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inorganic compounds\(\def\hfill{\hskip 5em}\def\hfil{\hskip 3em}\def\eqno#1{\hfil {#1}}\)

Journal logoCRYSTALLOGRAPHIC
COMMUNICATIONS
ISSN: 2056-9890
Volume 68| Part 8| August 2012| Page i66
https://doi.org/10.1107/S1600536812033259

Dilead(II) trimanganese(II) bis­(hydrogenphosphate) bis­(phosphate)

Abderrazzak Assani,a Mohamed Saadi,a Mohammed Zriouila* and Lahcen El Ammaria

aLaboratoire de Chimie du Solide Appliquée, Faculté des Sciences, Université Mohammed V-Agdal, Avenue Ibn Battouta, BP 1014, Rabat, Morocco
*Correspondence e-mail: m_zriouil@yahoo.fr

(Received 19 June 2012; accepted 23 July 2012; online 28 July 2012)

The title compound, Pb2Mn3(HPO4)2(PO4)2, was synthesized by a hydro­thermal method. All atoms are in general positions except for one Mn atom which is located on an inversion center. The framework of the structure is built up from PO4 tetra­hedra and two types of MnO6 octa­hedra, one almost ideal and the other very distorted with one very long Mn—O bond [2.610 (4) Å compared an average of 2.161 Å for the other bonds]. The centrosymetric octa­hedron is linked to two distorted MnO6 octa­hedra by an edge common, forming infinite zigzag Mn3O14 chains running along the b axis. Adjacent chains are linked by PO4 and PO3(OH) tetra­hedra through vertices or by edge sharing, forming sheets perpendicular to [100]. The Pb2+ cations are sandwiched between the layers and ensure the cohesion of the crystal structure. O—H⋯O hydrogen bonding between the layers is also observed.

Related literature

For properties of phosphates and their potential applications, see: Gao & Gao (2005[Gao, D. & Gao, Q. (2005). Micropor. Mesopor. Mater. 85, 365-373.]); Viter & Nagornyi (2009[Viter, V. N. & Nagornyi, P. G. (2009). Russ. J. Appl. Chem. 82, 935-939.]); Clearfield (1988[Clearfield, A. (1988). Chem. Rev. 88, 125-148.]); Trad et al. (2010[Trad, K., Carlier, D., Croguennec, L., Wattiaux, A., Ben Amara, M. & Delmas, C. (2010). Chem. Mater. 22, 5554-5562.]). For compounds with related structures, see: Assani et al. (2010[Assani, A., Saadi, M., Zriouil, M. & El Ammari, L. (2010). Acta Cryst. E66, i86-i87.], 2011a[Assani, A., Saadi, M., Zriouil, M. & El Ammari, L. (2011a). Acta Cryst. E67, i5.],b[Assani, A., El Ammari, L., Zriouil, M. & Saadi, M. (2011b). Acta Cryst. E67, i40.],c[Assani, A., El Ammari, L., Zriouil, M. & Saadi, M. (2011c). Acta Cryst. E67, i41.], 2012[Assani, A., Saadi, M., Zriouil, M. & El Ammari, L. (2012). Acta Cryst. E68, i30.]); Effenberger (1999[Effenberger, H. (1999). J. Solid State Chem. 142, 6-13.]). For bond-valence analysis, see: Brown & Altermatt (1985[Brown, I. D. & Altermatt, D. (1985). Acta Cryst. B41, 244-247.]).

Experimental

Crystal data

  • Pb2Mn3(HPO4)2(PO4)2

  • Mr = 961.10

  • Monoclinic, P 21 /c

  • a = 7.9449 (2) Å

  • b = 8.8911 (2) Å

  • c = 9.5718 (3) Å

  • β = 100.917 (2)°

  • V = 663.90 (3) Å3

  • Z = 2

  • Mo Kα radiation

  • μ = 28.63 mm−1

  • T = 296 K

  • 0.18 × 0.12 × 0.08 mm
Data collection

  • Bruker X8 APEXII diffractometer

  • Absorption correction: multi-scan (SADABS; Sheldrick, 2003)[Sheldrick, G. M. (2003). SADABS. University of Göttingen, Germany.] Tmin = 0.029, Tmax = 0.117

