Tetra-aqua-bis(pyridine-3-sulfonato-κN)nickel(II).

In the mol-ecule of the title compound, [Ni(C(5)H(4)NO(3)S)(2)(H(2)O)(4)], the Ni(II) cation is located on an inversion center and is coordinated by four water mol-ecules and two pyridine-3-sulfonate anions with an NiN(2)O(4) distorted octa-hedral geometry. The face-to-face separation of 3.561 (5) Å between parallel pyridine rings indicates the existence of weak π-π stacking between the pyridine rings. The structure also contains inter-molecular O-H⋯O hydrogen bonding and weak C-H⋯O hydrogen bonding.

Related literature

For general background, see: Deisenhofer & Michel (1989 ▶); Su & Xu (2004 ▶); Liu et al. (2004 ▶); Li et al. (2005 ▶). For a related structure, see: Walsh & Hathaway (1980 ▶). For related literature, see: Cotton & Wilkinson (1972 ▶).

Experimental

Crystal data

[Ni(C5H4NO3S)2(H2O)4]

M = 447.08

Monoclinic,

a = 7.5399 (8) Å

b = 12.6939 (15) Å

c = 8.7810 (8) Å

β = 97.419 (12)°

V = 833.40 (15) Å3

Z = 2

Mo Kα radiation

μ = 1.47 mm−1

T = 295 (2) K

0.32 × 0.22 × 0.20 mm

Data collection

Rigaku R-AXIS RAPID IP diffractometer

Absorption correction: multi-scan (ABSCOR; Higashi, 1995 ▶) T min = 0.660, T max = 0.745

8877 measured reflections

1524 independent reflections

1449 reflections with I > 2σ(I)

R int = 0.019

Refinement

R[F 2 > 2σ(F 2)] = 0.024

wR(F 2) = 0.065

S = 1.06

1524 reflections

115 parameters

H-atom parameters constrained

Δρmax = 0.29 e Å−3

Δρmin = −0.37 e Å−3

Data collection: PROCESS-AUTO (Rigaku, 1998 ▶); cell refinement: PROCESS-AUTO; data reduction: CrystalStructure (Rigaku/MSC, 2002 ▶); program(s) used to solve structure: SIR92 (Altomare et al., 1993 ▶); program(s) used to refine structure: SHELXL97 (Sheldrick, 2008 ▶); molecular graphics: ORTEP-3 for Windows (Farrugia, 1997 ▶); software used to prepare material for publication: WinGX (Farrugia, 1999 ▶).

Crystal structure: contains datablocks I, global. DOI: 10.1107/S1600536808010076/om2227sup1.cif

Structure factors: contains datablocks I. DOI: 10.1107/S1600536808010076/om2227Isup2.hkl

Additional supplementary materials: crystallographic information; 3D view; checkCIF report

[Ni(C5H4NO3S)2(H2O)4]	F000 = 460
Mr = 447.08	Dx = 1.782 Mg m−3
Monoclinic, P21/n	Mo Kα radiation λ = 0.71073 Å
Hall symbol: -P 2yn	Cell parameters from 5256 reflections
a = 7.5399 (8) Å	θ = 2.8–24.0º
b = 12.6939 (15) Å	µ = 1.47 mm−1
c = 8.7810 (8) Å	T = 295 (2) K
β = 97.419 (12)º	Prism, blue
V = 833.40 (15) Å3	0.32 × 0.22 × 0.20 mm
Z = 2

Rigaku R-AXIS RAPID IP diffractometer	1524 independent reflections
Radiation source: fine-focus sealed tube	1449 reflections with I > 2σ(I)
Monochromator: graphite	Rint = 0.019
Detector resolution: 10.0 pixels mm-1	θmax = 25.4º
T = 295(2) K	θmin = 2.8º
ω scans	h = −9→9
Absorption correction: multi-scan(ABSCOR; Higashi, 1995)	k = −15→15
Tmin = 0.660, Tmax = 0.745	l = −9→10
8877 measured reflections

