Related literature
For background to hydrogen-bonded networks, see: Tai et al. (2007
).
Experimental
Crystal data
[Co(H2O)6](C7H8NO3S)2 Mr = 539.43 Monoclinic, P 21 /n a = 6.309 (1) Å b = 7.0513 (11) Å c = 24.262 (4) Å β = 94.080 (2)° V = 1076.6 (3) Å3 Z = 2 Mo Kα radiation μ = 1.06 mm−1 T = 293 K 0.21 × 0.16 × 0.12 mm
|
Data collection
Bruker SMART CCD diffractometer Absorption correction: multi-scan (SADABS; Bruker, 2000 ) Tmin = 0.809, Tmax = 0.884 5530 measured reflections 1921 independent reflections 1690 reflections with I > 2σ(I) Rint = 0.019
|
Co1—O6 | 2.0515 (14) | Co1—O4 | 2.0866 (13) | Co1—O5 | 2.0868 (13) | | |
D—H⋯A | D—H | H⋯A | D⋯A | D—H⋯A | N1—H1A⋯O2i | 0.86 | 2.47 | 3.214 (2) | 145 | N1—H1B⋯O4 | 0.86 | 2.56 | 3.129 (2) | 125 | O4—H7⋯O2i | 0.85 | 2.00 | 2.8300 (19) | 167 | O4—H8⋯O3ii | 0.85 | 1.92 | 2.7675 (19) | 176 | O5—H9⋯O1iii | 0.85 | 1.94 | 2.7828 (19) | 170 | O5—H10⋯O3iv | 0.85 | 1.95 | 2.7963 (19) | 174 | O6—H11⋯O1iv | 0.85 | 1.93 | 2.7711 (19) | 169 | O6—H12⋯O2ii | 0.85 | 1.90 | 2.7419 (19) | 173 | Symmetry codes: (i) ; (ii) ; (iii) ; (iv) . | |
Data collection: SMART (Bruker, 2000
); cell refinement: SAINT (Bruker, 2000
); data reduction: SAINT; 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.
Supporting information
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 Co(CH3COO)24H2O in 5 ml e thanol at room temperature. The mixture was refluxed for 4 h with stirring, then the resulting precipitate was filtered, washed, and dried in vacuo over P4O10 for 48 h. Pink blocks of (I) were obtained by slowly evaporating from methanol at room temperature.
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).
Hexaaquacobalt(II) bis(4-amino-3-methylbenzenesulfonate)
top Crystal data top [Co(H2O)6](C7H8NO3S)2 | F(000) = 562 |
Mr = 539.43 | Dx = 1.664 Mg m−3 |
Monoclinic, P21/n | Mo Kα radiation, λ = 0.71073 Å |
Hall symbol: -P 2yn | Cell parameters from 3103 reflections |
a = 6.309 (1) Å | θ = 3.3–28.3° |
b = 7.0513 (11) Å | µ = 1.06 mm−1 |
c = 24.262 (4) Å | T = 293 K |
β = 94.080 (2)° | Block, pink |
V = 1076.6 (3) Å3 | 0.21 × 0.16 × 0.12 mm |
Z = 2 | |
Data collection top Bruker SMART CCD diffractometer | 1921 independent reflections |
Radiation source: fine-focus sealed tube | 1690 reflections with I > 2σ(I) |
Graphite monochromator | Rint = 0.019 |
ϕ and ω scans | θmax = 25.1°, θmin = 1.7° |
Absorption correction: multi-scan (SADABS; Bruker, 2000) | h = −7→7 |