  • 8738 measured reflections

  • 1225 independent reflections

  • 1202 reflections with I > 2σ(I)

  • Rint = 0.044
Refinement

  • R[F2 > 2σ(F2)] = 0.020

  • wR(F2) = 0.051

  • S = 1.10

  • 1225 reflections

  • 116 parameters

  • H-atom parameters constrained

  • Δρmax = 1.37 e Å−3

  • Δρmin = −2.03 e Å−3

Table 1
Hydrogen-bond geometry (Å, °)

D—H⋯A D—H H⋯A D⋯A D—H⋯A
O8—H8⋯O4 0.86 1.60 2.437 (5) 164
O8—H8⋯O1 0.86 2.76 3.393 (5) 132

Data collection: APEX2 (Bruker, 2005[Bruker (2005). APEX2 and SAINT. Bruker AXS Inc., Madison, Wisconsin, USA.]); cell refinement: SAINT (Bruker, 2005[Bruker (2005). APEX2 and SAINT. Bruker AXS Inc., Madison, Wisconsin, USA.]); data reduction: SAINT; program(s) used to solve structure: SHELXS97 (Sheldrick, 2008[Sheldrick, G. M. (2008). Acta Cryst. A64, 112-122.]); program(s) used to refine structure: SHELXL97 (Sheldrick, 2008[Sheldrick, G. M. (2008). Acta Cryst. A64, 112-122.]); molecular graphics: ORTEP-3 for Windows (Farrugia, 1997[Farrugia, L. J. (1997). J. Appl. Cryst. 30, 565.]) and DIAMOND (Brandenburg, 2006[Brandenburg, K. (2006). DIAMOND. Crystal Impact GbR, Bonn, Germany.]); software used to prepare material for publication: PLATON (Spek, 2009[Spek, A. L. (2009). Acta Cryst. D65, 148-155.]) and publCIF (Westrip, 2010[Westrip, S. P. (2010). J. Appl. Cryst. 43, 920-925.]).

Supporting information

Crystal structure: contains datablocks I, global. DOI: https://doi.org/10.1107/S1600536812033259/hp2043sup1.cif

Structure factors: contains datablock I. DOI: https://doi.org/10.1107/S1600536812033259/hp2043Isup2.hkl

checkCIF report


Comment top

Owing to their remarkable variety of structures and to their outstanding potentialities in widespread applications such as catalysis (Viter & Nagornyi, 2009; Gao & Gao, 2005) and ion-exchangers (Clearfield, 1988) and in batteries performance (Trad et al., (2010)), transition metal based phosphates have received great attention and still remains in the forefront of the developed scientific axes in our laboratory. Within this family of compounds, the resulting anionic frameworks, generally constructed from the alternation of PO4 tetrahedra connected to metal cations in different coordinate geometry MOn (with n=4, 5 and 6), generate pores and channels offering suitable environment to accommodate different other cations. Accordingly, we have succeeded to isolate new silver metal based orthophosphates for instance, AgMg3(PO4)(HPO4)2 wich represent a new member of the well known alluaudite-like structure family (Assani et al. 2011a); silver (nickel or cobalt) phosphate, namely, Ag2M3(HPO4)(PO4)2 with M=Ni, Co (Assani et al. 2011b; Assani et al. 2011c). Furthermore, a special attention have been paid to the ternary system MO—M'O—P2O5 with M=Ba, Ca, Cd, Pb and Sr and M'= transition metals, Mg and Zn. Our recent investigation has allowed to the isolate the compounds Ni2Sr(PO4)2.2H2O (Assani et al. 2010) and Co2Pb(HPO4)(PO4)OH H2O (Assani et al. 2012).

Inline with the focus of our research, the present paper aims to develop the hydrothermal synthesis and the structural characterization of a new layered lead manganese orthophosphate, namely, PbMn1.5(PO4)(HPO4), which is characterized by Mn/P ratio =3/4, rarely encountered in the literature with the exception of some copper based orthophosphates, Pb3Cu3(PO4)4 and Sr3Cu3(PO4)4 (Effenberger 1999).

