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Acta Crystallogr Sect E Struct Rep Online. 2009 April 1; 65(Pt 4): m387–m388.
Published online 2009 March 11. doi:  10.1107/S1600536809008174
PMCID: PMC2968916

Poly[octa-μ-aqua-tetra­aqua­bis(μ-5-sul­fon­atobenzene-1,3-dicarboxyl­ato)cobalt(II)tetra­sodium]

Abstract

The title compound, [CoNa4(C8H3O7S)2(H2O)12]n, is a three-dimensional coordination polymer bridged by sulfoisophthalate trianions and water mol­ecules. The CoII atom, located on an inversion centre, is coordinated by two carboxyl­ate groups of the sulfoisophthalate trianions and by four water mol­ecules in a distorted CoO6 octa­hedral geometry. Two independent NaI atoms also have a distorted octa­hedral coordination geometry formed by water, carboxyl­ate O and sulfonate O atoms. An extensive O—H(...)O and C—H(...)O hydrogen-bonding network is present in the crystal structure, as well as weak π-π stacking [centroid–centroid distance = 3.9553 (11) Å].

Related literature

For the role played by π–π stacking between aromatic rings in the electron-transfer process in some biological systems, see: Deisenhofer & Michel (1989 [triangle]); Su & Xu (2004 [triangle]); Liu et al. (2004 [triangle]); Pan et al. (2006 [triangle]). For a related structure, see: Zhang et al. (2008 [triangle]).

An external file that holds a picture, illustration, etc.
Object name is e-65-0m387-scheme1.jpg

Experimental

Crystal data

  • [CoNa4(C8H3O7S)2(H2O)12]
  • M r = 853.41
  • Monoclinic, An external file that holds a picture, illustration, etc.
Object name is e-65-0m387-efi10.jpg
  • a = 7.8756 (12) Å
  • b = 17.294 (3) Å
  • c = 11.7700 (18) Å
  • β = 93.281 (5)°
  • V = 1600.5 (4) Å3
  • Z = 2
  • Mo Kα radiation
  • μ = 0.82 mm−1
  • T = 295 K
  • 0.35 × 0.32 × 0.25 mm

Data collection

  • Rigaku R-AXIS RAPID IP diffractometer
  • Absorption correction: multi-scan (ABSCOR; Higashi, 1995 [triangle]) T min = 0.756, T max = 0.819
  • 9383 measured reflections
  • 3120 independent reflections
  • 2899 reflections with I > 2σ(I)
  • R int = 0.016

Refinement

  • R[F 2 > 2σ(F 2)] = 0.025
  • wR(F 2) = 0.066
  • S = 1.08
  • 3120 reflections
  • 223 parameters
  • H-atom parameters constrained
  • Δρmax = 0.42 e Å−3
  • Δρmin = −0.40 e Å−3

Data collection: PROCESS-AUTO (Rigaku, 1998 [triangle]); cell refinement: PROCESS-AUTO; data reduction: CrystalStructure (Rigaku/MSC, 2002 [triangle]); program(s) used to solve structure: SHELXS97 (Sheldrick, 2008 [triangle]); program(s) used to refine structure: SHELXL97 (Sheldrick, 2008 [triangle]); molecular graphics: ORTEP-3 for Windows (Farrugia, 1997 [triangle]); software used to prepare material for publication: WinGX (Farrugia, 1999 [triangle]).

Table 1
Selected bond lengths (Å)
Table 2
Hydrogen-bond geometry (Å, °)

Supplementary Material

Crystal structure: contains datablocks I, global. DOI: 10.1107/S1600536809008174/is2394sup1.cif

Structure factors: contains datablocks I. DOI: 10.1107/S1600536809008174/is2394Isup2.hkl

Additional supplementary materials: crystallographic information; 3D view; checkCIF report

Acknowledgments

The work was supported by the ZIJIN project of Zhejiang University, China.

supplementary crystallographic information

Comment

As π-π stacking between aromatic rings plays an important role in electron transfer process in some biological system (Deisenhofer & Michel, 1989), π-π stacking has attracted our much attention in past years (Su & Xu, 2004; Liu et al., 2004; Pan et al., 2006). In order to investigate the influence of substituents of the aromatic compounds on stacking between parallel aromatic rings, the title CoII compound incorporating sulfoisophthalate ligand has recently been prepared and its crystal structure is reported here.