Tmin = 0.809, Tmax = 0.884 | k = −8→6 |
5530 measured reflections | l = −25→28 |
Refinement top Refinement on F2 | Secondary atom site location: difference Fourier map |
Least-squares matrix: full | Hydrogen site location: inferred from neighbouring sites |
R[F2 > 2σ(F2)] = 0.025 | H-atom parameters constrained |
wR(F2) = 0.073 | w = 1/[σ2(Fo2) + (0.035P)2 + 0.4723P] where P = (Fo2 + 2Fc2)/3 |
S = 1.10 | (Δ/σ)max < 0.001 |
1921 reflections | Δρmax = 0.42 e Å−3 |
143 parameters | Δρmin = −0.33 e Å−3 |
0 restraints | Extinction correction: SHELXL97 (Sheldrick, 2008), Fc*=kFc[1+0.001xFc2λ3/sin(2θ)]-1/4 |
Primary atom site location: structure-invariant direct methods | Extinction coefficient: 0.0268 (16) |
Crystal data top [Co(H2O)6](C7H8NO3S)2 | V = 1076.6 (3) Å3 |
Mr = 539.43 | Z = 2 |
Monoclinic, P21/n | Mo Kα radiation |
a = 6.309 (1) Å | µ = 1.06 mm−1 |
b = 7.0513 (11) Å | T = 293 K |
c = 24.262 (4) Å | 0.21 × 0.16 × 0.12 mm |
β = 94.080 (2)° | |
Data collection top Bruker SMART CCD diffractometer | 1921 independent reflections |
Absorption correction: multi-scan (SADABS; Bruker, 2000) | 1690 reflections with I > 2σ(I) |
Tmin = 0.809, Tmax = 0.884 | Rint = 0.019 |
5530 measured reflections | |
Refinement top R[F2 > 2σ(F2)] = 0.025 | 0 restraints |
wR(F2) = 0.073 | H-atom parameters constrained |
S = 1.10 | Δρmax = 0.42 e Å−3 |
1921 reflections | Δρmin = −0.33 e Å−3 |
143 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 | x | y | z | Uiso*/Ueq | |
Co1 | 0.5000 | 0.5000 | 0.0000 | 0.02153 (14) | |
S1 | 0.59383 (7) | 0.51047 (6) | 0.403529 (19) | 0.02233 (15) | |
O1 | 0.5037 (2) | 0.66812 (19) | 0.43304 (5) | 0.0324 (3) | |
O2 | 0.5014 (2) | 0.32921 (19) | 0.41856 (5) | 0.0315 (3) | |
O3 | 0.8256 (2) | 0.50668 (17) | 0.41067 (6) | 0.0311 (3) | |
O4 | 0.3989 (2) | 0.73519 (19) | 0.04326 (6) | 0.0363 (3) | |
H7 | 0.2775 | 0.7762 | 0.0506 | 0.054* | |
H8 | 0.4888 | 0.8156 | 0.0567 | 0.054* | |
O5 | 0.4048 (2) | 0.3100 (2) | 0.05939 (6) | 0.0365 (4) | |
H9 | 0.2842 | 0.2560 | 0.0589 | 0.055* | |
H10 | 0.4924 | 0.2201 | 0.0664 | 0.055* | |
O6 | 0.7970 (2) | 0.50949 (18) | 0.04025 (7) | 0.0418 (4) | |
H12 | 0.8684 | 0.6054 | 0.0519 | 0.063* | |
H11 | 0.8706 | 0.4134 | 0.0507 | 0.063* | |
N1 | 0.3463 (3) | 0.6380 (3) | 0.16739 (7) | 0.0474 (5) | |
H1A | 0.2229 | 0.6845 | 0.1580 | 0.057* | |
H1B | 0.4320 | 0.6115 | 0.1425 | 0.057* | |
C1 | 0.5244 (3) | 0.5467 (2) | 0.33285 (7) | 0.0232 (4) | |