A partial three-dimensional plot of the crystal structure of PbMn1.5(PO4)(HPO4) is represented in Fig. 1. A l l atoms of this structure are in general positions, except one manganese Mn1 located in symmetry center (1) 2a (0 0 0; 0 1/2 1/2) of P21/c space group. The network is built up from two different types of polyhedra more or less distorted, viz. PO4, HPO4 tetrahedra and Mn1O6 (1 symmetry), Mn2O6 octahedra. Moreover, the edge-sharing Mn1O6 and Mn2O5(OH) octahedra form an infinite zigzag chains 1∞ [Mn3O14] running parallel to [010], as shown in Fig. 2. Adjacent chains are connected by PO4 and HPO4 tetrahedra via vertices in the way to build layers parallel to (100). These layers are in turn linked by Pb2+ cations as shown in Fig.2. The strong hydrogen bonding between the layers is also involved in the stability of this structure (Fig. 2 and Table 2).

Bond valence sum calculations (Brown & Altermatt, 1985) for Pb12+, Mn12+, Mb22+, P15+ and P25+ ions are as expected, viz. 1.82, 2.13, 1.97, 4.95 and 5.01 valence units, respectively. The values of the bond valence sums calculated for all oxygen atoms are between 1.93 and 2.05 except O4 and O8 which shown low values: 1.62 and 1.50 respectively. These atoms are considerably undersaturated and thus act as an acceptor with a very short H-bond (Table 2, Fig.1).

Related literature top

For properties of phosphates and their potential applications, see: Gao & Gao (2005); Viter & Nagornyi (2009); Clearfield (1988); Trad et al., (2010). For compounds with related structures, see: Assani et al. (2010, 2011a,b,c, 2012); Effenberger (1999). For bond-valence analysis, see: Brown & Altermatt (1985).

Experimental top

The crystals of the title compound is isolated from the hydrothermal treatment of the reaction mixture of lead oxide, metallic manganese and 85wt% phosphoric acid in a proportion corresponding to the molar ratio Pb:Mn:P = 1,5: 3:3.

The hydrothermal reaction was conducted in a 23 ml Teflon-lined autoclave, filled to 50% with distilled water and under autogeneous pressure at 483 K for twenty hours. After being filtered off, washed with deionized water and air dried, the reaction product consists of a light brown solid and colorless sheet shaped crystals corresponding to the title compound.

Refinement top

The O-bound H atoms were initially located in a difference map and refined with O—H distance restraints of 0.86 (1). In the last cycle they were refined in the riding model approximation with Uiso(H) set to 1.2Ueq(O). The highest peak and the deepest hole in the final Fourier map are at 0.62 Å and 0.67 Å, respectively, from Pb1. The not significants bonds and angles were removed from the CIF file.

Structure description top

Owing to their remarkable variety of structures and to their outstanding potentialities in widespread applications such as catalysis (Viter & Nagornyi, 2009; Gao & Gao, 2005) and ion-exchangers (Clearfield, 1988) and in batteries performance (Trad et al., (2010)), transition metal based phosphates have received great attention and still remains in the forefront of the developed scientific axes in our laboratory. Within this family of compounds, the resulting anionic frameworks, generally constructed from the alternation of PO4 tetrahedra connected to metal cations in different coordinate geometry MOn (with n=4, 5 and 6), generate pores and channels offering suitable environment to accommodate different other cations. Accordingly, we have succeeded to isolate new silver metal based orthophosphates for instance, AgMg3(PO4)(HPO4)2 wich represent a new member of the well known alluaudite-like structure family (Assani et al. 2011a); silver (nickel or cobalt) phosphate, namely, Ag2M3(HPO4)(PO4)2 with M=Ni, Co (Assani et al. 2011b; Assani et al. 2011c). Furthermore, a special attention have been paid to the ternary system MO—M'O—P2O5 with M=Ba, Ca, Cd, Pb and Sr and M'= transition metals, Mg and Zn. Our recent investigation has allowed to the isolate the compounds Ni2Sr(PO4)2.2H2O (Assani et al. 2010) and Co2Pb(HPO4)(PO4)OH H2O (Assani et al. 2012).

