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The structure of the title compound, sodium calcium niobate oxide arsenate, NaCa1.5(NbO)2O2(AsO4)2, is built up from chains of NbO6 octahedra, parallel to the c axis, corner-sharing with AsO4. There are two types of AsO4 tetrahedron; one is connected to three different NbO6 octahedra, whereas the other is linked to two NbO6 octahedra only. The non-bonded O atoms point towards the inter-layer space where the sodium and calcium ions are located. A relationship between the structure of the title compound and the related Na3SbO(PO4)2 (one-dimensional), Na2NbO2AsO4(two-dimensional) and NaVOAsO4 and SbOPO4 (three-dimensional) structures is discussed.

Supporting information

cif

Crystallographic Information File (CIF) https://doi.org/10.1107/S1600536805031429/dn6243sup1.cif
Contains datablocks I, global

hkl

Structure factor file (CIF format) https://doi.org/10.1107/S1600536805031429/dn6243Isup2.hkl
Contains datablock I

Key indicators

  • Single-crystal X-ray study
  • T = 298 K
  • Mean [sigma](As-O) = 0.002 Å
  • R factor = 0.019
  • wR factor = 0.051
  • Data-to-parameter ratio = 16.4

checkCIF/PLATON results

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Alert level C PLAT042_ALERT_1_C Calc. and Rep. MoietyFormula Strings Differ .... ? PLAT301_ALERT_3_C Main Residue Disorder ......................... 2.00 Perc.
0 ALERT level A = In general: serious problem 0 ALERT level B = Potentially serious problem 2 ALERT level C = Check and explain 0 ALERT level G = General alerts; check 1 ALERT type 1 CIF construction/syntax error, inconsistent or missing data 0 ALERT type 2 Indicator that the structure model may be wrong or deficient 1 ALERT type 3 Indicator that the structure quality may be low 0 ALERT type 4 Improvement, methodology, query or suggestion

Computing details top

Data collection: CAD-4 EXPRESS (Duisenberg, 1992; Macíček & Yordanov, 1992; Enraf–Nonius, 1994); cell refinement: CAD-4 EXPRESS; data reduction: XCAD4 (Harms & Wocadlo, 1995); program(s) used to solve structure: SHELXS97 (Sheldrick, 1997); program(s) used to refine structure: SHELXL97 (Sheldrick, 1997); molecular graphics: DIAMOND (Brandenburg, 1998), ORTEPIII (Burnett & Johnson, 1996) and ORTEP-3 for Windows (Farrugia, 1997); software used to prepare material for publication: SHELXL97.

