Supporting information
Crystallographic Information File (CIF) https://doi.org/10.1107/S1600536811030777/tk2770sup1.cif | |
Structure factor file (CIF format) https://doi.org/10.1107/S1600536811030777/tk2770Isup2.hkl |
CCDC reference: 845210
Key indicators
- Single-crystal X-ray study
- T = 200 K
- Mean (C-C) = 0.002 Å
- R factor = 0.032
- wR factor = 0.086
- Data-to-parameter ratio = 13.9
checkCIF/PLATON results
No syntax errors found
Alert level B PLAT420_ALERT_2_B D-H Without Acceptor O2W - H22W ... ?
Alert level C PLAT042_ALERT_1_C Calc. and Reported MoietyFormula Strings Differ ? PLAT910_ALERT_3_C Missing # of FCF Reflections Below Th(Min) ..... 2 PLAT912_ALERT_4_C Missing # of FCF Reflections Above STh/L= 0.600 370
Alert level G PLAT005_ALERT_5_G No _iucr_refine_instructions_details in CIF .... ?
0 ALERT level A = Most likely a serious problem - resolve or explain 1 ALERT level B = A potentially serious problem, consider carefully 3 ALERT level C = Check. Ensure it is not caused by an omission or oversight 1 ALERT level G = General information/check it is not something unexpected 1 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 1 ALERT type 4 Improvement, methodology, query or suggestion 1 ALERT type 5 Informative message, check
The title compound was synthesized by heating 218 mg (1 mmol) of 3-carboxy-4-hydroxybenzenesulfonic acid (5-sulfosalicylic acid) with an excess of MgCO3 in 50 ml of 1:1 ethanol–water under reflux for 10 min. After completion of the reaction, the unreacted MgCO3 was removed by filtration and the solution was allowed evaporate to incipient dryness at room temperature, giving small colourless prisms of the title compound from which a specimen was cleaved for the X-ray analysis.
Hydrogen atoms involved in hydrogen-bonding interactions were located by difference methods and their positional and isotropic displacement parameters were refined. Other H-atoms were included in the refinement at calculated positions [C–H = 0.93 Å and with Uiso(H) = 1.2Ueq(C), using a riding-model approximation.
Data collection: CrysAlis PRO (Oxford Diffraction, 2010); cell refinement: CrysAlis PRO (Oxford Diffraction, 2010); data reduction: CrysAlis PRO (Oxford Diffraction, 2010); program(s) used to solve structure: SIR92 (Altomare et al., 1994); program(s) used to refine structure: SHELXL97 (Sheldrick, 2008) within WinGX (Farrugia, 1999); molecular graphics: PLATON (Spek, 2009); software used to prepare material for publication: PLATON (Spek, 2009).
[Mg(H2O)6](C7H5O6S)2·2H2O | Z = 1 |
Mr = 602.78 | F(000) = 314 |
Triclinic, P1 | Dx = 1.613 Mg m−3 |