Inline with the focus of our research, the present paper aims to develop the hydrothermal synthesis and the structural characterization of a new layered lead manganese orthophosphate, namely, PbMn1.5(PO4)(HPO4), which is characterized by Mn/P ratio =3/4, rarely encountered in the literature with the exception of some copper based orthophosphates, Pb3Cu3(PO4)4 and Sr3Cu3(PO4)4 (Effenberger 1999).

A partial three-dimensional plot of the crystal structure of PbMn1.5(PO4)(HPO4) is represented in Fig. 1. A l l atoms of this structure are in general positions, except one manganese Mn1 located in symmetry center (1) 2a (0 0 0; 0 1/2 1/2) of P21/c space group. The network is built up from two different types of polyhedra more or less distorted, viz. PO4, HPO4 tetrahedra and Mn1O6 (1 symmetry), Mn2O6 octahedra. Moreover, the edge-sharing Mn1O6 and Mn2O5(OH) octahedra form an infinite zigzag chains 1∞ [Mn3O14] running parallel to [010], as shown in Fig. 2. Adjacent chains are connected by PO4 and HPO4 tetrahedra via vertices in the way to build layers parallel to (100). These layers are in turn linked by Pb2+ cations as shown in Fig.2. The strong hydrogen bonding between the layers is also involved in the stability of this structure (Fig. 2 and Table 2).

Bond valence sum calculations (Brown & Altermatt, 1985) for Pb12+, Mn12+, Mb22+, P15+ and P25+ ions are as expected, viz. 1.82, 2.13, 1.97, 4.95 and 5.01 valence units, respectively. The values of the bond valence sums calculated for all oxygen atoms are between 1.93 and 2.05 except O4 and O8 which shown low values: 1.62 and 1.50 respectively. These atoms are considerably undersaturated and thus act as an acceptor with a very short H-bond (Table 2, Fig.1).

For properties of phosphates and their potential applications, see: Gao & Gao (2005); Viter & Nagornyi (2009); Clearfield (1988); Trad et al., (2010). For compounds with related structures, see: Assani et al. (2010, 2011a,b,c, 2012); Effenberger (1999). For bond-valence analysis, see: Brown & Altermatt (1985).

Computing details top

Data collection: APEX2 (Bruker, 2005); cell refinement: SAINT (Bruker, 2005); data reduction: SAINT (Bruker, 2005); 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, 1997) and DIAMOND (Brandenburg, 2006); software used to prepare material for publication: PLATON (Spek, 2009) and publCIF (Westrip, 2010).

