Acta Cryst. (2008). E64, m815 [ doi:10.1107/S1600536808014037 ]
![[mu]](/logos/entities/mu_rmgif.gif)
-aqua-6-methylenedisulfonato-5-methylenedisulfonato-tetrasodium(I)]The title compound, [Na4(CH2O6S2)2(H2O)5]n, was crystallized from an aqueous solution. The sodium ions are surrounded and bridged by O atoms from coordinated water molecules and sulfonate ions in a three-dimensional neutral network. The crystal structure is also stabilized by an intricate system of hydrogen bonds.
An 1 mol L-1 NaOH aqueous solution was droped into one of mdsH2 (0.14 g, 1 mmol in 20 ml H2O) until the pH value of the solution reached 7 to 9. Slow evaporation for several days yieled colorless prismlike crystals of the title compound. Anal. Calcd for C2H14O17Na4S4 (530.34): C 4.51, H 2.69%; Found: C 4.53, H 2.66%.
All the non-hydrogen atoms were located from the Fourier maps, and were refined anisotropically. H atoms from µ2-H2O can be suitably placed in calculated positions, so all the H atoms, including those attached to carbon atoms and from water molecules, were positioned geometrically, and the isotropic vibration parameters related to the atoms which they are bonded to with Uiso = 1.2 Ueq.
Data collection: APEX2 (Bruker, 2004); cell refinement: SAINT (Bruker, 2004); data reduction: SAINT (Bruker, 2004); 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, 1997); software used to prepare material for publication: SHELXL97 (Sheldrick, 2008) and PLATON (Spek, 2003).
![[Figure 1]](./zl2114fig1thm.gif)
| Fig. 1. The asymmetric unit of I with atom labels and 50% probability displacement ellipsoids for non-H atoms. H atoms attached to carbon atoms are omitted for clarity. Symmetry codes: (i) -1+x, y, z; (ii) 1+x, y, z; (iii) -x, 2-y, 2-z. (iv) 1-x, 1-y, 1-z; (v) 1-x, 1-y, 2-z; (vi) 1-x, 2-y, 1-z; (vii) 1-x, 2-y, 2-z; (viii) 2-x, 2-y, 1-z; |
![[Figure 2]](./zl2114fig2thm.gif)
| Fig. 2. Packing diagram of compound I. Na—O bond is showed by black line, H atoms are omitted for clarity. |
| [Na4(CH2O6S2)2(H2O)5] | Z = 2 |
| Mr = 530.33 | F000 = 540 |
| Triclinic, P1 | Dx = 2.048 Mg m−3 |
| Hall symbol: -P 1 | Mo Kα radiation λ = 0.71073 Å |
| a = 8.7758 (7) Å | Cell parameters from 202 reflections |
| b = 9.5339 (7) Å | θ = 2.6–21.1º |
| c = 10.7878 (8) Å | µ = 0.74 mm−1 |
| α = 81.425 (2)º | T = 296 (2) K |
| β = 74.545 (2)º | Prismlike, colourless |
| γ = 87.227 (2)º | 0.30 × 0.25 × 0.25 mm |
| V = 860.19 (11) Å3 |
| Bruker SMART APEX2 diffractometer | 3321 independent reflections |
| Radiation source: fine-focus sealed tube | 3050 reflections with I > 2σ(I) |
| Monochromator: graphite | Rint = 0.022 |
| T = 296(2) K | θmax = 26.0º |
