catena-Poly[[triaqua-(pyridine-κN)nickel(II)]-μ-sulfato-κO:O'].

The title compound, [Ni(SO(4))(C(5)H(5)N)(H(2)O)(3)](n), was synthesized by the hydro-thermal reaction of NiSO(4)·6H(2)O, pyridine and water. The central Ni(II) atom is coordinated in a distorted octa-hedral environment by a pyridine N atom, three aqua O atoms and two O atoms of bridging sulfate anions, yielding a zigzag chain. A three-dimensional network is generated via complex hydrogen bonds involving the sulfate and aqua ligands and a pyridine C-H group.

Related literature

For the structures of related nickel(II) complexes, see: Wang et al. (2006 ▶); Stein et al. (2007 ▶).

Experimental

Crystal data

[Ni(SO4)(C5H5N)(H2O)3]

M = 287.92

Monoclinic,

a = 11.868 (3) Å

b = 7.5745 (14) Å

c = 11.420 (3) Å

β = 110.724 (4)°

V = 960.2 (3) Å3

Z = 4

Mo Kα radiation

μ = 2.26 mm−1

T = 193 K

0.30 × 0.20 × 0.14 mm

Data collection

Rigaku Mercury CCD diffractometer

Absorption correction: multi-scan (REQAB; Jacobson, 1998 ▶) T min = 0.465, T max = 0.729

8854 measured reflections

1746 independent reflections

1641 reflections with I > 2σ(I)

R int = 0.040

Refinement

R[F 2 > 2σ(F 2)] = 0.036

wR(F 2) = 0.110

S = 1.16

1746 reflections

161 parameters

6 restraints

H atoms treated by a mixture of independent and constrained refinement

Δρmax = 0.57 e Å−3

Δρmin = −0.84 e Å−3

Data collection: CrystalClear (Rigaku, 1999 ▶); cell refinement: CrystalClear; data reduction: CrystalStructure (Rigaku/MSC & Rigaku, 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.

Crystal structure: contains datablocks I, global. DOI: 10.1107/S1600536809049605/pk2206sup1.cif

Structure factors: contains datablocks I. DOI: 10.1107/S1600536809049605/pk2206Isup2.hkl

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

[Ni(SO4)(C5H5N)(H2O)3]	F(000) = 592
Mr = 287.92	Dx = 1.992 Mg m−3
Monoclinic, P21/c	Mo Kα radiation, λ = 0.71070 Å
Hall symbol: -P 2ybc	Cell parameters from 3550 reflections
a = 11.868 (3) Å	θ = 3.1–25.3°
b = 7.5745 (14) Å	µ = 2.26 mm−1
c = 11.420 (3) Å	T = 193 K
β = 110.724 (4)°	Block, light-green
V = 960.2 (3) Å3	0.30 × 0.20 × 0.14 mm
Z = 4

Rigaku Mercury CCD diffractometer	1746 independent reflections
Radiation source: fine-focus sealed tube	1641 reflections with I > 2σ(I)
graphite	Rint = 0.040
Detector resolution: 7.31 pixels mm-1	θmax = 25.3°, θmin = 3.3°
ω scans	h = −14→13
Absorption correction: multi-scan (REQAB; Jacobson, 1998)	k = −9→9
Tmin = 0.465, Tmax = 0.729	l = −13→12
8854 measured reflections

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)] = 0.036	Hydrogen site location: inferred from neighbouring sites
wR(F2) = 0.110	H atoms treated by a mixture of independent and constrained refinement
S = 1.16	w = 1/[σ2(Fo2) + (0.0672P)2 + 0.4274P] where P = (Fo2 + 2Fc2)/3
1746 reflections	(Δ/σ)max = 0.001
161 parameters	Δρmax = 0.57 e Å−3
6 restraints	Δρmin = −0.84 e Å−3

