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In the title mol­ecular salt, [Mg(H2O)6](C7H8NO3S)2, the Mg2+ cation lies on an inversion centre. In the crystal, the components are linked by N—H...O and O—H...O hydrogen bonds, thereby generating sheets parallel to (001).

Supporting information

cif

Crystallographic Information File (CIF) https://doi.org/10.1107/S1600536809046595/hb5189sup1.cif
Contains datablocks global, I

hkl

Structure factor file (CIF format) https://doi.org/10.1107/S1600536809046595/hb5189Isup2.hkl
Contains datablock I

CCDC reference: 758660

Key indicators

  • Single-crystal X-ray study
  • T = 273 K
  • Mean [sigma](C-C) = 0.006 Å
  • R factor = 0.054
  • wR factor = 0.138
  • Data-to-parameter ratio = 13.3

checkCIF/PLATON results

No syntax errors found



Alert level B PLAT930_ALERT_2_B Check Twin Law ( 0 0 1)[ 1 0 4] Estimated BASF 0.06 PLAT930_ALERT_2_B Check Twin Law ( 0 0 1)[ 1 0 4] Estimated BASF 0.06
Alert level C PLAT340_ALERT_3_C Low Bond Precision on C-C Bonds (x 1000) Ang .. 6 PLAT911_ALERT_3_C Missing # FCF Refl Between THmin & STh/L= 0.596 5 PLAT042_ALERT_1_C Calc. and Reported MoietyFormula Strings Differ ?
Alert level G PLAT860_ALERT_3_G Note: Number of Least-Squares Restraints ....... 9 PLAT128_ALERT_4_G Non-standard setting of Space-group P21/c .... P21/n PLAT199_ALERT_1_G Check the Reported _cell_measurement_temperature 273 K PLAT200_ALERT_1_G Check the Reported _diffrn_ambient_temperature 273 K PLAT931_ALERT_5_G Check Twin Law ( )[ 1 0 4] Estimated BASF 0.06 PLAT931_ALERT_5_G Check Twin Law ( 0 0 1)[ ] Estimated BASF 0.06
0 ALERT level A = In general: serious problem 2 ALERT level B = Potentially serious problem 3 ALERT level C = Check and explain 6 ALERT level G = General alerts; check 3 ALERT type 1 CIF construction/syntax error, inconsistent or missing data 2 ALERT type 2 Indicator that the structure model may be wrong or deficient 3 ALERT type 3 Indicator that the structure quality may be low 1 ALERT type 4 Improvement, methodology, query or suggestion 2 ALERT type 5 Informative message, check
checkCIF publication errors
Alert level G PUBL013_ALERT_1_G The _publ_section_comment (discussion of study) is missing. This is required for a full paper submission (but is optional for an electronic paper).
0 ALERT level A = Data missing that is essential or data in wrong format 1 ALERT level G = General alerts. Data that may be required is missing

Related literature top

For the isostructural cobalt-containing compound, see: Zhang & Chen (2009).

Experimental top

A solution of 1.0 mmol 4-amino-3-methyl-benzenesulfonic acid and 1.0 mmol NaOH in 10 ml ethanol was added to a solution of 0.5 mmol MgCl26H2O in 5 ml ethanol at room temperature. The mixture was refluxed for 3 h with stirring, then the resulting precipitate was filtered, washed, and dried in vacuo over P4O10 for 48 h. Colourless blocks of (I) were obtained by slowly evaporating from ethanol at room temperature.

Refinement top

The H atoms were positioned geometrically (C—H = 0.93–0.96, N—H = 0.86, O—H = 0.85Å) and refined as riding with Uiso(H)= 1.2 Ueq(C,N) or 1.5 Ueq(O).

Computing details top

Data collection: SMART (Bruker, 2000); cell refinement: SAINT (Bruker, 2000); data reduction: SAINT (Bruker, 2000); program(s) used to solve structure: SHELXS97 (Sheldrick, 2008); program(s) used to refine structure: SHELXL97 (Sheldrick, 2008); molecular graphics: SHELXTL (Sheldrick, 2008); software used to prepare material for publication: SHELXTL (Sheldrick, 2008).