The title compound is a three dimensional polymeric complex bridged by sulfoisophthalate trianions and water molecules (Fig. 1). The Co atom occupies a special position in an inversion centre and is coordinated by four water molecules and two carboxyl groups from sulfoisophthalate trianions in a distorted CoO6 octahedral geometry (Table 1). The crystal structure contains two independent NaI atoms, both in distorted octahedral coordination geometry. The Na1 atom is coordinated by five water molecules and one sulfonate O atom, while the Na2 atom is coordinated by three water molecules, two sulfonate O atoms and one carboxy O atom. The C8-carboxy group of the sulfoisophthalate ligand is not coordinated to the metal atom in the structure.

The extensive O—H···O hydrogen bonding network presents in the crystal structure (Table 2), weak C—H···O hydrogen bonding also helps to stabilize the crystal structure. A partial overlapped arrangement between centro-symmetric benzene rings is observed in the crystal structure (Fig. 2), perpendicular distance of the centroid of the C2-benzne ring on the C2vbenzene ring is 3.563 Å, [symmetry code: (v) 1 - x,1 - y,-z], which suggests a weak π-π stacking involving sulfoisophthalate ligand (Zhang et al., 2008).

Experimental

A water-ethanol solution (25 ml, 3:2) containing monosodium 5-sulfoisophthalate (0.270 g, 1 mmol), Na2CO3 (0.212 g, 2 mmol), NaOH (0.081 g, 2 mmol) and CoCl2.6H2O (0.595 g, 2.5 mmol) was refluxed for 7.5 h and filtered after cooling to room temperature. The single crystals of the title compound were obtained from the filtrate after one month.

Refinement

Water H atoms were located in a difference Fourier map and refined as riding in as-found relative positions, with Uiso(H) = 1.5Ueq(O). Other H atoms were placed in calculated positions (C—H = 0.93 Å) and refined in riding mode, with Uiso(H) = 1.2Ueq(C).

Figures

Fig. 1.
A part of the polymeric structure of the title compound with 50% probability displacement (arbitrary spheres for H atoms) [symmetry codes: (i) -x + 3/2,+y - 1/2,-z + 1/2; (ii) -x + 1/2,+y - 1/2,-z + 1/2; (iii) -x + 1,-y + 1,-z + 1; (iv) x - 1/2,-y + 1/2,+z ...
Fig. 2.
π-π stacking between benzene rings [symmetry code: (v) -x + 1,-y + 1,-z].

Crystal data

[CoNa4(C8H3O7S)2(H2O)12]F(000) = 874
Mr = 853.41Dx = 1.771 Mg m3
Monoclinic, P21/nMo Kα radiation, λ = 0.71073 Å
Hall symbol: -P 2ynCell parameters from 2508 reflections
a = 7.8756 (12) Åθ = 2.5–25.0°
b = 17.294 (3) ŵ = 0.82 mm1
c = 11.7700 (18) ÅT = 295 K
β = 93.281 (5)°Chuck, red
V = 1600.5 (4) Å30.35 × 0.32 × 0.25 mm
Z = 2

Data collection

Rigaku R-AXIS RAPID IP diffractometer3120 independent reflections
Radiation source: fine-focus sealed tube2899 reflections with I > 2σ(I)
graphiteRint = 0.016
Detector resolution: 10.0 pixels mm-1θmax = 26.0°, θmin = 2.1°
ω scansh = −9→9
Absorption correction: multi-scan (ABSCOR; Higashi, 1995)k = −21→21
Tmin = 0.756, Tmax = 0.819l = −14→14
9383 measured reflections

Refinement

Refinement on F2Primary atom site location: structure-invariant direct methods
Least-squares matrix: fullSecondary atom site location: difference Fourier map
R[F2 > 2σ(F2)] = 0.025Hydrogen site location: inferred from neighbouring sites
wR(F2) = 0.066H-atom parameters constrained
S = 1.08w = 1/[σ2(Fo2) + (0.035P)2 + 0.6342P] where P = (Fo2 + 2Fc2)/3
3120 reflections(Δ/σ)max = 0.002
223 parametersΔρmax = 0.42 e Å3
0 restraintsΔρmin = −0.40 e Å3

