Fmoc-L-Phg(4-Br)-OH

The crystal structure of the new double CuII complex salt, [Cu(L)(H2O)2][Cu(L)]Br4·2H2O (L = 3,14-diethyl-2,6,13,17-tetra-aza-tri-cyclo-[16.4.0.07,12]docosane, C22H44N4) has been determined using synchrotron radiation. The asymmetric unit contains one half of a [Cu(L)(H2O)2]2+ cation, one half of a [Cu(L)]2+ cation (both completed by crystallographic inversion symmetry), two bromide anions and one water solvent mol-ecule. The CuII atom in the first complex exists in a tetra-gonally distorted octa-hedral environment with the four N atoms of the macrocyclic ligand in equatorial and two aqua ligands in axial positions, whereas the CuII atom in the second complex exists in a square-planar environment defined by the four nitro-gen atoms of the macrocyclic ligand. The two macrocyclic rings adopt the most stable trans-III configuration with normal Cu-N bond lengths from 2.016 (3) to 2.055 (3) Å and an axial Cu-O bond length of 2.658 (4) Å. The crystal structure is stabilized by inter-molecular hydrogen bonds involving the macrocycle N-H or C-H groups and the O-H groups of water mol-ecules as donor groups, and the O atoms of water mol-ecules and bromide anions as acceptor groups, giving rise to a one-dimensional network extending parallel to [100].

In the centrosymmetric title compound, [Sn(4)Br(2)(C(6)H(5))(8)O(2)(OH)(2)], the four tin(IV) atoms are bridged by the hydroxo and oxo ligands, forming a ladder-like array of three edge-connected Sn(2)O(2) squares. The two independent tin atoms show distorted trigonal-bipyramidal SnC(2)O(3) and SnC(2)O(2)Br coordination geometries.

A new thulium(III)-copper(I) heterometallic coordination polymer, [Cu(4)Tm(2)Br(3)(C(6)H(4)NO(2))(6)(OH)(H(2)O)(4)](n), has been prepared by a hydro-thermal method. The Tm and both Cu atoms lie on mirror planes. The Tm atom is seven-coordinate with a capped distorted trigonal-prismatic coordination geometry, while the Cu atoms adopt trigonal CuBrN(2) and tetra-hedral CuBr(3)N coordination modes, respectively. The Cu atom in the trigonal coordination environment is disordered over two sites of equal occupancy. The crystal structure is constructed from two distinct units of dimeric [Tm(2)(μ(2)-OH(IN)(6)(H(2)O)(4)] cores (IN = isonicotinate) and one-dimensional inorganic [Cu(4)Br(3)](n) chains, which are linked together, forming heterometallic Cu-halide-lanthanide-organic layers.