In the title molecular salt, [Co(H
2O)
6](C
7H
8NO
3S)
2, the Co
2+ 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
CCDC reference: 758659
Key indicators
- Single-crystal X-ray study
- T = 293 K
- Mean
(C-C) = 0.003 Å
- R factor = 0.025
- wR factor = 0.073
- Data-to-parameter ratio = 13.4
checkCIF/PLATON results
No syntax errors found
Alert level C
PLAT242_ALERT_2_C Check Low Ueq as Compared to Neighbors for Co1
PLAT911_ALERT_3_C Missing # FCF Refl Between THmin & STh/L= 0.596 3
PLAT042_ALERT_1_C Calc. and Reported MoietyFormula Strings Differ ?
Alert level G
PLAT128_ALERT_4_G Non-standard setting of Space-group P21/c .... P21/n
PLAT199_ALERT_1_G Check the Reported _cell_measurement_temperature 293 K
PLAT200_ALERT_1_G Check the Reported _diffrn_ambient_temperature 293 K
PLAT380_ALERT_4_G Check Incorrectly? Oriented X(sp2)-Methyl Moiety C7
0 ALERT level A = In general: serious problem
0 ALERT level B = Potentially serious problem
3 ALERT level C = Check and explain
4 ALERT level G = General alerts; check
3 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
2 ALERT type 4 Improvement, methodology, query or suggestion
0 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 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. |