



Supporting information
![]() | Crystallographic Information File (CIF) https://doi.org/10.1107/S1600536809046595/hb5189sup1.cif |
![]() | Structure factor file (CIF format) https://doi.org/10.1107/S1600536809046595/hb5189Isup2.hkl |
CCDC reference: 758660
Key indicators
- Single-crystal X-ray study
- T = 273 K
- Mean
(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
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.
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).
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).
![]() | Fig. 1. The molecular structure of (I) showing 30% displacement ellipsoids. Atoms with the suffix A are generated by (–x, –y, –z). |
[Mg(H2O)6](C7H8NO3S)2 | F(000) = 532 |
Mr = 504.81 | Dx = 1.555 Mg m−3 |
Monoclinic, P21/n | Mo Kα radiation, λ = 0.71073 Å |
Hall symbol: -P 2yn | Cell parameters from 3577 reflections |
a = 6.3048 (13) Å | θ = 3.0–28.6° |
b = 7.0395 (15) Å | µ = 0.34 mm−1 |
c = 24.356 (5) Å | T = 273 K |
β = 93.921 (3)° | Block, colourless |
V = 1078.5 (4) Å3 | 0.23 × 0.16 × 0.12 mm |
Z = 2 |
Bruker SMART CCD diffractometer | 1918 independent reflections |
Radiation source: fine-focus sealed tube | 1779 reflections with I > 2σ(I) |
Graphite monochromator | Rint = 0.020 |
ω scans | θmax = 25.1°, θmin = 1.7° |
Absorption correction: multi-scan (SADABS; Bruker, 2000) | h = −6→7 |
Tmin = 0.926, Tmax = 0.960 | k = −8→8 |
5398 measured reflections | l = −28→25 |
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)] = 0.054 | Hydrogen site location: inferred from neighbouring sites |
wR(F2) = 0.138 | H-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 parameters | Δρmax = 0.37 e Å−3 |
9 restraints | Δρmin = −0.42 e Å−3 |
[Mg(H2O)6](C7H8NO3S)2 | V = 1078.5 (4) Å3 |
Mr = 504.81 | Z = 2 |
Monoclinic, P21/n | Mo Kα radiation |
a = 6.3048 (13) Å | µ = 0.34 mm−1 |
b = 7.0395 (15) Å | T = 273 K |
c = 24.356 (5) Å | 0.23 × 0.16 × 0.12 mm |
β = 93.921 (3)° |
Bruker SMART CCD diffractometer | 1918 independent reflections |
Absorption correction: multi-scan (SADABS; Bruker, 2000) | 1779 reflections with I > 2σ(I) |
Tmin = 0.926, Tmax = 0.960 | Rint = 0.020 |
5398 measured reflections |
R[F2 > 2σ(F2)] = 0.054 | 9 restraints |
wR(F2) = 0.138 | H-atom parameters constrained |
S = 1.27 | Δρmax = 0.37 e Å−3 |
1918 reflections | Δρmin = −0.42 e Å−3 |
144 parameters |
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. |
x | y | z | Uiso*/Ueq | ||
Mg1 | 0.0000 | 0.0000 | 0.0000 | 0.0216 (4) | |