Figures top
[Figure 1] Fig. 1. The molecular structure of (I) showing 30% displacement ellipsoids. Atoms with the suffix A are generated by (–x, –y, –z).
Hexaaquamagnesium bis(4-amino-3-methylbenzenesulfonate) top
Crystal data top
[Mg(H2O)6](C7H8NO3S)2F(000) = 532
Mr = 504.81Dx = 1.555 Mg m3
Monoclinic, P21/nMo Kα radiation, λ = 0.71073 Å
Hall symbol: -P 2ynCell parameters from 3577 reflections
a = 6.3048 (13) Åθ = 3.0–28.6°
b = 7.0395 (15) ŵ = 0.34 mm1
c = 24.356 (5) ÅT = 273 K
β = 93.921 (3)°Block, colourless
V = 1078.5 (4) Å30.23 × 0.16 × 0.12 mm
Z = 2
Data collection top
Bruker SMART CCD
diffractometer
1918 independent reflections
Radiation source: fine-focus sealed tube1779 reflections with I > 2σ(I)
Graphite monochromatorRint = 0.020
ω scansθmax = 25.1°, θmin = 1.7°
Absorption correction: multi-scan
(SADABS; Bruker, 2000)
h = 67
Tmin = 0.926, Tmax = 0.960k = 88
5398 measured reflectionsl = 2825
Refinement top
Refinement on F2Primary atom site location: structure-invariant direct methods
Least-squares matrix: fullSecondary atom site location: difference Fourier map
R[F2 > 2σ(F2)] = 0.054Hydrogen site location: inferred from neighbouring sites
wR(F2) = 0.138H-atom parameters constrained
S = 1.27 w = 1/[σ2(Fo2) + (0.0175P)2 + 3.9593P]
where P = (Fo2 + 2Fc2)/3
1918 reflections(Δ/σ)max < 0.001
144 parametersΔρmax = 0.37 e Å3
9 restraintsΔρmin = 0.42 e Å3
Crystal data top
[Mg(H2O)6](C7H8NO3S)2V = 1078.5 (4) Å3
Mr = 504.81Z = 2
Monoclinic, P21/nMo Kα radiation
a = 6.3048 (13) ŵ = 0.34 mm1
b = 7.0395 (15) ÅT = 273 K
c = 24.356 (5) Å0.23 × 0.16 × 0.12 mm
β = 93.921 (3)°
Data collection top
Bruker SMART CCD
diffractometer
1918 independent reflections
Absorption correction: multi-scan
(SADABS; Bruker, 2000)
1779 reflections with I > 2σ(I)
Tmin = 0.926, Tmax = 0.960Rint = 0.020
5398 measured reflections
Refinement top
R[F2 > 2σ(F2)] = 0.0549 restraints
wR(F2) = 0.138H-atom parameters constrained
S = 1.27Δρmax = 0.37 e Å3
1918 reflectionsΔρmin = 0.42 e Å3
144 parameters
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
Mg10.00000.00000.00000.0216 (4)
S10.40358 (14)0.50773 (14)0.09733 (4)0.0218 (3)
O10.4934 (5)0.6661 (4)0.06800 (11)0.0317 (7)
O20.1712 (4)0.5034 (4)0.09088 (12)0.0297 (7)
O30.4968 (4)0.3258 (4)0.08251 (12)0.0304 (7)
O40.2913 (5)0.0074 (4)0.04083 (13)0.0375 (8)
H70.35750.10510.05330.056*
H80.36470.08830.05190.056*
O50.0976 (5)0.1937 (4)0.05737 (13)0.0366 (8)
H90.01460.28810.06240.055*
H100.22220.24010.05640.055*
O60.1022 (5)0.2297 (4)0.04427 (13)0.0340 (7)
H120.22510.27210.04980.052 (16)*
H110.01470.30330.06180.11 (3)*
N10.6584 (7)0.6327 (6)0.33201 (15)0.0465 (11)
H1A0.78280.67790.34080.056*
H1B0.57390.60700.35730.056*
C10.4753 (6)0.5435 (5)0.16775 (16)0.0217 (8)
C20.3351 (6)0.5006 (6)0.20762 (16)0.0248 (8)
H20.20130.45190.19710.030*
C30.3929 (6)0.5297 (5)0.26277 (16)0.0254 (9)
C40.5949 (7)0.6021 (6)0.27807 (16)0.0280 (9)
C50.7335 (7)0.6445 (6)0.23738 (17)0.0305 (9)
H50.86750.69360.24740.037*
C60.6748 (6)0.6147 (6)0.18287 (17)0.0276 (9)
H60.76890.64240.15620.033*
C70.2434 (7)0.4831 (7)0.30672 (18)0.0363 (10)
H7A0.11930.42090.29030.054*
H7B0.20220.59820.32430.054*
H7C0.31360.40060.33360.054*
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
Mg10.0199 (9)0.0211 (9)0.0240 (9)0.0004 (8)0.0032 (7)0.0008 (8)
