>4</sub>L<sup>1</sup><sub>2</sub>}<sup>4+</sup>), <b>3</b>·4PF<sub>6</sub>¯·8CH<sub>3</sub>CN·H<sub>2</sub>O (<b>3</b> = {[(bpy)Pd]<sub>4</sub>L<sup>2</sup><sub>2</sub>}<sup>4+</sup>), and <b>7</b>·4PF<sub>6</sub>¯·6H<sub>2</sub>O (<b>7</b> = {[(bpy)Pd]<sub>4</sub>L<sup>5</sup><sub>2</sub>}<sup>4+</sup>). The 1:1 host−guest complexation for anthracene-based dipyrazolate-bridged macrocycles with aromatic guests was investigated via UV−vis and fluorescent titration.