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The title compound, {[Na(C8H4NO6)(H2O)3].H2O}n, forms polymeric chains by way of edge-sharing via pairs of water mol­ecules between NaO(H2O)5 octahedra. The chains are crosslinked by O—H...O hydrogen bonds, resulting in a three-dimensional network.

Supporting information

cif

Crystallographic Information File (CIF) https://doi.org/10.1107/S1600536804026273/hb6105sup1.cif
Contains datablocks I, publication_text

hkl

Structure factor file (CIF format) https://doi.org/10.1107/S1600536804026273/hb6105Isup2.hkl
Contains datablock I

CCDC reference: 255444

Key indicators

  • Single-crystal X-ray study
  • T = 293 K
  • Mean [sigma](C-C) = 0.003 Å
  • R factor = 0.048
  • wR factor = 0.132
  • Data-to-parameter ratio = 13.6

checkCIF/PLATON results

No syntax errors found



Alert level C PLAT029_ALERT_3_C _diffrn_measured_fraction_theta_full Low ....... 0.98 PLAT242_ALERT_2_C Check Low U(eq) as Compared to Neighbors for N1
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 0 ALERT type 1 CIF construction/syntax error, inconsistent or missing data 1 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: SMART (Bruker 1997); cell refinement: SMART; data reduction: SAINT (Bruker 1997); program(s) used to solve structure: SHELXTL (Sheldrick, 2001); program(s) used to refine structure: SHELXTL; molecular graphics: SHELXTL; software used to prepare material for publication: SHELXTL.