S1 | 0.40358 (14) | 0.50773 (14) | 0.09733 (4) | 0.0218 (3) | |
O1 | 0.4934 (5) | 0.6661 (4) | 0.06800 (11) | 0.0317 (7) | |
O2 | 0.1712 (4) | 0.5034 (4) | 0.09088 (12) | 0.0297 (7) | |
O3 | 0.4968 (4) | 0.3258 (4) | 0.08251 (12) | 0.0304 (7) | |
O4 | 0.2913 (5) | 0.0074 (4) | 0.04083 (13) | 0.0375 (8) | |
H7 | 0.3575 | 0.1051 | 0.0533 | 0.056* | |
H8 | 0.3647 | −0.0883 | 0.0519 | 0.056* | |
O5 | −0.0976 (5) | −0.1937 (4) | 0.05737 (13) | 0.0366 (8) | |
H9 | −0.0146 | −0.2881 | 0.0624 | 0.055* | |
H10 | −0.2222 | −0.2401 | 0.0564 | 0.055* | |
O6 | −0.1022 (5) | 0.2297 (4) | 0.04427 (13) | 0.0340 (7) | |
H12 | −0.2251 | 0.2721 | 0.0498 | 0.052 (16)* | |
H11 | −0.0147 | 0.3033 | 0.0618 | 0.11 (3)* | |
N1 | 0.6584 (7) | 0.6327 (6) | 0.33201 (15) | 0.0465 (11) | |
H1A | 0.7828 | 0.6779 | 0.3408 | 0.056* | |
H1B | 0.5739 | 0.6070 | 0.3573 | 0.056* | |
C1 | 0.4753 (6) | 0.5435 (5) | 0.16775 (16) | 0.0217 (8) | |
C2 | 0.3351 (6) | 0.5006 (6) | 0.20762 (16) | 0.0248 (8) | |
H2 | 0.2013 | 0.4519 | 0.1971 | 0.030* | |
C3 | 0.3929 (6) | 0.5297 (5) | 0.26277 (16) | 0.0254 (9) | |
C4 | 0.5949 (7) | 0.6021 (6) | 0.27807 (16) | 0.0280 (9) | |
C5 | 0.7335 (7) | 0.6445 (6) | 0.23738 (17) | 0.0305 (9) | |
H5 | 0.8675 | 0.6936 | 0.2474 | 0.037* | |
C6 | 0.6748 (6) | 0.6147 (6) | 0.18287 (17) | 0.0276 (9) | |
H6 | 0.7689 | 0.6424 | 0.1562 | 0.033* | |
C7 | 0.2434 (7) | 0.4831 (7) | 0.30672 (18) | 0.0363 (10) | |
H7A | 0.1193 | 0.4209 | 0.2903 | 0.054* | |
H7B | 0.2022 | 0.5982 | 0.3243 | 0.054* | |
H7C | 0.3136 | 0.4006 | 0.3336 | 0.054* |
U11 | U22 | U33 | U12 | U13 | U23 | |
Mg1 | 0.0199 (9) | 0.0211 (9) | 0.0240 (9) | −0.0004 (8) | 0.0032 (7) | 0.0008 (8) |
S1 | 0.0198 (5) | 0.0208 (5) | 0.0249 (5) | −0.0004 (4) | 0.0011 (3) | −0.0008 (4) |
O1 | 0.0331 (16) | 0.0318 (16) | 0.0304 (15) | −0.0064 (13) | 0.0045 (12) | 0.0080 (13) |
O2 | 0.0208 (14) | 0.0326 (16) | 0.0351 (16) | 0.0015 (13) | −0.0024 (11) | −0.0017 (13) |
O3 | 0.0299 (16) | 0.0279 (16) | 0.0335 (16) | 0.0043 (13) | 0.0021 (12) | −0.0089 (13) |
O4 | 0.0303 (16) | 0.0275 (16) | 0.0527 (19) | −0.0020 (13) | −0.0117 (14) | −0.0009 (15) |
O5 | 0.0264 (16) | 0.0361 (17) | 0.0486 (19) | 0.0009 (13) | 0.0121 (14) | 0.0161 (15) |
O6 | 0.0273 (16) | 0.0312 (16) | 0.0442 (18) | 0.0002 (14) | 0.0083 (13) | −0.0131 (14) |
N1 | 0.051 (2) | 0.060 (3) | 0.028 (2) | −0.018 (2) | −0.0021 (17) | −0.004 (2) |
C1 | 0.0220 (19) | 0.0166 (18) | 0.0266 (19) | 0.0008 (15) | 0.0018 (15) | −0.0004 (15) |