Figures top
[Figure 1] Fig. 1. A partial three-dimensional plot of the crystal structure of the title compound. Displacement ellipsoids are drawn at the 50% probability level. Symmetry codes:(i) x, -y + 3/2, z + 1/2; (ii) -x + 1, -y + 1, -z + 1; (iii) -x + 1, y - 1/2, -z + 3/2; (iv) -x, y - 1/2, -z + 1/2; (v) x - 1, y, z; (vi) -x, -y + 1, -z + 1; (vii) x, -y + 1/2, z + 1/2; (viii) x, -y + 1/2, z - 1/2; (ix) -x, y + 1/2, -z + 1/2; (x) x, -y + 3/2, z - 1/2; (xi) -x + 1, y + 1/2, -z + 3/2; (xii) x + 1, y, z.
[Figure 2] Fig. 2. A three-dimensional polyhedral view of the crystal structure of the PbMn1.5(PO4)(HPO4), showing the stacking of layers along the a axis and the hydrogen bonding scheme (dashed lines).
Dilead(II) trimanganese(II) bis(hydrogenphosphate) bis(phosphate) top
Crystal data top
Pb2Mn3(HPO4)2(PO4)2F(000) = 858
Mr = 961.10Dx = 4.808 Mg m−3
Monoclinic, P21/cMo Kα radiation, λ = 0.71073 Å
Hall symbol: -P 2ybcCell parameters from 1225 reflections
a = 7.9449 (2) Åθ = 2.6–25.4°
b = 8.8911 (2) ŵ = 28.63 mm−1
c = 9.5718 (3) ÅT = 296 K
β = 100.917 (2)°Prism, pink
V = 663.90 (3) Å30.18 × 0.12 × 0.08 mm
Z = 2
Data collection top
Bruker X8 APEXII
diffractometer		1225 independent reflections
Radiation source: fine-focus sealed tube1202 reflections with I > 2σ(I)
Graphite monochromatorRint = 0.044
φ and ω scansθmax = 25.4°, θmin = 2.6°
Absorption correction: multi-scan
(SADABS; Sheldrick, 2003)		h = −9→9
Tmin = 0.029, Tmax = 0.117k = −10→10
8738 measured reflectionsl = −11→11
Refinement top
Refinement on F2Secondary atom site location: difference Fourier map
Least-squares matrix: fullHydrogen site location: inferred from neighbouring sites
R[F2 > 2σ(F2)] = 0.020H-atom parameters constrained
wR(F2) = 0.051 w = 1/[σ2(Fo2) + (0.0232P)2 + 2.912P]
where P = (Fo2 + 2Fc2)/3
S = 1.10(Δ/σ)max = 0.001
1225 reflectionsΔρmax = 1.37 e Å−3
116 parametersΔρmin = −2.03 e Å−3
0 restraintsExtinction correction: SHELXL97 (Sheldrick, 2008), Fc*=kFc[1+0.001xFc2λ3/sin(2θ)]-1/4
Primary atom site location: structure-invariant direct methodsExtinction coefficient: 0.0091 (4)
Crystal data top
Pb2Mn3(HPO4)2(PO4)2V = 663.90 (3) Å3
Mr = 961.10Z = 2
Monoclinic, P21/cMo Kα radiation
a = 7.9449 (2) ŵ = 28.63 mm−1
b = 8.8911 (2) ÅT = 296 K
c = 9.5718 (3) Å0.18 × 0.12 × 0.08 mm
β = 100.917 (2)°
Data collection top
Bruker X8 APEXII
diffractometer		1225 independent reflections
Absorption correction: multi-scan
(SADABS; Sheldrick, 2003)		1202 reflections with I > 2σ(I)
Tmin = 0.029, Tmax = 0.117Rint = 0.044
8738 measured reflections
Refinement top
R[F2 > 2σ(F2)] = 0.0200 restraints
wR(F2) = 0.051H-atom parameters constrained
S = 1.10Δρmax = 1.37 e Å−3
1225 reflectionsΔρmin = −2.03 e Å−3
116 parameters
Special details top

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.

Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top
xyzUiso*/Ueq
Pb10.41097 (3)0.52400 (2)0.75343 (2)0.01734 (13)
Mn10.00000.50000.50000.0091 (2)
Mn20.10770 (9)0.13892 (8)0.59303 (7)0.00981 (19)
P10.14019 (16)0.70441 (14)0.23105 (12)0.0076 (3)
P20.65619 (16)0.70724 (14)0.56583 (12)0.0087 (3)
O10.0496 (5)0.6808 (4)0.3570 (4)0.0123 (7)
O20.0740 (5)0.5969 (4)0.1080 (3)0.0122 (7)
O30.1156 (5)0.8690 (4)0.1828 (4)0.0127 (7)
O40.3370 (5)0.6828 (4)0.2816 (4)0.0133 (7)
O50.7064 (5)0.6754 (5)0.7236 (4)0.0208 (9)
O60.7536 (5)0.6118 (4)0.4742 (4)0.0152 (8)
O70.6777 (5)0.8718 (4)0.5276 (4)0.0212 (9)
O80.4617 (5)0.6642 (4)0.5341 (4)0.0146 (7)
H80.40020.66670.44990.022*
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
Pb10.01783 (17)0.01676 (17)0.01923 (17)0.00271 (7)0.00812 (10)0.00201 (7)
Mn10.0108 (6)0.0084 (5)0.0080 (5)0.0006 (4)0.0018 (4)0.0002 (4)
Mn20.0096 (4)0.0107 (4)0.0082 (4)0.0003 (3)−0.0008 (3)−0.0006 (3)
P10.0080 (6)0.0090 (6)0.0055 (6)−0.0004 (5)0.0003 (5)0.0003 (4)
P20.0080 (6)0.0111 (6)0.0067 (6)−0.0007 (5)0.0009 (5)−0.0005 (4)
O10.0154 (19)0.0110 (17)0.0120 (17)−0.0005 (14)0.0068 (14)0.0016 (13)
O20.0154 (19)0.0111 (17)0.0076 (16)0.0002 (14)−0.0045 (14)−0.0020 (13)
O30.0154 (19)0.0099 (17)0.0120 (17)0.0005 (14)0.0008 (14)0.0026 (14)
O40.0083 (18)0.0234 (19)0.0078 (16)0.0002 (14)0.0004 (13)−0.0002 (14)
O50.015 (2)0.038 (2)0.0076 (18)0.0013 (17)−0.0021 (14)0.0035 (16)
O60.0113 (18)0.0200 (19)0.0153 (17)0.0061 (15)0.0048 (14)0.0015 (15)
O70.030 (2)0.0118 (18)0.026 (2)−0.0036 (16)0.0151 (18)−0.0013 (16)
O80.0087 (17)0.0261 (19)0.0079 (16)−0.0034 (15)−0.0012 (14)0.0016 (15)
Geometric parameters (Å, º) top
Pb1—O3i2.504 (4)P1—O31.536 (3)
Pb1—O82.539 (4)P1—O41.559 (4)
Pb1—O6ii2.614 (4)P2—O51.514 (4)
Pb1—O4i2.697 (4)P2—O71.526 (4)
Pb1—O7iii2.698 (4)P2—O61.532 (4)
Pb1—O52.767 (4)P2—O81.565 (4)
Pb1—O4ii2.785 (4)O1—Mn2vi2.141 (4)
Mn1—O3iv2.157 (3)O2—Mn2viii2.122 (4)
Mn1—O3i2.157 (3)O2—Mn2ix2.208 (3)
Mn1—O6ii2.168 (3)O3—Mn1ix2.157 (3)
Mn1—O6v2.168 (3)O3—Pb1x2.504 (4)
Mn1—O12.195 (3)O4—Pb1x2.697 (4)
Mn1—O1vi2.195 (3)O4—Pb1ii2.785 (4)
Mn2—O5iii2.094 (4)O5—Mn2xi2.094 (4)
Mn2—O2vii2.122 (4)O6—Mn1xii2.168 (3)
Mn2—O1vi2.141 (4)O6—Mn2ii2.610 (4)
Mn2—O2iv2.208 (3)O6—Pb1ii2.614 (4)
Mn2—O7ii2.235 (4)O7—Mn2ii2.235 (4)
Mn2—O6ii2.610 (4)O7—Pb1xi2.698 (4)
P1—O21.530 (3)O8—H80.8600
P1—O11.531 (3)
O3i—Pb1—O882.97 (11)O3i—Mn1—O1vi89.35 (13)
O3i—Pb1—O6ii69.84 (11)O6ii—Mn1—O1vi81.84 (13)
O8—Pb1—O6ii70.75 (11)O6v—Mn1—O1vi98.16 (13)
O3i—Pb1—O4i56.56 (11)O1—Mn1—O1vi180.000 (1)
O8—Pb1—O4i71.32 (11)O5iii—Mn2—O2vii100.04 (15)
O6ii—Pb1—O4i116.47 (11)O5iii—Mn2—O1vi92.62 (15)
O3i—Pb1—O7iii91.78 (12)O2vii—Mn2—O1vi129.62 (14)
O8—Pb1—O7iii173.95 (12)O5iii—Mn2—O2iv176.09 (15)
O6ii—Pb1—O7iii104.65 (12)O2vii—Mn2—O2iv79.73 (13)
O4i—Pb1—O7iii108.25 (11)O1vi—Mn2—O2iv90.49 (14)
O3i—Pb1—O5123.87 (12)O5iii—Mn2—O7ii87.34 (15)
O8—Pb1—O553.50 (11)O2vii—Mn2—O7ii96.38 (14)
O6ii—Pb1—O5116.03 (11)O1vi—Mn2—O7ii133.01 (14)
O4i—Pb1—O575.23 (12)O2iv—Mn2—O7ii88.81 (14)
O7iii—Pb1—O5132.49 (12)O5iii—Mn2—O6ii79.12 (14)
O3i—Pb1—O4ii151.26 (10)O2vii—Mn2—O6ii157.01 (13)
O8—Pb1—O4ii89.67 (11)O1vi—Mn2—O6ii73.21 (12)
O6ii—Pb1—O4ii81.50 (10)O2iv—Mn2—O6ii99.54 (12)
O4i—Pb1—O4ii145.63 (8)O7ii—Mn2—O6ii60.65 (12)
O7iii—Pb1—O4ii93.55 (11)O2—P1—O1112.1 (2)
O5—Pb1—O4ii70.46 (12)O2—P1—O3111.0 (2)
O3iv—Mn1—O3i180.000 (1)O1—P1—O3108.4 (2)
O3iv—Mn1—O6ii94.68 (14)O2—P1—O4109.9 (2)
O3i—Mn1—O6ii85.32 (14)O1—P1—O4109.4 (2)
O3iv—Mn1—O6v85.32 (14)O3—P1—O4105.9 (2)
O3i—Mn1—O6v94.68 (14)O5—P2—O7113.5 (2)
O6ii—Mn1—O6v180.00 (19)O5—P2—O6113.7 (2)
O3iv—Mn1—O189.35 (13)O7—P2—O6107.6 (2)
O3i—Mn1—O190.65 (13)O5—P2—O8102.2 (2)
O6ii—Mn1—O198.16 (13)O7—P2—O8109.8 (2)
O6v—Mn1—O181.84 (13)O6—P2—O8109.9 (2)
O3iv—Mn1—O1vi90.65 (13)
Symmetry codes: (i) x, −y+3/2, z+1/2; (ii) −x+1, −y+1, −z+1; (iii) −x+1, y−1/2, −z+3/2; (iv) −x, y−1/2, −z+1/2; (v) x−1, y, z; (vi) −x, −y+1, −z+1; (vii) x, −y+1/2, z+1/2; (viii) x, −y+1/2, z−1/2; (ix) −x, y+1/2, −z+1/2; (x) x, −y+3/2, z−1/2; (xi) −x+1, y+1/2, −z+3/2; (xii) x+1, y, z.
Hydrogen-bond geometry (Å, º) top
D—H···AD—HH···AD···AD—H···A
O8—H8···O40.861.602.437 (5)164
O8—H8···O10.862.763.393 (5)132

