Diaqua­bis­(pyridine-2-sulfonato-κ2N,O)cobalt(II)

Li, Z.-S.; Ng, S.W.

doi:10.1107/S1600536811048203

metal-organic compounds

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Volume 67| Part 12| December 2011| Page m1781

https://doi.org/10.1107/S1600536811048203

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Diaquabis(pyridine-2-sulfonato-κ²N,O)cobalt(II)

Zong-Sheng Li ^a and Seik Weng Ng ^b,^c ^*

^aCollege of Safety and Environment Engineering, Capital University of Economics and Business, Beijing 100070, People's Republic of China, ^bDepartment of Chemistry, University of Malaya, 50603 Kuala Lumpur, Malaysia, and ^cChemistry Department, Faculty of Science, King Abdulaziz University, PO Box 80203 Jeddah, Saudi Arabia
^*Correspondence e-mail: seikweng@um.edu.my

(Received 8 November 2011; accepted 14 November 2011; online 19 November 2011)

The title complex, [Co(C₅H₄NO₃S)₂(H₂O)₂], lies on a twofold rotation axis that relates the two water molecules and the two pyridine-2-sulfonate ions. The Co^II atom exists in an slightly distorted octahedral environment. The N-donor atoms are cis to each other. In the crystal, adjacent molecules are linked by O—H⋯O hydrogen bonds into a layer motif extending along (001).

Related literature

For the isotypic manganese(II), zinc and cadmium analogs, see: Lobana et al. (2004 ); Xiao (2007 ); Xiao & Liu (2004 ).

Experimental

Crystal data

[Co(C₅H₄NO₃S)₂(H₂O)₂]
M_r = 411.29
Monoclinic, C 2/c
a = 13.7009 (9) Å
b = 7.1127 (5) Å
c = 16.0180 (11) Å
β = 106.734 (1)°
V = 1494.86 (18) Å³
Z = 4
Mo Kα radiation
μ = 1.47 mm⁻¹
T = 296 K
0.25 × 0.20 × 0.15 mm

Data collection

Bruker SMART APEX diffractometer
Absorption correction: multi-scan (SADABS; Sheldrick, 1996 ) T_min = 0.710, T_max = 0.810
4331 measured reflections
1695 independent reflections
1590 reflections with I > 2σ(I)
R_int = 0.016

Refinement

R[F² > 2σ(F²)] = 0.024
wR(F²) = 0.067
S = 1.03
1695 reflections
113 parameters
3 restraints
H atoms treated by a mixture of independent and constrained refinement
Δρ_max = 0.35 e Å⁻³
Δρ_min = −0.34 e Å⁻³

Table 1
Hydrogen-bond geometry (Å, °)

D—H⋯A	D—H	H⋯A	D⋯A	D—H⋯A
O1w—H11⋯O2ⁱ	0.83 (1)	1.90 (1)	2.735 (2)	177 (3)
O1w—H12⋯O3ⁱⁱ	0.83 (1)	1.88 (1)	2.703 (2)	172 (3)
Symmetry codes: (i) $[-x+1, y+1, -z+{\script{3\over 2}}]$ ; (ii) $[x+{\script{1\over 2}}, y+{\script{1\over 2}}, z]$ .

Data collection: APEX2 (Bruker, 2007 ); cell refinement: SAINT (Bruker, 2007); data reduction: SAINT; program(s) used to solve structure: SHELXS97 (Sheldrick, 2008 ); program(s) used to refine structure: SHELXL97 (Sheldrick, 2008); molecular graphics: X-SEED (Barbour, 2001 ); software used to prepare material for publication: publCIF (Westrip, 2010 ).

