Decaaqua­dioxidobis[μ3-N-(phospho­n­atometh­yl)imino­diacetato]­dizinc(II)­divanadium(IV) dihydrate

The title compound, [Zn2V2(C5H6NO7P)2O2(H2O)10]·2H2O, contains a [V2O2(pmida)2]4− dimeric anionic unit [where H4pmida is N-(phosphono­meth­yl)imino­diacetic acid] lying on a centre of symmetry which is exo-coordinated via the two deprotonated phospho­nate groups to two Zn2+ cations, with the coordination environment of Zn completed by five water mol­ecules. The crystal packing is mediated by an extensive network of strong and highly directional O—H⋯O hydrogen bonds involving the water mol­ecules (coordinated and uncoordinated) and the functional groups of pmida4−, leading to a three-dimensional supra­molecular network

catena-[1,3-diammoniopropane di-mu2-hydroxodi-mu4-phosphato-trioxotrivanadium dihydrate]: a redetermination at 180 (2) K

The crystal structure of the title compound, (C3H12N2)- [V3O3(OH)2(PO4)2] 2H2O, has been reported by Soghomonian et al. [Chem. Mater. (1993), 5, 1690±1691]. We present here a redetermination of greatly improved precision and at a low temperature of 180 (2) K. The H atoms connected to oxygen have been successfully located and the coordination environments of the two crystallographically independent vanadium centres have been properly elucidated. Large channels, running along the a direction, contain water molecules and 1,3-diammoniopropane cations that are strongly hydrogen bonded to the anionic framework through N+ÐH O and OÐH O interactions. One vanadyl (V O) bond and the central ±CH2± group of 1,3-diammoniopropane are located on a mirror plane

Heterodimetallic germanium(IV) complex structures with transition metals

The hydrothermal synthesis and structural characterization of a number of complex compounds containing the divalent tris(oxalato-O,O¢)germanate anion, [Ge(C2O4)3]2-, or the neutral bis(oxalate-O,O¢)germanium fragment, [Ge(C2O4)2], with transition-metal (M) cationic complexes of 1,10¢-phenanthroline (phen) is reported: [M(phen)3]- [Ge(C2O4)3]âxH2O [where M2+ ) Cu2+ (1a and 1b), Fe2+ (2a and 2b), Ni2+ (3), Co2+ (4); x ) 0.2 for 2b], [MGe- (phen)2(í2-OH)2(C2O4)2] [where M2+ ) Cd2+ (5) and Cu2+ (6)]. The isolation of two polymorphs with Cu2+ (1a and 1b) and other pseudo-polymorphs for Fe2+ (2a and 2b) was rationalized based on slightly different molar ratios for the starting materials. All compounds have been characterized using EDS, SEM, vibrational spectroscopy (FT-IR and FT-Raman), thermogravimetry, and CHN elemental composition and their structure determined on the basis of single-crystal X-ray diffraction studies. The crystal packing of the different chemical moieties for each series of compounds was discussed on the basis of the various intermolecular interactions present (strong C-Hâââð and weak C-HâââO hydrogen-bonding interactions, C-Hâââð and ð-ð contacts).FCT - SFRH/BPD/9309/2002FCT - SFRH/BPD/14410/2003FEDERPOCI - 201

Transposition of chirality from diphosphonate metal-organic framework precursors onto porous lanthanide pyrophosphates

Chiral porous inorganic materials, lanthanide pyrophosphates, were prepared from chiral porous metal-organic framework precursors, which upon thermal decomposition transpose their chirality and porosity onto the inorganic framework. It is argued that this synthesis concept may be extended to other chiral porous inorganic solids

Synthesis and characterisation of the first three-dimensional mixed-metal-center inorganic-organic hybrid framework with N-(phosphonomethyl)iminodiacetate

Using crystal engineering concepts, the first three-dimensional (3D) mixed-metal-centre inorganic-organic hybrid frameworks incorporating N-(phosphonomethyl)iminodiacetate (pmida4−) were synthesised under mild hydrothermal conditions (100 °C) and characterised structurally. The crystal structures, obtained by the displacement of the coordinated water molecules in [Co2V2O2(pmida)2(H2O)10]·2(H2O) (1) [P21/c monoclinic space group, Z = 2, a = 9.996(2)A° , b = 14.854(3)A° , c = 10.781(2)A° , β = 110.90(3)° and V = 1495.5(5)A° 3] by the rod-like bridging 4,4 -bipyridine (4,4 - bpy) ligand — [CdVO(pmida)(4,4 -bpy)(H2O)2]·(4,4 - bpy)0.5·H2O (2) and [CoVO(pmida)(4,4 -bpy)(H2O)2]·(4,4 - bpy)0.5 (3) — are isostructural and were also determined in the P21/c monoclinic space group (Z = 4) by single-crystal Xray diffraction studies at low temperature (180 K): for 2, a = 9.1267(18)A° , b = 17.610(4)A° , c = 15.361(3)A° , β = 93.06(3)° and V = 2465.3(9)A° 3; for 3, a = 8.7734(18)A° , b = 17.264(4)A° , c = 15.507(3)A° , β = 93.94(3)° and V = 2343.2(8)A° 3. All the crystal structures contain centrosymmetric dimeric [V2O2(pmida)2]4− units connected to neighbouring M2+ cations (Cd2+ for 2, and Co2+ for 1 and 3) through the phosphonate group. In 2 and 3, extended two-dimensional [MVO(pmida)( H2O)2]n layers are formed, with the 4,4 -bpy molecules acting as pillars between adjacent layers, leading to porous 3D supramolecular structures, [MVO(pmida)(4,4 - bpy)(H2O)2] , with a topology resembling that of the NbO net