sodium calcium niobate oxide arsenate top
Crystal data top
NaCa1.5(NbO)2O2(AsO4)2F(000) = 1140
Mr = 610.78Dx = 3.977 Mg m3
Monoclinic, C2/cMo Kα radiation, λ = 0.71073 Å
Hall symbol: -C 2ycCell parameters from 25 reflections
a = 6.730 (2) Åθ = 12–14°
b = 22.302 (3) ŵ = 9.54 mm1
c = 7.4309 (9) ÅT = 298 K
β = 113.827 (1)°Prisme, colorless
V = 1020.3 (4) Å30.16 × 0.12 × 0.10 mm
Z = 4
Data collection top
Enraf–Nonius CAD-4
diffractometer
1337 reflections with I > 2σ(I)
Radiation source: fine-focus sealed tubeRint = 0.015
Graphite monochromatorθmax = 30.0°, θmin = 3.4°
ω/2θ scansh = 89
Absorption correction: ψ scan
(North et al., 1968)
k = 131
Tmin = 0.261, Tmax = 0.386l = 101
1683 measured reflections2 standard reflections every 120 min
1495 independent reflections intensity decay: 1.2%
Refinement top
Refinement on F20 restraints
Least-squares matrix: fullPrimary atom site location: structure-invariant direct methods
R[F2 > 2σ(F2)] = 0.019Secondary atom site location: difference Fourier map
wR(F2) = 0.051 w = 1/[σ2(Fo2) + (0.0195P)2 + 2.343P]
where P = (Fo2 + 2Fc2)/3
S = 1.10(Δ/σ)max = 0.021
1495 reflectionsΔρmax = 0.65 e Å3
91 parametersΔρmin = 0.75 e Å3
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 > σ(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*/UeqOcc. (<1)
Nb0.00565 (4)0.357919 (10)0.51029 (3)0.00618 (8)
As10.50000.417962 (18)0.25000.00927 (10)
As20.00000.221982 (17)0.25000.00575 (9)
Na0.50000.44084 (10)0.75000.0347 (6)
Ca10.00000.48192 (4)0.25000.00806 (16)0.87
Ca20.50000.27733 (7)0.25000.0219 (3)0.63
O10.0977 (3)0.26328 (9)0.3858 (3)0.0134 (4)
O20.00000.32411 (13)0.75000.0086 (5)
O30.0752 (4)0.43450 (10)0.5814 (3)0.0132 (4)
O40.3221 (3)0.36857 (10)0.4147 (3)0.0122 (4)
O50.3118 (3)0.32501 (11)0.5945 (3)0.0179 (5)
O60.6303 (4)0.45972 (11)0.3518 (4)0.0212 (5)
O70.00000.37148 (13)0.25000.0092 (5)
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
Nb0.00677 (12)0.00712 (13)0.00501 (12)0.00071 (8)0.00274 (9)0.00041 (8)
As10.00533 (17)0.00707 (18)0.0140 (2)0.0000.00240 (15)0.000
As20.00513 (17)0.00619 (17)0.00617 (17)0.0000.00254 (13)0.000
Na0.0201 (10)0.0183 (10)0.0600 (16)0.0000.0104 (11)0.000