Supporting information

Crystal structure: contains datablocks global, I. DOI: https://doi.org/10.1107/S1600536811048203/zs2164sup1.cif

Structure factors: contains datablock I. DOI: https://doi.org/10.1107/S1600536811048203/zs2164Isup2.hkl

checkCIF report

Comment top

Diaquabis(pyridine-2-sulfonate)cobalt(II) (Scheme I) is isostructural with the manganese, zinc (Lobana et al., 2004; Xiao & Liu, 2004) and cadmium (Xiao, 2007) analogs. The molecule lies on a twofold rotation axis that relates the two water molecules and the two pyridine-2-sulfonate ions and the Co^II atom exist in an slightly distorted octahedral environment. The N donor atoms are cis to each other (Fig. 1). Adjacent molecules are linked by water O–H···O_sulfonate hydrogen bonds (Table 1) into a layer motif extending along (0 0 1) (Fig. 2).

Related literature top

For the isotypic manganese(II), zinc(II) and cadmium(II) analogs, see: Lobana et al. (2004); Xiao (2007); Xiao & Liu (2004).

Experimental top

Pyridine-2-sulfonic acid (0.4 mmol, 0.0641 g) was dissolved in 0.1 M sodium hydroxide (4 ml); cobalt(II) chloride hexahydrate (0.2 mmol, 0.0476 g) and 4,4'-bipyridine-N,N'-dioxide (0.2 mmol, 0.0446 g) were added to the solution. The clear solution was allowed to evaporate at ambient conditions, affording red block-shaped crystals after one week, in 40% yield.

Structure description top

For the isotypic manganese(II), zinc(II) and cadmium(II) analogs, see: Lobana et al. (2004); Xiao (2007); Xiao & Liu (2004).

Computing details top

Data collection: APEX2 (Bruker, 2007); cell refinement: SAINT (Bruker, 2007); data reduction: SAINT (Bruker, 2007); program(s) used to solve structure: SHELXS97 (Sheldrick, 2008); program(s) used to refine structure: SHELXL97 (Sheldrick, 2008); molecular graphics: X-SEED (Barbour, 2001); software used to prepare material for publication: publCIF (Westrip, 2010).

Figures top

	Fig. 1. Thermal ellipsoid plot (Barbour, 2001) of [Co(H₂O)₂(C₅H₄NO₃S)₂] at the 50% probability level. Hydrogen atoms are drawn as spheres of arbitrary radius. The unlabeled atoms are related to the labeled ones by twofold rotational symmetry (symmetry code -x + 1, y, -z + 3/2).
	Fig. 2. The hydrogen-bonded layer structure.

Diaquabis(pyridine-2-sulfonato-κ²N,O)cobalt(II) top

Crystal data top

[Co(C₅H₄NO₃S)₂(H₂O)₂]	F(000) = 836
M_r = 411.29	D_x = 1.827 Mg m⁻³
Monoclinic, C2/c	Mo Kα radiation, λ = 0.71073 Å
Hall symbol: -C 2yc	Cell parameters from 3169 reflections
a = 13.7009 (9) Å	θ = 3.1–27.6°
b = 7.1127 (5) Å	µ = 1.47 mm⁻¹
c = 16.0180 (11) Å	T = 296 K
β = 106.734 (1)°	Prism, yellow
V = 1494.86 (18) Å³	0.25 × 0.20 × 0.15 mm
Z = 4

Data collection top

Bruker SMART APEX diffractometer	1695 independent reflections
Radiation source: fine-focus sealed tube	1590 reflections with I > 2σ(I)
Graphite monochromator	R_int = 0.016
ω scans	θ_max = 27.5°, θ_min = 2.7°
Absorption correction: multi-scan (SADABS; Sheldrick, 1996)	h = −17→11
T_min = 0.710, T_max = 0.810	k = −9→9
4331 measured reflections	l = −13→20

Refinement top

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)] = 0.024	Hydrogen site location: inferred from neighbouring sites
wR(F²) = 0.067	H atoms treated by a mixture of independent and constrained refinement
S = 1.03	w = 1/[σ²(F_o²) + (0.0362P)² + 1.5779P] where P = (F_o² + 2F_c²)/3
1695 reflections	(Δ/σ)_max = 0.001
113 parameters	Δρ_max = 0.35 e Å⁻³
3 restraints	Δρ_min = −0.34 e Å⁻³