Tcatena-Poly[[[aqua(2-carboxy-6-nitrobenzoato-κO)sodium]-di-µ-aqua] monohydrate] top
Crystal data top
[Na(C8H4NO6)(H2O)3]·H2OZ = 2
Mr = 305.18F(000) = 316
Triclinic, P1Dx = 1.610 Mg m3
Hall symbol: -P 1Mo Kα radiation, λ = 0.71073 Å
a = 6.9258 (19) ÅCell parameters from 766 reflections
b = 7.513 (2) Åθ = 3.0–26.2°
c = 12.907 (4) ŵ = 0.18 mm1
α = 77.622 (8)°T = 293 K
β = 83.212 (9)°Block, colorless
γ = 74.103 (8)°0.26 × 0.22 × 0.16 mm
V = 629.6 (3) Å3
Data collection top
Bruker SMART CCD area-detector
diffractometer
2536 independent reflections
Radiation source: fine-focus sealed tube1968 reflections with I > 2σ(I)
Graphite monochromatorRint = 0.019
φ and ω scansθmax = 26.4°, θmin = 1.6°
Absorption correction: multi-scan
(SADABS; Sheldrick, 1996)
h = 88
Tmin = 0.916, Tmax = 0.972k = 98
3650 measured reflectionsl = 1610
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)] = 0.048H atoms treated by a mixture of independent and constrained refinement
wR(F2) = 0.132 w = 1/[σ2(Fo2) + (0.0497P)2 + 0.4847P]
where P = (Fo2 + 2Fc2)/3
S = 1.11(Δ/σ)max = 0.002
2536 reflectionsΔρmax = 0.38 e Å3
186 parametersΔρmin = 0.26 e Å3
1 restraintExtinction correction: SHELXTL, Fc*=kFc[1+0.001xFc2λ3/sin(2θ)]-1/4
Primary atom site location: structure-invariant direct methodsExtinction coefficient: 0.093 (8)
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*/Ueq
Na10.25379 (15)0.48339 (14)0.50904 (8)0.0394 (3)
N10.0779 (4)1.3039 (3)0.12749 (18)0.0392 (5)
O10.2926 (3)0.5920 (3)0.30923 (14)0.0434 (5)
O20.4893 (3)0.4801 (3)0.17703 (15)0.0474 (5)
H20.514 (5)0.380 (3)0.225 (2)0.059 (10)*
O30.0303 (3)0.9333 (2)0.32176 (14)0.0352 (4)
O40.2506 (3)1.0075 (3)0.34047 (14)0.0379 (5)
O50.0434 (4)1.3153 (3)0.2012 (2)0.0740 (8)
O60.1387 (4)1.4371 (3)0.0782 (2)0.0709 (7)
C10.2956 (3)0.7906 (3)0.13895 (18)0.0274 (5)
C20.1982 (3)0.9588 (3)0.17311 (18)0.0246 (5)
C30.1632 (4)1.1215 (3)0.09543 (19)0.0304 (5)
C40.2083 (4)1.1223 (4)0.0114 (2)0.0376 (6)
H40.18261.23460.06080.045*
C50.2923 (4)0.9531 (4)0.0430 (2)0.0392 (6)
H50.31740.94920.11500.047*
C60.3394 (4)0.7897 (4)0.03115 (19)0.0347 (6)
H60.40170.67660.00900.042*
C70.3560 (4)0.6117 (3)0.21803 (19)0.0298 (5)
C80.1348 (4)0.9665 (3)0.28874 (18)0.0273 (5)
O70.4256 (3)0.7172 (3)0.50762 (14)0.0392 (5)
H7A0.41300.76030.56450.047*
H7B0.36830.80210.45790.047*
O80.2153 (3)0.3517 (3)0.69776 (16)0.0530 (6)
H8A0.16290.43820.73320.064*
H8B0.13880.27860.70320.064*
O90.0640 (3)0.2796 (3)0.47933 (14)0.0378 (5)
H9A0.05310.20660.53870.045*
H9B0.10800.21560.43060.045*
O100.4202 (3)0.8509 (2)0.69551 (14)0.0397 (5)
H10A0.30260.92330.70030.048*
H10B0.50900.91250.68660.048*
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
Na10.0319 (6)0.0378 (6)0.0490 (7)0.0098 (4)0.0013 (4)0.0091 (5)
N10.0461 (14)0.0249 (11)0.0439 (13)0.0042 (10)0.0123 (11)0.0023 (10)
O10.0544 (12)0.0319 (10)0.0329 (10)0.0002 (9)0.0046 (9)0.0009 (8)
O20.0539 (13)0.0351 (11)0.0397 (11)0.0108 (9)0.0002 (9)0.0089 (9)
O30.0297 (10)0.0360 (10)0.0365 (10)0.0060 (8)0.0046 (7)0.0062 (8)
O40.0412 (11)0.0437 (11)0.0339 (10)0.0126 (8)0.0053 (8)0.0147 (8)
O50.0871 (19)0.0352 (12)0.0822 (17)0.0013 (12)0.0300 (15)0.0150 (12)
O60.099 (2)0.0393 (13)0.0785 (17)0.0309 (13)0.0032 (14)0.0046 (12)
C10.0233 (12)0.0293 (12)0.0298 (12)0.0060 (9)0.0001 (9)0.0082 (10)
C20.0222 (11)0.0260 (12)0.0264 (11)0.0068 (9)0.0029 (9)0.0050 (9)
C30.0300 (13)0.0269 (12)0.0338 (13)0.0060 (10)0.0067 (10)0.0043 (10)
C40.0435 (15)0.0384 (15)0.0286 (13)0.0130 (12)0.0082 (11)0.0052 (11)
C50.0461 (16)0.0479 (16)0.0250 (13)0.0136 (13)0.0009 (11)0.0088 (11)
C60.0371 (14)0.0385 (14)0.0294 (13)0.0080 (11)0.0010 (10)0.0124 (11)
