catena-Poly[[(2,9-dimethyl-1,10-phenanthroline-κ2 N,N′)lead(II)]-di-μ-2-hydroxy­benzoato-κ3 O 1,O 1′:O 2;κ3 O 2:O 1,O 1′]. Corrigendum

Corrigendum to Acta Cryst. (2007), E63, m2678

Di-μ-benzoato-κ3 O,O′:O;κ3 O:O,O′-bis­[(acetato-κO)(1,10-phenanthroline-κ2 N,N′)lead(II)] dihydrate

The title compound, [Pb2(CH3COO)2(C7H5O2)2(C12H8N2)2]·2H2O, consists of dimeric units built up around a crystallographic centre of symmetry and two non-coordinating water mol­ecules. Each PbII unit is six-coordinated by a bidentate 1,10-phenanthroline (phen) ligand, a monodentate acetate anion and a bidentate benzoate anion, which also acts as a bridge linking the two PbII atoms. The crystal packing is stabilized by O—H⋯O hydrogen bonds and by π–π inter­actions between the phen rings of neighboring mol­ecules, with a centroid–centroid distance of 3.577 (3) Å

Poly[bis­(μ3-acetato-κ4 O,O′:O:O′)bis­(μ2-acetato-κ3 O,O′:O)(μ2-2,5-dimethyl­benzene-1,4-diol-κ2 O:O′)dilead(II)]

The title compound, [Pb2(C2H3O2)4(C8H10O2)]n, has a polymeric structure, with acetatolead(II) chains and 2,5-dimethyl­benzene-1,4-diol mol­ecules forming bridges between two PbII ions from neighbouring chains. Each PbII centre is surrounded by eight O atoms; four belong to bidentate acetate ions, three to neighbouring bridging acetate groups and one to the 2,5-dimethyl­benzene-1,4-diol mol­ecule. The PbII ions are chelated symmetrically and asymmetrically by acetate ligands. The coordination environment of the PbII ion can be described as a hemidirected PbIIO6 core with the empty space around the metal ion filled by the stereochemically active 6s 2 electron pair and two longer Pb—O contacts. The Pb—O distances are in the range of 2.355 (3)–2.994 (3) Å. Additionally, the crystal structure is stabilized by O—H⋯O hydrogen bonds

catena-Poly[[[aqua­[(2-hydroxy­phen­yl)acetato-κ2 O,O′]lead(II)]-μ3-[(2-hydroxy­phen­yl)acetato-κ4 O:O,O′:O′]] monohydrate]

In the title complex, {[Pb(C8H7O3)2(H2O)]·H2O}n, the PbII atom is seven-coordinated by six carboxyl­ate O atoms from four different 2-hydroxy­phenyl­acetate (2-dph) ligands and one water mol­ecule, displaying a hemidirected irregular geometry, with the empty side of the metal ion capped by a benzene ring forming a Pb⋯π contact [Pb⋯centroid distance = 3.342 (2) Å]. One 2-dph ligand functions in a bridging mode and connects Pb ions into a linear chain. The crystal packing is governed by intra- and inter­molecular O—H⋯O hydrogen bonds

Bis(μ-3-hydroxy­benzoato-κ3 O,O′:O)bis­[aqua­(3-hydroxy­benzoato-κ2 O,O′)(1,10-phenanthroline-κ2 N,N′)lead(II)] monohydrate

In the centrosymmetric binuclear title complex, [Pb2(C7H5O3)4(C12H8N2)2(H2O)2]·H2O, each Pb atom is eight-coordinated in a PbO6N2 environment by two N atoms from the 1,10-phenanthroline (phen) ligand, five carboxylate O atoms from four 3-hydroxy­benzoate anions and one O atom from the coordinated water mol­ecule in a distorted bicapped trigonal-prismatic geometry. The benzoate groups coordinate each PbII atom in two different ways. Two benzoate ions behave as bidentate ligands to the Pb atom, and another benzoate ion bridges the Pb atoms, forming a binuclear structure. The dimeric units are packed via O—H⋯O hydrogen bonds and π–π inter­actions between the aromatic rings of neighboring mol­ecules, with centroid–centroid distances of 3.552 (2) and 3.641 (2) Å

Poly[ethyl­enediaminium [di-μ-aqua-(μ6-benzene-1,2,4,5-tetra­carboxyl­ato-κ10 O 1,O 1′:O 2,O 2′:O 2′:O 4,O 4′:O 5:O 5,O 5′)dithallium(I)]]

The title compound, {(C2H10N2)[Tl2(C10H2O8)(H2O)2)]}n, was prepared using (enH2)2(btc)·2H2O and thallium(I) nitrate (en = ethyl­enediamine and btcH4 = benzene-1,2,4,5-tetra­carboxylic acid). The enH2 cation and btc ligand are each located on an inversion centre. The TlI atom is seven-coordinated by three btc ligands and two water mol­ecules in an irregular geometry due to the stereochemically active lone pair on the Tl centre. The water mol­ecule and btc ligand are bonded to the Tl atoms in μ- and μ6-forms, respectively, leading to a three-dimensional structure. The crystal structure involves O—H⋯O, N—H⋯O and C—H⋯O hydrogen bonds, and also a Tl⋯π inter­action of 3.537 (1) Å

Macrocyclic receptor showing improved PbII/ZnII and PbII/CaII selectivities

[Abstract] Herein we report on the macrocyclic receptor N,N′‐bis[(6‐carboxy‐2‐pyridyl)methyl]‐1,10‐diaza‐15‐crown‐5 (H2bp15c5) and its coordination properties towards ZnII, CdII, PbII, and CaII. The stability constants of these complexes determined by pH‐potentiometric titration at 25 °C in 0.1 M KNO3 vary in the following order: PbII > CdII >> ZnII > CaII. As a result, bp15c5 presents very important PbII/ZnII and PbII/CaII selectivities. These results are in contrast to those reported for the related receptor derived from 1,7‐diaza‐12‐crown‐4, which provides very similar complex stabilities for ZnII and PbII. The X‐ray crystal structure of [Cd(Hbp15c5)]+ shows heptadentate binding of the ligand to the metal ion, with two oxygen atoms of the macrocyclic unit remaining uncoordinated. The 1H NMR spectra of the complexes formed with PbII, ZnII, and CaII (D2O) show very broad peaks in the region 2–5 ppm, indicating an important degree of flexibility of the crownmoiety in these complexes. On the contrary, the 1H and 13C NMR spectra recorded for the CdII complex are well resolved and could be fully assigned. A detailed conformational investigation using theoretical calculations performed at the DFT (B3LYP) level predict a minimum energy conformation for [Cd(bp15c5)] that is very similar to that observed in the solid state. Analogous calculations performed on the [M(bp15c5)] (M = Zn or Pb) systems predict hexadentate binding of the ligand to these metal ions. In the case of the PbII complex our calculations indicate that the 6s lone pair is stereochemically active, which results in a hemidirected coordination geometry around the metal ion. The minimum energy conformations calculated for the ZnII, CdII, and PbII complexes are compatible with the experimental NMR spectra obtained in D2O solution.Xunta de Galicia; PGIDIT06TAM10301PRXunta de Galicia; INCITE09E1R103013E