| ω scans | θmin = 2.0º |
| Absorption correction: multi-scan (SADABS; Bruker, 2000) | h = −10→10 |
| Tmin = 0.81, Tmax = 0.84 | k = −11→11 |
| 10702 measured reflections | l = −13→13 |
| Refinement on F2 | Hydrogen site location: inferred from neighbouring sites |
| Least-squares matrix: full | H-atom parameters constrained |
| R[F2 > 2σ(F2)] = 0.030 | w = 1/[σ2(Fo2) + (0.0428P)2 + 0.7023P] where P = (Fo2 + 2Fc2)/3 |
| wR(F2) = 0.093 | (Δ/σ)max = 0.001 |
| S = 1.00 | Δρmax = 0.47 e Å−3 |
| 3321 reflections | Δρmin = −0.56 e Å−3 |
| 244 parameters | Extinction correction: SHELXL97 (Sheldrick, 2008), F*=F(1+0.002xF2(sin(2θ))-0.25 |
| Primary atom site location: structure-invariant direct methods | Extinction coefficient: 0.00025 (5) |
| Secondary atom site location: difference Fourier map |
| [Na4(CH2O6S2)2(H2O)5] | γ = 87.227 (2)º |
| Mr = 530.33 | V = 860.19 (11) Å3 |
| Triclinic, P1 | Z = 2 |
| a = 8.7758 (7) Å | Mo Kα |
| b = 9.5339 (7) Å | µ = 0.74 mm−1 |
| c = 10.7878 (8) Å | T = 296 (2) K |
| α = 81.425 (2)º | 0.30 × 0.25 × 0.25 mm |
| β = 74.545 (2)º |
| Bruker SMART APEX2 diffractometer | 3321 independent reflections |
| Absorption correction: multi-scan (SADABS; Bruker, 2000) | 3050 reflections with I > 2σ(I) |
| Tmin = 0.81, Tmax = 0.84 | Rint = 0.022 |
| 10702 measured reflections |
| R[F2 > 2σ(F2)] = 0.030 | 244 parameters |
| wR(F2) = 0.093 | H-atom parameters constrained |
| S = 1.00 | Δρmax = 0.47 e Å−3 |
| 3321 reflections | Δρmin = −0.56 e Å−3 |
Geometry. All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds 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. |
| x | y | z | Uiso*/Ueq | ||
| C1 | 0.4436 (2) | 1.0561 (2) | 0.8451 (2) | 0.0189 (4) | |
| H1A | 0.4297 | 0.9743 | 0.9121 | 0.023* | |
| H1B | 0.5440 | 1.0983 | 0.8394 | 0.023* | |
| C2 | 0.9094 (3) | 0.4391 (2) | 0.8842 (2) | 0.0217 (4) | |
| H2A | 1.0010 | 0.3786 | 0.8863 | 0.026* | |
| H2B | 0.8798 | 0.4796 | 0.9647 | 0.026* | |
| Na1 | 0.55562 (10) | 0.66480 (9) | 0.86815 (9) | 0.0253 (2) | |
| Na2 | 0.85901 (11) | 0.87496 (9) | 0.59357 (9) | 0.0268 (2) | |
| Na3 | 0.54875 (13) | 0.67712 (11) | 0.52620 (12) | 0.0421 (3) | |
| Na4 | 0.08149 (10) | 0.88263 (9) | 0.88189 (8) | 0.0240 (2) | |
| O1 | 0.57149 (19) | 0.87897 (16) | 0.69116 (15) | 0.0261 (4) | |
| O2 | 0.5103 (2) | 1.11297 (17) | 0.59433 (15) | 0.0278 (4) | |
| O3 | 0.29960 (18) | 0.94639 (19) | 0.70181 (15) | 0.0287 (4) | |
| O4 | 0.3169 (2) | 1.21026 (19) | 1.01825 (16) | 0.0334 (4) | |
| O5 | 0.3122 (2) | 1.30241 (17) | 0.79628 (18) | 0.0353 (4) | |
| O6 | 0.13991 (19) | 1.11171 (17) | 0.91904 (17) | 0.0290 (4) | |
| O7 | 0.82527 (18) | 0.65404 (17) | 0.73482 (15) | 0.0259 (4) | |
