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

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ISSN: 2056-9890

Distrontium trimanganese(II) bis­­(hydro­gen­phosphate) bis­­(ortho­phosphate)

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

(Received 4 July 2013; accepted 8 July 2013; online 13 July 2013)

The title compound, Sr2Mn3(HPO4)2(PO4)2, was synthesized under hydro­thermal conditions. In the structure, one of two Mn atoms is located on an inversion centre, whereas all others atoms are located in general positions. The framework structure is built up from two types of MnO6 octa­hedra (one almost undistorted, one considerably distorted), one PO3OH and one PO4 tetra­hedron. The centrosymmetric MnO6 octa­hedron is linked to two other MnO6 octa­hedra by edge-sharing, forming infinite zigzag chains parallel to [010]. The PO3OH and PO4 tetra­hedra connect these chains through common vertices or edges, resulting in the formation of sheets parallel to (100). The Sr2+ cation is located in the inter­layer space and is bonded to nine O atoms in form of a distorted polyhedron and enhances the cohesion of the layers. Additional stabilization is achieved by a strong inter­layer O—H⋯O hydrogen bond between the PO3OH and PO4 units. The structure of the title phosphate is isotypic to that of Pb2Mn3(HPO4)2(PO4)2.

Related literature

For isotypic Pb2Mn3(HPO4)2(PO4)2, see: Assani et al. (2012b[Assani, A., Saadi, M., Zriouil, M. & El Ammari, L. (2012b). Acta Cryst. E68, i66.]). For related structures, see: Assani et al. (2012a[Assani, A., Saadi, M., Zriouil, M. & El Ammari, L. (2012a). Acta Cryst. E68, i30.]); Effenberger (1999[Effenberger, H. (1999). J. Solid State Chem. 142, 6-13.]). For the thermal stability of similar compounds, see: Morozov et al. (2003[Morozov, V. A., Pokholok, K. V., Lazoryak, B. I., Malakho, A. P., Lachgar, A., Lebedev, O. I. & Van Tendeloo, G. (2003). J. Solid State Chem. 170, 411-417.]). For applications of phosphates, see: Cheetham et al. (1999[Cheetham, A. K., Férey, G. & Loiseau, T. (1999). Angew. Chem. Int. Ed. 38, 3268-3292.]); Viter & Nagornyi (2009[Viter, V. N. & Nagornyi, P. G. (2009). Russ. J. Appl. Chem. 82, 935-939.]); Forster et al. (2003[Forster, P. M., Eckert, J., Chang, J.-S., Park, J.-S., Férey, G. & Cheatham, A. K. (2003). J. Am. Chem. Soc. 125, 1309-1312.]); Clearfield (1988[Clearfield, A. (1988). Chem. Rev. 88, 125-148.]); Joschi et al. (2008[Joschi, R., Patel, H. & Chudasama, U. (2008). Indian J. Chem. Technol. 15, 238-243.]); Trad et al. (2010[Trad, K., Carlier, D., Croguennec, L., Wattiaux, A., Ben Amara, M. & Delmas, C. (2010). Chem. Mater. 22, 5554-5562.]).

Experimental

Crystal data
  • Sr2Mn3(HPO4)2(PO4)2

  • Mr = 721.96

  • Monoclinic, P 21 /c

  • a = 7.8535 (1) Å

  • b = 8.7793 (2) Å

  • c = 9.6165 (2) Å

  • β = 101.434 (1)°

  • V = 649.88 (2) Å3

  • Z = 2

  • Mo Kα radiation

  • μ = 11.58 mm−1

  • T = 296 K

  • 0.33 × 0.24 × 0.12 mm

Data collection
  • Bruker APEXII CCD diffractometer

  • Absorption correction: multi-scan (SADABS; Bruker, 2009[Bruker (2009). APEX2, SAINT and SADABS. Bruker AXS Inc., Madison, Wisconsin, USA.]) Tmin = 0.046, Tmax = 0.215

