The title compound, lead trimanganese tris(orthophosphate), has been synthesized by hydro-thermal methods. In this structure, only two O atoms are in general positions and all others atoms are in the special positions of the Imma space group. Indeed, the atoms in the Wyckoff positions are namely: Pb1 and P1 on 4e (mm2); Mn1 on 4b (2/m); Mn2 and P2 on 8g (2); O1 on 8h (m); O2 on 8i (m). The crystal structure can be viewed as a three-dimensional network of corner- and edge-sharing PO4 tetra-hedra and MnO6 octa-hedra, building two types of chains running along the b axis. The first is an infinite linear chain, formed by alternating Mn(III)O6 octa-hedra and PO4 tetra-hedra which share one vertex. The second chain is built up from two adjacent edge-sharing octa-hedra (Mn(II) 2O10 dimers) whose ends are linked to two PO4 tetra-hedra by a common edge. These chains are linked together by common vertices of polyhedra in such a way as to form porous layers parallel to (001). These sheets are bonded by the first linear chains, leading to the appearance of two types of tunnels, one propagating along the a axis and the other along b. The Pb(II) ions are located within the inter-sections of the tunnels with eight neighbouring O atoms in form of a trigonal prism that is capped by two O atoms on one side. The three-dimensional framework of this structure is compared with similar phosphates such as Ag2Co3(HPO4)(PO4)2 and Ag2Ni3(HPO4)(PO4)2.
The title compound, lead trimanganese tris(orthophosphate), has been synthesized by hydro-thermal methods. In this structure, only two O atoms are in general positions and all others atoms are in the special positions of the Imma space group. Indeed, the atoms in the Wyckoff positions are namely: Pb1 and P1 on 4e (mm2); Mn1 on 4b (2/m); Mn2 and P2 on 8g (2); O1 on 8h (m); O2 on 8i (m). The crystal structure can be viewed as a three-dimensional network of corner- and edge-sharing PO4tetra-hedra and MnO6 octa-hedra, building two types of chains running along the b axis. The first is an infinite linear chain, formed by alternating Mn(III)O6 octa-hedra and PO4tetra-hedra which share one vertex. The second chain is built up from two adjacent edge-sharing octa-hedra (Mn(II) 2O10 dimers) whose ends are linked to two PO4tetra-hedra by a common edge. These chains are linked together by common vertices of polyhedra in such a way as to form porous layers parallel to (001). These sheets are bonded by the first linear chains, leading to the appearance of two types of tunnels, one propagating along the a axis and the other along b. The Pb(II) ions are located within the inter-sections of the tunnels with eight neighbouring O atoms in form of a trigonal prism that is capped by two O atoms on one side. The three-dimensional framework of this structure is compared with similar phosphates such as Ag2Co3(HPO4)(PO4)2 and Ag2Ni3(HPO4)(PO4)2.
For compounds with related structures see: Assani et al. (2011a
▶,b
▶,c
▶); Moore & Ito (1979 ▶). For applications of related compounds, see: Trad et al. (2010 ▶). For compounds with mixed-valence manganese(II/III) lead(II) triphosphates(V), see: Adam et al. (2009 ▶). For bond-valence analysis, see: Brown & Altermatt (1985 ▶).
Bruker X8 APEX diffractometerAbsorption correction: multi-scan (SADABS; Bruker, 2009 ▶) T
min = 0.046, T
max = 0.2154704 measured reflections787 independent reflections771 reflections with I > 2σ(I)R
int = 0.028
Refinement
R[F
2 > 2σ(F
2)] = 0.016wR(F
2) = 0.040S = 1.11787 reflections53 parametersΔρmax = 2.54 e Å−3Δρmin = −0.98 e Å−3Data collection: APEX2 (Bruker, 2009 ▶); cell refinement: SAINT (Bruker, 2009 ▶); data reduction: SAINT; program(s) used to solve structure: SHELXS97 (Sheldrick, 2008 ▶); program(s) used to refine structure: SHELXL97 (Sheldrick, 2008 ▶); molecular graphics: ORTEP-3 for Windows (Farrugia, 2012 ▶) and DIAMOND (Brandenburg, 2006 ▶); software used to prepare material for publication: publCIF (Westrip, 2010 ▶).Crystal structure: contains datablock(s) I, global. DOI: 10.1107/S1600536813016504/br2227sup1.cifStructure factors: contains datablock(s) I. DOI: 10.1107/S1600536813016504/br2227Isup2.hklAdditional supplementary materials: crystallographic information; 3D view; checkCIF report
Primary atom site location: structure-invariant direct methods
R[F2 > 2σ(F2)] = 0.016
Secondary atom site location: difference Fourier map
wR(F2) = 0.040
w = 1/[σ2(Fo2) + (0.0205P)2 + 2.635P] where P = (Fo2 + 2Fc2)/3
S = 1.11
(Δ/σ)max < 0.001
787 reflections
Δρmax = 2.54 e Å−3
53 parameters
Δρmin = −0.98 e Å−3
Geometry. All s.u.'s (except the s.u. in the dihedral angle between two l.s. planes) are
estimated using the full covariance matrix. The cell s.u.'s are taken into
account individually in the estimation of s.u.'s in distances, angles and
torsion angles; correlations between s.u.'s in cell parameters are only used
when they are defined by crystal symmetry. An approximate (isotropic)
treatment of cell s.u.'s is used for estimating s.u.'s involving l.s. planes.
Refinement. Refinement of F2 against all reflections. The weighted R-factor
wR and goodness of fit S are based on F2, conventional
R-factors R are based on F, with F set to zero for
negative F2. The threshold expression of F2 >
2σ(F2) is used only for calculating R-factors(gt) etc.
and is not relevant to the choice of reflections for refinement.
R-factors based on F2 are statistically about twice as large
as those based on F, and R- factors based on all data will be
even larger.
Authors: Adam Bouraima; Thomas Makani; Abderrazzak Assani; Mohamed Saadi; Lahcen El Ammari Journal: Acta Crystallogr E Crystallogr Commun Date: 2016-07-19