Special details

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)

xyzUiso*/Ueq
Co0.50000.50000.50000.01857 (9)
Na10.82210 (8)0.33026 (4)0.45527 (6)0.02963 (16)
Na20.40642 (9)0.26855 (4)0.19976 (5)0.02861 (16)
S0.28585 (5)0.72991 (2)0.01806 (3)0.01880 (10)
O10.42263 (15)0.52219 (6)0.33357 (9)0.0254 (2)
O20.42504 (18)0.40595 (6)0.25165 (9)0.0338 (3)
O30.1617 (2)0.37979 (7)−0.13019 (11)0.0444 (4)
O40.11425 (17)0.47988 (7)−0.24435 (10)0.0324 (3)
O50.45517 (15)0.74752 (7)−0.01734 (10)0.0274 (3)
O60.25309 (16)0.76048 (6)0.12948 (10)0.0294 (3)
O70.15486 (14)0.75313 (6)−0.06860 (10)0.0266 (3)
O80.75313 (16)0.52064 (8)0.46031 (11)0.0384 (3)
H8A0.82140.54390.50620.058*
H8B0.78120.53100.39290.058*
O90.53565 (14)0.38179 (6)0.46304 (9)0.0240 (2)
H9A0.46720.35210.49630.036*
H9B0.50480.37720.39410.036*
O100.70112 (17)0.26175 (7)0.28516 (10)0.0334 (3)
H10A0.75400.26170.22630.050*
H10B0.69970.21400.30270.050*
O110.68645 (15)0.21915 (7)0.55730 (11)0.0322 (3)
H11A0.57800.22600.57090.048*
H11B0.68040.18600.50180.048*
O120.86980 (15)0.37242 (7)0.64918 (10)0.0315 (3)
H12A0.79160.40450.65730.047*
H12B0.95420.39620.68850.047*
O131.03883 (16)0.40306 (7)0.36711 (11)0.0354 (3)
H13A1.00310.43250.31410.053*
H13B1.11130.37130.33710.053*
C10.4040 (2)0.47732 (9)0.24890 (13)0.0208 (3)
C20.3461 (2)0.51502 (9)0.13824 (13)0.0210 (3)
C30.3431 (2)0.59494 (8)0.12797 (12)0.0208 (3)
H30.38440.62600.18790.025*
C40.27793 (19)0.62793 (8)0.02779 (12)0.0190 (3)
C50.2182 (2)0.58293 (9)−0.06349 (13)0.0212 (3)
H50.17470.6061−0.13030.025*
C60.2241 (2)0.50268 (8)−0.05391 (13)0.0222 (3)
C70.2891 (2)0.46985 (9)0.04690 (13)0.0238 (3)
H70.29440.41630.05320.029*
C80.1620 (2)0.45023 (9)−0.15059 (13)0.0244 (3)

Atomic displacement parameters (Å2)

U11U22U33U12U13U23
Co0.02424 (17)0.01734 (15)0.01366 (15)0.00223 (11)−0.00299 (11)−0.00032 (10)
Na10.0267 (4)0.0352 (4)0.0267 (3)0.0019 (3)−0.0009 (3)0.0029 (3)
Na20.0307 (4)0.0317 (4)0.0234 (3)−0.0005 (3)0.0014 (3)−0.0039 (3)
S0.0222 (2)0.01579 (17)0.01856 (19)−0.00060 (13)0.00249 (14)0.00052 (13)
O10.0398 (7)0.0203 (5)0.0152 (5)0.0030 (5)−0.0061 (5)−0.0009 (4)
O20.0610 (9)0.0191 (6)0.0200 (6)0.0054 (5)−0.0091 (5)0.0002 (4)
O30.0828 (11)0.0193 (6)0.0289 (7)−0.0026 (6)−0.0164 (7)−0.0035 (5)
O40.0490 (8)0.0294 (6)0.0178 (6)0.0020 (5)−0.0087 (5)−0.0020 (5)
O50.0246 (6)0.0290 (6)0.0288 (6)−0.0064 (5)0.0045 (5)−0.0014 (5)
O60.0445 (7)0.0214 (5)0.0233 (6)−0.0008 (5)0.0098 (5)−0.0034 (4)
O70.0267 (6)0.0243 (5)0.0284 (6)0.0028 (5)−0.0010 (5)0.0059 (5)
O80.0302 (7)0.0608 (8)0.0242 (6)−0.0087 (6)0.0021 (5)−0.0028 (6)
O90.0324 (6)0.0194 (5)0.0196 (5)0.0014 (4)−0.0048 (4)−0.0005 (4)
O100.0469 (8)0.0290 (6)0.0246 (6)0.0013 (5)0.0035 (5)0.0039 (5)
O110.0273 (7)0.0309 (6)0.0379 (7)0.0038 (5)−0.0036 (5)−0.0058 (5)
O120.0329 (7)0.0296 (6)0.0315 (6)0.0027 (5)−0.0013 (5)−0.0076 (5)
O130.0377 (7)0.0306 (6)0.0380 (7)0.0067 (5)0.0035 (6)0.0064 (5)
C10.0270 (8)0.0190 (7)0.0159 (7)0.0000 (6)−0.0023 (6)0.0005 (6)
C20.0270 (8)0.0202 (7)0.0155 (7)0.0008 (6)−0.0020 (6)−0.0001 (6)
C30.0268 (8)0.0199 (7)0.0155 (7)−0.0013 (6)−0.0002 (6)−0.0027 (6)
C40.0219 (8)0.0158 (7)0.0196 (7)−0.0004 (6)0.0026 (6)0.0004 (6)
C50.0264 (8)0.0210 (7)0.0158 (7)0.0004 (6)−0.0018 (6)0.0022 (6)
C60.0284 (9)0.0216 (8)0.0163 (8)−0.0006 (6)−0.0015 (6)−0.0010 (6)
C70.0344 (9)0.0171 (7)0.0195 (8)−0.0004 (6)−0.0025 (6)0.0006 (6)
C80.0315 (9)0.0229 (8)0.0182 (8)0.0004 (6)−0.0030 (6)−0.0023 (6)