C2 | 0.6647 (3) | 0.5036 (2) | 0.29306 (8) | 0.0247 (4) | |
H2 | 0.7980 | 0.4545 | 0.3039 | 0.030* | |
C3 | 0.6088 (3) | 0.5326 (2) | 0.23743 (8) | 0.0260 (4) | |
C4 | 0.4060 (3) | 0.6062 (3) | 0.22179 (8) | 0.0289 (4) | |
C5 | 0.2676 (3) | 0.6489 (3) | 0.26221 (8) | 0.0307 (4) | |
H5 | 0.1341 | 0.6985 | 0.2518 | 0.037* | |
C6 | 0.3248 (3) | 0.6188 (3) | 0.31715 (8) | 0.0289 (4) | |
H6 | 0.2301 | 0.6467 | 0.3437 | 0.035* | |
C7 | 0.7578 (4) | 0.4865 (3) | 0.19380 (9) | 0.0360 (5) | |
H7A | 0.8888 | 0.4387 | 0.2110 | 0.054* | |
H7B | 0.7854 | 0.5991 | 0.1733 | 0.054* | |
H7C | 0.6945 | 0.3923 | 0.1693 | 0.054* | |
Atomic displacement parameters (Å2) top | U11 | U22 | U33 | U12 | U13 | U23 |
Co1 | 0.0198 (2) | 0.0217 (2) | 0.0232 (2) | −0.00091 (13) | 0.00196 (14) | −0.00005 (12) |
S1 | 0.0203 (3) | 0.0220 (3) | 0.0245 (3) | −0.00008 (16) | −0.00023 (18) | 0.00040 (16) |
O1 | 0.0316 (7) | 0.0326 (7) | 0.0328 (7) | 0.0041 (6) | 0.0005 (6) | −0.0082 (6) |
O2 | 0.0299 (7) | 0.0284 (7) | 0.0359 (8) | −0.0036 (6) | 0.0002 (6) | 0.0071 (6) |
O3 | 0.0220 (7) | 0.0343 (8) | 0.0362 (8) | 0.0004 (5) | −0.0024 (6) | 0.0012 (5) |
O4 | 0.0278 (7) | 0.0340 (8) | 0.0476 (9) | −0.0019 (6) | 0.0072 (6) | −0.0164 (6) |
O5 | 0.0270 (7) | 0.0361 (8) | 0.0474 (9) | 0.0027 (6) | 0.0088 (6) | 0.0160 (7) |
O6 | 0.0311 (8) | 0.0281 (8) | 0.0633 (11) | −0.0004 (6) | −0.0171 (7) | −0.0025 (6) |
N1 | 0.0528 (12) | 0.0596 (13) | 0.0288 (9) | 0.0205 (10) | −0.0043 (8) | 0.0047 (9) |
C1 | 0.0247 (9) | 0.0198 (8) | 0.0248 (9) | −0.0011 (7) | −0.0006 (7) | 0.0021 (7) |
C2 | 0.0236 (9) | 0.0197 (9) | 0.0307 (10) | 0.0007 (7) | 0.0009 (8) | 0.0008 (7) |
C3 | 0.0304 (10) | 0.0196 (9) | 0.0283 (10) | −0.0003 (7) | 0.0041 (8) | −0.0009 (7) |
C4 | 0.0375 (11) | 0.0222 (9) | 0.0263 (10) | 0.0008 (8) | −0.0019 (8) | 0.0025 (7) |
C5 | 0.0268 (10) | 0.0306 (10) | 0.0338 (11) | 0.0077 (8) | −0.0042 (8) | 0.0003 (8) |
C6 | 0.0261 (10) | 0.0307 (10) | 0.0299 (10) | 0.0031 (8) | 0.0031 (8) | −0.0011 (8) |
C7 | 0.0418 (12) | 0.0335 (11) | 0.0334 (11) | 0.0050 (9) | 0.0085 (10) | 0.0004 (8) |
Geometric parameters (Å, º) top Co1—O6i | 2.0515 (14) | N1—C4 | 1.365 (2) |
Co1—O6 | 2.0515 (14) | N1—H1A | 0.8600 |
Co1—O4i | 2.0866 (13) | N1—H1B | 0.8600 |
Co1—O4 | 2.0866 (13) | C1—C6 | 1.386 (2) |
Co1—O5 | 2.0868 (13) | C1—C2 | 1.389 (3) |
Co1—O5i | 2.0868 (13) | C2—C3 | 1.386 (3) |
S1—O1 | 1.4593 (13) | C2—H2 | 0.9300 |