Hall symbol: -P 1 | Mo Kα radiation, λ = 0.71073 Å |
a = 6.8694 (4) Å | Cell parameters from 4714 reflections |
b = 6.9069 (4) Å | θ = 3.2–28.9° |
c = 14.3950 (8) Å | µ = 0.33 mm−1 |
α = 77.472 (5)° | T = 200 K |
β = 78.120 (4)° | Prism, colourless |
γ = 70.131 (5)° | 0.40 × 0.12 × 0.10 mm |
V = 620.51 (6) Å3 |
Oxford Diffraction Gemini-S CCD-detector diffractometer | 2899 independent reflections |
Radiation source: Enhance (Mo) X-ray source | 2553 reflections with I > 2σ(I) |
Graphite monochromator | Rint = 0.023 |
ω scans | θmax = 28.8°, θmin = 3.2° |
Absorption correction: multi-scan (CrysAlis PRO; Oxford Diffraction, 2010) | h = −9→9 |
Tmin = 0.96, Tmax = 0.99 | k = −9→8 |
8134 measured reflections | l = −19→18 |
Refinement on F2 | Primary atom site location: structure-invariant direct methods |
Least-squares matrix: full | Secondary atom site location: difference Fourier map |
R[F2 > 2σ(F2)] = 0.032 | Hydrogen site location: inferred from neighbouring sites |
wR(F2) = 0.086 | H atoms treated by a mixture of independent and constrained refinement |
S = 1.14 | w = 1/[σ2(Fo2) + (0.0388P)2 + 0.10P] where P = (Fo2 + 2Fc2)/3 |
2899 reflections | (Δ/σ)max = 0.001 |
209 parameters | Δρmax = 0.34 e Å−3 |
0 restraints | Δρmin = −0.43 e Å−3 |
[Mg(H2O)6](C7H5O6S)2·2H2O | γ = 70.131 (5)° |
Mr = 602.78 | V = 620.51 (6) Å3 |
Triclinic, P1 | Z = 1 |
a = 6.8694 (4) Å | Mo Kα radiation |
b = 6.9069 (4) Å | µ = 0.33 mm−1 |
c = 14.3950 (8) Å | T = 200 K |
α = 77.472 (5)° | 0.40 × 0.12 × 0.10 mm |
β = 78.120 (4)° |
Oxford Diffraction Gemini-S CCD-detector diffractometer | 2899 independent reflections |
Absorption correction: multi-scan (CrysAlis PRO; Oxford Diffraction, 2010) | 2553 reflections with I > 2σ(I) |
Tmin = 0.96, Tmax = 0.99 | Rint = 0.023 |
8134 measured reflections |
R[F2 > 2σ(F2)] = 0.032 | 0 restraints |
wR(F2) = 0.086 | H atoms treated by a mixture of independent and constrained refinement |
S = 1.14 | Δρmax = 0.34 e Å−3 |
2899 reflections | Δρmin = −0.43 e Å−3 |
209 parameters |
Geometry. Bond distances, angles etc. have been calculated using the rounded fractional coordinates. All su's are estimated from the variances of the (full) variance-covariance matrix. The cell e.s.d.'s are taken into account in the estimation of distances, angles and torsion angles |
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 | ||
S5 | 0.32291 (6) | 0.27288 (6) | 0.24107 (3) | 0.0205 (1) | |
O2 | −0.30636 (17) | 0.30257 (19) | 0.58938 (9) | 0.0293 (4) | |
O11 | 0.33290 (17) | 0.10533 (19) | 0.60809 (9) | 0.0282 (4) | |
O12 | 0.00797 (17) | 0.16915 (18) | 0.68922 (8) | 0.0285 (3) | |