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)] = 0.024	H-atom parameters constrained
wR(F2) = 0.065	w = 1/[σ2(Fo2) + (0.0323P)2 + 0.5265P] where P = (Fo2 + 2Fc2)/3
S = 1.06	(Δ/σ)max < 0.001
1524 reflections	Δρmax = 0.29 e Å−3
115 parameters	Δρmin = −0.37 e Å−3
Primary atom site location: structure-invariant direct methods	Extinction correction: none

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
Ni	0.5000	0.5000	0.5000	0.02883 (13)
S	0.45204 (7)	0.75905 (4)	−0.03581 (6)	0.03407 (15)
N1	0.5850 (2)	0.54221 (13)	0.28948 (18)	0.0307 (3)
O1	0.76142 (19)	0.48676 (11)	0.60868 (18)	0.0388 (3)
H1B	0.8326	0.5397	0.5900	0.058*
H1A	0.8182	0.4333	0.5998	0.058*
O2	0.50231 (19)	0.34035 (11)	0.45010 (17)	0.0411 (3)
H2A	0.5076	0.3156	0.3615	0.062*
H2B	0.4194	0.3021	0.4815	0.062*
O3	0.5370 (3)	0.76975 (16)	−0.1732 (2)	0.0687 (6)
O4	0.4828 (2)	0.85025 (12)	0.0624 (2)	0.0554 (5)
O5	0.2658 (2)	0.73019 (12)	−0.06337 (19)	0.0481 (4)
C1	0.7217 (3)	0.49242 (15)	0.2368 (3)	0.0370 (5)
H1	0.7768	0.4372	0.2943	0.044*
C2	0.7839 (3)	0.51907 (18)	0.1020 (3)	0.0452 (5)
H2	0.8783	0.4819	0.0693	0.054*
C3	0.7053 (3)	0.60162 (17)	0.0150 (3)	0.0405 (5)
H3	0.7461	0.6218	−0.0762	0.049*
C4	0.5641 (2)	0.65298 (14)	0.0684 (2)	0.0298 (4)
C5	0.5074 (3)	0.62143 (15)	0.2044 (2)	0.0320 (4)
H5	0.4116	0.6565	0.2384	0.038*

	U11	U22	U33	U12	U13	U23
Ni	0.0309 (2)	0.0273 (2)	0.0284 (2)	0.00105 (13)	0.00426 (14)	0.00418 (13)
S	0.0419 (3)	0.0278 (3)	0.0317 (3)	0.0027 (2)	0.0018 (2)	0.00399 (19)
N1	0.0329 (8)	0.0290 (8)	0.0302 (8)	0.0016 (7)	0.0037 (6)	0.0034 (7)
O1	0.0336 (7)	0.0355 (8)	0.0467 (9)	0.0018 (6)	0.0031 (6)	0.0056 (6)
O2	0.0512 (9)	0.0328 (8)	0.0409 (8)	−0.0017 (6)	0.0122 (7)	−0.0002 (6)
O3	0.0861 (14)	0.0758 (13)	0.0491 (11)	0.0261 (11)	0.0269 (10)	0.0305 (9)
O4	0.0591 (10)	0.0297 (8)	0.0707 (11)	0.0048 (7)	−0.0174 (8)	−0.0095 (8)
O5	0.0441 (9)	0.0358 (8)	0.0600 (10)	0.0039 (7)	−0.0103 (7)	−0.0022 (7)
C1	0.0360 (11)	0.0328 (11)	0.0417 (12)	0.0064 (8)	0.0034 (9)	0.0061 (8)
C2	0.0417 (12)	0.0431 (12)	0.0542 (14)	0.0126 (10)	0.0188 (10)	0.0065 (10)
C3	0.0455 (12)	0.0393 (11)	0.0395 (12)	0.0036 (9)	0.0154 (9)	0.0055 (9)
C4	0.0337 (9)	0.0255 (9)	0.0295 (10)	−0.0002 (7)	0.0016 (8)	0.0005 (7)
C5	0.0333 (9)	0.0314 (10)	0.0313 (10)	0.0041 (8)	0.0047 (8)	0.0004 (8)