| O8 | 1.06688 (19) | 0.66657 (17) | 0.80084 (17) | 0.0286 (4) | |
| O9 | 1.0542 (2) | 0.51641 (18) | 0.64174 (16) | 0.0325 (4) | |
| O10 | 0.6110 (2) | 0.41828 (18) | 0.9018 (2) | 0.0366 (4) | |
| O11 | 0.7435 (2) | 0.21996 (18) | 0.99171 (18) | 0.0352 (4) | |
| O12 | 0.7916 (2) | 0.27615 (19) | 0.75861 (17) | 0.0367 (4) | |
| O13 | 0.3962 (2) | 0.59164 (17) | 0.74448 (17) | 0.0316 (4) | |
| H13A | 0.2921 | 0.6356 | 0.7642 | 0.038* | |
| H13B | 0.3854 | 0.4893 | 0.7581 | 0.038* | |
| O14 | 0.8268 (2) | 0.7545 (2) | 0.42866 (17) | 0.0361 (4) | |
| H14A | 0.8993 | 0.6746 | 0.4159 | 0.043* | |
| H14B | 0.8388 | 0.8170 | 0.3470 | 0.043* | |
| O15 | 1.1401 (2) | 0.88559 (19) | 0.51526 (17) | 0.0338 (4) | |
| H15A | 1.1832 | 0.8177 | 0.4560 | 0.041* | |
| H15B | 1.1927 | 0.8759 | 0.5846 | 0.041* | |
| O16 | 0.6570 (2) | 0.43211 (19) | 0.54436 (17) | 0.0355 (4) | |
| H16A | 0.7614 | 0.4243 | 0.4860 | 0.043* | |
| H16B | 0.6587 | 0.3945 | 0.6326 | 0.043* | |
| O17 | −0.1158 (2) | 0.97729 (18) | 0.77543 (16) | 0.0308 (4) | |
| H17A | −0.2173 | 0.9697 | 0.8396 | 0.037* | |
| H17B | −0.0951 | 1.0776 | 0.7471 | 0.037* | |
| S1 | 0.45658 (6) | 0.99467 (5) | 0.69417 (5) | 0.01723 (13) | |
| S2 | 0.29091 (6) | 1.18145 (5) | 0.89699 (5) | 0.02035 (14) | |
| S3 | 0.96766 (6) | 0.58056 (5) | 0.75349 (5) | 0.01822 (14) | |
| S4 | 0.75141 (6) | 0.33016 (5) | 0.88177 (5) | 0.01945 (14) |
| U11 | U22 | U33 | U12 | U13 | U23 | |
| C1 | 0.0163 (10) | 0.0213 (10) | 0.0196 (9) | −0.0008 (8) | −0.0062 (8) | −0.0015 (8) |
| C2 | 0.0201 (11) | 0.0206 (10) | 0.0249 (10) | −0.0059 (8) | −0.0097 (9) | 0.0031 (8) |
| Na1 | 0.0236 (5) | 0.0240 (5) | 0.0298 (5) | −0.0020 (3) | −0.0086 (4) | −0.0049 (4) |
| Na2 | 0.0269 (5) | 0.0246 (5) | 0.0278 (5) | −0.0050 (4) | −0.0061 (4) | −0.0010 (4) |
| Na3 | 0.0352 (6) | 0.0290 (5) | 0.0592 (7) | −0.0041 (4) | −0.0151 (5) | 0.0090 (5) |
| Na4 | 0.0222 (5) | 0.0225 (4) | 0.0275 (4) | −0.0026 (3) | −0.0064 (4) | −0.0035 (3) |
| O1 | 0.0236 (8) | 0.0227 (8) | 0.0298 (8) | 0.0048 (6) | −0.0047 (6) | −0.0026 (6) |
| O2 | 0.0333 (9) | 0.0226 (8) | 0.0217 (8) | 0.0005 (7) | −0.0009 (7) | 0.0034 (6) |
| O3 | 0.0179 (8) | 0.0449 (10) | 0.0253 (8) | −0.0059 (7) | −0.0055 (6) | −0.0102 (7) |
| O4 | 0.0336 (10) | 0.0408 (10) | 0.0289 (9) | −0.0089 (8) | −0.0056 (7) | −0.0161 (8) |
| O5 | 0.0451 (11) | 0.0193 (8) | 0.0410 (10) | 0.0027 (7) | −0.0139 (8) | 0.0013 (7) |
| O6 | 0.0177 (8) | 0.0302 (9) | 0.0412 (9) | −0.0024 (7) | −0.0055 (7) | −0.0149 (7) |
| O7 | 0.0199 (8) | 0.0258 (8) | 0.0296 (8) | 0.0012 (6) | −0.0064 (6) | 0.0031 (6) |
| O8 | 0.0241 (8) | 0.0224 (8) | 0.0401 (9) | −0.0078 (6) | −0.0080 (7) | −0.0050 (7) |