C2 | 0.0227 (19) | 0.0198 (19) | 0.032 (2) | −0.0004 (16) | 0.0019 (16) | 0.0006 (17) |
C3 | 0.032 (2) | 0.0158 (19) | 0.029 (2) | 0.0006 (16) | 0.0067 (16) | 0.0000 (16) |
C4 | 0.034 (2) | 0.022 (2) | 0.028 (2) | −0.0019 (17) | 0.0015 (17) | −0.0017 (17) |
C5 | 0.027 (2) | 0.029 (2) | 0.035 (2) | −0.0064 (18) | −0.0047 (18) | −0.0018 (18) |
C6 | 0.023 (2) | 0.030 (2) | 0.031 (2) | −0.0028 (17) | 0.0046 (16) | 0.0009 (18) |
C7 | 0.047 (3) | 0.030 (2) | 0.033 (2) | −0.006 (2) | 0.012 (2) | 0.002 (2) |
Mg1—O4i | 2.029 (3) | N1—C4 | 1.364 (5) |
Mg1—O4 | 2.029 (3) | N1—H1A | 0.8600 |
Mg1—O6i | 2.071 (3) | N1—H1B | 0.8600 |
Mg1—O6 | 2.071 (3) | C1—C6 | 1.380 (5) |
Mg1—O5 | 2.075 (3) | C1—C2 | 1.390 (5) |
Mg1—O5i | 2.075 (3) | C2—C3 | 1.383 (6) |
S1—O1 | 1.459 (3) | C2—H2 | 0.9300 |
S1—O2 | 1.463 (3) | C3—C4 | 1.399 (6) |
S1—O3 | 1.465 (3) | C3—C7 | 1.510 (6) |
S1—C1 | 1.762 (4) | C4—C5 | 1.398 (6) |
O4—H7 | 0.8499 | C5—C6 | 1.370 (6) |
O4—H8 | 0.8500 | C5—H5 | 0.9300 |
O5—H9 | 0.8500 | C6—H6 | 0.9300 |
O5—H10 | 0.8500 | C7—H7A | 0.9600 |
O6—H12 | 0.8500 | C7—H7B | 0.9600 |
O6—H11 | 0.8500 | C7—H7C | 0.9600 |
O4i—Mg1—O4 | 180.0 | H12—O6—H11 | 105.9 |
O4i—Mg1—O6i | 91.62 (13) | C4—N1—H1A | 120.0 |
O4—Mg1—O6i | 88.38 (13) | C4—N1—H1B | 120.0 |
O4i—Mg1—O6 | 88.38 (13) | H1A—N1—H1B | 120.0 |
O4—Mg1—O6 | 91.62 (13) | C6—C1—C2 | 120.3 (4) |
O6i—Mg1—O6 | 180.0 | C6—C1—S1 | 118.7 (3) |
O4i—Mg1—O5 | 90.75 (12) | C2—C1—S1 | 121.0 (3) |
O4—Mg1—O5 | 89.25 (12) | C3—C2—C1 | 120.6 (4) |
O6i—Mg1—O5 | 87.41 (12) | C3—C2—H2 | 119.7 |
O6—Mg1—O5 | 92.59 (12) | C1—C2—H2 | 119.7 |
O4i—Mg1—O5i | 89.25 (12) | C2—C3—C4 | 119.2 (4) |
O4—Mg1—O5i | 90.75 (12) | C2—C3—C7 | 121.4 (4) |
O6i—Mg1—O5i | 92.59 (12) | C4—C3—C7 | 119.4 (4) |
O6—Mg1—O5i | 87.41 (12) | N1—C4—C5 | 119.5 (4) |
O5—Mg1—O5i | 180.0 | N1—C4—C3 | 121.1 (4) |
O1—S1—O2 | 112.49 (18) | C5—C4—C3 | 119.4 (4) |
O1—S1—O3 | 111.84 (17) | C6—C5—C4 | 120.9 (4) |
O2—S1—O3 | 111.78 (17) | C6—C5—H5 | 119.5 |
O1—S1—C1 | 106.55 (17) | C4—C5—H5 | 119.5 |
O2—S1—C1 | 107.23 (17) | C5—C6—C1 | 119.7 (4) |
O3—S1—C1 | 106.52 (17) | C5—C6—H6 | 120.2 |
Mg1—O4—H7 | 127.0 | C1—C6—H6 | 120.2 |
Mg1—O4—H8 | 126.1 | C3—C7—H7A | 109.5 |
H7—O4—H8 | 106.5 | C3—C7—H7B | 109.5 |
Mg1—O5—H9 | 113.8 | H7A—C7—H7B | 109.5 |
Mg1—O5—H10 | 123.4 | C3—C7—H7C | 109.5 |
H9—O5—H10 | 105.2 | H7A—C7—H7C | 109.5 |
Mg1—O6—H12 | 132.6 | H7B—C7—H7C | 109.5 |
Mg1—O6—H11 | 121.5 | ||
O1—S1—C1—C6 | −38.2 (4) | C2—C3—C4—N1 | −179.9 (4) |
