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

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Dicobalt(II) lead(II) hydrogenphos­phate(V) phos­phate(V) hydroxide monohydrate

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 21 March 2012; accepted 4 April 2012; online 18 April 2012)

The title compound, Co2Pb(HPO4)(PO4)OH·H2O, which was synthesized under hydro­thermal conditions, crystallizes in a new structure type. Except for two O atoms in general positions and two Co atoms on centres of symmetry, all other atoms in the asymmetric unit (1 Pb, 2 Co, 2 P, 8 O and 4 H) are located on mirror planes. The structure is built up from two infinite linear chains, viz. 1[CoO2/1(H2O)2/2O2/2] and 1[CoO2/1(OH)2/2O2/2], of edge-sharing CoO6 octa­hedra running along [010]. Adjacent chains are linked to each other through PO4 and PO3(OH) tetra­hedra, leading to the formation of layers parallel to (100). The three-dimensional framework is formed by stacking along [100] of adjacent layers that are held together by distorted PbO8 polyhedra. Hydrogen bonds of the type O—H⋯O involving the water mol­ecule are very strong, while those O atoms involving the OH groups form weak bifurcated and trifurcated hydrogen bonds.

Related literature

For catalytic properties of phosphates, see: Cheetham et al. (1999[Cheetham, A. K., Férey, G. & Loiseau, T. (1999). Angew. Chem. Int. Ed. 111, 3466-3492.]); 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: Yakubovich et al. (2001[Yakubovich, O. V., Massa, W., Liferovich, R. P. & McCammon, C. A. (2001). Can. Mineral. 39, 1317-1324.]); Lee et al. (2008[Lee, Y. H., Clegg, J. K., Lindoy, L. F., Lu, G. Q. M., Park, Y.-C. & Kim, Y. (2008). Acta Cryst. E64, i67-i68.]); Effenberger (1999[Effenberger, H. (1999). J. Solid State Chem. 142, 6-13.]); Britvin et al. (2002[Britvin, S. N., Ferraris, G., Ivaldi, G., Bogdanova, A. N. & Chukanov, N. V. (2002). Neues Jahrb. Miner. Monatsh. 4, 160-168.]); Assani et al. (2010[Assani, A., Saadi, M. & El Ammari, L. (2010). Acta Cryst. E66, i44.]). For bond-valence analysis, see: Brown & Altermatt (1985[Brown, I. D. & Altermatt, D. (1985). Acta Cryst. B41, 244-247.]). For background to the Inorganic Crystal Structure Database (ICSD), see: Belsky et al. (2002[Belsky, A., Hellenbrandt, M., Karen, V. L. & Luksch, P. (2002). Acta Cryst. B58, 364-369.]).

Experimental

Crystal data
  • Co2Pb(HPO4)(PO4)OH·H2O

  • Mr = 551.02

  • Monoclinic, P 21 /m

  • a = 7.4299 (1) Å

  • b = 6.2949 (1) Å

  • c = 8.9057 (1) Å

  • β = 113.936 (1)°

  • V = 380.70 (1) Å3

  • Z = 2

  • Mo Kα radiation

  • μ = 26.83 mm−1

  • T = 296 K

  • 0.18 × 0.12 × 0.08 mm

Data collection
  • Bruker X8 APEXII diffractometer

  • Absorption correction: multi-scan (SADABS; Sheldrick, 1999[Sheldrick, G. M. (1999). SADABS. University of Göttingen, Germany.]) Tmin = 0.029, Tmax = 0.117

  • 8321 measured reflections

  • 1601 independent reflections

  • 1558 reflections with I > 2σ(I)

  • Rint = 0.027

Refinement
  • R[F2 > 2σ(F2)] = 0.016

  • wR(F2) = 0.039

  • S = 1.11

  • 1601 reflections

  • 86 parameters

  • H-atom parameters constrained

  • Δρmax = 1.76 e Å−3

  • Δρmin = −1.49 e Å−3

Table 1
Hydrogen-bond geometry (Å, °)