  • 12425 measured reflections

  • 3138 independent reflections

  • 2874 reflections with I > 2σ(I)

  • Rint = 0.025

Refinement
  • R[F2 > 2σ(F2)] = 0.019

  • wR(F2) = 0.045

  • S = 1.06

  • 3138 reflections

  • 115 parameters

  • H-atom parameters constrained

  • Δρmax = 0.58 e Å−3

  • Δρmin = −0.54 e Å−3

Table 1
Hydrogen-bond geometry (Å, °)

D—H⋯A D—H H⋯A DA D—H⋯A
O8—H8⋯O4 0.82 1.66 2.4828 (14) 177

Data collection: APEX2 (Bruker, 2009[Bruker (2009). APEX2, SAINT and SADABS. Bruker AXS Inc., Madison, Wisconsin, USA.]); cell refinement: SAINT (Bruker, 2009[Bruker (2009). APEX2, SAINT and SADABS. 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, 2012[Farrugia, L. J. (2012). J. Appl. Cryst. 45, 849-854.]) and DIAMOND (Brandenburg, 2006[Brandenburg, K. (2006). DIAMOND. Crystal Impact GbR, Bonn, Germany.]); software used to prepare material for publication: publCIF (Westrip, 2010[Westrip, S. P. (2010). J. Appl. Cryst. 43, 920-925.]).

Supporting information


Comment top

Widespread studies were devoted to metal-based phosphates, either with open-framework structures, or in terms of porous materials. Within those materials, the anionic framework, generally constructed from PO4 tetrahedra connected to metal (M) cations in different coordination environments MOn (with n = 4, 5 and 6), can generate pores and channels offering a suitable environment to accommodate various other cations. Besides their high chemical activity and their thermal stability (Morozov et al., 2003), such metal-based phosphates have some interesting properties leading to applications such as in catalysis (Cheetham et al., 1999; Viter & Nagornyi, 2009), ion-exchangers (Clearfield, 1988; Joschi et al., 2008), gas sorption (Forster et al., 2003), or batteries (Trad et al., 2010).

Our interest is particularly focused on hydrothermally synthesized orthophosphates within the ternary systems MO–M'O–P2O5 with M and M' = divalent cations. We have recently characterized some new lead cobalt or manganese phosphates, viz. Co2Pb(HPO4)(PO4)OH.H2O (Assani et al., 2012a) and Pb2Mn3(HPO4)2(PO4)2 (Assani et al., 2012b). In line with the focus of our research, the present paper describes the hydrothermal synthesis and the structural characterization of a new strontium manganese phosphate, Sr2Mn3(HPO4)2(PO4)2, that is isotypic with its lead analogue, Pb2Mn3(HPO4)2(PO4)2. These two phosphates are characterized by an Mn:P ratio = 3:4, which is rarely observed, with the exception of some copper-based orthophosphates, Pb3Cu3(PO4)4 and Sr3Cu3(PO4)4 (Effenberger, 1999), also with Cu:P = 3:4.

In the structure of the title compound, one of the two manganese sites (Mn1) is located on a centre of inversion, while all remaining atoms are in general positions. A part of the structure, as given in Fig. 1, shows the different types of polyhedra around the metal positions and the P atoms. The centrosymmetric Mn1O6 octahedron is linked to two distorted Mn2O6 octahedra by a common edge, thus forming infinite zigzag chains with composition [Mn3O14] running parallel to [010] (Fig. 2). Adjacent chains are linked to each other through PO4 and PO3OH tetrahedra, via common corners or edges, leading to the formation of layers parallel to (100). The cohesion of the crystal structure is ensured on one hand by the presence of the Sr2+ cations in the interlayer space and on the other hand by strong O—H···O hydrogen bonds between sheets (Fig. 2 and Table 2).

