The complexes of 2, 11-dithia-4,5,6,7,8,9-hexahydro[3.3]paracyclophane (dthhpcp) with Cu(I), i.e. [Cu 2 I 2 (dthhpcp) 2 ]×2H 2 O 1, or with Ag(I), i.e. [Ag(dthhpcp)(NO 3 )]×thf 2 and [Ag(dthpcp)(CF 3 COO)] 3, were prepared for structural study by single-crystal X-ray diffraction analysis. For these three complexes, dthhpcp serves as a bridging group in the polymeric structure through bridging sulfur atoms via metal, while the bonding of anion with the second metal atom forms the multi-diminished structures. Complex 1 is a novel two-dimensional coordination polymer composed of Cu 6 motifs, in which Cu 2 I 2 formed a square planar unit to link the dthhpcp molecule. The two oxygen atoms of the nitrate anion as a bridge for two Ag atoms in complex 2 provides a three-dimensional channel framework of silver(I) with a tetrahydrofuran molecule as a guest inside the open cavities. In contrast, the analogous reaction with silver triflouroacetate gave a complex 3, which is composed of infinite linear chains of -Ag-dthhpcp-Ag-dthhpcp-along the a axis. Unit cell data: complex 1, orthorhombic system, space group P2 (1)2(1)2(1), a = 19.2982(11) Å b = 16.5661(10) Å, c = 25.3006(15) Å, b = 90°, Z = 8; complex 2, orthorhombic system, space group Pna2(1), a = 8.8595(6) Å, b = 12.6901(9) Å, c = 19.8449(14) Å, b = 90°, Z = 4; complex 3, monoclinic system, space group P2(1)/n, a = 8.845(3) Å, b = 20.841(6) Å, c = 11.061(3) Å, b = 107.832(6)°, Z = 4.
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