Ca10.0090 (4)0.0075 (4)0.0091 (4)0.0000.0051 (3)0.000
Ca20.0189 (7)0.0120 (6)0.0320 (8)0.0000.0074 (6)0.000
O10.0196 (10)0.0080 (9)0.0197 (10)0.0023 (8)0.0152 (9)0.0044 (8)
O20.0124 (13)0.0089 (12)0.0045 (12)0.0000.0036 (10)0.000
O30.0172 (10)0.0118 (10)0.0126 (9)0.0012 (8)0.0081 (8)0.0019 (8)
O40.0066 (9)0.0140 (9)0.0148 (10)0.0020 (8)0.0033 (8)0.0043 (8)
O50.0102 (10)0.0254 (12)0.0195 (11)0.0093 (9)0.0074 (9)0.0130 (9)
O60.0119 (10)0.0182 (11)0.0325 (13)0.0025 (9)0.0081 (10)0.0122 (10)
O70.0131 (13)0.0092 (12)0.0068 (12)0.0000.0056 (10)0.000
Geometric parameters (Å, º) top
Nb—O31.793 (2)Na—As1iii3.149 (2)
Nb—O71.9428 (6)Na—Nbx3.5880 (14)
Nb—O21.9488 (12)Na—Ca1xii3.7802 (14)
Nb—O52.033 (2)Ca1—O6ii2.342 (2)
Nb—O42.040 (2)Ca1—O6viii2.342 (2)
Nb—O12.297 (2)Ca1—O3iii2.411 (2)
Nb—Ca13.3661 (8)Ca1—O3xiii2.411 (2)
Nb—Ca2i3.5111 (13)Ca1—O72.463 (3)
Nb—Na3.5880 (14)Ca1—O3v2.536 (2)
Nb—Ca23.6378 (11)Ca1—O32.536 (2)
As1—O61.657 (2)Ca1—Nbv3.3661 (8)
As1—O6ii1.657 (2)Ca1—As1viii3.6548 (10)
As1—O4ii1.721 (2)Ca1—Naxii3.7802 (14)
As1—O41.721 (2)Ca2—O2i2.262 (3)
As1—Ca23.1363 (16)Ca2—O42.426 (3)
As1—Naiii3.149 (2)Ca2—O4ii2.426 (3)
As1—Ca13.6548 (10)Ca2—O1ii2.498 (2)
As1—Ca1iv3.6548 (10)Ca2—O12.498 (2)
As2—O11.684 (2)Ca2—O1vi2.672 (2)
As2—O1v1.684 (2)Ca2—O1i2.672 (2)
As2—O5vi1.690 (2)Ca2—Nbvi3.5111 (13)
As2—O5vii1.690 (2)Ca2—Nbi3.5111 (13)
As2—Ca2viii3.5843 (11)Ca2—As2iv3.5843 (11)
As2—Ca23.5843 (11)O1—Ca2i2.672 (2)
Na—O6ix2.607 (3)O2—Nbxi1.9488 (11)
Na—O6iii2.607 (3)O2—Ca2i2.262 (3)
Na—O32.621 (2)O3—Ca1iii2.411 (2)
Na—O3x2.621 (2)O5—As2vii1.690 (2)
Na—O6xi2.758 (3)O6—Ca1iv2.342 (2)
Na—O6viii2.758 (3)O6—Naiii2.607 (3)
Na—O52.903 (3)O6—Naiv2.758 (3)
Na—O5x2.903 (3)O7—Nbv1.9428 (6)
O3—Nb—O792.45 (11)O3xiii—Ca1—O7140.63 (5)
O3—Nb—O2101.45 (10)O6ii—Ca1—O3v80.14 (8)
O7—Nb—O2166.04 (12)O6viii—Ca1—O3v89.71 (8)
O3—Nb—O598.13 (10)O3iii—Ca1—O3v145.65 (8)
O7—Nb—O588.43 (7)O3xiii—Ca1—O3v79.59 (8)
O2—Nb—O588.30 (7)O7—Ca1—O3v65.35 (5)
O3—Nb—O496.24 (9)O6ii—Ca1—O389.71 (8)
O7—Nb—O492.97 (6)O6viii—Ca1—O380.14 (8)
O2—Nb—O486.88 (6)O3iii—Ca1—O379.59 (8)
O5—Nb—O4165.49 (9)O3xiii—Ca1—O3145.65 (8)
O3—Nb—O1174.00 (9)O7—Ca1—O365.35 (5)
O7—Nb—O182.02 (10)O3v—Ca1—O3130.70 (10)