In the structure of the title compound, the Sr2+ cation is surrounded by nine O atoms instead of eight as in the case of Pb2Mn3(HPO4)2(PO4)2. All other bond lengths and angles are similar in the two structures, with the exception of the Mn2—O bond lengths. In the title structure, four medium-long bonds in the range 2.1189 (10) to 2.1875 (9) Å and two longer bonds of 2.4079 (12) and 2.4609 (11) Å are observed, whereas in the lead analogue five medium-long bonds in the range 2.094 (4) to 2.235 (4) Å and one considerably long bond of 2.610 (4) Å is observed.

Related literature top

For isotypic Pb2Mn3(HPO4)2(PO4)2, see: Assani et al. (2012b). For related structures, see: Assani et al. (2012a); Effenberger (1999). For the thermal stability of similar compounds, see: Morozov et al. (2003). For applications of phosphates, see: Cheetham et al. (1999); Viter & Nagornyi (2009); Forster et al. (2003); Clearfield (1988); Joschi et al. (2008); Trad et al. (2010).

Experimental top

Transparent crystals of Sr2Mn3(HPO4)2(PO4)2 were isolated from hydrothermal treatment of the reaction mixture of strontium, manganese, sodium and phosphate precursors in a proportion corresponding to the molar ratio Sr: Mn: Na: P: = 4: 4.5: 1: 6. The hydrothermal reaction was conducted in a 23 ml Teflon-lined autoclave filled to 50% with distilled water and under autogenously pressure at 473 K for five days. After being filtered off, washed with deionized water and air-dried, the reaction product consisted of colourless crystals with a platy form.

Refinement top

The O-bound H atom was initially located in a difference map and refined with O—H distance restraint of 0.82 (1) Å. In the last cycle it was refined in the riding model approximation with Uiso(H) set to 1.5Ueq(O). The highest peak and the deepest hole in the final Fourier map are at 0.64 Å and 0.55 Å, from Mn2.

Computing details top

Data collection: APEX2 (Bruker, 2009); cell refinement: SAINT (Bruker, 2009); data reduction: SAINT (Bruker, 2009); 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).

