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The title compound, Na+·C5H4NOS-·2H2O, (I), contains extended cationic chains of empirical formula [Na3(C5H4NOS)2(H2O)6]+, linked by C5H4NOS- moieties via an extensive hydrogen-bond network.

Supporting information

cif

Crystallographic Information File (CIF) https://doi.org/10.1107/S1600536802015003/bt6179sup1.cif
Contains datablocks global, I

hkl

Structure factor file (CIF format) https://doi.org/10.1107/S1600536802015003/bt6179Isup2.hkl
Contains datablock I

CCDC reference: 197453

Key indicators

  • Single-crystal X-ray study
  • T = 296 K
  • Mean [sigma](C-C) = 0.005 Å
  • R factor = 0.042
  • wR factor = 0.113
  • Data-to-parameter ratio = 8.9

checkCIF results

No syntax errors found

ADDSYM reports no extra symmetry


Red Alert Alert Level A:
THETM_01 Alert A The value of sine(theta_max)/wavelength is less than 0.550 Calculated sin(theta_max)/wavelength = 0.5309
Amber Alert Alert Level B:
PLAT_420 Alert B D-H Without Acceptor O(9) - H(9B) ?
Yellow Alert Alert Level C:
REFNR_01 Alert C Ratio of reflections to parameters is < 10 for a centrosymmetric structure sine(theta)/lambda 0.5309 Proportion of unique data used 1.0000 Ratio reflections to parameters 8.8932 PLAT_731 Alert C Bond Calc 0.81(5), Rep 0.82(2) .... 2.50 s.u-Ratio O9 -H9A 1.555 1.555
1 Alert Level A = Potentially serious problem
1 Alert Level B = Potential problem
2 Alert Level C = Please check

Comment top

NO COMMENT

Experimental top

Sodium pyrithione hydrate was obtained from the Aldrich Company and a single-crystal of (I) was grown by slow evaporation of an ethanolic solution. The crystal structure of (I) was shown to be representative of the bulk sample by comparison of simulated and measured powder XRD profiles (available from the author on request). Powder XRD measurements also show that an additional anhydrous sodium pyrithione phase with stoichiometry Na(C5H4NOS) is present in the bulk sample (as supplied by Aldrich). Powder XRD at 373 K shows that the hydrate (I) reverts to this anhydrous phase at elevated temperatures. On standing in air, spontaneous rehydration is observed to regenerate polycrystalline (I).

Refinement top

Exactly one hemisphere of unique data were collected, with no Friedel pairs measured; a merging R factor cannot therefore be calculated. Attempts were made at a later date to re-collect data using Mo Kα radiation, but crystals were observed to become opaque and cease diffracting in the X-ray beam. H atoms bound to C atoms were placed geometrically and allowed to ride with Ueq(H) = 1.2Ueq(C). Water H atoms were located in difference Fourier maps and refined with a common isotropic displacement parameter. The O—H distances were restrained to be equivalent, with s.u. values of 0.01 Å, with the distance refined as a single variable [final value: 0.81 (2) Å]. The H···H distances were also restrained to be 1.633 times this variable to ensure chemically reasonable H—O—H bond angles.

Computing details top

Data collection: DIF4 (Stoe & Cie, 1992); cell refinement: DIF4; data reduction: REDU4 (Stoe & Cie, 1992); program(s) used to solve structure: SHELXS97 (Sheldrick, 1997); program(s) used to refine structure: SHELXL97; molecular graphics: XP (Sheldrick, 1993); software used to prepare material for publication: SHELXL97.