Experimental details

Crystal data
Chemical formulaPb2Mn3(HPO4)2(PO4)2
Mr961.10
Crystal system, space groupMonoclinic, P21/c
Temperature (K)296
a, b, c (Å)7.9449 (2), 8.8911 (2), 9.5718 (3)
β (°) 100.917 (2)
V (Å3)663.90 (3)
Z2
Radiation typeMo Kα
µ (mm−1)28.63
Crystal size (mm)0.18 × 0.12 × 0.08
Data collection
DiffractometerBruker X8 APEXII
Absorption correctionMulti-scan
(SADABS; Sheldrick, 2003)
Tmin, Tmax0.029, 0.117
No. of measured, independent and
observed [I > 2σ(I)] reflections		8738, 1225, 1202
Rint0.044
(sin θ/λ)max (Å−1)0.602
Refinement
R[F2 > 2σ(F2)], wR(F2), S 0.020, 0.051, 1.10
No. of reflections1225
No. of parameters116
H-atom treatmentH-atom parameters constrained
Δρmax, Δρmin (e Å−3)1.37, −2.03

Computer programs: APEX2 (Bruker, 2005), SAINT (Bruker, 2005), SHELXS97 (Sheldrick, 2008), SHELXL97 (Sheldrick, 2008), ORTEP-3 for Windows (Farrugia, 1997) and DIAMOND (Brandenburg, 2006), PLATON (Spek, 2009) and publCIF (Westrip, 2010).

Hydrogen-bond geometry (Å, º) top
D—H···AD—HH···AD···AD—H···A
O8—H8···O40.861.602.437 (5)163.7
O8—H8···O10.862.763.393 (5)131.5
 

Acknowledgements

The authors thank the Unit of Support for Technical and Scientific Research (UATRS, CNRST) for the X-ray measurements.

References

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ISSN: 2056-9890
Volume 68| Part 8| August 2012| Page i66
https://doi.org/10.1107/S1600536812033259
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