The third-generation bis(1-pyrazolyl)methane ligands p-C6H4[CH2OCH2CH(pz)(2)](2) (L-p, pz=pyrazolyl ring) and rn-C6H4[CH2OCH2CH(pz)(2)](2) (L-m) have been synthesized by the reaction of (pz)(2)CHCH2OH with NaH followed by alpha,alpha '-dibromo-p-xylene or alpha,alpha '-dibromo-m-xylene. The reaction of L-p with AgBF4, AgPF6, and AgO3SCF3 yields the new compounds {Ag[p-C6H4(CH2OCH2CH(pz)(2))(2)]}BF4, {Ag[p-C6H4(CH2OCH2CH(pz)(2))(2)]}PF6, and {Ag[p-C6H4(CH2OCH2CH(pz)(2))(2)]}O3SCF3, respectively. A similar reaction of L-m with AgBF4 and AgPF6 yields {Ag[m-C6H4(CH2OCH2CH(pz)(2))(2)]}BF4 and (Ag[m-C6H4(CH2OCH2CH(pz)(2))(2)]}PF6. These compounds were crystallized from both acetone and acetonitrile to yield nine crystalline forms of (LAg)(+) that differ in counterion and solvent of crystallization. In all complexes, the four pyrazolyl rings of the ligand chelate a single silver(I) cation in a distorted tetrahedral environment to form mononuclear metallacycles. This arrangement has not previously been observed with the analogous ligands based on tris(1-pyrazolyl)methane units and is unique because of the ring sizes (16-member rings in L-m and 17-member rings in L-p). The dominant feature in all of these solid state structures, regardless of solvent or anion, is this cationic metallacyclic architecture, which does not readily lend itself to strong supramolecular organization.