| O9 | 0.0320 (9) | 0.0296 (9) | 0.0299 (9) | −0.0016 (7) | 0.0049 (7) | −0.0088 (7) |
| O10 | 0.0195 (8) | 0.0249 (9) | 0.0626 (12) | −0.0013 (7) | −0.0085 (8) | −0.0010 (8) |
| O11 | 0.0371 (10) | 0.0292 (9) | 0.0376 (9) | −0.0137 (8) | −0.0151 (8) | 0.0151 (7) |
| O12 | 0.0471 (11) | 0.0332 (10) | 0.0309 (9) | −0.0113 (8) | −0.0073 (8) | −0.0097 (7) |
| O13 | 0.0273 (9) | 0.0237 (8) | 0.0458 (10) | −0.0008 (7) | −0.0128 (8) | −0.0051 (7) |
| O14 | 0.0411 (11) | 0.0366 (10) | 0.0339 (9) | 0.0084 (8) | −0.0144 (8) | −0.0096 (8) |
| O15 | 0.0280 (9) | 0.0371 (10) | 0.0331 (9) | 0.0018 (7) | −0.0063 (7) | 0.0011 (7) |
| O16 | 0.0296 (9) | 0.0405 (10) | 0.0330 (9) | −0.0025 (8) | −0.0060 (7) | 0.0020 (8) |
| O17 | 0.0318 (9) | 0.0290 (9) | 0.0328 (9) | −0.0004 (7) | −0.0097 (7) | −0.0061 (7) |
| S1 | 0.0149 (3) | 0.0180 (3) | 0.0175 (2) | −0.00013 (19) | −0.00291 (19) | −0.00080 (19) |
| S2 | 0.0192 (3) | 0.0183 (3) | 0.0247 (3) | −0.0022 (2) | −0.0057 (2) | −0.0062 (2) |
| S3 | 0.0165 (3) | 0.0157 (3) | 0.0210 (3) | −0.00201 (19) | −0.00272 (19) | −0.00110 (19) |
| S4 | 0.0192 (3) | 0.0153 (3) | 0.0240 (3) | −0.00369 (19) | −0.0073 (2) | 0.00080 (19) |
| C1—S2 | 1.783 (2) | Na4—O17 | 2.3942 (19) |
| C1—S1 | 1.785 (2) | Na4—O11ii | 2.3972 (19) |
| C1—H1A | 0.9700 | Na4—O6viii | 2.4881 (18) |
| C1—H1B | 0.9700 | Na4—Na4viii | 3.6050 (17) |
| C2—S4 | 1.780 (2) | Na4—Na2vii | 4.1000 (13) |
| C2—S3 | 1.785 (2) | O1—S1 | 1.4562 (16) |
| C2—H2A | 0.9700 | O2—S1 | 1.4398 (16) |
| C2—H2B | 0.9700 | O2—Na3v | 2.3339 (18) |
| Na1—O4i | 2.3382 (19) | O3—S1 | 1.4512 (16) |
| Na1—O13 | 2.3644 (19) | O4—S2 | 1.4528 (17) |
| Na1—O10 | 2.3709 (19) | O4—Na1i | 2.3382 (19) |
| Na1—O7 | 2.4260 (18) | O5—S2 | 1.4437 (18) |
| Na1—O10ii | 2.552 (2) | O6—S2 | 1.4577 (17) |
| Na1—O1 | 2.5607 (18) | O6—Na4viii | 2.4881 (18) |
| Na1—O11ii | 2.913 (2) | O7—S3 | 1.4492 (16) |
| Na1—S4ii | 3.2699 (10) | O8—S3 | 1.4569 (16) |
| Na1—Na3 | 3.6898 (15) | O8—Na4iii | 2.3763 (18) |
| Na1—Na2 | 3.7975 (13) | O9—S3 | 1.4460 (16) |
| Na1—Na1ii | 3.8822 (18) | O10—S4 | 1.4432 (17) |
| Na2—O14 | 2.3389 (19) | O10—Na1ii | 2.552 (2) |
| Na2—O17iii | 2.3816 (19) | O11—S4 | 1.4515 (17) |
| Na2—O15 | 2.3866 (19) | O11—Na4ii | 2.3972 (19) |
| Na2—O7 | 2.3893 (18) | O11—Na1ii | 2.913 (2) |
| Na2—O15iv | 2.4057 (19) | O12—S4 | 1.4462 (17) |
| Na2—O1 | 2.4623 (18) | O13—H13A | 0.9700 |
| Na2—Na2iv | 3.5152 (18) | O13—H13B | 0.9700 |
| Na2—Na3 | 3.6688 (15) | O14—H14A | 0.9700 |
| Na2—Na4iii | 4.1000 (13) | O14—H14B | 0.9700 |
| Na3—O2v | 2.3339 (18) | O15—Na2iv | 2.4057 (19) |
| Na3—O13 | 2.420 (2) | O15—H15A | 0.9700 |
| Na3—O16vi | 2.465 (2) | O15—H15B | 0.9700 |