Figures top
[Figure 1] Fig. 1. The asymmetric unit in (I), showing displacement ellipsoids at the 50% probability level for non-H atoms.
Sodium 1-hydroxypyridine-2(1H)-thiolate dihydrate top
Crystal data top
Na+·C5H4NOS·2H2OZ = 6
Mr = 185.17F(000) = 576
Triclinic, P1Dx = 1.540 Mg m3
a = 7.916 (4) ÅCu Kα radiation, λ = 1.5418 Å
b = 12.114 (6) ÅCell parameters from 25 reflections
c = 13.280 (7) Åθ = 40–50°
α = 106.19 (2)°µ = 3.83 mm1
β = 98.18 (1)°T = 296 K
γ = 95.43 (2)°Block, colourless
V = 1198.4 (11) Å30.30 × 0.15 × 0.15 mm
Data collection top
Stoe STADI-4
diffractometer
2387 reflections with I > 2σ(I)
Radiation source: fine-focus sealed tubeRint = 0.000
Graphite monochromatorθmax = 54.9°, θmin = 7.7°
ωθ scansh = 88
Absorption correction: ψ scan
(North et al., 1968)
k = 1212
Tmin = 0.333, Tmax = 0.563l = 014
2997 measured reflections3 standard reflections every 100 reflections
2997 independent reflections intensity decay: none
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)] = 0.042H atoms treated by a mixture of independent and constrained refinement
wR(F2) = 0.113 w = 1/[σ2(Fo2) + (0.0731P)2 + 0.4893P]
where P = (Fo2 + 2Fc2)/3
S = 1.05(Δ/σ)max = 0.008
2997 reflectionsΔρmax = 0.36 e Å3
337 parametersΔρmin = 0.32 e Å3
18 restraintsExtinction correction: SHELXL97, Fc*=kFc[1+0.001xFc2λ3/sin(2θ)]-1/4
Primary atom site location: structure-invariant direct methodsExtinction coefficient: 0.0206 (10)
Crystal data top
Na+·C5H4NOS·2H2Oγ = 95.43 (2)°
Mr = 185.17V = 1198.4 (11) Å3
Triclinic, P1Z = 6
a = 7.916 (4) ÅCu Kα radiation
b = 12.114 (6) ŵ = 3.83 mm1
c = 13.280 (7) ÅT = 296 K
α = 106.19 (2)°0.30 × 0.15 × 0.15 mm
β = 98.18 (1)°
Data collection top
Stoe STADI-4
diffractometer
2387 reflections with I > 2σ(I)
Absorption correction: ψ scan
(North et al., 1968)
Rint = 0.000
Tmin = 0.333, Tmax = 0.563θmax = 54.9°
2997 measured reflections3 standard reflections every 100 reflections
2997 independent reflections intensity decay: none
Refinement top
R[F2 > 2σ(F2)] = 0.04218 restraints
wR(F2) = 0.113H atoms treated by a mixture of independent and constrained refinement
S = 1.05Δρmax = 0.36 e Å3
2997 reflectionsΔρmin = 0.32 e Å3
337 parameters
Special details top

Experimental. Exactly one hemisphere of unique data were collected, with no Friedel pairs measured; a merging R-factor cannot be therefore calculated. Attempts were made at a later date to re-collect data using Mo Kα radiation, but crystals were observed to become opaque and cease diffracting in the X-ray beam.