D—H⋯A D—H H⋯A DA D—H⋯A
O2—H2⋯O6i 0.86 2.28 3.027 (3) 145
O2—H2⋯O6ii 0.86 2.28 3.027 (3) 145
O7—H7⋯O2iii 0.86 2.20 2.915 (3) 140
O7—H7⋯O3 0.86 2.53 2.986 (2) 114
O7—H7⋯O3iv 0.86 2.53 2.986 (2) 114
O8—H8A⋯O4v 0.86 1.79 2.649 (3) 177
O8—H8B⋯O7 0.86 1.65 2.489 (3) 165
Symmetry codes: (i) -x, -y, -z; (ii) [-x, y-{\script{1\over 2}}, -z]; (iii) -x, -y, -z+1; (iv) [x, -y+{\script{1\over 2}}, z]; (v) x-1, y, z.

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


Comment top

Metal based phosphates are of great interest owing to either their remarkable diversity of structures or their properties and applications in catalysis, as ion-exchangers (Cheetham et al., 1999; Clearfield, 1988) or as positive electrode materials in lithium- and sodium-containing batteries (Trad et al., 2010)). Mainly, our focus of investigation is focused on orthophosphates with (mixed) divalent metals with general formula (M,M')3(PO4)2.nH2O (Assani et al., 2010). It has been pointed out that the structural diversity of this family of compounds depends on the size difference of the divalent cations (Effenberger, 1999) and on the degree of hydratation (Yakubovich et al., 2001; Lee et al., 2008. The highest water content known up to date is realised for Mg3(PO4)2.22H2O (Britvin et al., 2002). In this work, a new dicobalt lead phosphate(V)] with formula Co2Pb(HPO4)(PO4)OH.H2O, was hydrothermally synthesized and structurally characterized.

A search in the ICSD (Belsky et al., 2002) reveals that the crystal structure of this phosphate represents a new structure type. A plot of the crystal structure illustrating the most important coordination polyhedra and their mutual connections is represented in Fig. 1. All atoms are in special positions, except two oxygen atoms (O3,O6) in general position of the P21/m space group. The crystal structure is built up from three different types of polyhedra more or less distorted, viz. two PbO8 polyhedra (m symmetry), PO4 and PO3(OH) tetrahedra (both with m symmetry) and two CoO6 octahedra (both with 1 symmetry). The CoO6 octahedra share edges and form 1[Co(1)O2/1(H2O)2/2O2/2] and 1[Co(2)O2/1(OH)2/2O2/2] chains running parallel to [010], as shown in Fig. 2. Adjacent chains are connected by PO4 and HPO4 tetrahedra via vertices, leading to the formation of layers parallel to (100). These layers are in turn linked by sheets of distorted PbO8 polyhedra as also shown in Fig.2.

Bond valence sum calculations (Brown & Altermatt, 1985) for Pb12+, Co12+, Co22+, P15+ and P25+ ions are as expected, viz. 1.92, 2.03, 1.93, 5.05 and 5.05 valence units, respectively. The values of the bond valence sums calculated for the oxygen atoms show low values for O2, O7 and O8 when the contribution of H atoms are not considered (i.e. 1.23, 0.88 and 0.75 valence units, respectively). Hence these O atoms are associated with protons and are involved in O—H···O hydrogen bonding (Table 1). H atoms of the water molecule form very strong hydrogen bonds, especially O8–H8B···O7 with an D···A distance less than 2.5 Å. The H atom of the OH- group (O7) and the hydrogenphosphate group (O2) form weak bifurcated (O2) and trifurcated (O7) hydrogen bonds (Fig. 2, Table 1).