O51 | 0.21125 (18) | 0.34405 (17) | 0.15798 (8) | 0.0282 (3) | |
O52 | 0.4428 (2) | 0.4036 (2) | 0.24880 (9) | 0.0358 (4) | |
O53 | 0.45513 (17) | 0.05481 (18) | 0.24189 (8) | 0.0288 (3) | |
C1 | 0.0565 (2) | 0.2280 (2) | 0.51806 (10) | 0.0168 (4) | |
C2 | −0.1584 (2) | 0.2911 (2) | 0.51141 (11) | 0.0198 (4) | |
C3 | −0.2240 (2) | 0.3455 (2) | 0.42131 (12) | 0.0235 (5) | |
C4 | −0.0799 (2) | 0.3391 (2) | 0.33881 (11) | 0.0223 (4) | |
C5 | 0.1338 (2) | 0.2784 (2) | 0.34503 (11) | 0.0182 (4) | |
C6 | 0.2005 (2) | 0.2238 (2) | 0.43408 (11) | 0.0176 (4) | |
C11 | 0.1284 (2) | 0.1655 (2) | 0.61309 (11) | 0.0193 (4) | |
Mg1 | 0.00000 | 0.00000 | 0.00000 | 0.0200 (2) | |
O1W | 0.0127 (2) | 0.0693 (2) | 0.12890 (9) | 0.0323 (4) | |
O2W | 0.3193 (2) | −0.1459 (2) | −0.01676 (11) | 0.0338 (4) | |
O3W | 0.0515 (2) | 0.27534 (19) | −0.06749 (9) | 0.0307 (4) | |
O4W | 0.5409 (2) | 0.7353 (2) | 0.13401 (10) | 0.0313 (4) | |
H2 | −0.244 (3) | 0.264 (3) | 0.6383 (17) | 0.045 (6)* | |
H3 | −0.36580 | 0.38640 | 0.41680 | 0.0280* | |
H4 | −0.12490 | 0.37510 | 0.27890 | 0.0270* | |
H6 | 0.34260 | 0.18390 | 0.43800 | 0.0210* | |
H11 | 0.369 (4) | 0.070 (3) | 0.6595 (18) | 0.049 (7)* | |
H11W | −0.002 (3) | −0.002 (3) | 0.1845 (18) | 0.049 (6)* | |
H12W | 0.067 (4) | 0.155 (4) | 0.1343 (17) | 0.050 (7)* | |
H21W | 0.395 (4) | −0.180 (4) | 0.025 (2) | 0.061 (8)* | |
H22W | 0.383 (5) | −0.180 (4) | −0.068 (2) | 0.083 (10)* | |
H31W | −0.028 (4) | 0.370 (4) | −0.0898 (17) | 0.044 (7)* | |
H32W | 0.177 (4) | 0.293 (4) | −0.0885 (17) | 0.055 (7)* | |
H41W | 0.490 (4) | 0.826 (4) | 0.1655 (18) | 0.058 (8)* | |
H42W | 0.514 (4) | 0.631 (4) | 0.1686 (18) | 0.055 (7)* |
U11 | U22 | U33 | U12 | U13 | U23 | |
S5 | 0.0224 (2) | 0.0251 (2) | 0.0139 (2) | −0.0083 (2) | −0.0034 (1) | −0.0009 (1) |
O2 | 0.0175 (6) | 0.0402 (7) | 0.0254 (7) | −0.0054 (5) | 0.0016 (5) | −0.0055 (5) |
O11 | 0.0199 (6) | 0.0418 (7) | 0.0185 (6) | −0.0022 (5) | −0.0075 (5) | −0.0035 (5) |
O12 | 0.0263 (6) | 0.0358 (6) | 0.0176 (6) | −0.0060 (5) | −0.0002 (5) | −0.0007 (5) |
O51 | 0.0354 (6) | 0.0288 (6) | 0.0177 (6) | −0.0063 (5) | −0.0106 (5) | 0.0022 (4) |
O52 | 0.0433 (7) | 0.0494 (8) | 0.0254 (6) | −0.0322 (6) | −0.0010 (6) | −0.0027 (5) |
O53 | 0.0267 (6) | 0.0321 (6) | 0.0212 (6) | 0.0025 (5) | −0.0061 (5) | −0.0074 (5) |
C1 | 0.0171 (7) | 0.0134 (6) | 0.0189 (7) | −0.0034 (5) | −0.0042 (6) | −0.0014 (5) |
C2 | 0.0177 (7) | 0.0166 (7) | 0.0237 (8) | −0.0040 (6) | −0.0007 (6) | −0.0048 (6) |
C3 | 0.0154 (7) | 0.0246 (8) | 0.0301 (9) | −0.0028 (6) | −0.0067 (6) | −0.0058 (6) |