C70.0294 (13)0.0267 (12)0.0333 (13)0.0042 (10)0.0043 (10)0.0083 (10)
C80.0293 (13)0.0199 (11)0.0291 (12)0.0006 (9)0.0011 (10)0.0065 (9)
O70.0425 (11)0.0388 (10)0.0361 (10)0.0062 (8)0.0099 (8)0.0083 (8)
O80.0586 (13)0.0522 (13)0.0557 (13)0.0194 (10)0.0025 (10)0.0232 (10)
O90.0430 (11)0.0382 (10)0.0330 (10)0.0105 (8)0.0034 (8)0.0114 (8)
O100.0323 (10)0.0347 (10)0.0491 (11)0.0027 (8)0.0028 (8)0.0089 (8)
Geometric parameters (Å, º) top
Na1—O72.373 (2)C2—C31.388 (3)
Na1—O92.386 (2)C2—C81.514 (3)
Na1—O82.437 (2)C3—C41.376 (4)
Na1—O12.538 (2)C4—C51.372 (4)
Na1—O7i2.333 (3)C4—H40.9300
Na1—O9ii2.435 (3)C5—C61.371 (4)
Na1—H7B2.6533C5—H50.9300
N1—O51.194 (3)C6—H60.9300
N1—O61.216 (3)O7—Na1i2.333 (2)
N1—C31.463 (3)O7—H7A0.8500
O1—C71.200 (3)O7—H7B0.8500
O2—C71.311 (3)O8—H8A0.8500
O2—H20.859 (10)O8—H8B0.8500
O3—C81.244 (3)O9—Na1ii2.435 (2)
O4—C81.239 (3)O9—H9A0.8500
C1—C61.390 (3)O9—H9B0.8500
C1—C21.396 (3)O10—H10A0.8500
C1—C71.493 (3)O10—H10B0.8500
O7i—Na1—O785.18 (8)C5—C4—H4120.8
O7i—Na1—O998.15 (8)C3—C4—H4120.8
O7—Na1—O9169.63 (8)C6—C5—C4120.2 (2)
O7i—Na1—O9ii173.92 (8)C6—C5—H5119.9
O7—Na1—O9ii88.98 (7)C4—C5—H5119.9
O9—Na1—O9ii87.33 (7)C5—C6—C1121.0 (2)
O7i—Na1—O892.13 (8)C5—C6—H6119.5
O7—Na1—O8102.85 (8)C1—C6—H6119.5
O9—Na1—O886.90 (7)O1—C7—O2123.9 (2)
O9ii—Na1—O890.81 (8)O1—C7—C1123.7 (2)
O7i—Na1—O185.94 (7)O2—C7—C1112.3 (2)
O7—Na1—O181.80 (7)O4—C8—O3126.6 (2)
O9—Na1—O188.61 (7)O4—C8—C2117.0 (2)
O9ii—Na1—O191.57 (7)O3—C8—C2116.4 (2)
O8—Na1—O1174.82 (8)Na1i—O7—Na194.82 (8)
Na1i—Na1—Na1ii170.09 (7)Na1i—O7—H7A109.6
O5—N1—O6123.0 (3)Na1—O7—H7A116.3
O5—N1—C3119.4 (2)Na1i—O7—H7B124.9
O6—N1—C3117.5 (2)Na1—O7—H7B99.8
C7—O1—Na1163.82 (18)H7A—O7—H7B110.4
C7—O2—H2108 (2)Na1—O8—H8A111.0
C6—C1—C2120.0 (2)Na1—O8—H8B106.3
C6—C1—C7119.7 (2)H8A—O8—H8B110.1
C2—C1—C7120.2 (2)Na1—O9—Na1ii92.67 (7)
C3—C2—C1116.6 (2)Na1—O9—H9A105.8
C3—C2—C8121.0 (2)Na1ii—O9—H9A99.1
C1—C2—C8122.4 (2)Na1—O9—H9B118.0
C4—C3—C2123.6 (2)Na1ii—O9—H9B127.8
C4—C3—N1117.3 (2)H9A—O9—H9B110.1
C2—C3—N1119.1 (2)H10A—O10—H10B111.1
C5—C4—C3118.3 (2)
O7i—Na1—O1—C70.3 (7)C7—C1—C6—C5177.6 (2)
O7—Na1—O1—C785.4 (7)Na1—O1—C7—O226.5 (8)
O9—Na1—O1—C798.5 (7)Na1—O1—C7—C1151.9 (5)
O9ii—Na1—O1—C7174.2 (7)C6—C1—C7—O1165.5 (2)
Na1i—Na1—O1—C742.8 (7)C2—C1—C7—O115.5 (4)
Na1ii—Na1—O1—C7142.7 (7)C6—C1—C7—O215.8 (3)
C6—C1—C2—C34.6 (3)C2—C1—C7—O2163.2 (2)
C7—C1—C2—C3174.4 (2)C3—C2—C8—O483.1 (3)
C6—C1—C2—C8176.0 (2)C1—C2—C8—O496.2 (3)
C7—C1—C2—C84.9 (3)C3—C2—C8—O396.0 (3)
C1—C2—C3—C44.0 (4)C1—C2—C8—O384.7 (3)
C8—C2—C3—C4176.7 (2)O7i—Na1—O7—Na1i0.0
C1—C2—C3—N1174.6 (2)O9—Na1—O7—Na1i109.2 (4)
C8—C2—C3—N14.7 (3)O9ii—Na1—O7—Na1i178.32 (8)
O5—N1—C3—C4145.6 (3)O8—Na1—O7—Na1i91.09 (8)
O6—N1—C3—C435.9 (3)O1—Na1—O7—Na1i86.59 (7)
O5—N1—C3—C235.7 (4)Na1ii—Na1—O7—Na1i169.50 (9)
O6—N1—C3—C2142.7 (3)O7i—Na1—O9—Na1ii177.34 (8)
C2—C3—C4—C50.1 (4)O7—Na1—O9—Na1ii69.3 (4)
N1—C3—C4—C5178.7 (2)O9ii—Na1—O9—Na1ii0.0
C3—C4—C5—C63.5 (4)O8—Na1—O9—Na1ii90.96 (8)
C4—C5—C6—C12.8 (4)O1—Na1—O9—Na1ii91.63 (7)
C2—C1—C6—C51.4 (4)Na1i—Na1—O9—Na1ii166.76 (11)
Symmetry codes: (i) x+1, y+1, z+1; (ii) x, y+1, z+1.
Hydrogen-bond geometry (Å, º) top
D—H···AD—HH···AD···AD—H···A
O10—H10B···O4iii0.851.892.722 (3)166
O10—H10A···O3iv0.851.922.749 (3)165
O9—H9B···O4v0.852.112.939 (3)166
O9—H9A···O3ii0.851.892.740 (3)173
O8—H8B···O3ii0.852.032.846 (3)160
O8—H8A···O5iv0.852.122.962 (3)171
O7—H7B···O40.851.992.834 (3)176
O7—H7A···O100.851.962.809 (3)173
O2—H2···O10i0.86 (1)1.78 (1)2.631 (3)169 (3)
Symmetry codes: (i) x+1, y+1, z+1; (ii) x, y+1, z+1; (iii) x+1, y+2, z+1; (iv) x, y+2, z+1; (v) x, y1, z.
 

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