Geometric parameters (Å, °)

Co—O1i2.0541 (11)O4—C81.2550 (19)
Co—O12.0541 (11)O8—H8A0.8421
Co—O82.1039 (13)O8—H8B0.8549
Co—O8i2.1039 (13)O9—H9A0.8546
Co—O9i2.1122 (11)O9—H9B0.8373
Co—O92.1122 (11)O10—H10A0.8284
Na1—O5ii2.3477 (13)O10—H10B0.8512
Na1—O92.4322 (13)O11—H11A0.8860
Na1—O102.4702 (14)O11—H11B0.8680
Na1—O112.5343 (15)O12—H12A0.8381
Na1—O122.4048 (14)O12—H12B0.8887
Na1—O132.4037 (15)O13—H13A0.8406
Na2—O22.4557 (13)O13—H13B0.8803
Na2—O5iii2.4785 (13)C1—C21.504 (2)
Na2—O6iv2.4344 (13)C2—C71.383 (2)
Na2—O102.4787 (15)C2—C31.388 (2)
Na2—O11v2.3506 (14)C3—C41.382 (2)
Na2—O12v2.5222 (14)C3—H30.9300
S—O61.4508 (12)C4—C51.387 (2)
S—O51.4519 (12)C5—C61.393 (2)
S—O71.4647 (12)C5—H50.9300
S—C41.7688 (14)C6—C71.387 (2)
O1—C11.2648 (18)C6—C81.514 (2)
O2—C11.2456 (19)C7—H70.9300
O3—C81.242 (2)
O1i—Co—O1180.000 (1)S—O6—Na2vii153.39 (8)
O1—Co—O889.41 (5)Co—O8—H8A121.1
O1—Co—O8i90.59 (5)Co—O8—H8B122.7
O8—Co—O8i180.00 (8)H8A—O8—H8B107.8
O1—Co—O9i88.85 (4)Co—O9—Na1119.79 (5)
O8—Co—O9i91.17 (5)Co—O9—H9A113.1
O1—Co—O991.15 (4)Na1—O9—H9A114.1
O8—Co—O988.83 (5)Co—O9—H9B104.8
O9i—Co—O9180.0Na1—O9—H9B98.5
O5ii—Na1—O1385.25 (5)H9A—O9—H9B103.4
O5ii—Na1—O1279.41 (5)Na1—O10—Na2127.93 (6)
O13—Na1—O12100.06 (5)Na1—O10—H10A119.3
O5ii—Na1—O9152.84 (5)Na2—O10—H10A99.5
O13—Na1—O9120.49 (5)Na1—O10—H10B106.2
O12—Na1—O987.02 (4)Na2—O10—H10B96.8
O5ii—Na1—O10101.92 (5)H10A—O10—H10B102.5
O13—Na1—O1098.73 (5)Na2viii—O11—Na187.47 (5)
O12—Na1—O10161.21 (5)Na2viii—O11—H11A122.5
O9—Na1—O1083.72 (4)Na1—O11—H11A114.9
O5ii—Na1—O1173.63 (4)Na2viii—O11—H11B127.1
O13—Na1—O11158.54 (5)Na1—O11—H11B98.6
O12—Na1—O1180.06 (5)H11A—O11—H11B102.3
O9—Na1—O1180.96 (4)Na1—O12—Na2viii86.59 (4)
O10—Na1—O1182.35 (5)Na1—O12—H12A103.5
O11v—Na2—O6iv101.54 (5)Na2viii—O12—H12A133.4
O11v—Na2—O296.94 (5)Na1—O12—H12B134.9
O6iv—Na2—O282.90 (4)Na2viii—O12—H12B104.6
O11v—Na2—O5iii74.63 (5)H12A—O12—H12B99.6
O6iv—Na2—O5iii169.14 (5)Na1—O13—H13A114.9
O2—Na2—O5iii107.52 (5)Na1—O13—H13B109.8
O11v—Na2—O10158.18 (5)H13A—O13—H13B106.1
O6iv—Na2—O10100.25 (5)O2—C1—O1125.33 (14)
O2—Na2—O1084.48 (5)O2—C1—C2119.03 (13)
O5iii—Na2—O1084.15 (5)O1—C1—C2115.60 (13)
O11v—Na2—O12v81.34 (4)C7—C2—C3119.46 (14)
O6iv—Na2—O12v94.71 (4)C7—C2—C1119.83 (13)
O2—Na2—O12v176.74 (5)C3—C2—C1120.67 (13)
O5iii—Na2—O12v74.76 (4)C4—C3—C2119.29 (13)
O10—Na2—O12v98.15 (4)C4—C3—H3120.4
O11v—Na2—Na1v48.51 (4)C2—C3—H3120.4
O6iv—Na2—Na1v126.05 (4)C3—C4—C5121.49 (13)
O2—Na2—Na1v134.99 (4)C3—C4—S117.01 (11)
O5iii—Na2—Na1v43.99 (3)C5—C4—S121.40 (11)
O10—Na2—Na1v117.07 (4)C4—C5—C6119.21 (14)
O12v—Na2—Na1v45.26 (3)C4—C5—H5120.4
O6—S—O5113.37 (7)C6—C5—H5120.4
O6—S—O7112.02 (7)C7—C6—C5119.09 (14)
O5—S—O7111.38 (7)C7—C6—C8119.03 (13)
O6—S—C4107.22 (7)C5—C6—C8121.88 (14)
O5—S—C4105.31 (7)C2—C7—C6121.43 (14)
O7—S—C4107.00 (7)C2—C7—H7119.3
C1—O1—Co130.65 (10)C6—C7—H7119.3
C1—O2—Na2161.18 (11)O3—C8—O4124.55 (15)
S—O5—Na1vi136.11 (7)O3—C8—C6116.52 (14)
S—O5—Na2iii132.98 (7)O4—C8—C6118.93 (14)
Na1vi—O5—Na2iii88.86 (4)