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*/Ueq
S10.40949 (13)0.35563 (7)0.07946 (7)0.0397 (3)
N10.3175 (4)0.1299 (2)0.1883 (2)0.0291 (7)
O10.4022 (3)0.10627 (19)0.10342 (17)0.0346 (6)
C10.3009 (4)0.2423 (3)0.1851 (3)0.0297 (8)
C20.1925 (5)0.2561 (3)0.2734 (3)0.0371 (9)
H20.16880.33020.27230.044*
C30.1217 (5)0.1654 (3)0.3599 (3)0.0412 (9)
H30.05240.17770.41730.049*
C40.1529 (5)0.0553 (3)0.3621 (3)0.0424 (10)
H40.10930.00750.42200.051*
C50.2489 (5)0.0396 (3)0.2749 (3)0.0355 (9)
H50.26770.03510.27500.043*
S20.07976 (12)0.20546 (8)0.06565 (7)0.0399 (3)
N20.1286 (3)0.0046 (2)0.2068 (2)0.0290 (7)
O20.0256 (3)0.0356 (2)0.13287 (18)0.0365 (6)
C60.1688 (4)0.1057 (3)0.1845 (3)0.0290 (8)
C70.2830 (5)0.1290 (3)0.2652 (3)0.0403 (9)
H70.31540.20280.25330.048*
C80.3470 (5)0.0478 (4)0.3593 (3)0.0497 (11)
H80.42270.06620.41050.060*
C90.3005 (5)0.0624 (3)0.3797 (3)0.0471 (10)
H90.34180.11870.44460.057*
C100.1916 (5)0.0855 (3)0.3010 (3)0.0410 (9)
H100.15980.15940.31280.049*
S30.85021 (12)0.27850 (8)0.43341 (7)0.0406 (3)
N30.5290 (4)0.3313 (2)0.3939 (2)0.0307 (7)
O30.5486 (3)0.3138 (2)0.29239 (18)0.0403 (6)
C110.6583 (4)0.3166 (3)0.4672 (3)0.0306 (8)
C120.6248 (5)0.3356 (3)0.5712 (3)0.0377 (9)
H120.70860.32440.62260.045*
C130.4761 (5)0.3692 (4)0.6000 (3)0.0476 (10)
H130.45910.38200.67000.057*
C140.3498 (5)0.3841 (4)0.5232 (3)0.0506 (11)
H140.24580.40630.54070.061*
C150.3801 (5)0.3658 (3)0.4212 (3)0.0406 (9)
H150.29650.37720.36980.049*
Na10.62101 (17)0.22453 (11)0.03299 (10)0.0356 (4)
Na20.18860 (17)0.09622 (12)0.01362 (10)0.0375 (4)
Na30.00845 (19)0.40613 (12)0.16714 (11)0.0429 (4)
O40.4638 (3)0.1000 (2)0.12169 (19)0.0379 (6)
H4A0.492 (6)0.147 (3)0.180 (2)0.080 (5)*
H4B0.506 (6)0.041 (3)0.116 (3)0.080 (5)*
O50.8616 (4)0.2286 (2)0.17947 (19)0.0405 (6)
H5A0.914 (6)0.173 (3)0.166 (3)0.080 (5)*
H5B0.835 (6)0.239 (4)0.238 (2)0.080 (5)*
O60.7024 (4)0.4217 (2)0.1515 (2)0.0456 (7)
H6A0.679 (7)0.423 (4)0.210 (2)0.080 (5)*
H6B0.662 (6)0.475 (3)0.134 (3)0.080 (5)*
O70.2636 (4)0.3154 (3)0.1353 (2)0.0481 (7)
H7A0.345 (4)0.324 (5)0.184 (3)0.080 (5)*
H7B0.301 (5)0.341 (4)0.091 (3)0.080 (5)*
O80.0088 (5)0.4861 (3)0.3495 (2)0.0621 (9)
H8A0.040 (6)0.547 (3)0.396 (3)0.080 (5)*
H8B0.049 (6)0.442 (3)0.372 (3)0.080 (5)*
O90.1572 (6)0.5610 (4)0.1329 (4)0.0999 (14)
H9A0.102 (5)0.602 (4)0.106 (4)0.080 (5)*
