The synthesis and characterization are described of transition metal coordination with the novel pentadentate ligand 1,9-bis(3,5-dimethyl-1-pyrazolyl)-3,7-dithia-5-nonanol (Hbdnol). Most of the compounds are of the general formula [M(2)(bdnol)X(3)]. n(solvent) with M = Co2+, Ni2+, CU2+, Zn2+ and Cd2+ and X(-) = Cl-. Br-, NO3-, and NCS-, Additionally, a polymeric copper(I) compound of the formula [Cu2H(bdnol)(NCS)(2)] and an unusual trinuclear nickel compound of the formula [Ni-3(bdnol)Cl-5(EtOH)]. 3EtOH are described. Hbdnol acts as a pentadentate ligand in all compounds; the alcohol group is generally dehydronated and bridging between the metal ions, except in the case of the Copper(I) compound, where the alcohol group is noncoordinating. Single crystals of [Co-2(bdnol)(NCS)(3)]. MeCN (A), [Zn-2(bdnol)Cl(NCS)(2)]. 1/2MeCN (B), [Cu-2(bdnol)(NO3)(3)] (C), and [Cu-2(Hbdnol)(NCS)(2)] (D) were used for X-ray structure determinations, [Co-2(bdnol)(NCS)(3)]. MeCN orthorhombic, space group Pnma, a = 17.7487(7) Angstrom, b = 20.095(2) Angstrom, c = 8.569(2) Angstrom, Z = 4, and T = 150 K : R(F) = 0.060, wR2 = 0.108 for 3606 reflections, [Zn-2(bdnol)Cl(NCS)(2)]. 1/2MeCN : monoclinic, space group P2(1), a = 8.7369(7) Angstrom, b = 16.416(1) Angstrom, c = 11.222(1) Angstrom, beta = 108.84(1)degrees, Z = 2, and T = 293 K; R(F) = 0.051, R(W) = 0.062 for 2983 reflections. [Cu-2(bdnol)(NO3)(3)] : triclinic, space group P-1. a = 8.012(4) Angstrom, b = 12.430(6), Angstrom, c = 13.702(16) Angstrom, alpha = 95.61(7)degrees, beta = 102.34(5), gamma = 97.46(5)degrees, Z = 2, and T = 293 K : R(F) = 0.042, R(W) = 0.041 for 3805 reflections. [Cu-2(Hbdnol)(NCS)(2)] : triclinic space group P-1 a = 9.241(4) Angstrom, b = 10.32(2) Angstrom, c = 15.27(1) Angstrom, alpha = 103.1(1)degrees, beta = 98.92(8)degrees, gamma = 113.85(5)degrees Z = 2, and T = 293 K; R(F) = 0.050, R(W) = 0.052 for 2999 reflections.