Figures top
[Figure 1] Fig. 1. : A partial plot of the crystal structure of the title compound. Displacement ellipsoids are drawn at the 50% probability level. Symmetry codes: (i) -x + 1, y - 1/2, -z + 1/2; (ii) -x + 1, -y + 1, -z + 1; (iii) x, -y + 3/2, z - 1/2; (iv) -x + 2, -y + 1, -z + 1; (v) x + 1, -y + 3/2, z + 1/2; (vi) x + 1, y, z; (vii) -x + 1, y + 1/2, -z + 1/2; (viii) x, -y + 3/2, z + 1/2.
[Figure 2] Fig. 2. : Polyhedral representation of Sr2Mn3(HPO4)2(PO4)2, showing Sr2+ cations between layers and O—H···O hydrogen bonds (dashed lines) between the sheets.
Distrontium trimanganese(II) bis(hydrogenphosphate) bis(orthophosphate) top
Crystal data top
Sr2Mn3(HPO4)2(PO4)2F(000) = 682
Mr = 721.96Dx = 3.689 Mg m3
Monoclinic, P21/cMo Kα radiation, λ = 0.71073 Å
Hall symbol: -P 2ybcCell parameters from 3138 reflections
a = 7.8535 (1) Åθ = 2.7–36.3°
b = 8.7793 (2) ŵ = 11.58 mm1
c = 9.6165 (2) ÅT = 296 K
β = 101.434 (1)°Sheet, colourless
V = 649.88 (2) Å30.33 × 0.24 × 0.12 mm
Z = 2
Data collection top
Bruker APEXII CCD
diffractometer
3138 independent reflections
Radiation source: fine-focus sealed tube2874 reflections with I > 2σ(I)
Graphite monochromatorRint = 0.025
ϕ and ω scansθmax = 36.3°, θmin = 2.7°
Absorption correction: multi-scan
(SADABS; Bruker (2009)
h = 1312
Tmin = 0.046, Tmax = 0.215k = 1414
12425 measured reflectionsl = 1616
Refinement top
Refinement on F2Primary atom site location: structure-invariant direct methods
Least-squares matrix: fullSecondary atom site location: difference Fourier map
R[F2 > 2σ(F2)] = 0.019Hydrogen site location: difference Fourier map
wR(F2) = 0.045H-atom parameters constrained
S = 1.06 w = 1/[σ2(Fo2) + (0.0211P)2 + 0.239P]
where P = (Fo2 + 2Fc2)/3
3138 reflections(Δ/σ)max = 0.002
115 parametersΔρmax = 0.58 e Å3
0 restraintsΔρmin = 0.54 e Å3
Crystal data top
Sr2Mn3(HPO4)2(PO4)2V = 649.88 (2) Å3
Mr = 721.96Z = 2
Monoclinic, P21/cMo Kα radiation
a = 7.8535 (1) ŵ = 11.58 mm1
b = 8.7793 (2) ÅT = 296 K
c = 9.6165 (2) Å0.33 × 0.24 × 0.12 mm
β = 101.434 (1)°
Data collection top
Bruker APEXII CCD
diffractometer
3138 independent reflections
Absorption correction: multi-scan
(SADABS; Bruker (2009)
2874 reflections with I > 2σ(I)
Tmin = 0.046, Tmax = 0.215Rint = 0.025
12425 measured reflections
Refinement top
R[F2 > 2σ(F2)] = 0.0190 restraints
wR(F2) = 0.045H-atom parameters constrained
S = 1.06Δρmax = 0.58 e Å3
3138 reflectionsΔρmin = 0.54 e Å3
115 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
Sr10.573794 (17)0.478038 (15)0.234323 (14)0.00999 (3)
Mn11.00000.50000.50000.00677 (5)
Mn20.89650 (3)0.85638 (2)0.40357 (2)0.00891 (4)
P10.14462 (4)0.70256 (4)0.22974 (3)0.00542 (6)
P20.65079 (4)0.71451 (4)0.56233 (3)0.00649 (6)
O10.06059 (13)0.67784 (12)0.35944 (10)0.00966 (17)
O20.06622 (13)0.59473 (11)0.10796 (10)0.01019 (17)
O30.11920 (13)0.86980 (11)0.18530 (11)0.01016 (17)
O40.34252 (13)0.67330 (12)0.27411 (10)0.01050 (17)
O50.70244 (14)0.69325 (14)0.72158 (10)0.0141 (2)
O60.75819 (13)0.62546 (12)0.47491 (11)0.01179 (18)
O70.65059 (15)0.88211 (12)0.51673 (11)0.01383 (19)
O80.45824 (13)0.65486 (13)0.53325 (11)0.01209 (19)
H80.41690.66070.44820.018*
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
Sr10.00960 (6)0.01026 (6)0.01085 (5)0.00204 (4)0.00384 (4)0.00216 (4)