H9B0.257 (3)0.570 (4)0.124 (4)0.080 (5)*
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
S10.0529 (6)0.0272 (5)0.0320 (5)0.0053 (4)0.0094 (4)0.0063 (4)
N10.0355 (16)0.0298 (16)0.0204 (15)0.0055 (12)0.0031 (12)0.0085 (12)
O10.0472 (15)0.0295 (13)0.0241 (13)0.0072 (11)0.0091 (11)0.0102 (10)
C10.0322 (18)0.032 (2)0.0258 (18)0.0085 (15)0.0012 (15)0.0114 (15)
C20.043 (2)0.040 (2)0.032 (2)0.0076 (17)0.0034 (17)0.0197 (17)
C30.042 (2)0.052 (3)0.028 (2)0.0015 (19)0.0085 (16)0.0180 (19)
C40.053 (2)0.046 (2)0.0195 (19)0.0013 (19)0.0051 (17)0.0047 (16)
C50.044 (2)0.0282 (19)0.030 (2)0.0026 (16)0.0016 (17)0.0063 (16)
S20.0467 (6)0.0387 (6)0.0261 (5)0.0162 (4)0.0054 (4)0.0009 (4)
N20.0328 (16)0.0291 (16)0.0225 (15)0.0028 (12)0.0033 (12)0.0080 (12)
O20.0464 (15)0.0323 (14)0.0294 (13)0.0091 (11)0.0069 (11)0.0122 (11)
C60.0342 (19)0.0292 (19)0.0223 (18)0.0042 (15)0.0001 (14)0.0082 (15)
C70.046 (2)0.039 (2)0.035 (2)0.0119 (18)0.0052 (17)0.0122 (18)
C80.056 (3)0.058 (3)0.031 (2)0.004 (2)0.0139 (18)0.017 (2)
C90.062 (3)0.042 (2)0.025 (2)0.0034 (19)0.0132 (18)0.0036 (17)
C100.048 (2)0.032 (2)0.035 (2)0.0020 (17)0.0050 (18)0.0044 (17)
S30.0457 (6)0.0460 (6)0.0310 (5)0.0171 (4)0.0028 (4)0.0112 (4)
N30.0380 (17)0.0255 (15)0.0255 (16)0.0032 (12)0.0001 (13)0.0056 (12)
O30.0533 (16)0.0430 (15)0.0228 (14)0.0106 (12)0.0019 (11)0.0096 (11)
C110.040 (2)0.0197 (17)0.0289 (19)0.0000 (14)0.0007 (15)0.0062 (14)
C120.052 (2)0.034 (2)0.0255 (19)0.0001 (17)0.0020 (17)0.0100 (15)
C130.060 (3)0.047 (2)0.033 (2)0.001 (2)0.015 (2)0.0067 (18)
C140.046 (2)0.043 (2)0.060 (3)0.0078 (19)0.021 (2)0.005 (2)
C150.036 (2)0.033 (2)0.046 (2)0.0057 (17)0.0033 (18)0.0068 (17)
Na10.0398 (8)0.0316 (8)0.0302 (7)0.0047 (6)0.0045 (6)0.0064 (6)
Na20.0384 (8)0.0436 (8)0.0295 (7)0.0072 (6)0.0023 (6)0.0129 (6)
Na30.0458 (9)0.0397 (8)0.0414 (9)0.0083 (6)0.0012 (7)0.0114 (7)
O40.0459 (15)0.0354 (15)0.0301 (14)0.0132 (12)0.0056 (11)0.0097 (11)
O50.0577 (17)0.0387 (15)0.0291 (14)0.0193 (13)0.0099 (12)0.0111 (11)
O60.0576 (17)0.0346 (15)0.0408 (16)0.0178 (13)0.0055 (14)0.0085 (12)
O70.0465 (16)0.0561 (18)0.0417 (17)0.0134 (13)0.0004 (13)0.0161 (14)
O80.079 (2)0.054 (2)0.0402 (17)0.0119 (16)0.0072 (16)0.0019 (14)
O90.107 (3)0.080 (3)0.152 (4)0.035 (3)0.050 (3)0.076 (3)
Geometric parameters (Å, º) top