C4 | 0.0218 (7) | 0.0224 (7) | 0.0223 (8) | −0.0029 (6) | −0.0105 (6) | −0.0025 (6) |
C5 | 0.0192 (7) | 0.0174 (7) | 0.0173 (7) | −0.0052 (6) | −0.0030 (6) | −0.0017 (5) |
C6 | 0.0152 (7) | 0.0177 (7) | 0.0192 (7) | −0.0038 (5) | −0.0044 (6) | −0.0016 (5) |
C11 | 0.0206 (7) | 0.0168 (7) | 0.0190 (7) | −0.0033 (6) | −0.0036 (6) | −0.0029 (6) |
Mg1 | 0.0227 (4) | 0.0233 (4) | 0.0142 (4) | −0.0084 (3) | −0.0045 (3) | 0.0007 (3) |
O1W | 0.0492 (8) | 0.0395 (7) | 0.0156 (6) | −0.0245 (6) | −0.0067 (5) | −0.0005 (5) |
O2W | 0.0254 (6) | 0.0455 (8) | 0.0245 (7) | −0.0053 (6) | −0.0017 (6) | −0.0042 (6) |
O3W | 0.0247 (6) | 0.0250 (6) | 0.0371 (7) | −0.0078 (5) | −0.0063 (6) | 0.0079 (5) |
O4W | 0.0300 (7) | 0.0287 (7) | 0.0357 (7) | −0.0114 (6) | −0.0048 (6) | −0.0022 (6) |
S5—O51 | 1.4584 (15) | O2W—H21W | 0.82 (3) |
S5—O52 | 1.4466 (17) | O2W—H22W | 0.82 (3) |
S5—O53 | 1.4699 (15) | O3W—H32W | 0.89 (3) |
S5—C5 | 1.7661 (19) | O3W—H31W | 0.75 (3) |
Mg1—O1W | 2.0396 (17) | O4W—H42W | 0.84 (3) |
Mg1—O2W | 2.0664 (19) | O4W—H41W | 0.79 (3) |
Mg1—O3W | 2.0494 (17) | C1—C11 | 1.476 (2) |
Mg1—O1Wi | 2.0396 (17) | C1—C6 | 1.394 (2) |
Mg1—O2Wi | 2.0664 (19) | C1—C2 | 1.408 (2) |
Mg1—O3Wi | 2.0494 (17) | C2—C3 | 1.393 (2) |
O2—C2 | 1.347 (2) | C3—C4 | 1.379 (2) |
O11—C11 | 1.314 (2) | C4—C5 | 1.399 (2) |
O12—C11 | 1.229 (2) | C5—C6 | 1.382 (2) |
O2—H2 | 0.85 (2) | C3—H3 | 0.9300 |
O11—H11 | 0.79 (3) | C4—H4 | 0.9300 |
O1W—H11W | 0.85 (2) | C6—H6 | 0.9300 |
O1W—H12W | 0.82 (3) | ||
S5···H12W | 2.96 (3) | O1W···H22Wi | 2.83 (4) |
S5···H42W | 3.08 (3) | O2···H3v | 2.5300 |
S5···H11ii | 2.92 (2) | O2W···H32W | 2.87 (3) |
S5···H22Wiii | 2.91 (3) | O3W···H12W | 2.86 (2) |
O1W···O2W | 2.907 (3) | O4W···H32Wx | 1.87 (3) |
O1W···O3W | 2.879 (2) | O4W···H21Wxi | 1.91 (3) |
O1W···O51 | 2.824 (2) | O11···H6 | 2.3800 |
O1W···O12iv | 2.779 (2) | O11···H6ii | 2.5200 |
O1W···O2Wi | 2.900 (3) | O12···H11Wiv | 1.93 (2) |
O1W···O3Wi | 2.903 (2) | O12···H2 | 1.87 (2) |
O2···C3v | 3.324 (3) | O51···H4 | 2.5600 |
O2···O11vi | 3.151 (3) | O51···H31Wix | 2.10 (3) |
O2···O12 | 2.632 (2) | O51···H22Wiii | 2.78 (3) |
O2···O52vii | 3.207 (3) | O51···H12W | 2.00 (3) |
O2W···O3Wi | 2.926 (3) | O52···H6 | 2.8900 |
O2W···O1W | 2.907 (3) | O52···H2vii | 2.89 (2) |
O2W···O3W | 2.894 (2) | O52···H42W | 1.88 (3) |
O2W···O1Wi | 2.900 (3) | O53···H11ii | 1.92 (3) |
O2W···O4Wviii | 2.728 (3) | O53···H22Wiii | 2.61 (3) |
O3W···O2W | 2.894 (2) | O53···H41Wviii | 2.04 (3) |
O3W···O1W | 2.879 (2) | C1···C2iv | 3.515 (3) |
O3W···O51ix | 2.850 (2) | C1···C1vii | 3.511 (3) |
O3W···O1Wi | 2.903 (2) | C1···C2vii | 3.543 (3) |