S10.0198 (5)0.0208 (5)0.0249 (5)0.0004 (4)0.0011 (3)0.0008 (4)
O10.0331 (16)0.0318 (16)0.0304 (15)0.0064 (13)0.0045 (12)0.0080 (13)
O20.0208 (14)0.0326 (16)0.0351 (16)0.0015 (13)0.0024 (11)0.0017 (13)
O30.0299 (16)0.0279 (16)0.0335 (16)0.0043 (13)0.0021 (12)0.0089 (13)
O40.0303 (16)0.0275 (16)0.0527 (19)0.0020 (13)0.0117 (14)0.0009 (15)
O50.0264 (16)0.0361 (17)0.0486 (19)0.0009 (13)0.0121 (14)0.0161 (15)
O60.0273 (16)0.0312 (16)0.0442 (18)0.0002 (14)0.0083 (13)0.0131 (14)
N10.051 (2)0.060 (3)0.028 (2)0.018 (2)0.0021 (17)0.004 (2)
C10.0220 (19)0.0166 (18)0.0266 (19)0.0008 (15)0.0018 (15)0.0004 (15)
C20.0227 (19)0.0198 (19)0.032 (2)0.0004 (16)0.0019 (16)0.0006 (17)
C30.032 (2)0.0158 (19)0.029 (2)0.0006 (16)0.0067 (16)0.0000 (16)
C40.034 (2)0.022 (2)0.028 (2)0.0019 (17)0.0015 (17)0.0017 (17)
C50.027 (2)0.029 (2)0.035 (2)0.0064 (18)0.0047 (18)0.0018 (18)
C60.023 (2)0.030 (2)0.031 (2)0.0028 (17)0.0046 (16)0.0009 (18)
C70.047 (3)0.030 (2)0.033 (2)0.006 (2)0.012 (2)0.002 (2)
Geometric parameters (Å, º) top
Mg1—O4i2.029 (3)N1—C41.364 (5)
Mg1—O42.029 (3)N1—H1A0.8600
Mg1—O6i2.071 (3)N1—H1B0.8600
Mg1—O62.071 (3)C1—C61.380 (5)
Mg1—O52.075 (3)C1—C21.390 (5)
Mg1—O5i2.075 (3)C2—C31.383 (6)
S1—O11.459 (3)C2—H20.9300
S1—O21.463 (3)C3—C41.399 (6)
S1—O31.465 (3)C3—C71.510 (6)
S1—C11.762 (4)C4—C51.398 (6)
O4—H70.8499C5—C61.370 (6)
O4—H80.8500C5—H50.9300
O5—H90.8500C6—H60.9300
O5—H100.8500C7—H7A0.9600
O6—H120.8500C7—H7B0.9600
O6—H110.8500C7—H7C0.9600
O4i—Mg1—O4180.0H12—O6—H11105.9
O4i—Mg1—O6i91.62 (13)C4—N1—H1A120.0
O4—Mg1—O6i88.38 (13)C4—N1—H1B120.0
O4i—Mg1—O688.38 (13)H1A—N1—H1B120.0
O4—Mg1—O691.62 (13)C6—C1—C2120.3 (4)
O6i—Mg1—O6180.0C6—C1—S1118.7 (3)
O4i—Mg1—O590.75 (12)C2—C1—S1121.0 (3)
O4—Mg1—O589.25 (12)C3—C2—C1120.6 (4)
O6i—Mg1—O587.41 (12)C3—C2—H2119.7
O6—Mg1—O592.59 (12)C1—C2—H2119.7
O4i—Mg1—O5i89.25 (12)C2—C3—C4119.2 (4)
O4—Mg1—O5i90.75 (12)C2—C3—C7121.4 (4)
O6i—Mg1—O5i92.59 (12)C4—C3—C7119.4 (4)
O6—Mg1—O5i87.41 (12)N1—C4—C5119.5 (4)
O5—Mg1—O5i180.0N1—C4—C3121.1 (4)
O1—S1—O2112.49 (18)C5—C4—C3119.4 (4)
O1—S1—O3111.84 (17)C6—C5—C4120.9 (4)
O2—S1—O3111.78 (17)C6—C5—H5119.5
O1—S1—C1106.55 (17)C4—C5—H5119.5
O2—S1—C1107.23 (17)C5—C6—C1119.7 (4)
O3—S1—C1106.52 (17)C5—C6—H6120.2
Mg1—O4—H7127.0C1—C6—H6120.2
Mg1—O4—H8126.1C3—C7—H7A109.5
H7—O4—H8106.5C3—C7—H7B109.5
Mg1—O5—H9113.8H7A—C7—H7B109.5
Mg1—O5—H10123.4C3—C7—H7C109.5
H9—O5—H10105.2H7A—C7—H7C109.5
Mg1—O6—H12132.6H7B—C7—H7C109.5
Mg1—O6—H11121.5
O1—S1—C1—C638.2 (4)C2—C3—C4—N1179.9 (4)
O2—S1—C1—C6158.9 (3)C7—C3—C4—N10.5 (6)
O3—S1—C1—C681.3 (3)C2—C3—C4—C50.4 (6)
O1—S1—C1—C2142.0 (3)C7—C3—C4—C5179.8 (4)
O2—S1—C1—C221.4 (4)N1—C4—C5—C6179.8 (4)
O3—S1—C1—C298.4 (3)C3—C4—C5—C60.5 (6)
C6—C1—C2—C30.4 (6)C4—C5—C6—C10.6 (6)
S1—C1—C2—C3179.8 (3)C2—C1—C6—C50.5 (6)
C1—C2—C3—C40.3 (6)S1—C1—C6—C5179.7 (3)
C1—C2—C3—C7179.7 (4)
Symmetry code: (i) x, y, z.
Hydrogen-bond geometry (Å, º) top
D—H···AD—HH···AD···AD—H···A
N1—H1A···O3ii0.862.483.208 (5)143
N1—H1B···O6iii0.862.543.133 (5)127
O4—H7···O30.851.902.748 (4)178
O4—H8···O1iv0.851.942.778 (4)169
O5—H9···O2iv0.851.972.810 (4)168
O5—H10···O1v0.851.952.790 (4)170
O6—H11···O20.851.942.776 (4)169
O6—H12···O3vi0.852.012.835 (4)163
Symmetry codes: (ii) x+3/2, y+1/2, z+1/2; (iii) x+1/2, y+1/2, z+1/2; (iv) x, y1, z; (v) x1, y1, z; (vi) x1, y, z.