S1—C11.718 (3)C14—C151.370 (6)
N1—O11.343 (3)C14—H140.930
N1—C51.350 (4)C15—H150.930
N1—C11.369 (4)Na1—O62.433 (3)
C1—C21.411 (5)Na1—O42.503 (3)
C2—C31.355 (5)Na1—O52.508 (3)
C2—H20.930Na1—S2i2.863 (2)
C3—C41.373 (6)Na1—S12.944 (2)
C3—H30.930Na1—O12.350 (3)
C4—C51.361 (5)Na2—O12.471 (3)
C4—H40.930Na2—S22.836 (2)
C5—H50.930Na2—O2ii2.401 (3)
S2—C61.705 (3)Na2—O22.455 (3)
N2—O21.344 (3)Na2—O42.421 (3)
N2—C101.350 (5)Na2—O72.655 (3)
N2—C61.364 (4)Na3—S23.290 (2)
C6—C71.409 (5)Na3—O92.307 (4)
C7—C81.351 (5)Na3—O82.344 (3)
C7—H70.930Na3—O5iii2.404 (3)
C8—C91.383 (6)Na3—O72.423 (3)
C8—H80.930Na3—O6iii2.431 (3)
C9—C101.365 (5)O4—H4A0.81 (2)
C9—H90.930O4—H4B0.81 (2)
C10—H100.930O5—H5A0.82 (2)
S3—C111.713 (4)O5—H5B0.81 (2)
N3—O31.339 (4)O6—H6A0.82 (2)
N3—C151.351 (5)O6—H6B0.82 (2)
N3—C111.369 (4)O7—H7A0.82 (2)
C11—C121.403 (5)O7—H7B0.82 (2)
C12—C131.352 (6)O8—H8A0.82 (2)
C12—H120.930O8—H8B0.81 (2)
C13—C141.385 (6)O9—H9A0.82 (2)
C13—H130.930O9—H9B0.82 (2)
C1—S1—Na199.08 (12)O6—Na1—O570.35 (9)
O1—N1—C5117.7 (3)O4—Na1—O581.28 (10)
O1—N1—C1120.3 (3)O1—Na1—S2i102.60 (9)
C5—N1—C1122.0 (3)O6—Na1—S2i98.62 (9)
N1—O1—Na1129.15 (18)O4—Na1—S2i133.53 (8)
N1—O1—Na2105.74 (18)O5—Na1—S2i75.27 (8)
Na1—O1—Na295.39 (10)O1—Na1—S166.41 (7)
N1—C1—C2115.4 (3)O6—Na1—S178.28 (8)
N1—C1—S1120.5 (2)O4—Na1—S1116.23 (8)
C2—C1—S1124.1 (3)O5—Na1—S1148.06 (8)
C3—C2—C1122.4 (3)S2i—Na1—S1104.38 (6)
C3—C2—H2118.8O2ii—Na2—O493.65 (10)
C1—C2—H2118.8O2ii—Na2—O287.09 (10)
C2—C3—C4119.6 (3)O4—Na2—O2140.85 (10)
C2—C3—H3120.2O2ii—Na2—O1161.94 (10)
C4—C3—H3120.2O4—Na2—O175.14 (10)
C5—C4—C3118.8 (3)O2—Na2—O192.80 (10)
C5—C4—H4120.6O2ii—Na2—O794.21 (10)
C3—C4—H4120.6O4—Na2—O776.69 (9)
N1—C5—C4121.5 (3)O2—Na2—O7142.36 (10)
N1—C5—H5119.3O1—Na2—O796.82 (10)
C4—C5—H5119.3O2ii—Na2—S293.35 (8)
C6—S2—Na2102.54 (13)O4—Na2—S2152.60 (9)
C6—S2—Na1iii99.33 (12)O2—Na2—S265.98 (7)
Na2—S2—Na1iii118.92 (6)O1—Na2—S2103.11 (8)
C6—S2—Na3168.07 (12)O7—Na2—S276.40 (8)
Na2—S2—Na386.88 (5)O9—Na3—O899.98 (17)
Na1iii—S2—Na369.42 (5)O9—Na3—O5iii172.00 (16)
O2—N2—C10118.2 (3)O8—Na3—O5iii87.71 (11)
O2—N2—C6119.8 (2)O9—Na3—O784.31 (14)
C10—N2—C6122.0 (3)O8—Na3—O7111.78 (13)
N2—O2—Na2ii110.92 (19)O5iii—Na3—O790.81 (11)
N2—O2—Na2125.86 (18)O9—Na3—O6iii110.73 (14)
Na2ii—O2—Na292.91 (10)O8—Na3—O6iii83.37 (12)
N2—C6—C7115.8 (3)O5iii—Na3—O6iii72.13 (10)