Mn10.00742 (11)0.00597 (11)0.00692 (11)0.00076 (8)0.00144 (8)0.00002 (8)
Mn20.00962 (9)0.00758 (9)0.00837 (8)0.00006 (6)0.00103 (6)0.00030 (6)
P10.00572 (12)0.00557 (12)0.00475 (12)0.00013 (10)0.00052 (9)0.00000 (9)
P20.00632 (13)0.00796 (13)0.00540 (12)0.00034 (10)0.00167 (10)0.00007 (10)
O10.0108 (4)0.0108 (4)0.0085 (4)0.0003 (3)0.0047 (3)0.0012 (3)
O20.0137 (4)0.0079 (4)0.0073 (4)0.0001 (3)0.0019 (3)0.0020 (3)
O30.0126 (4)0.0057 (4)0.0109 (4)0.0000 (3)0.0007 (3)0.0021 (3)
O40.0064 (4)0.0154 (5)0.0093 (4)0.0019 (3)0.0007 (3)0.0004 (3)
O50.0105 (4)0.0256 (6)0.0055 (4)0.0009 (4)0.0002 (3)0.0008 (4)
O60.0109 (4)0.0151 (5)0.0104 (4)0.0054 (4)0.0047 (3)0.0002 (3)
O70.0202 (5)0.0076 (4)0.0148 (4)0.0001 (4)0.0061 (4)0.0003 (3)
O80.0074 (4)0.0203 (5)0.0083 (4)0.0033 (4)0.0008 (3)0.0009 (3)
Geometric parameters (Å, º) top
Sr1—O3i2.5641 (10)Mn2—O1vi2.1248 (10)
Sr1—O42.5806 (10)Mn2—O5iii2.1256 (10)
Sr1—O8ii2.5775 (11)Mn2—O2v2.1875 (9)
Sr1—O7iii2.5981 (11)Mn2—O72.4079 (12)
Sr1—O5ii2.7409 (11)Mn2—O62.4609 (11)
Sr1—O4i2.7599 (11)P1—O31.5312 (10)
Sr1—O62.7923 (10)P1—O21.5365 (10)
Sr1—O7i2.8207 (11)P1—O11.5377 (10)
Sr1—O5iii3.0680 (12)P1—O41.5494 (10)
Mn1—O62.1670 (10)P2—O51.5160 (10)
Mn1—O6iv2.1670 (10)P2—O61.5201 (11)
Mn1—O3v2.1672 (9)P2—O71.5352 (11)
Mn1—O3i2.1672 (9)P2—O81.5721 (11)
Mn1—O1ii2.1786 (10)P2—Sr1viii3.2838 (4)
Mn1—O1vi2.1786 (10)O8—H80.8200
Mn2—O2vii2.1189 (10)
O3i—Sr1—O4148.09 (3)O6iv—Mn1—O3i92.85 (4)
O3i—Sr1—O8ii79.54 (3)O3v—Mn1—O3i180.0
O4—Sr1—O8ii88.83 (3)O6—Mn1—O1ii97.99 (4)
O3i—Sr1—O7iii93.63 (3)O6iv—Mn1—O1ii82.01 (4)
O4—Sr1—O7iii95.05 (3)O3v—Mn1—O1ii88.84 (4)
O8ii—Sr1—O7iii172.09 (3)O3i—Mn1—O1ii91.16 (4)
O3i—Sr1—O5ii118.41 (3)O6—Mn1—O1vi82.01 (4)
O4—Sr1—O5ii74.91 (4)O6iv—Mn1—O1vi97.99 (4)
O8ii—Sr1—O5ii53.21 (3)O3v—Mn1—O1vi91.16 (4)
O7iii—Sr1—O5ii134.52 (3)O3i—Mn1—O1vi88.84 (4)
O3i—Sr1—O4i55.56 (3)O1ii—Mn1—O1vi180.0
O4—Sr1—O4i145.79 (2)O2vii—Mn2—O1vi128.50 (4)
O8ii—Sr1—O4i69.60 (3)O2vii—Mn2—O5iii104.08 (4)
O7iii—Sr1—O4i109.86 (3)O1vi—Mn2—O5iii92.78 (4)
O5ii—Sr1—O4i70.92 (3)O2vii—Mn2—O2v77.72 (4)
O3i—Sr1—O667.65 (3)O1vi—Mn2—O2v92.21 (4)
O4—Sr1—O680.44 (3)O5iii—Mn2—O2v171.78 (4)
O8ii—Sr1—O667.36 (3)O2vii—Mn2—O793.58 (4)
O7iii—Sr1—O6106.45 (3)O1vi—Mn2—O7137.06 (4)
O5ii—Sr1—O6114.99 (3)O5iii—Mn2—O783.28 (4)
O4i—Sr1—O6112.72 (3)O2v—Mn2—O788.62 (4)
O3i—Sr1—O7i122.54 (3)O2vii—Mn2—O6154.34 (4)
O4—Sr1—O7i89.23 (3)O1vi—Mn2—O676.51 (4)
O8ii—Sr1—O7i117.08 (3)O5iii—Mn2—O677.09 (4)
O7iii—Sr1—O7i69.95 (4)O2v—Mn2—O697.77 (4)
O5ii—Sr1—O7i65.75 (3)O7—Mn2—O660.88 (4)
O4i—Sr1—O7i78.31 (3)O3—P1—O2111.57 (5)
O6—Sr1—O7i168.81 (3)O3—P1—O1107.97 (6)
O3i—Sr1—O5iii93.62 (3)O2—P1—O1111.08 (6)
O4—Sr1—O5iii68.17 (3)O3—P1—O4107.70 (6)
O8ii—Sr1—O5iii123.36 (3)O2—P1—O4109.65 (6)
O7iii—Sr1—O5iii52.59 (3)O1—P1—O4108.76 (6)
O5ii—Sr1—O5iii143.06 (3)O5—P2—O6115.38 (6)
O4i—Sr1—O5iii145.93 (3)O5—P2—O7113.04 (6)
O6—Sr1—O5iii58.42 (3)O6—P2—O7107.71 (6)
O7i—Sr1—O5iii113.67 (3)O5—P2—O8101.19 (6)
O6—Mn1—O6iv180.0O6—P2—O8110.48 (6)
O6—Mn1—O3v92.85 (4)O7—P2—O8108.78 (6)
O6iv—Mn1—O3v87.15 (4)O5—P2—Mn2120.08 (4)
O6—Mn1—O3i87.15 (4)
Symmetry codes: (i) x+1, y1/2, z+1/2; (ii) x+1, y+1, z+1; (iii) x, y+3/2, z1/2; (iv) x+2, y+1, z+1; (v) x+1, y+3/2, z+1/2; (vi) x+1, y, z; (vii) x+1, y+1/2, z+1/2; (viii) x, y+3/2, z+1/2.
Hydrogen-bond geometry (Å, º) top
D—H···AD—HH···AD···AD—H···A
O8—H8···O40.821.662.4828 (14)177