Crystal data top

[Co(C₅H₄NO₃S)₂(H₂O)₂]	V = 1494.86 (18) Å³
M_r = 411.29	Z = 4
Monoclinic, C2/c	Mo Kα radiation
a = 13.7009 (9) Å	µ = 1.47 mm⁻¹
b = 7.1127 (5) Å	T = 296 K
c = 16.0180 (11) Å	0.25 × 0.20 × 0.15 mm
β = 106.734 (1)°

Data collection top

Bruker SMART APEX diffractometer	1695 independent reflections
Absorption correction: multi-scan (SADABS; Sheldrick, 1996)	1590 reflections with I > 2σ(I)
T_min = 0.710, T_max = 0.810	R_int = 0.016
4331 measured reflections

Refinement top

R[F² > 2σ(F²)] = 0.024	3 restraints
wR(F²) = 0.067	H atoms treated by a mixture of independent and constrained refinement
S = 1.03	Δρ_max = 0.35 e Å⁻³
1695 reflections	Δρ_min = −0.34 e Å⁻³
113 parameters

Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å²) top

	x	y	z	U_iso*/U_eq
Co1	0.5000	0.69090 (4)	0.7500	0.02354 (11)
S1	0.33529 (3)	0.39913 (6)	0.66183 (2)	0.02716 (12)
O1	0.38590 (11)	0.4900 (2)	0.74481 (7)	0.0379 (3)
O2	0.37681 (13)	0.21672 (19)	0.65256 (10)	0.0474 (4)
O3	0.22560 (11)	0.3995 (3)	0.64164 (10)	0.0504 (4)
O1W	0.59993 (12)	0.9037 (2)	0.74438 (11)	0.0467 (4)
H11	0.6059 (18)	1.001 (2)	0.7743 (14)	0.055 (7)*
H12	0.6431 (16)	0.902 (3)	0.7169 (15)	0.060 (8)*
N1	0.44352 (10)	0.6597 (2)	0.61055 (9)	0.0255 (3)
C1	0.36597 (12)	0.5407 (2)	0.58114 (9)	0.0237 (3)
C2	0.31435 (14)	0.5162 (3)	0.49417 (11)	0.0339 (4)
H2	0.2589	0.4352	0.4769	0.041*
C3	0.34772 (16)	0.6160 (3)	0.43366 (11)	0.0398 (4)
H3	0.3149	0.6034	0.3744	0.048*
C4	0.43020 (15)	0.7344 (3)	0.46221 (12)	0.0384 (4)
H4	0.4551	0.7998	0.4224	0.046*
C5	0.47534 (14)	0.7548 (3)	0.55036 (12)	0.0344 (4)
H5	0.5299	0.8374	0.5691	0.041*

Atomic displacement parameters (Å²) top

	U¹¹	U²²	U³³	U¹²	U¹³	U²³
Co1	0.02474 (17)	0.02440 (17)	0.02083 (16)	0.000	0.00555 (11)	0.000
S1	0.0294 (2)	0.0293 (2)	0.0240 (2)	−0.00801 (15)	0.00954 (16)	0.00137 (14)
O1	0.0506 (8)	0.0432 (7)	0.0214 (5)	−0.0189 (6)	0.0125 (5)	−0.0010 (5)
O2	0.0711 (11)	0.0282 (7)	0.0465 (8)	0.0001 (7)	0.0228 (7)	0.0063 (6)
O3	0.0306 (7)	0.0803 (12)	0.0433 (8)	−0.0137 (7)	0.0154 (6)	0.0049 (7)
O1W	0.0496 (9)	0.0409 (8)	0.0625 (9)	−0.0211 (7)	0.0367 (8)	−0.0254 (7)
N1	0.0268 (7)	0.0279 (7)	0.0218 (6)	−0.0028 (5)	0.0068 (5)	0.0036 (5)
C1	0.0262 (7)	0.0245 (7)	0.0216 (7)	0.0003 (6)	0.0088 (6)	0.0013 (6)
C2	0.0371 (9)	0.0382 (9)	0.0246 (8)	−0.0068 (8)	0.0060 (7)	−0.0044 (7)
C3	0.0489 (11)	0.0493 (11)	0.0201 (7)	0.0006 (9)	0.0081 (7)	0.0008 (7)
C4	0.0488 (11)	0.0418 (10)	0.0291 (8)	0.0012 (9)	0.0184 (8)	0.0109 (8)
C5	0.0364 (9)	0.0346 (9)	0.0335 (9)	−0.0077 (8)	0.0119 (7)	0.0070 (7)