N2—C6—S2119.9 (2)O7—Na3—O6iii157.11 (12)
C7—C6—S2124.3 (3)O9—Na3—S2103.73 (15)
C8—C7—C6122.2 (4)O8—Na3—S2156.29 (10)
C8—C7—H7118.9O5iii—Na3—S268.61 (8)
C6—C7—H7118.9O7—Na3—S271.17 (8)
C7—C8—C9120.3 (3)O6iii—Na3—S288.09 (8)
C7—C8—H8119.9Na2—O4—Na192.80 (10)
C9—C8—H8119.9Na2—O4—H4A120 (3)
C10—C9—C8117.5 (3)Na1—O4—H4A94 (4)
C10—C9—H9121.2Na2—O4—H4B120 (3)
C8—C9—H9121.2Na1—O4—H4B110 (4)
N2—C10—C9122.2 (4)H4A—O4—H4B113 (3)
N2—C10—H10118.9Na3i—O5—Na191.59 (10)
C9—C10—H10118.9Na3i—O5—H5A115 (4)
O3—N3—C15117.9 (3)Na1—O5—H5A114 (4)
O3—N3—C11120.4 (3)Na3i—O5—H5B110 (4)
C15—N3—C11121.7 (3)Na1—O5—H5B115 (4)
N3—C11—C12116.2 (3)H5A—O5—H5B110 (3)
N3—C11—S3121.6 (3)Na3i—O6—Na192.77 (10)
C12—C11—S3122.2 (3)Na3i—O6—H6A105 (4)
C13—C12—C11123.0 (4)Na1—O6—H6A109 (4)
C13—C12—H12118.5Na3i—O6—H6B122 (4)
C11—C12—H12118.5Na1—O6—H6B119 (4)
C12—C13—C14118.7 (4)H6A—O6—H6B108 (3)
C12—C13—H13120.7Na3—O7—Na2112.58 (12)
C14—C13—H13120.7Na3—O7—H7A121 (4)
C15—C14—C13119.1 (4)Na2—O7—H7A112 (4)
C15—C14—H14120.4Na3—O7—H7B105 (4)
C13—C14—H14120.4Na2—O7—H7B96 (4)
N3—C15—C14121.2 (4)H7A—O7—H7B107 (3)
N3—C15—H15119.4Na3—O8—H8A139 (3)
C14—C15—H15119.4Na3—O8—H8B111 (3)
O1—Na1—O6142.23 (10)H8A—O8—H8B110 (3)
O1—Na1—O475.79 (9)Na3—O9—H9A118 (3)
O6—Na1—O4110.46 (11)Na3—O9—H9B129 (3)
O1—Na1—O5145.47 (10)H9A—O9—H9B109 (3)
C5—N1—O1—Na1154.8 (2)Na2ii—O2—Na2—S294.97 (8)
C1—N1—O1—Na126.0 (4)N1—O1—Na2—O2ii138.7 (3)
C5—N1—O1—Na294.4 (3)Na1—O1—Na2—O2ii88.0 (3)
C1—N1—O1—Na284.9 (3)N1—O1—Na2—O4168.23 (19)
O1—N1—C1—C2172.8 (3)Na1—O1—Na2—O434.96 (9)
C5—N1—C1—C26.4 (5)N1—O1—Na2—O249.55 (18)
O1—N1—C1—S17.9 (4)Na1—O1—Na2—O2177.18 (8)
C5—N1—C1—S1172.9 (3)N1—O1—Na2—O794.00 (18)
Na1—S1—C1—N16.7 (3)Na1—O1—Na2—O739.27 (10)
Na1—S1—C1—C2172.5 (3)N1—O1—Na2—S216.43 (18)
N1—C1—C2—C35.6 (5)Na1—O1—Na2—S2116.84 (8)
S1—C1—C2—C3173.7 (3)C6—S2—Na2—O2ii101.12 (14)
C1—C2—C3—C41.1 (6)Na1iii—S2—Na2—O2ii7.10 (9)
C2—C3—C4—C52.7 (6)Na3—S2—Na2—O2ii71.49 (8)
O1—N1—C5—C4176.3 (3)C6—S2—Na2—O4154.3 (2)
C1—N1—C5—C42.9 (5)Na1iii—S2—Na2—O497.5 (2)
C3—C4—C5—N11.9 (6)Na3—S2—Na2—O433.1 (2)
C10—N2—O2—Na2ii93.6 (3)C6—S2—Na2—O215.80 (14)
C6—N2—O2—Na2ii85.3 (3)Na1iii—S2—Na2—O292.41 (9)
C10—N2—O2—Na2156.3 (2)Na3—S2—Na2—O2156.80 (8)
C6—N2—O2—Na224.7 (4)C6—S2—Na2—O171.39 (14)
O2—N2—C6—C7177.6 (3)Na1iii—S2—Na2—O1179.61 (7)
C10—N2—C6—C71.3 (5)Na3—S2—Na2—O1116.00 (8)