| Na3—O16 | 2.479 (2) | O16—Na3vi | 2.465 (2) |
| Na3—O14 | 2.486 (2) | O16—H16A | 0.9700 |
| Na3—O1 | 2.856 (2) | O16—H16B | 0.9700 |
| Na3—Na3vi | 3.683 (2) | O17—Na2vii | 2.3816 (19) |
| Na4—O3 | 2.3635 (18) | O17—H17A | 0.9700 |
| Na4—O8vii | 2.3763 (18) | O17—H17B | 0.9700 |
| Na4—O6 | 2.3816 (18) | S4—Na1ii | 3.2699 (10) |
| S2—C1—S1 | 117.32 (11) | O13—Na3—Na2 | 100.89 (6) |
| S2—C1—H1A | 108.0 | O16vi—Na3—Na2 | 172.47 (6) |
| S1—C1—H1A | 108.0 | O16—Na3—Na2 | 101.22 (6) |
| S2—C1—H1B | 108.0 | O14—Na3—Na2 | 39.03 (5) |
| S1—C1—H1B | 108.0 | O1—Na3—Na2 | 42.08 (4) |
| H1A—C1—H1B | 107.2 | O2v—Na3—Na3vi | 123.29 (7) |
| S4—C2—S3 | 117.32 (12) | O13—Na3—Na3vi | 81.18 (5) |
| S4—C2—H2A | 108.0 | O16vi—Na3—Na3vi | 41.99 (5) |
| S3—C2—H2A | 108.0 | O16—Na3—Na3vi | 41.70 (5) |
| S4—C2—H2B | 108.0 | O14—Na3—Na3vi | 116.43 (7) |
| S3—C2—H2B | 108.0 | O1—Na3—Na3vi | 151.94 (6) |
| H2A—C2—H2B | 107.2 | Na2—Na3—Na3vi | 142.60 (5) |
| O4i—Na1—O13 | 166.18 (8) | O2v—Na3—Na1 | 121.20 (6) |
| O4i—Na1—O10 | 111.23 (8) | O13—Na3—Na1 | 38.99 (5) |
| O13—Na1—O10 | 82.42 (7) | O16vi—Na3—Na1 | 124.37 (6) |
| O4i—Na1—O7 | 80.23 (6) | O16—Na3—Na1 | 85.67 (5) |
| O13—Na1—O7 | 105.45 (7) | O14—Na3—Na1 | 96.42 (5) |
| O10—Na1—O7 | 78.58 (6) | O1—Na3—Na1 | 43.79 (4) |
| O4i—Na1—O10ii | 81.40 (7) | Na2—Na3—Na1 | 62.14 (3) |
| O13—Na1—O10ii | 100.65 (7) | Na3vi—Na3—Na1 | 109.09 (4) |
| O10—Na1—O10ii | 75.97 (7) | O3—Na4—O8vii | 88.53 (6) |
| O7—Na1—O10ii | 140.45 (7) | O3—Na4—O6 | 78.83 (6) |
| O4i—Na1—O1 | 91.18 (7) | O8vii—Na4—O6 | 167.28 (7) |
| O13—Na1—O1 | 78.18 (6) | O3—Na4—O17 | 95.65 (7) |
| O10—Na1—O1 | 142.97 (7) | O8vii—Na4—O17 | 87.86 (6) |
| O7—Na1—O1 | 76.66 (6) | O6—Na4—O17 | 92.01 (6) |
| O10ii—Na1—O1 | 138.45 (6) | O3—Na4—O11ii | 90.43 (7) |
| O4i—Na1—O11ii | 88.36 (6) | O8vii—Na4—O11ii | 92.18 (7) |
| O13—Na1—O11ii | 82.51 (6) | O6—Na4—O11ii | 89.29 (7) |
| O10—Na1—O11ii | 120.57 (6) | O17—Na4—O11ii | 173.92 (7) |
| O7—Na1—O11ii | 160.46 (6) | O3—Na4—O6viii | 163.22 (7) |
| O10ii—Na1—O11ii | 51.33 (5) | O8vii—Na4—O6viii | 108.07 (6) |
| O1—Na1—O11ii | 87.86 (5) | O6—Na4—O6viii | 84.51 (6) |
| O4i—Na1—S4ii | 85.44 (5) | O17—Na4—O6viii | 82.85 (6) |
| O13—Na1—S4ii | 90.84 (5) | O11ii—Na4—O6viii | 91.36 (7) |
| O10—Na1—S4ii | 97.33 (5) | O3—Na4—Na4viii | 122.20 (6) |
| O7—Na1—S4ii | 162.36 (5) | O8vii—Na4—Na4viii | 149.15 (6) |
| O10ii—Na1—S4ii | 25.03 (4) | O6—Na4—Na4viii | 43.39 (4) |
| O1—Na1—S4ii | 114.07 (5) | O17—Na4—Na4viii | 86.40 (5) |
| O11ii—Na1—S4ii | 26.35 (3) | O11ii—Na4—Na4viii | 90.47 (6) |
| O4i—Na1—Na3 | 135.93 (6) | O6viii—Na4—Na4viii | 41.12 (4) |
| O13—Na1—Na3 | 40.08 (5) | O3—Na4—Na2vii | 81.93 (5) |