O2—S1—C1—C6 | −158.9 (3) | C7—C3—C4—N1 | −0.5 (6) |
O3—S1—C1—C6 | 81.3 (3) | C2—C3—C4—C5 | 0.4 (6) |
O1—S1—C1—C2 | 142.0 (3) | C7—C3—C4—C5 | 179.8 (4) |
O2—S1—C1—C2 | 21.4 (4) | N1—C4—C5—C6 | 179.8 (4) |
O3—S1—C1—C2 | −98.4 (3) | C3—C4—C5—C6 | −0.5 (6) |
C6—C1—C2—C3 | 0.4 (6) | C4—C5—C6—C1 | 0.6 (6) |
S1—C1—C2—C3 | −179.8 (3) | C2—C1—C6—C5 | −0.5 (6) |
C1—C2—C3—C4 | −0.3 (6) | S1—C1—C6—C5 | 179.7 (3) |
C1—C2—C3—C7 | −179.7 (4) |
Symmetry code: (i) −x, −y, −z. |
D—H···A | D—H | H···A | D···A | D—H···A |
N1—H1A···O3ii | 0.86 | 2.48 | 3.208 (5) | 143 |
N1—H1B···O6iii | 0.86 | 2.54 | 3.133 (5) | 127 |
O4—H7···O3 | 0.85 | 1.90 | 2.748 (4) | 178 |
O4—H8···O1iv | 0.85 | 1.94 | 2.778 (4) | 169 |
O5—H9···O2iv | 0.85 | 1.97 | 2.810 (4) | 168 |
O5—H10···O1v | 0.85 | 1.95 | 2.790 (4) | 170 |
O6—H11···O2 | 0.85 | 1.94 | 2.776 (4) | 169 |
O6—H12···O3vi | 0.85 | 2.01 | 2.835 (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, y−1, z; (v) x−1, y−1, z; (vi) x−1, y, z. |
Experimental details
Crystal data | |
Chemical formula | [Mg(H2O)6](C7H8NO3S)2 |
Mr | 504.81 |
Crystal system, space group | Monoclinic, P21/n |
Temperature (K) | 273 |
a, b, c (Å) | 6.3048 (13), 7.0395 (15), 24.356 (5) |
β (°) | 93.921 (3) |
V (Å3) | 1078.5 (4) |
Z | 2 |
Radiation type | Mo Kα |
µ (mm−1) | 0.34 |
Crystal size (mm) | 0.23 × 0.16 × 0.12 |
Data collection | |
Diffractometer | Bruker SMART CCD diffractometer |
Absorption correction | Multi-scan (SADABS; Bruker, 2000) |
Tmin, Tmax | 0.926, 0.960 |
No. of measured, independent and observed [I > 2σ(I)] reflections | 5398, 1918, 1779 |
Rint | 0.020 |
(sin θ/λ)max (Å−1) | 0.596 |
Refinement | |
R[F2 > 2σ(F2)], wR(F2), S | 0.054, 0.138, 1.27 |
No. of reflections | 1918 |
No. of parameters | 144 |
No. of restraints | 9 |
H-atom treatment | H-atom parameters constrained |
Δρmax, Δρmin (e Å−3) | 0.37, −0.42 |
Computer programs: SMART (Bruker, 2000), SAINT (Bruker, 2000), SHELXS97 (Sheldrick, 2008), SHELXL97 (Sheldrick, 2008), SHELXTL (Sheldrick, 2008).
D—H···A | D—H | H···A | D···A | D—H···A |
N1—H1A···O3i | 0.86 | 2.48 | 3.208 (5) | 143 |
N1—H1B···O6ii | 0.86 | 2.54 | 3.133 (5) | 127 |
O4—H7···O3 | 0.85 | 1.90 | 2.748 (4) | 178 |
O4—H8···O1iii | 0.85 | 1.94 | 2.778 (4) | 169 |
O5—H9···O2iii | 0.85 | 1.97 | 2.810 (4) | 168 |
O5—H10···O1iv | 0.85 | 1.95 | 2.790 (4) | 170 |
O6—H11···O2 | 0.85 | 1.94 | 2.776 (4) | 169 |
O6—H12···O3v | 0.85 | 2.01 | 2.835 (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, y−1, z; (iv) x−1, y−1, z; (v) x−1, y, z. |