O2—N2—C6—S23.2 (4)C6—S2—Na2—O7165.35 (14)
C10—N2—C6—S2177.9 (3)Na1iii—S2—Na2—O786.43 (9)
Na2—S2—C6—N213.5 (3)Na3—S2—Na2—O722.04 (7)
Na1iii—S2—C6—N2109.1 (3)C6—S2—Na3—O9113.5 (6)
Na3—S2—C6—N2128.0 (5)Na2—S2—Na3—O9103.96 (13)
Na2—S2—C6—C7165.6 (3)Na1iii—S2—Na3—O9133.51 (12)
Na1iii—S2—C6—C771.8 (3)C6—S2—Na3—O866.1 (7)
Na3—S2—C6—C752.8 (8)Na2—S2—Na3—O876.5 (3)
N2—C6—C7—C80.9 (5)Na1iii—S2—Na3—O846.1 (3)
S2—C6—C7—C8178.4 (3)C6—S2—Na3—O5iii69.0 (6)
C6—C7—C8—C90.4 (6)Na2—S2—Na3—O5iii73.63 (9)
C7—C8—C9—C101.2 (6)Na1iii—S2—Na3—O5iii48.91 (8)
O2—N2—C10—C9178.4 (3)C6—S2—Na3—O7167.6 (6)
C6—N2—C10—C90.6 (6)Na2—S2—Na3—O724.98 (8)
C8—C9—C10—N20.8 (6)Na1iii—S2—Na3—O7147.51 (9)
O3—N3—C11—C12179.2 (3)C6—S2—Na3—O6iii2.6 (6)
C15—N3—C11—C122.1 (5)Na2—S2—Na3—O6iii145.16 (8)
O3—N3—C11—S31.3 (4)Na1iii—S2—Na3—O6iii22.63 (8)
C15—N3—C11—S3177.4 (3)O2ii—Na2—O4—Na1161.93 (9)
N3—C11—C12—C131.6 (5)O2—Na2—O4—Na1108.20 (16)
S3—C11—C12—C13177.9 (3)O1—Na2—O4—Na132.44 (8)
C11—C12—C13—C141.0 (6)O7—Na2—O4—Na168.46 (10)
C12—C13—C14—C150.8 (6)S2—Na2—O4—Na157.4 (2)
O3—N3—C15—C14179.2 (3)O1—Na1—O4—Na234.21 (9)
C11—N3—C15—C142.1 (5)O6—Na1—O4—Na2106.67 (10)
C13—C14—C15—N31.3 (6)O5—Na1—O4—Na2171.81 (10)
N1—O1—Na1—O643.7 (3)S2i—Na1—O4—Na2128.21 (9)
Na2—O1—Na1—O671.62 (18)S1—Na1—O4—Na219.99 (11)
N1—O1—Na1—O4148.9 (3)O1—Na1—O5—Na3i153.99 (16)
Na2—O1—Na1—O433.56 (9)O6—Na1—O5—Na3i41.90 (10)
N1—O1—Na1—O5161.2 (2)O4—Na1—O5—Na3i157.38 (10)
Na2—O1—Na1—O583.48 (19)S2i—Na1—O5—Na3i63.08 (8)
N1—O1—Na1—S2i78.9 (2)S1—Na1—O5—Na3i30.58 (19)
Na2—O1—Na1—S2i165.74 (7)O1—Na1—O6—Na3i153.32 (14)
N1—O1—Na1—S121.5 (2)O4—Na1—O6—Na3i113.60 (11)
Na2—O1—Na1—S193.89 (8)O5—Na1—O6—Na3i41.36 (9)
C1—S1—Na1—O111.60 (14)S2i—Na1—O6—Na3i29.55 (9)
C1—S1—Na1—O6177.89 (14)S1—Na1—O6—Na3i132.56 (9)
C1—S1—Na1—O470.69 (15)O9—Na3—O7—Na2135.81 (17)
C1—S1—Na1—O5171.22 (18)O8—Na3—O7—Na2125.69 (13)
C1—S1—Na1—S2i86.09 (13)O5iii—Na3—O7—Na237.83 (12)
N2—O2—Na2—O2ii118.5 (3)O6iii—Na3—O7—Na23.1 (4)
N2—O2—Na2—O4149.3 (2)S2—Na3—O7—Na229.20 (9)
Na2ii—O2—Na2—O492.21 (17)O2ii—Na2—O7—Na358.98 (13)
N2—O2—Na2—O179.5 (2)O4—Na2—O7—Na3151.74 (14)
Na2ii—O2—Na2—O1161.92 (10)O2—Na2—O7—Na331.7 (2)
N2—O2—Na2—O725.4 (3)O1—Na2—O7—Na3135.34 (12)
Na2ii—O2—Na2—O793.13 (16)S2—Na2—O7—Na333.45 (10)
N2—O2—Na2—S223.6 (2)
Symmetry codes: (i) x+1, y, z; (ii) x, y, z; (iii) x1, y, z.