Related literature top

For catalytic properties of phosphates, see: Cheetham et al. (1999); Clearfield (1988); Trad et al. (2010). For compounds with related structures, see: Yakubovich et al. (2001); Lee et al. (2008); Effenberger (1999); Britvin et al. (2002); Assani et al. (2010). For bond-valence analysis, see: Brown & Altermatt (1985). For background to the Inorganic Crystal Structure Database (ICSD), see: Belsky et al. (2002).

Experimental top

The title compound, Co2Pb(HPO4)(PO4)OH.H2O, was obtained from the hydrothermal treatment of a reaction mixture of Pb(NO3)2, metallic cobalt and 85wt% phosphoric acid in the molar ratio Pb:Co:P = 1:3:3. The hydrothermal reaction was conducted in a 23 ml Teflon-lined autoclave under autogeneous pressure at 473 K for three days. The product was filtered off, washed with deionized water and air dried. The resulting product consists of pink crystals besides some pink powder.

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 a the last cycle they were refined in the riding model approximation with Uiso(H) set to 1.2Ueq(O). The highest remaining positive and negative electron densities observed in the final Fourier map are 0.76 Å and 0.78 Å, respectively, from Pb1.

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 Co2Pb(HPO4)(PO4)OH.H2O. Displacement ellipsoids are drawn at the 50% probability level. Symmetry codes:(i) -x, y + 1/2, -z; (ii) -x, -y, -z; (iii) x, -y + 1/2, z; (iv) -x, -y, -z + 1; (v) -x - 1, -y, -z; (vi) x + 1, y, z; (vii) -x, -y + 1, -z + 1; (viii) x + 1, -y + 1/2, z + 1; (ix) x + 1, y + 1, z; (x) x, -y - 1/2, z; (xi) x - 1, y - 1, z; (xii) -x, y - 1/2, -z + 1; (xiii) -x - 1, y + 1/2, -z;
[Figure 2] Fig. 2. A three-dimensional polyhedral view of the crystal structure of Co2Pb(HPO4)(PO4)OH.H2O, showing the stacking of layers along the [100] axis and the hydrogen bonding scheme (dashed lines).
Dicobalt(II) lead(II) hydrogenphosphate(V) phosphate(V) hydroxide monohydrate top
Crystal data top
Co2Pb(HPO4)(PO4)OH·H2OF(000) = 500
Mr = 551.02Dx = 4.807 Mg m3
Monoclinic, P21/mMo Kα radiation, λ = 0.71073 Å
Hall symbol: -P 2ybCell parameters from 1601 reflections
a = 7.4299 (1) Åθ = 2.5–33.5°
b = 6.2949 (1) ŵ = 26.83 mm1
c = 8.9057 (1) ÅT = 296 K
β = 113.936 (1)°Prism, pink
V = 380.70 (1) Å30.18 × 0.12 × 0.08 mm
Z = 2
Data collection top
Bruker X8 APEXII
diffractometer
1601 independent reflections
Radiation source: fine-focus sealed tube1558 reflections with I > 2σ(I)
Graphite monochromatorRint = 0.027
ϕ and ω scansθmax = 33.5°, θmin = 2.5°
Absorption correction: multi-scan
(SADABS; Sheldrick, 1999)
h = 911
Tmin = 0.029, Tmax = 0.117k = 99
8321 measured reflectionsl = 1313
Refinement top
Refinement on F2Secondary atom site location: difference Fourier map
Least-squares matrix: fullHydrogen site location: difference Fourier map
R[F2 > 2σ(F2)] = 0.016H-atom parameters constrained
wR(F2) = 0.039 w = 1/[σ2(Fo2) + (0.0153P)2 + 0.885P]
where P = (Fo2 + 2Fc2)/3
S = 1.11(Δ/σ)max = 0.001
1601 reflectionsΔρmax = 1.76 e Å3
86 parametersΔρmin = 1.49 e Å3
0 restraintsExtinction correction: SHELXL97 (Sheldrick, 2008), Fc*=kFc[1+0.001xFc2λ3/sin(2θ)]-1/4
Primary atom site location: structure-invariant direct methodsExtinction coefficient: 0.0061 (3)
Crystal data top
Co2Pb(HPO4)(PO4)OH·H2OV = 380.70 (1) Å3
Mr = 551.02Z = 2
Monoclinic, P21/mMo Kα radiation
a = 7.4299 (1) ŵ = 26.83 mm1
b = 6.2949 (1) ÅT = 296 K
c = 8.9057 (1) Å0.18 × 0.12 × 0.08 mm
β = 113.936 (1)°
Data collection top
Bruker X8 APEXII
diffractometer
1601 independent reflections
Absorption correction: multi-scan
(SADABS; Sheldrick, 1999)
1558 reflections with I > 2σ(I)
Tmin = 0.029, Tmax = 0.117Rint = 0.027
8321 measured reflections
Refinement top
R[F2 > 2σ(F2)] = 0.0160 restraints
wR(F2) = 0.039H-atom parameters constrained
S = 1.11Δρmax = 1.76 e Å3
1601 reflectionsΔρmin = 1.49 e Å3
86 parameters
Special details top