O2—Nb—O184.15 (9)O6ii—Ca1—Nbv82.92 (7)
O5—Nb—O184.07 (9)O6viii—Ca1—Nbv77.05 (6)
O4—Nb—O181.82 (8)O3iii—Ca1—Nbv167.89 (5)
O3—Nb—Ca147.76 (7)O3xiii—Ca1—Nbv107.01 (5)
O7—Nb—Ca146.28 (9)O7—Ca1—Nbv34.759 (11)
O2—Nb—Ca1147.48 (8)O3v—Ca1—Nbv31.56 (5)
O5—Nb—Ca1104.38 (6)O3—Ca1—Nbv99.60 (6)
O4—Nb—Ca186.83 (6)O6ii—Ca1—Nb77.05 (6)
O1—Nb—Ca1126.32 (6)O6viii—Ca1—Nb82.92 (7)
O3—Nb—Ca2i136.38 (7)O3iii—Ca1—Nb107.01 (5)
O7—Nb—Ca2i129.72 (9)O3xiii—Ca1—Nb167.89 (5)
O2—Nb—Ca2i36.45 (8)O7—Ca1—Nb34.759 (11)
O5—Nb—Ca2i75.58 (6)O3v—Ca1—Nb99.60 (6)
O4—Nb—Ca2i92.57 (6)O3—Ca1—Nb31.56 (5)
O1—Nb—Ca2i49.56 (6)Nbv—Ca1—Nb69.52 (2)
Ca1—Nb—Ca2i175.859 (16)O6ii—Ca1—As119.90 (6)
O7—Nb—Na93.17 (5)O6viii—Ca1—As1140.83 (7)
O2—Nb—Na95.87 (4)O3iii—Ca1—As185.13 (5)
O5—Nb—Na53.99 (8)O3xiii—Ca1—As1133.50 (5)
O4—Nb—Na140.20 (7)O7—Ca1—As167.028 (16)
O1—Nb—Na137.98 (6)O3v—Ca1—As190.83 (5)
Ca1—Nb—Na69.80 (3)O3—Ca1—As170.12 (5)
Ca2i—Nb—Na112.88 (3)Nbv—Ca1—As183.262 (18)
O3—Nb—Ca2134.75 (7)Nb—Ca1—As158.402 (12)
O7—Nb—Ca284.82 (5)O6ii—Ca1—As1viii140.83 (7)
O2—Nb—Ca286.29 (4)O6viii—Ca1—As1viii19.90 (6)
O5—Nb—Ca2126.83 (8)O3iii—Ca1—As1viii133.50 (5)
O4—Nb—Ca239.16 (7)O3xiii—Ca1—As1viii85.13 (5)
O1—Nb—Ca242.76 (6)O7—Ca1—As1viii67.028 (16)
Ca1—Nb—Ca2108.023 (19)O3v—Ca1—As1viii70.12 (5)
Ca2i—Nb—Ca269.254 (14)O3—Ca1—As1viii90.83 (5)
Na—Nb—Ca2177.76 (2)Nbv—Ca1—As1viii58.402 (12)
O6—As1—O6ii111.60 (18)Nb—Ca1—As1viii83.262 (18)
O6—As1—O4ii109.89 (11)As1—Ca1—As1viii134.06 (3)
O6ii—As1—O4ii112.30 (12)O6ii—Ca1—Naxii157.77 (6)
O6—As1—O4112.30 (12)O6viii—Ca1—Naxii42.86 (7)
O6ii—As1—O4109.89 (11)O3iii—Ca1—Naxii91.23 (6)
O4ii—As1—O4100.39 (15)O3xiii—Ca1—Naxii43.44 (6)
O6—As1—Ca2124.20 (9)O7—Ca1—Naxii117.11 (3)
O6ii—As1—Ca2124.20 (9)O3v—Ca1—Naxii91.07 (5)
O4ii—As1—Naiii129.80 (7)O3—Ca1—Naxii111.19 (5)
O4—As1—Naiii129.80 (7)Nbv—Ca1—Naxii100.24 (3)
Ca2—As1—Naiii180.0Nb—Ca1—Naxii124.81 (3)
O6—As1—Ca1115.97 (9)As1—Ca1—Naxii175.86 (4)
O4ii—As1—Ca1128.74 (7)As1viii—Ca1—Naxii50.08 (3)
O4—As1—Ca182.75 (7)O2i—Ca2—O4146.99 (5)
Ca2—As1—Ca1112.972 (16)O2i—Ca2—O4ii146.99 (5)
Naiii—As1—Ca167.028 (16)O4—Ca2—O4ii66.03 (10)
O6ii—As1—Ca1iv115.97 (9)O2i—Ca2—O1ii82.79 (6)
O4ii—As1—Ca1iv82.75 (7)O4—Ca2—O1ii122.85 (8)
