Poly[[[μ-1,4-bis(pyridin-4-ylmethyl)piperazine][μ-4-(2-carboxylatoethyl)benzoato]copper(II)] monohydrate], a coordination polymer with twofold interpenetrated cds topology networks

A divalent copper tri-periodic coordination polymer with twofold interpenetrating 658 cds topology, {[Cu(ceb)(bpmp)]·H2O] n , was structurally characterized by single-crystal X-ray diffraction.

The asymmetric unit of the title compound contains a Cu II atom disordered over two positions, a fully deprotonated ceb ligand whose carboxylatoethyl group is disordered over two sets of sites, a bpmp ligand, and two disordered water molecules of crystallization.All disordered parts in the crystal structure are present in a refined ratio of 0.655 (6):0.345(6).The Cu II atom is coordinated in an {N 2 O 2 } square-planar fashion by two trans-oriented pyridyl N-atom donors from two bpmp ligands, and two trans-oriented carboxylate O-atom donors from two ceb ligands (Fig. 1).Pertinent bond length and angle information for the coordination sphere is listed in Table 1.

Figure 5
Twofold interpenetration of cds topology networks in the title compound.
The Cu atoms are depicted as 4-connected nodes.The rods represent through-ligand contacts between Cu atom nodes.Symmetry codes are as listed in Table 1.

Refinement
Crystal data, data collection and structure refinement details are summarized in Table 2.All H atoms attached to C were placed in calculated positions and refined with a riding model.The H atoms of the disordered water molecules of crystallization could not be found from difference-Fourier maps, and attempts to use calculated positions did not give chemically reasonable interactions.Disorder of the Cu II atoms, water molecules of crystallization and ceb ligands was found and refined in a 0.655 (6):0.345( 6) ratio for all disorder components.EADP commands were used to restrain the atomic displacement parameters for the disordered components.Without these restraints, substantial numbers of non-positive definite ADPs occurred.In addition, DFIX commands were used to restrain bond lengths within the disordered parts of the ceb ligands.Otherwise, unreasonable bond lengths were occurring.Computer programs: COSMO (Bruker, 2009), SAINT (Bruker, 2014), SHELXT (Sheldrick, 2015a), SHELXL (Sheldrick, 2015b), CrystalMaker X (Palmer, 2020), and OLEX2 (Dolomanov et al., 2009).Crystal data

Special details
Experimental.Data was collected using a BRUKER CCD (charge coupled device) based diffractometer equipped with an Oxford low-temperature apparatus operating at 173 K.A suitable crystal was chosen and mounted on a nylon loop using Paratone oil.Data were measured using omega scans of 0.5° per frame for 30 s.The total number of images were based on results from the program COSMO where redundancy was expected to be 4 and completeness to 0.83Å to 100%.Cell parameters were retrieved using APEX II software and refined using SAINT on all observed reflections.Data reduction was performed using the SAINT software which corrects for Lp.Scaling and absorption corrections were applied using SADABS6 multi-scan technique, supplied by George Sheldrick.The structure was solved by the direct method using the SHELXT program and refined by least squares method on F2, SHELXL, incorporated in OLEX2.Geometry.All esds (except the esd in the dihedral angle between two l.s.planes) are estimated using the full covariance matrix.The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry.An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s.planes.Refinement.The structure was refined by Least Squares using version 2018/3 of XL (Sheldrick, 2015) incorporated in Olex2 (Dolomanov et al., 2009).All non-hydrogen atoms were refined anisotropically.Hydrogen atom positions were calculated geometrically and refined using the riding model, except for the Hydrogen atom on the nitrogen atom which was found by difference Fourier methods and refined isotropically.

Figure 3 A
Figure 3 A [Cu(ceb)(bpmp)] n cds coordination polymer network in the title compound.The [Cu(ceb)] n coordination polymer chains are depicted in red.

Figure 1
Figure 1 Copper coordination environment in the title compound with full ceb and bpmp ligands.Displacement ellipsoids are drawn at the 50% probability level.Color code: Cu, dark blue; O, red; N, light blue; C, black.The minor disorder components are shown in teal.H-atom positions are shown as sticks.Symmetry codes are as listed inTable 1.

Figure 4
Figure 4 Twofold interpenetration of [Cu(ceb)(bpmp)] n tri-periodic coordination polymer networks in the title compound.Each network is shown in a different color.Unit-cell outlines are shown.

Table 2
Experimental details.