| O10—Na1—Na3 | 95.38 (6) | O8vii—Na4—Na2vii | 60.20 (5) |
| O7—Na1—Na3 | 71.14 (5) | O6—Na4—Na2vii | 115.90 (5) |
| O10ii—Na1—Na3 | 140.70 (6) | O17—Na4—Na2vii | 30.76 (4) |
| O1—Na1—Na3 | 50.52 (4) | O11ii—Na4—Na2vii | 151.34 (6) |
| O11ii—Na1—Na3 | 108.04 (5) | O6viii—Na4—Na2vii | 103.86 (5) |
| S4ii—Na1—Na3 | 126.48 (3) | Na4viii—Na4—Na2vii | 117.00 (4) |
| O4i—Na1—Na2 | 78.15 (5) | S1—O1—Na2 | 131.01 (10) |
| O13—Na1—Na2 | 98.51 (5) | S1—O1—Na1 | 125.55 (9) |
| O10—Na1—Na2 | 114.45 (6) | Na2—O1—Na1 | 98.21 (6) |
| O7—Na1—Na2 | 37.60 (4) | S1—O1—Na3 | 114.45 (9) |
| O10ii—Na1—Na2 | 159.32 (5) | Na2—O1—Na3 | 86.90 (5) |
| O1—Na1—Na2 | 39.92 (4) | Na1—O1—Na3 | 85.68 (5) |
| O11ii—Na1—Na2 | 124.52 (4) | S1—O2—Na3v | 148.85 (11) |
| S4ii—Na1—Na2 | 147.72 (3) | S1—O3—Na4 | 131.30 (9) |
| Na3—Na1—Na2 | 58.66 (3) | S2—O4—Na1i | 150.62 (11) |
| O4i—Na1—Na1ii | 97.06 (6) | S2—O6—Na4 | 130.70 (10) |
| O13—Na1—Na1ii | 92.35 (5) | S2—O6—Na4viii | 123.77 (9) |
| O10—Na1—Na1ii | 39.63 (5) | Na4—O6—Na4viii | 95.49 (6) |
| O7—Na1—Na1ii | 112.71 (5) | S3—O7—Na2 | 116.86 (9) |
| O10ii—Na1—Na1ii | 36.33 (4) | S3—O7—Na1 | 134.13 (9) |
| O1—Na1—Na1ii | 168.41 (6) | Na2—O7—Na1 | 104.11 (6) |
| O11ii—Na1—Na1ii | 84.25 (4) | S3—O8—Na4iii | 144.64 (11) |
| S4ii—Na1—Na1ii | 58.81 (2) | S4—O10—Na1 | 135.88 (11) |
| Na3—Na1—Na1ii | 124.47 (4) | S4—O10—Na1ii | 106.52 (10) |
| Na2—Na1—Na1ii | 150.21 (4) | Na1—O10—Na1ii | 104.03 (7) |
| O14—Na2—O17iii | 174.53 (8) | S4—O11—Na4ii | 136.83 (11) |
| O14—Na2—O15 | 94.48 (7) | S4—O11—Na1ii | 90.67 (9) |
| O17iii—Na2—O15 | 87.48 (7) | Na4ii—O11—Na1ii | 117.01 (7) |
| O14—Na2—O7 | 88.36 (7) | Na1—O13—Na3 | 100.93 (7) |
| O17iii—Na2—O7 | 86.24 (6) | Na1—O13—H13A | 111.6 |
| O15—Na2—O7 | 101.40 (7) | Na3—O13—H13A | 111.6 |
| O14—Na2—O15iv | 99.06 (7) | Na1—O13—H13B | 111.6 |
| O17iii—Na2—O15iv | 86.17 (7) | Na3—O13—H13B | 111.6 |
| O15—Na2—O15iv | 85.64 (7) | H13A—O13—H13B | 109.4 |
| O7—Na2—O15iv | 169.40 (7) | Na2—O14—Na3 | 98.94 (7) |
| O14—Na2—O1 | 91.38 (7) | Na2—O14—H14A | 112.0 |
| O17iii—Na2—O1 | 86.73 (6) | Na3—O14—H14A | 112.0 |
| O15—Na2—O1 | 174.12 (7) | Na2—O14—H14B | 112.0 |
| O7—Na2—O1 | 79.24 (6) | Na3—O14—H14B | 112.0 |
| O15iv—Na2—O1 | 92.95 (6) | H14A—O14—H14B | 109.7 |
| O14—Na2—Na2iv | 99.26 (6) | Na2—O15—Na2iv | 94.36 (7) |
| O17iii—Na2—Na2iv | 85.67 (6) | Na2—O15—H15A | 112.9 |
| O15—Na2—Na2iv | 43.03 (5) | Na2iv—O15—H15A | 112.9 |
| O7—Na2—Na2iv | 143.79 (6) | Na2—O15—H15B | 112.9 |
| O15iv—Na2—Na2iv | 42.61 (5) | Na2iv—O15—H15B | 112.9 |
| O1—Na2—Na2iv | 135.28 (6) | H15A—O15—H15B | 110.3 |
| O14—Na2—Na3 | 42.03 (5) | Na3vi—O16—Na3 | 96.30 (7) |
| O17iii—Na2—Na3 | 134.64 (6) | Na3vi—O16—H16A | 112.5 |