Optimised hydrothermal synthesis of multi-dimensional hybrid coordination polymers containing flexible organic ligands

In this paper, we summarise our recent research interest in the hydrothermal synthesis and structural characterisation of multi-dimensional coordination polymers. The use of N-(phosphonomethyl)iminodiacetic acid (also referred to as H4pmida) in the literature as a versatile chelating organic ligand is briefly reviewed. This molecule plays an important role in the formation of centrosymmetric dimeric [V2O2(pmida)2]4 anionic units, which were first used by us as building blocks to construct novel coordination polymers. Starting with [V2O2(pmida)2]4 in solution, we have isolated [M2V2O2(pmida)2 (H2O)10] species (where M2þ ¼ Mn2þ, Co2þ or Cd2þ) via the hydrothermal synthetic approach, which were then employed for the construction of [CdVO(pmida)(4,4#-bpy)(H2O)2](4,4#-bpy)0.5(H2O), [CoVO(pmida)(4,4#-bpy)(H2O)2](4,4#-bpy)0.5, [Co(H2O)6][CoV2O2(pmida)2(pyr)(H2O)2]2(H2O) and [Cd2V2O2(pmida)2(pyr)2(H2O)4]$4(H2O) by the inclusion of bridging organic ligands in the reactive mixtures, such as pyrazine (pyr) and 4,4#-bipyridine (4,4#-bpy). These materials can contain channel systems, and exhibit magnetic behaviour, not only due to the V4þ centres but also to the transition metal centres which establish the links between neighbouring dimeric [V2O2(pmida)2]4 anionic units. A closely related anionic moiety, [Ge2(pmida)2(OH)2]2 , was engineered to allow the study of such crystalline hybrid materials using one- and two-dimensional high-resolution solid-state NMR

Hydrothermal synthesis and structural characterisation of a Ge-pmida binuclear complex: X-Ray diffraction and HETCOR MAS NMR with FS-LG decoupling

International audienc

A novel germanium(IV) oxalate complex: [Ge(OH)2(C2O4)2]2−

Two crystalline compounds, X [Ge(OH)2(C2O4)2] n(H2O) [where X ¼ C4H12N2þ 2 ðH2pipz2þÞ and n = 1 for compound I, and X ¼ C10H10N2þ 2 ðH2bipy2þÞ and n = 2 for II], were synthesised using hydrothermal synthetic approach and characterised structurally using single-crystal X-ray diffraction, vibrational spectroscopy (FT-IR and FT-Raman), thermogravimetric analysis (TGA) and CHN elemental composition. The crystalline compounds contain a novel anionic complex [Ge(OH)2(C2O4)2]2 , which co-crystallises with organic cations (piperazinium in I, and 4,40-bipyridinium in II) and water molecules of crystallisation. These chemical moieties are involved in extensive three-dimensional (3D) hydrogen bonding networks composed of strong and highly directional O–H O and N–H O interactions.FCT, MCTES - POCI-PPCDT/QUI/58377/2004FCT, MCTES - SFRH/BPD/ 14410/2003FCT, MCTES - SFRH/BPD/9309/200

Supramolecular salts containing the anionic [Ge(C(2)O(4))(3)](2-) complex and heteroaromatic amines

The crystalline compounds (Hbipy)2[Ge(C2O4)3] (1) and (Hphen)2[Ge(C2O4)3] 2(H2O) (2) [Hbipy+ is the 2,20-bipyridinium cation (C10H9N2), and Hphen+ is the 1,100-phenathrolinium cation (C12H9N2)] were isolated from mild hydrothermal syntheses and their structures were elucidated from single-crystal X-ray diffraction. The two compounds were further characterised by vibrational spectroscopy (FT-IR and FT-Raman), thermogravimetric analysis (TGA) and CHN elemental composition. Compounds 1 and 2 comprise the tris(oxalato-O,O0)germanate dianion complex, [Ge(C2O4)3]2 , which co-crystallises with Hbipy+ (in 1), or Hphen+ and water molecules (in 2). In 1, the germanium oxalate anionic complex, [Ge(C2O4)3]2 , and the Hbipy+ organic residues interact mutually via N–H O hydrogen bonding interactions, leading to supramolecular discrete hydrogen-bonded units which are further interconnected via p–p stacking. Compound 2, on the other hand, exhibits a more complex hydrogen bonding network due to the presence of the water molecules of crystallisation which, along with p–p stacking between neighbouring Hphen+ residues, mediate the crystal packing