Geometry. All e.s.d.'s (except the e.s.d. in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell e.s.d.'s are taken into account individually in the estimation of e.s.d.'s in distances, angles and torsion angles; correlations between e.s.d.'s in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell e.s.d.'s is used for estimating e.s.d.'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
Pb10.006473 (17)0.25000.232477 (15)0.01414 (5)
Co10.50000.00000.00000.00717 (8)
Co20.50000.50000.50000.00859 (8)
P10.22391 (12)0.25000.32517 (9)0.00646 (13)
P20.21025 (11)0.25000.16270 (9)0.00642 (13)
O10.3205 (3)0.25000.4478 (3)0.0088 (4)
O20.0058 (4)0.25000.4403 (3)0.0145 (5)
H20.06420.25000.37440.017*
O30.2656 (2)0.0469 (3)0.2228 (2)0.0102 (3)
O40.0041 (4)0.25000.0355 (3)0.0160 (5)
O50.3411 (3)0.25000.0638 (3)0.0096 (4)
O60.2489 (3)0.0525 (3)0.2742 (2)0.0135 (3)
O70.4341 (4)0.25000.3936 (3)0.0100 (4)
H70.31970.25000.39100.012*
O80.6059 (3)0.25000.0885 (3)0.0086 (4)
H8A0.73220.25000.05220.010*
H8B0.56600.25000.19370.010*
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
Pb10.01157 (7)0.02066 (8)0.01059 (7)0.0000.00492 (4)0.000
Co10.00890 (17)0.00553 (19)0.00703 (16)0.00041 (14)0.00319 (14)0.00011 (13)
Co20.01066 (18)0.0070 (2)0.00765 (16)0.00114 (14)0.00323 (14)0.00053 (13)
P10.0091 (3)0.0062 (3)0.0048 (3)0.0000.0035 (3)0.000
P20.0068 (3)0.0075 (3)0.0052 (3)0.0000.0028 (2)0.000
O10.0122 (10)0.0082 (10)0.0084 (9)0.0000.0067 (8)0.000
O20.0080 (10)0.0233 (14)0.0106 (10)0.0000.0022 (8)0.000
O30.0119 (7)0.0090 (7)0.0083 (6)0.0011 (6)0.0027 (5)0.0010 (6)
O40.0073 (10)0.0287 (15)0.0101 (10)0.0000.0016 (8)0.000
O50.0110 (10)0.0101 (10)0.0105 (9)0.0000.0071 (8)0.000
O60.0156 (8)0.0124 (8)0.0088 (6)0.0056 (7)0.0010 (6)0.0041 (6)
O70.0113 (10)0.0130 (11)0.0074 (9)0.0000.0055 (8)0.000
O80.0097 (9)0.0100 (10)0.0072 (9)0.0000.0047 (8)0.000
Geometric parameters (Å, º) top
Pb1—O42.380 (3)P1—O11.531 (2)
Pb1—O6i2.5429 (18)P1—O21.595 (3)
Pb1—O6ii2.5429 (18)P2—O41.535 (3)
Pb1—O32.7284 (17)P2—O61.5432 (18)
Pb1—O3iii2.7284 (17)P2—O6iii1.5432 (18)
Pb1—O52.846 (2)P2—O51.554 (2)
Pb1—O1iv2.857 (2)O1—Co2xi2.2302 (16)
Pb1—O2iv2.952 (3)O1—Co2xii2.2302 (16)
Co1—O82.0544 (14)O1—Pb1iv2.857 (2)
Co1—O8v2.0544 (14)O2—Pb1iv2.952 (3)
Co1—O3v2.0624 (16)O2—H20.8600
Co1—O32.0624 (16)O5—Co1xiii2.1766 (15)
Co1—O52.1766 (15)O6—Co2xiv2.1426 (17)
Co1—O5v2.1766 (15)O6—Pb1ii2.5429 (18)
Co2—O7vi1.9978 (14)O7—Co2xv1.9978 (14)
