10.1021/acs.inorgchem.5b00176.s001 Verónica Cámara Verónica Cámara Natalia Barquero Natalia Barquero Delia Bautista Delia Bautista Juan Gil-Rubio Juan Gil-Rubio José Vicente José Vicente Assembly of Heterometallic Rigid-Rod Complexes and Coordination Oligomers from Gold(I) Metalloligands American Chemical Society 2015 BF NMR diffusion spectroscopy 3P coordination oligomers Zn MX ClO Fe PPN complex Co 2015-07-06 00:00:00 Journal contribution https://acs.figshare.com/articles/journal_contribution/Assembly_of_Heterometallic_Rigid_Rod_Complexes_and_Coordination_Oligomers_from_Gold_I_Metalloligands/2152432 The reactions of TpylC<sub>6</sub>­H<sub>4</sub>CCAuL (Tpyl = 2,2′:6′,2″-terpyridin-4′-yl; L = PPh<sub>3</sub>, CNXy; Xy = 2,6-dimethylphenyl) with MX<sub>2</sub>·<i>n</i>H<sub>2</sub>O (M = Fe, X = ClO<sub>4</sub>; M = Co, X = BF<sub>4</sub>; M = Zn, X = TfO, ClO<sub>4</sub>) in a 2:1 molar ratio give complexes [M­(Tpyl­C<sub>6</sub>H<sub>4</sub>­CC­AuL)<sub>2</sub>]­X<sub>2</sub>. Similarly, the reactions of PPN­[(TpylC<sub>6</sub>H<sub>4</sub>­CC)<sub>2</sub>Au] (PPN = (Ph<sub>3</sub>P)<sub>2</sub>N) with an equimolar amount of MX<sub>2</sub>·<i>n</i>H<sub>2</sub>O give coordination oligomers [M­{(TpylC<sub>6</sub>H<sub>4</sub>­CC)<sub>2</sub>­Au}]<sub><i>n</i></sub>X<sub><i>n</i></sub> (M = Fe, Zn, X = ClO<sub>4</sub>; M = Co, X = BF<sub>4</sub>). The complexes and oligomers have been isolated and characterized. The crystal structures of [Fe­(Tpyl­C<sub>6</sub>H<sub>4</sub>­CC­AuCNXy)<sub>2</sub>]­(ClO<sub>4</sub>)<sub>2</sub> and [Co­(Tpyl­C<sub>6</sub>H<sub>4</sub>­CC­AuPPh<sub>3</sub>)<sub>2</sub>]­(BF<sub>4</sub>)<sub>2</sub> have been determined by X-ray diffraction. The hydrodynamic sizes of complexes [M­(Tpyl­C<sub>6</sub>H<sub>4</sub>­CC­AuPPh<sub>3</sub>)<sub>2</sub>]­X<sub>2</sub> and coordination oligomers [M­{(Tpyl­C<sub>6</sub>H<sub>4</sub>­CC)<sub>2</sub>­Au}]<sub><i>n</i></sub>X<sub><i>n</i></sub> have been studied by NMR diffusion spectroscopy and dynamic light scattering measurements.