| O15—Na2—Na3 | 134.80 (6) | Na3—O16—H16A | 112.5 |
| O7—Na2—Na3 | 71.87 (5) | Na3vi—O16—H16B | 112.5 |
| O15iv—Na2—Na3 | 108.79 (6) | Na3—O16—H16B | 112.5 |
| O1—Na2—Na3 | 51.02 (5) | H16A—O16—H16B | 110.0 |
| Na2iv—Na2—Na3 | 134.34 (4) | Na2vii—O17—Na4 | 118.30 (8) |
| O14—Na2—Na1 | 96.33 (6) | Na2vii—O17—H17A | 107.7 |
| O17iii—Na2—Na1 | 78.85 (5) | Na4—O17—H17A | 107.7 |
| O15—Na2—Na1 | 137.49 (5) | Na2vii—O17—H17B | 107.7 |
| O7—Na2—Na1 | 38.29 (4) | Na4—O17—H17B | 107.7 |
| O15iv—Na2—Na1 | 132.48 (5) | H17A—O17—H17B | 107.1 |
| O1—Na2—Na1 | 41.87 (4) | O2—S1—O3 | 113.99 (10) |
| Na2iv—Na2—Na1 | 164.30 (4) | O2—S1—O1 | 113.19 (9) |
| Na3—Na2—Na1 | 59.20 (3) | O3—S1—O1 | 112.55 (10) |
| O14—Na2—Na4iii | 146.42 (6) | O2—S1—C1 | 106.32 (10) |
| O17iii—Na2—Na4iii | 30.94 (5) | O3—S1—C1 | 106.12 (9) |
| O15—Na2—Na4iii | 66.79 (5) | O1—S1—C1 | 103.62 (10) |
| O7—Na2—Na4iii | 69.72 (5) | O5—S2—O4 | 114.42 (11) |
| O15iv—Na2—Na4iii | 106.56 (5) | O5—S2—O6 | 112.59 (11) |
| O1—Na2—Na4iii | 108.29 (5) | O4—S2—O6 | 111.20 (10) |
| Na2iv—Na2—Na4iii | 85.84 (3) | O5—S2—C1 | 107.49 (10) |
| Na3—Na2—Na4iii | 139.39 (3) | O4—S2—C1 | 102.79 (10) |
| Na1—Na2—Na4iii | 82.22 (3) | O6—S2—C1 | 107.57 (10) |
| O2v—Na3—O13 | 123.40 (7) | O9—S3—O7 | 113.00 (10) |
| O2v—Na3—O16vi | 86.03 (7) | O9—S3—O8 | 112.97 (10) |
| O13—Na3—O16vi | 85.41 (7) | O7—S3—O8 | 112.99 (10) |
| O2v—Na3—O16 | 152.16 (8) | O9—S3—C2 | 106.55 (10) |
| O13—Na3—O16 | 81.48 (6) | O7—S3—C2 | 107.55 (10) |
| O16vi—Na3—O16 | 83.70 (7) | O8—S3—C2 | 102.91 (10) |
| O2v—Na3—O14 | 83.66 (7) | O10—S4—O12 | 113.60 (12) |
| O13—Na3—O14 | 134.23 (8) | O10—S4—O11 | 111.27 (11) |
| O16vi—Na3—O14 | 136.85 (8) | O12—S4—O11 | 113.07 (11) |
| O16—Na3—O14 | 86.32 (7) | O10—S4—C2 | 106.45 (10) |
| O2v—Na3—O1 | 79.21 (6) | O12—S4—C2 | 107.98 (11) |
| O13—Na3—O1 | 71.68 (6) | O11—S4—C2 | 103.70 (10) |
| O16vi—Na3—O1 | 138.69 (7) | O10—S4—Na1ii | 48.45 (8) |
| O16—Na3—O1 | 124.33 (7) | O12—S4—Na1ii | 137.74 (8) |
| O14—Na3—O1 | 79.74 (6) | O11—S4—Na1ii | 62.98 (8) |
| O2v—Na3—Na2 | 87.04 (5) | C2—S4—Na1ii | 113.81 (8) |
| Symmetry codes: (i) −x+1, −y+2, −z+2; (ii) −x+1, −y+1, −z+2; (iii) x+1, y, z; (iv) −x+2, −y+2, −z+1; (v) −x+1, −y+2, −z+1; (vi) −x+1, −y+1, −z+1; (vii) x−1, y, z; (viii) −x, −y+2, −z+2. |
| D—H···A | D—H | H···A | D···A | D—H···A |
| O13—H13A···O8vii | 0.97 | 1.93 | 2.868 (2) | 163 |
| O13—H13B···O5ix | 0.97 | 1.87 | 2.824 (2) | 166 |
| O14—H14A···O9x | 0.97 | 2.00 | 2.871 (2) | 148 |
| O15—H15B···O3iii | 0.97 | 1.97 | 2.877 (2) | 155 |
| O16—H16A···O9x | 0.97 | 1.87 | 2.794 (2) | 158 |
| O16—H16B···O12 | 0.97 | 2.18 | 3.034 (3) | 147 |
| O17—H17A···O4viii | 0.97 | 2.17 | 2.879 (3) | 129 |
