Four-component intergrowth structures of the metal-ion cage complexes fac-(1,5,9,13,20-pentamethyl-3,7,11,15,18,22-hexaazabicyclo
The crystal structures of (1,5,9,13,20-pentamethyl-3,7,11,15,18,22-hexaazabicyclo[7.7.7]tricosane-kappa(6)N,N',N",N"',N"",N""')nickel(II) diperchlorate-x(water) (x = 0.530), [Ni(C(22)H(48)N(6))](ClO(4))(2).0.530H(2)O, and (1,5,9,13,20-pentamethyl-3,7,11,15,18,22-hexaazabicyclo[7.7.7]tricosane-kappa(6)N,N',N",N"',N"",N""')zinc(II) diperchlorate-x(water) (x = 0.608), [Zn(C(22)H(48)N(6))](ClO(4))(2).0.608H(2)O, are isomorphic and each is described as an intergrowth of four substructures, consistent with different modulations of an idealized parent structure of space group C2/c. Two substructures correspond to alternative orientations of a C1; structure for which x = 0 in the general formula [M(C(22)H(48)N(6))](ClO(4))(2).xH(2)O, and two substructures correspond to alternative origins of a P2(1)/n structure for which x = 1. Twinning also occurs. An analysis of the pseudosymmetry, a description of the refinement and a description of the refined structures are presented. The MN(6) coordination geometry is essentially octahedral, in contrast to the trigonal-prismatic geometry observed for the Cd(II) and Hg(II) complexes of the same ligand.
Haller
KJ
School of Chemistry, Suranaree University of Technology, Nakhon Ratchasima 30000, Thailand.
Rae
AD
Bygott
AM
Hockless
DC
Ralph
SF
Geue
RJ
Sargeson
AM