S1—O3 | 1.4603 (14) | C3—C4 | 1.407 (3) |
S1—O2 | 1.4617 (13) | C3—C7 | 1.500 (3) |
S1—C1 | 1.7580 (18) | C4—C5 | 1.392 (3) |
O4—H7 | 0.8498 | C5—C6 | 1.372 (3) |
O4—H8 | 0.8498 | C5—H5 | 0.9300 |
O5—H9 | 0.8500 | C6—H6 | 0.9300 |
O5—H10 | 0.8499 | C7—H7A | 0.9600 |
O6—H12 | 0.8499 | C7—H7B | 0.9600 |
O6—H11 | 0.8499 | C7—H7C | 0.9600 |
| | | |
O6i—Co1—O6 | 180.0 | H12—O6—H11 | 105.7 |
O6i—Co1—O4i | 92.07 (6) | C4—N1—H1A | 120.0 |
O6—Co1—O4i | 87.93 (6) | C4—N1—H1B | 120.0 |
O6i—Co1—O4 | 87.93 (6) | H1A—N1—H1B | 120.0 |
O6—Co1—O4 | 92.07 (6) | C6—C1—C2 | 120.05 (17) |
O4i—Co1—O4 | 180.0 | C6—C1—S1 | 118.67 (14) |
O6i—Co1—O5 | 90.56 (6) | C2—C1—S1 | 121.28 (14) |
O6—Co1—O5 | 89.44 (6) | C3—C2—C1 | 120.94 (17) |
O4i—Co1—O5 | 87.15 (6) | C3—C2—H2 | 119.5 |
O4—Co1—O5 | 92.85 (6) | C1—C2—H2 | 119.5 |
O6i—Co1—O5i | 89.44 (6) | C2—C3—C4 | 118.72 (17) |
O6—Co1—O5i | 90.56 (6) | C2—C3—C7 | 121.77 (18) |
O4i—Co1—O5i | 92.85 (6) | C4—C3—C7 | 119.51 (17) |
O4—Co1—O5i | 87.15 (6) | N1—C4—C5 | 120.13 (17) |
O5—Co1—O5i | 180.0 | N1—C4—C3 | 120.29 (18) |
O1—S1—O3 | 112.18 (8) | C5—C4—C3 | 119.58 (17) |
O1—S1—O2 | 111.56 (9) | C6—C5—C4 | 121.08 (17) |
O3—S1—O2 | 111.60 (7) | C6—C5—H5 | 119.5 |
O1—S1—C1 | 106.81 (8) | C4—C5—H5 | 119.5 |
O3—S1—C1 | 107.24 (8) | C5—C6—C1 | 119.63 (17) |
O2—S1—C1 | 107.10 (8) | C5—C6—H6 | 120.2 |
Co1—O4—H7 | 133.5 | C1—C6—H6 | 120.2 |
Co1—O4—H8 | 120.2 | C3—C7—H7A | 109.5 |
H7—O4—H8 | 106.2 | C3—C7—H7B | 109.5 |
Co1—O5—H9 | 125.3 | H7A—C7—H7B | 109.5 |
Co1—O5—H10 | 113.7 | C3—C7—H7C | 109.5 |
H9—O5—H10 | 103.7 | H7A—C7—H7C | 109.5 |
Co1—O6—H12 | 129.0 | H7B—C7—H7C | 109.5 |
Co1—O6—H11 | 125.2 | | |
| | | |
O1—S1—C1—C6 | −38.02 (17) | C2—C3—C4—N1 | 179.47 (17) |
O3—S1—C1—C6 | −158.47 (14) | C7—C3—C4—N1 | −0.9 (3) |
O2—S1—C1—C6 | 81.62 (16) | C2—C3—C4—C5 | 0.3 (3) |
O1—S1—C1—C2 | 142.30 (14) | C7—C3—C4—C5 | 179.96 (17) |
O3—S1—C1—C2 | 21.85 (16) | N1—C4—C5—C6 | −179.70 (19) |
O2—S1—C1—C2 | −98.06 (15) | C3—C4—C5—C6 | −0.6 (3) |
C6—C1—C2—C3 | 0.4 (3) | C4—C5—C6—C1 | 0.7 (3) |
S1—C1—C2—C3 | −179.97 (13) | C2—C1—C6—C5 | −0.6 (3) |
C1—C2—C3—C4 | −0.2 (3) | S1—C1—C6—C5 | 179.75 (15) |
C1—C2—C3—C7 | −179.85 (17) | | |
Symmetry code: (i) −x+1, −y+1, −z. |
Hydrogen-bond geometry (Å, º) top D—H···A | D—H | H···A | D···A | D—H···A |
N1—H1A···O2ii | 0.86 | 2.47 | 3.214 (2) | 145 |
N1—H1B···O4 | 0.86 | 2.56 | 3.129 (2) | 125 |
O4—H7···O2ii | 0.85 | 2.00 | 2.8300 (19) | 167 |