O4—As1—Ca1iv128.74 (7)O4ii—Ca2—O1ii70.61 (7)
Ca2—As1—Ca1iv112.972 (16)O2i—Ca2—O182.79 (6)
Naiii—As1—Ca1iv67.028 (16)O4—Ca2—O170.61 (7)
Ca1—As1—Ca1iv134.06 (3)O4ii—Ca2—O1122.85 (8)
O1—As2—O1v113.67 (14)O1ii—Ca2—O1165.59 (12)
O1—As2—O5vi112.50 (11)O2i—Ca2—O1vi70.19 (5)
O1v—As2—O5vi107.22 (11)O4—Ca2—O1vi131.65 (8)
O1—As2—O5vii107.22 (11)O4ii—Ca2—O1vi84.49 (7)
O1v—As2—O5vii112.50 (10)O1ii—Ca2—O1vi76.43 (7)
O5vi—As2—O5vii103.32 (18)O1—Ca2—O1vi98.61 (7)
O1—As2—Ca2viii113.93 (8)O2i—Ca2—O1i70.19 (5)
O5vi—As2—Ca2viii131.15 (7)O4—Ca2—O1i84.49 (7)
O5vii—As2—Ca2viii76.66 (8)O4ii—Ca2—O1i131.65 (8)
O1v—As2—Ca2113.93 (8)O1ii—Ca2—O1i98.61 (7)
O5vi—As2—Ca276.66 (8)O1—Ca2—O1i76.43 (7)
O5vii—As2—Ca2131.15 (7)O1vi—Ca2—O1i140.37 (11)
Ca2viii—As2—Ca2139.71 (5)O2i—Ca2—As1180.0
O6ix—Na—O6iii63.43 (11)O4—Ca2—As133.01 (5)
O6ix—Na—O375.81 (8)O4ii—Ca2—As133.01 (5)
O6iii—Na—O3109.70 (9)O1ii—Ca2—As197.21 (6)
O6ix—Na—O3x109.70 (9)O1—Ca2—As197.21 (6)
O6iii—Na—O3x75.81 (8)O1vi—Ca2—As1109.81 (5)
O3—Na—O3x173.81 (14)O1i—Ca2—As1109.81 (5)
O6ix—Na—O6xi63.71 (9)O2i—Ca2—Nbvi30.784 (14)
O6iii—Na—O6xi100.55 (8)O4—Ca2—Nbvi150.70 (5)
O3—Na—O6xi109.51 (7)O4ii—Ca2—Nbvi124.66 (5)
O3x—Na—O6xi71.49 (7)O1ii—Ca2—Nbvi85.38 (6)
O6ix—Na—O6viii100.55 (8)O1—Ca2—Nbvi82.24 (5)
O6iii—Na—O6viii63.71 (9)O1vi—Ca2—Nbvi40.85 (5)
O3—Na—O6viii71.49 (7)O1i—Ca2—Nbvi100.02 (6)
O3x—Na—O6viii109.51 (7)As1—Ca2—Nbvi149.216 (14)
O6xi—Na—O6viii162.44 (13)O2i—Ca2—Nbi30.784 (14)
O6ix—Na—O5136.76 (7)O4—Ca2—Nbi124.66 (5)
O6iii—Na—O5141.74 (7)O4ii—Ca2—Nbi150.70 (5)
O3—Na—O562.96 (7)O1ii—Ca2—Nbi82.24 (5)
O3x—Na—O5111.00 (9)O1—Ca2—Nbi85.38 (6)
O6xi—Na—O5117.47 (9)O1vi—Ca2—Nbi100.02 (6)
O6viii—Na—O579.07 (7)O1i—Ca2—Nbi40.85 (5)
O6ix—Na—O5x141.74 (7)As1—Ca2—Nbi149.216 (14)
O6iii—Na—O5x136.76 (7)Nbvi—Ca2—Nbi61.57 (3)
O3—Na—O5x111.00 (9)O2i—Ca2—As2iv69.86 (2)
O3x—Na—O5x62.96 (7)O4—Ca2—As2iv124.10 (5)
O6xi—Na—O5x79.07 (7)O4ii—Ca2—As2iv90.97 (5)
O6viii—Na—O5x117.47 (9)O1ii—Ca2—As2iv24.82 (5)
O5—Na—O5x54.32 (9)O1—Ca2—As2iv145.21 (7)
O6ix—Na—As1iii31.71 (6)O1vi—Ca2—As2iv92.08 (5)
O6iii—Na—As1iii31.71 (6)O1i—Ca2—As2iv74.34 (5)
O3—Na—As1iii93.10 (7)As1—Ca2—As2iv110.14 (2)
O3x—Na—As1iii93.10 (7)Nbvi—Ca2—As2iv84.65 (3)