Experimental details

Crystal data
Chemical formula[Mg(H2O)6](C7H8NO3S)2
Mr504.81
Crystal system, space groupMonoclinic, P21/n
Temperature (K)273
a, b, c (Å)6.3048 (13), 7.0395 (15), 24.356 (5)
β (°) 93.921 (3)
V3)1078.5 (4)
Z2
Radiation typeMo Kα
µ (mm1)0.34
Crystal size (mm)0.23 × 0.16 × 0.12
Data collection
DiffractometerBruker SMART CCD
diffractometer
Absorption correctionMulti-scan
(SADABS; Bruker, 2000)
Tmin, Tmax0.926, 0.960
No. of measured, independent and
observed [I > 2σ(I)] reflections
5398, 1918, 1779
Rint0.020
(sin θ/λ)max1)0.596
Refinement
R[F2 > 2σ(F2)], wR(F2), S 0.054, 0.138, 1.27
No. of reflections1918
No. of parameters144
No. of restraints9
H-atom treatmentH-atom parameters constrained
Δρmax, Δρmin (e Å3)0.37, 0.42

Computer programs: SMART (Bruker, 2000), SAINT (Bruker, 2000), SHELXS97 (Sheldrick, 2008), SHELXL97 (Sheldrick, 2008), SHELXTL (Sheldrick, 2008).

Selected bond lengths (Å) top
Mg1—O42.029 (3)Mg1—O52.075 (3)
Mg1—O62.071 (3)
Hydrogen-bond geometry (Å, º) top
D—H···AD—HH···AD···AD—H···A
N1—H1A···O3i0.862.483.208 (5)143
N1—H1B···O6ii0.862.543.133 (5)127
O4—H7···O30.851.902.748 (4)178
O4—H8···O1iii0.851.942.778 (4)169
O5—H9···O2iii0.851.972.810 (4)168
O5—H10···O1iv0.851.952.790 (4)170
O6—H11···O20.851.942.776 (4)169
O6—H12···O3v0.852.012.835 (4)163
Symmetry codes: (i) x+3/2, y+1/2, z+1/2; (ii) x+1/2, y+1/2, z+1/2; (iii) x, y1, z; (iv) x1, y1, z; (v) x1, y, z.
 

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