Geometric parameters (Å, º) top

Co1—O1W	2.0601 (14)	O1W—H12	0.832 (9)
Co1—O1Wⁱ	2.0601 (13)	N1—C1	1.334 (2)
Co1—O1	2.1018 (13)	N1—C5	1.349 (2)
Co1—O1ⁱ	2.1018 (13)	C1—C2	1.380 (2)
Co1—N1	2.1545 (13)	C2—C3	1.381 (3)
Co1—N1ⁱ	2.1545 (13)	C2—H2	0.9300
S1—O2	1.4414 (15)	C3—C4	1.378 (3)
S1—O3	1.4432 (14)	C3—H3	0.9300
S1—O1	1.4612 (13)	C4—C5	1.376 (3)
S1—C1	1.7814 (15)	C4—H4	0.9300
O1W—H11	0.833 (9)	C5—H5	0.9300

O1W—Co1—O1Wⁱ	85.45 (9)	Co1—O1W—H11	122.9 (16)
O1W—Co1—O1	173.62 (6)	Co1—O1W—H12	126.6 (16)
O1Wⁱ—Co1—O1	90.29 (6)	H11—O1W—H12	110.3 (15)
O1W—Co1—O1ⁱ	90.29 (6)	C1—N1—C5	117.02 (14)
O1Wⁱ—Co1—O1ⁱ	173.61 (6)	C1—N1—Co1	116.31 (10)
O1—Co1—O1ⁱ	94.34 (8)	C5—N1—Co1	126.58 (12)
O1W—Co1—N1	94.31 (6)	N1—C1—C2	124.14 (15)
O1Wⁱ—Co1—N1	94.36 (6)	N1—C1—S1	115.65 (11)
O1—Co1—N1	81.26 (5)	C2—C1—S1	120.12 (13)
O1ⁱ—Co1—N1	90.69 (5)	C1—C2—C3	117.83 (17)
O1W—Co1—N1ⁱ	94.36 (6)	C1—C2—H2	121.1
O1Wⁱ—Co1—N1ⁱ	94.31 (6)	C3—C2—H2	121.1
O1—Co1—N1ⁱ	90.69 (5)	C4—C3—C2	119.14 (16)
O1ⁱ—Co1—N1ⁱ	81.26 (5)	C4—C3—H3	120.4
N1—Co1—N1ⁱ	168.19 (8)	C2—C3—H3	120.4
O2—S1—O3	113.26 (10)	C3—C4—C5	119.23 (17)
O2—S1—O1	113.20 (9)	C3—C4—H4	120.4
O3—S1—O1	113.19 (9)	C5—C4—H4	120.4
O2—S1—C1	104.56 (8)	N1—C5—C4	122.56 (17)
O3—S1—C1	106.52 (8)	N1—C5—H5	118.7
O1—S1—C1	105.11 (7)	C4—C5—H5	118.7
S1—O1—Co1	119.31 (7)