O6xi—Na—As1iii81.22 (7)Nbi—Ca2—As2iv60.102 (18)
O6viii—Na—As1iii81.22 (7)O2i—Ca2—As269.86 (2)
O5—Na—As1iii152.84 (5)O4—Ca2—As290.97 (5)
O5x—Na—As1iii152.84 (5)O4ii—Ca2—As2124.10 (5)
O6ix—Na—Nb103.26 (5)O1ii—Ca2—As2145.21 (7)
O6iii—Na—Nb130.36 (6)O1—Ca2—As224.82 (5)
O3—Na—Nb28.50 (5)O1vi—Ca2—As274.34 (5)
O3x—Na—Nb145.40 (9)O1i—Ca2—As292.08 (5)
O6xi—Na—Nb116.14 (5)As1—Ca2—As2110.14 (2)
O6viii—Na—Nb73.55 (5)Nbvi—Ca2—As260.102 (18)
O5x—Na—Nb84.66 (7)Nbi—Ca2—As284.65 (3)
As1iii—Na—Nb121.03 (3)As2iv—Ca2—As2139.71 (5)
O6ix—Na—Nbx130.36 (6)As2—O1—Nb128.03 (11)
O6iii—Na—Nbx103.26 (5)As2—O1—Ca2116.65 (11)
O3—Na—Nbx145.40 (9)Nb—O1—Ca298.62 (8)
O3x—Na—Nbx28.50 (5)As2—O1—Ca2i115.19 (11)
O6xi—Na—Nbx73.55 (5)Nb—O1—Ca2i89.59 (8)
O6viii—Na—Nbx116.14 (5)Ca2—O1—Ca2i103.57 (7)
O5—Na—Nbx84.66 (7)Nbxi—O2—Nb134.47 (16)
O5x—Na—Nbx34.50 (4)Nbxi—O2—Ca2i112.77 (8)
As1iii—Na—Nbx121.03 (3)Nb—O2—Ca2i112.77 (8)
Nb—Na—Nbx117.95 (6)Nb—O3—Ca1iii143.58 (11)
O6ix—Na—Ca1xii90.93 (7)Nb—O3—Ca1100.68 (9)
O6iii—Na—Ca1xii37.68 (5)Ca1iii—O3—Ca1100.41 (8)
O3—Na—Ca1xii145.45 (7)Nb—O3—Na107.27 (11)
O3x—Na—Ca1xii39.25 (5)Ca1iii—O3—Na97.31 (8)
O6xi—Na—Ca1xii91.90 (5)Ca1—O3—Na101.13 (8)
O6viii—Na—Ca1xii80.08 (5)As1—O4—Nb131.75 (12)
O5—Na—Ca1xii130.59 (6)As1—O4—Ca296.79 (9)
O5x—Na—Ca1xii99.22 (5)Nb—O4—Ca2108.77 (9)
As1iii—Na—Ca1xii62.89 (3)As2vii—O5—Nb145.18 (13)
Nb—Na—Ca1xii151.852 (12)As2vii—O5—Na101.18 (11)
Nbx—Na—Ca1xii65.67 (2)Nb—O5—Na91.51 (9)
O6ii—Ca1—O6viii155.60 (13)As1—O6—Ca1iv131.33 (13)
O6ii—Ca1—O3iii84.99 (9)As1—O6—Naiii92.49 (11)
O6viii—Ca1—O3iii114.47 (8)Ca1iv—O6—Naiii99.46 (9)
O6ii—Ca1—O3xiii114.47 (8)As1—O6—Naiv113.99 (12)
O6viii—Ca1—O3xiii84.99 (9)Ca1iv—O6—Naiv102.40 (9)
O3iii—Ca1—O3xiii78.74 (10)Naiii—O6—Naiv116.29 (9)
O6ii—Ca1—O777.80 (6)Nbv—O7—Nb162.08 (17)
O6viii—Ca1—O777.80 (6)Nbv—O7—Ca198.96 (9)
O3iii—Ca1—O7140.63 (5)Nb—O7—Ca198.96 (9)
Symmetry codes: (i) x1/2, y+1/2, z+1; (ii) x1, y, z+1/2; (iii) x, y+1, z+1; (iv) x1, y, z; (v) x, y, z+1/2; (vi) x1/2, y+1/2, z1/2; (vii) x+1/2, y+1/2, z+1; (viii) x+1, y, z; (ix) x+1, y+1, z+1/2; (x) x+1, y, z+3/2; (xi) x, y, z+3/2; (xii) x+1, y+1, z+1; (xiii) x, y+1, z1/2.
 

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