Co2—O7vii1.9978 (14)O7—Co2xii1.9978 (14)
Co2—O6i2.1426 (17)O7—H70.8600
Co2—O6viii2.1426 (17)O7—H8B1.6474
Co2—O1ix2.2302 (16)O8—Co1xiii2.0544 (14)
Co2—O1iv2.2302 (16)O8—H8A0.8600
P1—O3x1.5274 (18)O8—H8B0.8600
P1—O31.5274 (18)
O4—Pb1—O6i82.12 (5)O3v—Co1—O588.92 (8)
O4—Pb1—O6ii82.12 (5)O3—Co1—O591.08 (8)
O6i—Pb1—O6ii97.00 (9)O8—Co1—O5v96.95 (6)
O4—Pb1—O3105.34 (5)O8v—Co1—O5v83.05 (6)
O6i—Pb1—O3171.63 (5)O3v—Co1—O5v91.08 (8)
O6ii—Pb1—O387.90 (7)O3—Co1—O5v88.92 (8)
O4—Pb1—O3iii105.34 (5)O5—Co1—O5v180.00 (12)
O6i—Pb1—O3iii87.90 (7)O7vi—Co2—O7vii180.0
O6ii—Pb1—O3iii171.63 (5)O7vi—Co2—O6i87.93 (9)
O3—Pb1—O3iii86.46 (8)O7vii—Co2—O6i92.07 (9)
O4—Pb1—O555.64 (7)O7vi—Co2—O6viii92.07 (9)
O6i—Pb1—O5117.25 (4)O7vii—Co2—O6viii87.93 (9)
O6ii—Pb1—O5117.25 (4)O6i—Co2—O6viii180.0
O3—Pb1—O565.72 (4)O7vi—Co2—O1ix100.06 (7)
O3iii—Pb1—O565.72 (4)O7vii—Co2—O1ix79.94 (7)
O4—Pb1—O1iv132.09 (7)O6i—Co2—O1ix93.55 (8)
O6i—Pb1—O1iv67.09 (5)O6viii—Co2—O1ix86.45 (8)
O6ii—Pb1—O1iv67.09 (5)O7vi—Co2—O1iv79.94 (7)
O3—Pb1—O1iv109.06 (5)O7vii—Co2—O1iv100.06 (7)
O3iii—Pb1—O1iv109.06 (5)O6i—Co2—O1iv86.45 (8)
O5—Pb1—O1iv172.27 (6)O6viii—Co2—O1iv93.55 (8)
O4—Pb1—O2iv178.00 (7)O1ix—Co2—O1iv180.0
O6i—Pb1—O2iv99.18 (5)O3x—P1—O3113.68 (14)
O6ii—Pb1—O2iv99.18 (5)O3x—P1—O1112.68 (8)
O3—Pb1—O2iv73.26 (5)O3—P1—O1112.68 (8)
O3iii—Pb1—O2iv73.26 (5)O3x—P1—O2106.78 (8)
O5—Pb1—O2iv122.36 (7)O3—P1—O2106.78 (8)
O1iv—Pb1—O2iv49.91 (6)O1—P1—O2103.32 (13)
O8—Co1—O8v180.00 (11)O4—P2—O6109.94 (9)
O8—Co1—O3v87.37 (8)O4—P2—O6iii109.94 (9)
O8v—Co1—O3v92.63 (8)O6—P2—O6iii107.30 (15)
O8—Co1—O392.63 (8)O4—P2—O5106.40 (14)
O8v—Co1—O387.37 (8)O6—P2—O5111.63 (9)
O3v—Co1—O3180.00 (13)O6iii—P2—O5111.63 (9)
O8—Co1—O583.05 (6)H8A—O8—H8B104.5
O8v—Co1—O596.95 (6)
Symmetry codes: (i) x, y+1/2, z; (ii) x, y, z; (iii) x, y+1/2, z; (iv) x, y, z+1; (v) x1, y, z; (vi) x+1, y, z; (vii) x, y+1, z+1; (viii) x+1, y+1/2, z+1; (ix) x+1, y+1, z; (x) x, y1/2, z; (xi) x1, y1, z; (xii) x, y1/2, z+1; (xiii) x1, y+1/2, z; (xiv) x, y1/2, z; (xv) x1, y, z.
Hydrogen-bond geometry (Å, º) top
D—H···AD—HH···AD···AD—H···A
O2—H2···O6ii0.862.283.027 (3)145
O2—H2···O6xiv0.862.283.027 (3)145
O7—H7···O2iv0.862.202.915 (3)140
O7—H7···O30.862.532.986 (2)114
O7—H7···O3iii0.862.532.986 (2)114
O8—H8A···O4xv0.861.792.649 (3)177
O8—H8B···O70.861.652.489 (3)165
Symmetry codes: (ii) x, y, z; (iii) x, y+1/2, z; (iv) x, y, z+1; (xiv) x, y1/2, z; (xv) x1, y, z.

