3-Methyl-5-methyl-sulfanyl-1,3,4-thia-diazole-2(3H)-thione.

The title compound, C(4)H(6)N(2)S(3), has two very similar mol-ecules per asymmetric unit. The nine non-H atoms in each mol-ecule are coplanar, both having comparable r.m.

Bis(2,S-dimethyl-dithio-carbazate-κ(2)N(3),S)(nitrato-κO)copper(II) nitrate.

The title complex, [Cu(NO(3))(C(3)H(8)N(2)S(2))(2)]NO(3), represents a low-symmetry polymorph (P-1, Z = 4) of a previously reported form [P-1, Z = 2; Ali et al. (2011 ▶). Polyhedron, 30, 542-548].

Benzyl 2-methyl-3-[(E)-(thio-phen-2-yl)methyl-idene]dithio-carbazate.

In the title compound, C(14)H(14)N(2)S(3), the thione S atom and methyl group are syn, as are the two thio-ether S atoms. The mol-ecule is twisted, the dihedral angles between the central (C(2)N(2)S(2)) residue and the pendent 2-thienyl and phenyl rings being 21.57 (6) and 77.

5,7,7,12,14,14-Hexamethyl-4,11-diaza-1,8-diazo-niacyclo-tetra-decane bis-(perchlorate) monohydrate.

In the title hydrated salt, C(16)H(38)N(4) (2+)·2ClO(4) (-)·H(2)O, the dication is protonated at the diagonally opposite N atoms proximate to the -C(CH(3))(2)- groups. Within the cavity, there are two ammonium-amine N-H⋯N hydrogen bonds. Supra-molecular layers are formed in the crystal packing whereby the water mol-ecule links two perchlorate anions, and the resultant aggregates are connected to the dications via N-H⋯O hydrogen bonds.

cis-(Nitrato-κ(2)O,O')(2,5,5,7,9,12,12,14-octa-methyl-1,4,8,11-tetra-aza-cyclo-tetra-decane-κ(4)N,N',N'',N''')cadmium nitrate hemihydrate.

The Cd(II) atom in the title complex, [Cd(NO(3))(C(18)H(40)N(4))]NO(3)·0.5H(2)O, is coordinated within a cis-N(4)O(2) donor set provided by the tetra-dentate macrocyclic ligand and two O atoms of a nitrate anion; the coordination geometry is distorted octa-hedral. The lattice water mol-ecule is located on a twofold rotation axis.

[(4E,11E)-5,7,12,14-Tetra-benzyl-7,14-dimethyl-1,4,8,11-tetra-aza-cyclo-tetra-deca-4,11-diene]copper(II) bis(per-chlorate).

The complete cation in the title compound, [Cu(C(40)H(48)N(4))](ClO(4))(2), is generated by the operation of a crystallographic centre of inversion. The Cu(II) ion exists in a tetra-gonally distorted trans-N(4)O(2) coordination geometry defined by the four N atoms of the macrocyclic ligand and two weakly bound perchlorate-O atoms from two anions. The N-H atoms form intra-molecular N-H⋯O(perchlorate) hydrogen bonds.

Dichlorido[(4E,11E)-5,7,12,14-tetra-benzyl-7,14-dimethyl-1,4,8,11-tetra-aza-cyclo-tetra-deca-4,11-diene]cobalt(III) perchlorate.

The Co(III) atom in the title complex, [CoCl(2)(C(40)H(48)N(4))]ClO(4), is octa-hedrally coordinated within a trans-Cl(2)N(4) donor set provided by the tetra-dentate macrocylic ligand and two chloride ions. The N-H atoms, which are orientated to one side of the N(4) plane, form hydrogen bonds with chloride ions and perchlorate-O atoms. These along with C-H⋯O inter-actions consolidate the three-dimensional crystal structure.

(Acetato-κO)(2,5,5,7,9,12,12,14-octa-methyl-1,4,8,11-tetra-aza-cyclo-tetra-decane-κN,N',N'',N''')zinc perchlorate.

The Zn(II) atom in the cation of the title salt, [Zn(C(2)H(3)O(2))(C(18)H(40)N(4))]ClO(4), is five-coordinated by the four N atoms of the macrocycle and the O atom of the monodentate acetate ligand. The N(4)O donor set is based on a trigonal bipyramid with two N atoms occupying axial positions [N-Zn-N = 170.89 (16)°].

3,10-C-meso-3,5,7,7,10,12,14,14-Octa-methyl-4,11-diaza-1,8-diazo-niacyclo-tetra-decane bis-(perchlorate).

The structure determination of the title salt, C(18)H(42)N(4) (2+)·2ClO(4) (-), reveals that protonation has occurred at diagonally opposite amine N atoms. Intra-molecular N-H⋯N hydrogen bonds stabilize the conformation of the dication. In the crystal, the dications are bridged by perchlorate ions via N-H⋯O hydrogen bonds into supra-molecular chains propagating along the c axis and weak C-H⋯O inter-actions cross-link the chains.

Synthesis and antimicrobial activities of isomers of N(4),N(11)-dimethyl-3,5,7,7,10,12,14,14-octamethyl-1,4,8,11-tetraazacyclotetradecane and their nickel(II) complexes.

The reactions of two isomers of 3,5,7,7,10,12,14,14-octamethyl-1,4,8,11-tetraazacyclotetradecane (differing in the orientation of the methyl groups on the chiral carbon atoms), designated as L(B) and L(C), with CH(3)I in the ratio of 1:4 resulted in the substitution of the N(4) and N(11) protons by CH(3) groups, forming the dimethyl derivatives L(BZ) and L(CZ), respectively. These ligands, on interaction with nickel(II) acetate tetrahydrate and subsequent addition of lithium perchlorate, produce square-planar yellow [NiL(BZ)][ClO(4)](2) and orange [NiL(C'Z)][ClO(4)](2). These nickel complexes undergo axial ligand addition reactions with NCS(-), Cl(-), Br(-), and I(-) as X(-) to form six-coordinate trans-diisothiocyanato, -dichloro, -dibromo, and -diiodo complexes of formula [NiLX(2)], where L = L(BZ) or L(C'Z), and X = SCN, Cl, Br, or I.