| O17—H17B···O12xi | 0.97 | 2.10 | 2.918 (3) | 141 |
| Symmetry codes: (vii) x−1, y, z; (ix) x, y−1, z; (x) −x+2, −y+1, −z+1; (iii) x+1, y, z; (viii) −x, −y+2, −z+2; (xi) x−1, y+1, z. |
| D—H···A | D—H | H···A | D···A | D—H···A |
| O13—H13A···O8i | 0.97 | 1.93 | 2.868 (2) | 163 |
| O13—H13B···O5ii | 0.97 | 1.87 | 2.824 (2) | 166 |
| O14—H14A···O9iii | 0.97 | 2.00 | 2.871 (2) | 148 |
| O15—H15B···O3iv | 0.97 | 1.97 | 2.877 (2) | 155 |
| O16—H16A···O9iii | 0.97 | 1.87 | 2.794 (2) | 158 |
| O16—H16B···O12 | 0.97 | 2.18 | 3.034 (3) | 147 |
| O17—H17A···O4v | 0.97 | 2.17 | 2.879 (3) | 129 |
| O17—H17B···O12vi | 0.97 | 2.10 | 2.918 (3) | 141 |
| Symmetry codes: (i) x−1, y, z; (ii) x, y−1, z; (iii) −x+2, −y+1, −z+1; (iv) x+1, y, z; (v) −x, −y+2, −z+2; (vi) x−1, y+1, z. |
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Due to the weak coordination strength of monosulfonate ions, most metal complexes of these ligands obtained from aqueous solution are water-coordinated metal sulfonate salts, and the coordination chemistry of the sulfonate ion has been less well investigated in comparison with other organic acidato anions such as carbonates and phosfonates (Côté & Shimizu, 2003). However, by employing disulfonates, which can provide multiple potentially chelating coordination sites, stable networks sustained by sulfonate-metal interactions can be obtained with various dimensionalities (Cai, 2004; Li et al., 2008; Mi et al., 2007; Videnova-Adrabinska, 2007).
The present structral study of the title compound {Na4(mds)2(H2O) 5}n (I) reveals the existence of sulfonate-sodium interactions. The asymmetric unit consists of four sodium ions, five coordinated µ2-H2O molecules and two CH3(SO3)22- ligands (Fig. 1). Of the four sodium ions, Na1, Na2 and Na4 are six-coordinated. Na3 is coordinated by five oxygen atoms (O2vi, O13, O14, O16 and O16iv). The Na—O bond lengths fall in the range of 2.334 (2) to 2.5609 (18) Å. All sulfonate oxygens are deprotonated. Three sulfonate oxygen atoms (O5, O9 and O12) are not coordinated to sodium atoms and do instead act as hydrogen bonding acceptors towards coordinated water molecules. All other hydrogen bonds are from water molecules towards Na coordinated sulfonate oxygen atoms (Table 1).
Each sodium atom is bridged to an equivalent neighbour, forming {Na2O2} dimers with inversion centers in the middle. O1 and O7 connect the dimers of Na1 and Na2 into an infinite chain. Na1-Na2 chains are joined to dimers of Na3 and Na4 through intricate bridges of oxygens from sulfonate groups and coordinated waters, and O—S—O connectivities, thus generating a three-dimensional network (Fig. 2).