O2—S1—O1—Co1	98.03 (11)	C5—N1—C1—C2	−3.1 (3)
O3—S1—O1—Co1	−131.35 (10)	Co1—N1—C1—C2	173.84 (14)
C1—S1—O1—Co1	−15.48 (11)	C5—N1—C1—S1	173.39 (13)
O1Wⁱ—Co1—O1—S1	104.28 (10)	Co1—N1—C1—S1	−9.71 (16)
O1ⁱ—Co1—O1—S1	−80.13 (9)	O2—S1—C1—N1	−103.32 (14)
N1—Co1—O1—S1	9.91 (10)	O3—S1—C1—N1	136.50 (14)
N1ⁱ—Co1—O1—S1	−161.41 (10)	O1—S1—C1—N1	16.13 (15)
O1W—Co1—N1—C1	−174.23 (12)	O2—S1—C1—C2	73.28 (16)
O1Wⁱ—Co1—N1—C1	−88.48 (12)	O3—S1—C1—C2	−46.89 (17)
O1—Co1—N1—C1	1.14 (12)	O1—S1—C1—C2	−167.27 (15)
O1ⁱ—Co1—N1—C1	95.43 (12)	N1—C1—C2—C3	2.6 (3)
N1ⁱ—Co1—N1—C1	48.64 (11)	S1—C1—C2—C3	−173.66 (14)
O1W—Co1—N1—C5	2.33 (15)	C1—C2—C3—C4	0.0 (3)
O1Wⁱ—Co1—N1—C5	88.09 (15)	C2—C3—C4—C5	−2.0 (3)
O1—Co1—N1—C5	177.71 (16)	C1—N1—C5—C4	0.9 (3)
O1ⁱ—Co1—N1—C5	−88.01 (15)	Co1—N1—C5—C4	−175.65 (14)
N1ⁱ—Co1—N1—C5	−134.79 (15)	C3—C4—C5—N1	1.6 (3)

Symmetry code: (i) −x+1, y, −z+3/2.

Hydrogen-bond geometry (Å, º) top

D—H···A	D—H	H···A	D···A	D—H···A
O1w—H11···O2ⁱⁱ	0.83 (1)	1.90 (1)	2.735 (2)	177 (3)
O1w—H12···O3ⁱⁱⁱ	0.83 (1)	1.88 (1)	2.703 (2)	172 (3)

Symmetry codes: (ii) −x+1, y+1, −z+3/2; (iii) x+1/2, y+1/2, z.

Experimental details

Crystal data
Chemical formula	[Co(C₅H₄NO₃S)₂(H₂O)₂]
M_r	411.29
Crystal system, space group	Monoclinic, C2/c
Temperature (K)	296
a, b, c (Å)	13.7009 (9), 7.1127 (5), 16.0180 (11)
β (°)	106.734 (1)
V (Å³)	1494.86 (18)
Z	4
Radiation type	Mo Kα
µ (mm⁻¹)	1.47
Crystal size (mm)	0.25 × 0.20 × 0.15

Data collection
Diffractometer	Bruker SMART APEX
Absorption correction	Multi-scan (SADABS; Sheldrick, 1996)
T_min, T_max	0.710, 0.810
No. of measured, independent and observed [I > 2σ(I)] reflections	4331, 1695, 1590
R_int	0.016
(sin θ/λ)_max (Å⁻¹)	0.650

Refinement
R[F² > 2σ(F²)], wR(F²), S	0.024, 0.067, 1.03
No. of reflections	1695
No. of parameters	113
No. of restraints	3
H-atom treatment	H atoms treated by a mixture of independent and constrained refinement
Δρ_max, Δρ_min (e Å⁻³)	0.35, −0.34

Computer programs: APEX2 (Bruker, 2007), SAINT (Bruker, 2007), SHELXS97 (Sheldrick, 2008), SHELXL97 (Sheldrick, 2008), X-SEED (Barbour, 2001), publCIF (Westrip, 2010).

Hydrogen-bond geometry (Å, º) top

D—H···A	D—H	H···A	D···A	D—H···A
O1w—H11···O2ⁱ	0.83 (1)	1.90 (1)	2.735 (2)	177 (3)
O1w—H12···O3ⁱⁱ	0.83 (1)	1.88 (1)	2.703 (2)	172 (3)

Symmetry codes: (i) −x+1, y+1, −z+3/2; (ii) x+1/2, y+1/2, z.

Acknowledgements

We thank Beijing Normal University and the University of Malaya for supporting this study.

References

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