Experimental details

Crystal data
Chemical formulaSr2Mn3(HPO4)2(PO4)2
Mr721.96
Crystal system, space groupMonoclinic, P21/c
Temperature (K)296
a, b, c (Å)7.8535 (1), 8.7793 (2), 9.6165 (2)
β (°) 101.434 (1)
V3)649.88 (2)
Z2
Radiation typeMo Kα
µ (mm1)11.58
Crystal size (mm)0.33 × 0.24 × 0.12
Data collection
DiffractometerBruker APEXII CCD
diffractometer
Absorption correctionMulti-scan
(SADABS; Bruker (2009)
Tmin, Tmax0.046, 0.215
No. of measured, independent and
observed [I > 2σ(I)] reflections
12425, 3138, 2874
Rint0.025
(sin θ/λ)max1)0.833
Refinement
R[F2 > 2σ(F2)], wR(F2), S 0.019, 0.045, 1.06
No. of reflections3138
No. of parameters115
H-atom treatmentH-atom parameters constrained
Δρmax, Δρmin (e Å3)0.58, 0.54

Computer programs: APEX2 (Bruker, 2009), SAINT (Bruker, 2009), SHELXS97 (Sheldrick, 2008), SHELXL97 (Sheldrick, 2008), ORTEP-3 for Windows (Farrugia, 2012) and DIAMOND (Brandenburg, 2006), publCIF (Westrip, 2010).

Hydrogen-bond geometry (Å, º) top
D—H···AD—HH···AD···AD—H···A
O8—H8···O40.821.662.4828 (14)177.3
 

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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