O3W···O2Wi | 2.926 (3) | C2···C1vii | 3.543 (3) |
O3W···O4Wx | 2.748 (3) | C2···C6iv | 3.570 (3) |
O4W···O2Wxi | 2.728 (3) | C2···C6vii | 3.509 (3) |
O4W···O53xi | 2.803 (2) | C2···C1iv | 3.515 (3) |
O4W···O52 | 2.717 (2) | C3···C11vii | 3.568 (3) |
O4W···O3Wx | 2.748 (3) | C3···C11iv | 3.490 (3) |
O11···O2xii | 3.151 (3) | C3···O2v | 3.324 (3) |
O11···O53ii | 2.678 (2) | C4···C11vii | 3.529 (3) |
O11···C6ii | 3.264 (3) | C4···C11iv | 3.519 (3) |
O12···O1Wiv | 2.779 (2) | C6···C2iv | 3.570 (3) |
O12···O2 | 2.632 (2) | C6···C2vii | 3.509 (3) |
O51···O1W | 2.824 (2) | C6···O11ii | 3.264 (3) |
O51···O3Wix | 2.850 (2) | C11···C4vii | 3.529 (3) |
O52···O4W | 2.717 (2) | C11···C3iv | 3.490 (3) |
O52···O2vii | 3.207 (3) | C11···C3vii | 3.568 (3) |
O53···O4Wviii | 2.803 (2) | C11···C4iv | 3.519 (3) |
O53···O11ii | 2.678 (2) | C11···H2 | 2.38 (2) |
O1W···H21W | 2.92 (3) | ||
O51—S5—O52 | 114.10 (7) | Mg1—O2W—H21W | 126.5 (19) |
O51—S5—O53 | 110.20 (7) | H21W—O2W—H22W | 113 (3) |
O51—S5—C5 | 107.36 (7) | Mg1—O3W—H32W | 125.3 (17) |
O52—S5—O53 | 111.08 (8) | Mg1—O3W—H31W | 126 (2) |
O52—S5—C5 | 106.81 (7) | H31W—O3W—H32W | 107 (3) |
O53—S5—C5 | 106.91 (7) | H41W—O4W—H42W | 105 (3) |
O2W—Mg1—O3Wi | 90.64 (6) | C2—C1—C11 | 120.22 (13) |
O1Wi—Mg1—O3W | 90.48 (5) | C6—C1—C11 | 120.43 (13) |
O2Wi—Mg1—O3W | 90.64 (6) | C2—C1—C6 | 119.35 (13) |
O3W—Mg1—O3Wi | 180.00 | O2—C2—C1 | 122.58 (14) |
O1Wi—Mg1—O2Wi | 90.12 (6) | C1—C2—C3 | 119.67 (14) |
O1Wi—Mg1—O3Wi | 89.53 (5) | O2—C2—C3 | 117.75 (13) |
O2Wi—Mg1—O3Wi | 89.36 (6) | C2—C3—C4 | 120.41 (14) |
O1Wi—Mg1—O2W | 89.88 (6) | C3—C4—C5 | 120.14 (14) |
O1W—Mg1—O2W | 90.12 (6) | C4—C5—C6 | 119.90 (14) |
O1W—Mg1—O3W | 89.53 (5) | S5—C5—C6 | 118.58 (11) |
O1W—Mg1—O1Wi | 180.00 | S5—C5—C4 | 121.52 (12) |
O1W—Mg1—O2Wi | 89.88 (6) | C1—C6—C5 | 120.53 (14) |
O1W—Mg1—O3Wi | 90.48 (5) | O11—C11—O12 | 123.56 (14) |
O2W—Mg1—O3W | 89.36 (6) | O11—C11—C1 | 113.42 (13) |
O2W—Mg1—O2Wi | 180.00 | O12—C11—C1 | 123.02 (14) |
C2—O2—H2 | 107.2 (15) | C2—C3—H3 | 120.00 |
C11—O11—H11 | 112 (2) | C4—C3—H3 | 120.00 |
Mg1—O1W—H11W | 128.1 (14) | C3—C4—H4 | 120.00 |
Mg1—O1W—H12W | 123.6 (17) | C5—C4—H4 | 120.00 |
H11W—O1W—H12W | 106 (2) | C1—C6—H6 | 120.00 |
Mg1—O2W—H22W | 121 (2) | C5—C6—H6 | 120.00 |
O51—S5—C5—C4 | 1.22 (13) | C2—C1—C11—O11 | 178.30 (13) |
O51—S5—C5—C6 | −177.90 (11) | C2—C1—C11—O12 | −1.5 (2) |
O52—S5—C5—C4 | 124.00 (12) | C6—C1—C11—O11 | −1.25 (19) |
O52—S5—C5—C6 | −55.12 (13) | C6—C1—C11—O12 | 178.95 (13) |
O53—S5—C5—C4 | −117.02 (12) | O2—C2—C3—C4 | 179.28 (13) |
O53—S5—C5—C6 | 63.86 (13) | C1—C2—C3—C4 | −0.4 (2) |