Symmetry codes: (i) −x+1, −y+1, −z+1; (ii) −x+3/2, y−1/2, −z+1/2; (iii) −x+1, −y+1, −z; (iv) −x+1/2, y−1/2, −z+1/2; (v) x−1/2, −y+1/2, z−1/2; (vi) −x+3/2, y+1/2, −z+1/2; (vii) −x+1/2, y+1/2, −z+1/2; (viii) x+1/2, −y+1/2, z+1/2.

Hydrogen-bond geometry (Å, °)

D—H···AD—HH···AD···AD—H···A
O8—H8A···O13ix0.842.022.8584 (19)172
O8—H8B···O4iii0.851.982.8028 (18)160
O9—H9A···O7iv0.862.162.9932 (16)164
O9—H9B···O20.841.832.6222 (16)158
O10—H10A···O7iii0.832.042.8602 (17)168
O10—H10B···O3viii0.851.842.6676 (18)165
O11—H11A···O7iv0.891.892.7621 (17)167
O11—H11B···O3viii0.871.922.7904 (19)175
O12—H12A···O1i0.842.122.9531 (17)174
O12—H12B···O4x0.892.052.9076 (18)162
O13—H13A···O4iii0.841.932.7277 (18)157
O13—H13B···O6ii0.882.222.9597 (17)142
C7—H7···O11v0.932.493.371 (2)157

Symmetry codes: (ix) −x+2, −y+1, −z+1; (iii) −x+1, −y+1, −z; (iv) −x+1/2, y−1/2, −z+1/2; (viii) x+1/2, −y+1/2, z+1/2; (i) −x+1, −y+1, −z+1; (x) x+1, y, z+1; (ii) −x+3/2, y−1/2, −z+1/2; (v) x−1/2, −y+1/2, z−1/2.

Footnotes

Supplementary data and figures for this paper are available from the IUCr electronic archives (Reference: IS2394).

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