Experimental details

Crystal data
Chemical formulaCo2Pb(HPO4)(PO4)OH·H2O
Mr551.02
Crystal system, space groupMonoclinic, P21/m
Temperature (K)296
a, b, c (Å)7.4299 (1), 6.2949 (1), 8.9057 (1)
β (°) 113.936 (1)
V3)380.70 (1)
Z2
Radiation typeMo Kα
µ (mm1)26.83
Crystal size (mm)0.18 × 0.12 × 0.08
Data collection
DiffractometerBruker X8 APEXII
diffractometer
Absorption correctionMulti-scan
(SADABS; Sheldrick, 1999)
Tmin, Tmax0.029, 0.117
No. of measured, independent and
observed [I > 2σ(I)] reflections
8321, 1601, 1558
Rint0.027
(sin θ/λ)max1)0.777
Refinement
R[F2 > 2σ(F2)], wR(F2), S 0.016, 0.039, 1.11
No. of reflections1601
No. of parameters86
H-atom treatmentH-atom parameters constrained
Δρmax, Δρmin (e Å3)1.76, 1.49

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
O2—H2···O6i0.862.283.027 (3)144.7
O2—H2···O6ii0.862.283.027 (3)144.7
O7—H7···O2iii0.862.202.915 (3)140.0
O7—H7···O30.862.532.986 (2)114.4
O7—H7···O3iv0.862.532.986 (2)114.4
O8—H8A···O4v0.861.792.649 (3)176.6
O8—H8B···O70.861.652.489 (3)165.4
Symmetry codes: (i) x, y, z; (ii) x, y1/2, z; (iii) x, y, z+1; (iv) x, y+1/2, z; (v) x1, y, z.
 

Acknowledgements

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

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