C6—C1—C2—O2 | −178.76 (13) | C2—C3—C4—C5 | −0.2 (2) |
C6—C1—C2—C3 | 0.9 (2) | C3—C4—C5—S5 | −178.80 (11) |
C11—C1—C2—O2 | 1.7 (2) | C3—C4—C5—C6 | 0.3 (2) |
C11—C1—C2—C3 | −178.65 (12) | S5—C5—C6—C1 | 179.34 (10) |
C2—C1—C6—C5 | −0.8 (2) | C4—C5—C6—C1 | 0.2 (2) |
C11—C1—C6—C5 | 178.75 (12) |
Symmetry codes: (i) −x, −y, −z; (ii) −x+1, −y, −z+1; (iii) −x+1, −y, −z; (iv) −x, −y, −z+1; (v) −x−1, −y+1, −z+1; (vi) x−1, y, z; (vii) −x, −y+1, −z+1; (viii) x, y−1, z; (ix) −x, −y+1, −z; (x) −x+1, −y+1, −z; (xi) x, y+1, z; (xii) x+1, y, z. |
D—H···A | D—H | H···A | D···A | D—H···A |
O2—H2···O12 | 0.85 (2) | 1.87 (2) | 2.632 (2) | 149 (2) |
O11—H11···O53ii | 0.79 (3) | 1.92 (3) | 2.678 (2) | 161 (3) |
O1W—H11W···O12iv | 0.85 (2) | 1.93 (2) | 2.779 (2) | 175 (2) |
O1W—H12W···O51 | 0.82 (3) | 2.00 (3) | 2.824 (2) | 175 (2) |
O2W—H21W···O4Wviii | 0.82 (3) | 1.91 (3) | 2.728 (3) | 173 (3) |
O3W—H31W···O51ix | 0.75 (3) | 2.10 (3) | 2.850 (2) | 171 (3) |
O3W—H32W···O4Wx | 0.89 (3) | 1.87 (3) | 2.748 (3) | 167 (2) |
O4W—H41W···O53xi | 0.79 (3) | 2.04 (3) | 2.803 (2) | 162 (3) |
O4W—H42W···O52 | 0.84 (3) | 1.88 (3) | 2.717 (2) | 178 (3) |
C3—H3···O2v | 0.93 | 2.53 | 3.324 (3) | 144 |
C4—H4···O51 | 0.93 | 2.56 | 2.940 (3) | 105 |
C6—H6···O11 | 0.93 | 2.38 | 2.705 (2) | 100 |
C6—H6···O11ii | 0.93 | 2.52 | 3.264 (3) | 137 |
Symmetry codes: (ii) −x+1, −y, −z+1; (iv) −x, −y, −z+1; (v) −x−1, −y+1, −z+1; (viii) x, y−1, z; (ix) −x, −y+1, −z; (x) −x+1, −y+1, −z; (xi) x, y+1, z. |
Experimental details
Crystal data | |
Chemical formula | [Mg(H2O)6](C7H5O6S)2·2H2O |
Mr | 602.78 |
Crystal system, space group | Triclinic, P1 |
Temperature (K) | 200 |
a, b, c (Å) | 6.8694 (4), 6.9069 (4), 14.3950 (8) |
α, β, γ (°) | 77.472 (5), 78.120 (4), 70.131 (5) |
V (Å3) | 620.51 (6) |
Z | 1 |
Radiation type | Mo Kα |
µ (mm−1) | 0.33 |
Crystal size (mm) | 0.40 × 0.12 × 0.10 |
Data collection | |
Diffractometer | Oxford Diffraction Gemini-S CCD-detector diffractometer |
Absorption correction | Multi-scan (CrysAlis PRO; Oxford Diffraction, 2010) |
Tmin, Tmax | 0.96, 0.99 |
No. of measured, independent and observed [I > 2σ(I)] reflections | 8134, 2899, 2553 |
Rint | 0.023 |
(sin θ/λ)max (Å−1) | 0.678 |
Refinement | |
R[F2 > 2σ(F2)], wR(F2), S | 0.032, 0.086, 1.14 |
No. of reflections | 2899 |
No. of parameters | 209 |
H-atom treatment | H atoms treated by a mixture of independent and constrained refinement |
Δρmax, Δρmin (e Å−3) | 0.34, −0.43 |
Computer programs: CrysAlis PRO (Oxford Diffraction, 2010), SIR92 (Altomare et al., 1994), SHELXL97 (Sheldrick, 2008) within WinGX (Farrugia, 1999), PLATON (Spek, 2009).