Experimental details

Crystal data
Chemical formulaNa+·C5H4NOS·2H2O
Mr185.17
Crystal system, space groupTriclinic, P1
Temperature (K)296
a, b, c (Å)7.916 (4), 12.114 (6), 13.280 (7)
α, β, γ (°)106.19 (2), 98.18 (1), 95.43 (2)
V3)1198.4 (11)
Z6
Radiation typeCu Kα
µ (mm1)3.83
Crystal size (mm)0.30 × 0.15 × 0.15
Data collection
DiffractometerStoe STADI-4
diffractometer
Absorption correctionψ scan
(North et al., 1968)
Tmin, Tmax0.333, 0.563
No. of measured, independent and
observed [I > 2σ(I)] reflections
2997, 2997, 2387
Rint0.000
θmax (°)54.9
(sin θ/λ)max1)0.531
Refinement
R[F2 > 2σ(F2)], wR(F2), S 0.042, 0.113, 1.05
No. of reflections2997
No. of parameters337
No. of restraints18
H-atom treatmentH atoms treated by a mixture of independent and constrained refinement
Δρmax, Δρmin (e Å3)0.36, 0.32

Computer programs: DIF4 (Stoe & Cie, 1992), DIF4, REDU4 (Stoe & Cie, 1992), SHELXS97 (Sheldrick, 1997), SHELXL97, XP (Sheldrick, 1993).

 

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