O4—H8···O3iii | 0.85 | 1.92 | 2.7675 (19) | 176 |
O5—H9···O1iv | 0.85 | 1.94 | 2.7828 (19) | 170 |
O5—H10···O3v | 0.85 | 1.95 | 2.7963 (19) | 174 |
O6—H11···O1v | 0.85 | 1.93 | 2.7711 (19) | 169 |
O6—H12···O2iii | 0.85 | 1.90 | 2.7419 (19) | 173 |
Symmetry codes: (ii) −x+1/2, y+1/2, −z+1/2; (iii) −x+3/2, y+1/2, −z+1/2; (iv) −x+1/2, y−1/2, −z+1/2; (v) −x+3/2, y−1/2, −z+1/2. |
Experimental details
Crystal data |
Chemical formula | [Co(H2O)6](C7H8NO3S)2 |
Mr | 539.43 |
Crystal system, space group | Monoclinic, P21/n |
Temperature (K) | 293 |
a, b, c (Å) | 6.309 (1), 7.0513 (11), 24.262 (4) |
β (°) | 94.080 (2) |
V (Å3) | 1076.6 (3) |
Z | 2 |
Radiation type | Mo Kα |
µ (mm−1) | 1.06 |
Crystal size (mm) | 0.21 × 0.16 × 0.12 |
|
Data collection |
Diffractometer | Bruker SMART CCD diffractometer |
Absorption correction | Multi-scan (SADABS; Bruker, 2000) |
Tmin, Tmax | 0.809, 0.884 |
No. of measured, independent and observed [I > 2σ(I)] reflections | 5530, 1921, 1690 |
Rint | 0.019 |
(sin θ/λ)max (Å−1) | 0.596 |
|
Refinement |
R[F2 > 2σ(F2)], wR(F2), S | 0.025, 0.073, 1.10 |
No. of reflections | 1921 |
No. of parameters | 143 |
H-atom treatment | H-atom parameters constrained |
Δρmax, Δρmin (e Å−3) | 0.42, −0.33 |
Selected bond lengths (Å) topCo1—O6 | 2.0515 (14) | Co1—O5 | 2.0868 (13) |
Co1—O4 | 2.0866 (13) | | |
Hydrogen-bond geometry (Å, º) top D—H···A | D—H | H···A | D···A | D—H···A |
N1—H1A···O2i | 0.86 | 2.47 | 3.214 (2) | 145 |
N1—H1B···O4 | 0.86 | 2.56 | 3.129 (2) | 125 |
O4—H7···O2i | 0.85 | 2.00 | 2.8300 (19) | 167 |
O4—H8···O3ii | 0.85 | 1.92 | 2.7675 (19) | 176 |
O5—H9···O1iii | 0.85 | 1.94 | 2.7828 (19) | 170 |
O5—H10···O3iv | 0.85 | 1.95 | 2.7963 (19) | 174 |
O6—H11···O1iv | 0.85 | 1.93 | 2.7711 (19) | 169 |
O6—H12···O2ii | 0.85 | 1.90 | 2.7419 (19) | 173 |
Symmetry codes: (i) −x+1/2, y+1/2, −z+1/2; (ii) −x+3/2, y+1/2, −z+1/2; (iii) −x+1/2, y−1/2, −z+1/2; (iv) −x+3/2, y−1/2, −z+1/2. |
Acknowledgements
The authors would like to thank the Program for New Century Excellent Talents in Universities for a research grant.
References
Bruker (2000). SMART, SAINT and SADABS. Bruker AXS Inc., Madison, Wisconsin, USA. Google Scholar
Sheldrick, G. M. (2008). Acta Cryst. A64, 112–122. Web of Science CrossRef CAS IUCr Journals Google Scholar
Tai, X. S., Yin, J., Feng, Y. M. & Kong, F. Y. (2007). Chin. J. Inorg. Chem. 24, 1812–1814. Google Scholar
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