Ni—O1i	2.0828 (14)	O1—H1B	0.8886
Ni—O1	2.0828 (14)	O1—H1A	0.8115
Ni—O2i	2.0739 (14)	O2—H2A	0.8450
Ni—O2	2.0739 (14)	O2—H2B	0.8642
Ni—N1i	2.1026 (16)	C1—C2	1.370 (3)
Ni—N1	2.1026 (16)	C1—H1	0.9300
S—O5	1.4412 (16)	C2—C3	1.384 (3)
S—O3	1.4438 (18)	C2—H2	0.9300
S—O4	1.4445 (16)	C3—C4	1.381 (3)
S—C4	1.7788 (19)	C3—H3	0.9300
N1—C1	1.341 (3)	C4—C5	1.379 (3)
N1—C5	1.341 (2)	C5—H5	0.9300
O2i—Ni—O2	180.0	C5—N1—Ni	121.36 (13)
O2i—Ni—O1i	89.12 (6)	Ni—O1—H1B	114.4
O2—Ni—O1i	90.88 (6)	Ni—O1—H1A	120.2
O2i—Ni—O1	90.88 (6)	H1B—O1—H1A	106.0
O2—Ni—O1	89.12 (6)	Ni—O2—H2A	124.1
O1i—Ni—O1	180.0	Ni—O2—H2B	117.1
O2i—Ni—N1i	92.95 (6)	H2A—O2—H2B	101.9
O2—Ni—N1i	87.05 (6)	N1—C1—C2	123.07 (19)
O1i—Ni—N1i	92.61 (6)	N1—C1—H1	118.5
O1—Ni—N1i	87.39 (6)	C2—C1—H1	118.5
O2i—Ni—N1	87.05 (6)	C1—C2—C3	119.6 (2)
O2—Ni—N1	92.95 (6)	C1—C2—H2	120.2
O1i—Ni—N1	87.39 (6)	C3—C2—H2	120.2
O1—Ni—N1	92.61 (6)	C4—C3—C2	117.6 (2)
N1i—Ni—N1	180.0	C4—C3—H3	121.2
O5—S—O3	114.30 (12)	C2—C3—H3	121.2
O5—S—O4	112.45 (10)	C5—C4—C3	119.71 (18)
O3—S—O4	111.67 (12)	C5—C4—S	119.06 (14)
O5—S—C4	106.36 (9)	C3—C4—S	121.23 (15)
O3—S—C4	105.58 (10)	N1—C5—C4	122.60 (18)
O4—S—C4	105.69 (9)	N1—C5—H5	118.7
C1—N1—C5	117.40 (17)	C4—C5—H5	118.7
C1—N1—Ni	121.22 (13)

D—H···A	D—H	H···A	D···A	D—H···A
O1—H1A···O3ii	0.81	2.39	3.162 (3)	158
O1—H1A···O4ii	0.81	2.44	3.119 (2)	142
O1—H1B···O4iii	0.89	1.83	2.722 (2)	177
O2—H2A···O3iv	0.84	1.97	2.787 (2)	163
O2—H2B···O5v	0.86	1.89	2.748 (2)	174
C1—H1···O4ii	0.93	2.34	3.212 (3)	155

Table 1

Selected bond lengths (Å)

Ni—O1	2.0828 (14)
Ni—O2	2.0739 (14)
Ni—N1	2.1026 (16)

Table 2

Hydrogen-bond geometry (Å, °)

D—H⋯A	D—H	H⋯A	D⋯A	D—H⋯A
O1—H1A⋯O3i	0.81	2.39	3.162 (3)	158
O1—H1A⋯O4i	0.81	2.44	3.119 (2)	142
O1—H1B⋯O4ii	0.89	1.83	2.722 (2)	177
O2—H2A⋯O3iii	0.84	1.97	2.787 (2)	163
O2—H2B⋯O5iv	0.86	1.89	2.748 (2)	174
C1—H1⋯O4i	0.93	2.34	3.212 (3)	155

Symmetry codes: (i) ; (ii) ; (iii) ; (iv) .