D—H···A | D—H | H···A | D···A | D—H···A |
O2—H2···O12 | 0.85 (2) | 1.87 (2) | 2.632 (2) | 149 (2) |
O11—H11···O53i | 0.79 (3) | 1.92 (3) | 2.678 (2) | 161 (3) |
O1W—H11W···O12ii | 0.85 (2) | 1.93 (2) | 2.779 (2) | 175 (2) |
O1W—H12W···O51 | 0.82 (3) | 2.00 (3) | 2.824 (2) | 175 (2) |
O2W—H21W···O4Wiii | 0.82 (3) | 1.91 (3) | 2.728 (3) | 173 (3) |
O3W—H31W···O51iv | 0.75 (3) | 2.10 (3) | 2.850 (2) | 171 (3) |
O3W—H32W···O4Wv | 0.89 (3) | 1.87 (3) | 2.748 (3) | 167 (2) |
O4W—H41W···O53vi | 0.79 (3) | 2.04 (3) | 2.803 (2) | 162 (3) |
O4W—H42W···O52 | 0.84 (3) | 1.88 (3) | 2.717 (2) | 178 (3) |
Symmetry codes: (i) −x+1, −y, −z+1; (ii) −x, −y, −z+1; (iii) x, y−1, z; (iv) −x, −y+1, −z; (v) −x+1, −y+1, −z; (vi) x, y+1, z. |
The title compound, [Mg(H2O)6]2+ 2(C7H5O6S-). 2(H2O) was obtained from the reaction of 3-carboxy-4-hydroxybenzenesulfonic acid (5-sulfosalicylic acid, 5-SSA) with MgCO3 and the structure is reported here In the structure of this compound (Fig. 1), the octahedral cationic Mg complex cations lie on crystallographic inversion centres [Mg—O, 2.0396 (17)–2.0664 (19) Å]. This complex is isomorphous with other divalent first transition metal–5-SSA complexes with the same basic dihydrate formula [M(H2O)6] 2(5-SSA-). 2(H2O), [M = Mn (Ma et al., 2003a); Co (Abdelhak et al., 2005); Cu (Ma et al., 2003d)]. These complexes are also similar to the tetrahydrate analogues {[M(H2O)6] 2(5-SSA-). 4(H2O)}, having triclinic unit cells with comparable cell parameters e.g. CoII (Ma et al., 2003b) and Ni (Ma et al., 2003c) and Zn (Ma et al., 2003e).
The coordinated water molecules are involved in a number of O—H···O hydrogen-bonding interactions with sulfonate and carboxylate O acceptors of the uncoordinated 5-SSA monoanions and the water molecules of solvation (Table 1) and together with a carboxylic acid O—H···Osulfonate hydrogen bond form a three-dimensional structure (Fig. 2). In the anion there is the intramolecular cyclic phenol O—H···Ocarboxyl hydrogen bond which is invariably present in this monoanion (Ma et al., 2003a). One H of one of the coordinated water molecules (H22W) has no reasonable acceptor in the structure.