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
Ni1	0.65136 (3)	0.59664 (5)	0.21049 (4)	0.0112 (2)
S1	0.37812 (7)	0.51034 (10)	0.20733 (7)	0.0111 (2)
O1	0.4632 (2)	0.5757 (3)	0.1473 (2)	0.0144 (5)
O2	0.3600 (2)	0.3178 (3)	0.1818 (2)	0.0148 (5)
O3	0.2651 (2)	0.6067 (3)	0.1535 (2)	0.0185 (6)
O4	0.4322 (2)	0.5392 (3)	0.3441 (2)	0.0163 (5)
O5	0.6504 (2)	0.3741 (3)	0.1062 (2)	0.0139 (5)
H5A	0.626 (3)	0.283 (3)	0.128 (3)	0.017 (10)*
H5B	0.619 (4)	0.381 (6)	0.0300 (11)	0.033 (13)*
O6	0.6708 (2)	0.4525 (3)	0.3691 (2)	0.0165 (5)
H6A	0.687 (4)	0.3472 (19)	0.367 (4)	0.037 (13)*
H6B	0.611 (2)	0.435 (5)	0.387 (4)	0.028 (12)*
O7	0.6283 (2)	0.7484 (3)	0.0563 (2)	0.0212 (6)
H7A	0.632 (4)	0.724 (5)	−0.0120 (19)	0.034 (12)*
H7B	0.609 (4)	0.850 (2)	0.064 (4)	0.031 (12)*
N1	0.8352 (3)	0.6199 (4)	0.2656 (3)	0.0179 (7)
C1	0.9028 (3)	0.6672 (5)	0.3822 (3)	0.0247 (8)
H1	0.8637	0.6950	0.4394	0.030*
C2	1.0269 (3)	0.6774 (6)	0.4232 (4)	0.0325 (9)
H2	1.0718	0.7112	0.5069	0.039*
C3	1.0846 (3)	0.6379 (6)	0.3407 (4)	0.0345 (10)
H3	1.1699	0.6441	0.3664	0.041*
C4	1.0165 (4)	0.5894 (5)	0.2207 (5)	0.0331 (10)
H4	1.0539	0.5612	0.1620	0.040*
C5	0.8929 (3)	0.5822 (5)	0.1867 (4)	0.0255 (9)
H5C	0.8464	0.5490	0.1034	0.031*

	U11	U22	U33	U12	U13	U23
Ni1	0.0115 (3)	0.0107 (3)	0.0109 (3)	−0.00030 (14)	0.0035 (2)	0.00009 (15)
S1	0.0122 (4)	0.0103 (4)	0.0114 (4)	−0.0005 (3)	0.0050 (3)	−0.0009 (3)
O1	0.0123 (12)	0.0198 (13)	0.0129 (12)	−0.0013 (9)	0.0066 (10)	0.0014 (9)
O2	0.0222 (13)	0.0097 (12)	0.0127 (11)	−0.0012 (9)	0.0064 (10)	−0.0036 (10)
O3	0.0172 (13)	0.0147 (13)	0.0259 (14)	0.0034 (9)	0.0103 (11)	0.0035 (10)
O4	0.0226 (13)	0.0160 (12)	0.0113 (12)	−0.0048 (10)	0.0071 (10)	−0.0043 (10)
O5	0.0188 (13)	0.0144 (12)	0.0081 (12)	−0.0028 (10)	0.0042 (10)	0.0010 (10)
O6	0.0158 (13)	0.0135 (13)	0.0198 (13)	−0.0005 (11)	0.0058 (10)	0.0022 (11)
O7	0.0361 (15)	0.0135 (14)	0.0175 (14)	0.0053 (11)	0.0139 (12)	0.0009 (11)
N1	0.0154 (15)	0.0150 (15)	0.0223 (16)	−0.0002 (11)	0.0053 (12)	0.0016 (12)
C1	0.0198 (19)	0.029 (2)	0.0217 (19)	−0.0036 (16)	0.0025 (15)	−0.0012 (17)
C2	0.020 (2)	0.035 (2)	0.033 (2)	−0.0033 (17)	−0.0025 (17)	0.002 (2)
C3	0.0139 (19)	0.028 (2)	0.057 (3)	−0.0045 (16)	0.007 (2)	0.004 (2)
C4	0.024 (2)	0.028 (2)	0.056 (3)	−0.0004 (17)	0.025 (2)	0.002 (2)
C5	0.0198 (19)	0.029 (2)	0.030 (2)	−0.0035 (15)	0.0124 (17)	−0.0038 (17)

Ni1—O7	2.039 (2)	O6—H6B	0.82 (3)
Ni1—N1	2.053 (3)	O7—H7A	0.82 (3)
Ni1—O6	2.056 (2)	O7—H7B	0.815 (10)
Ni1—O5	2.062 (2)	N1—C1	1.337 (5)
Ni1—O1	2.096 (2)	N1—C5	1.342 (5)
Ni1—O2i	2.110 (2)	C1—C2	1.380 (5)
S1—O3	1.458 (2)	C1—H1	0.9500
S1—O4	1.479 (2)	C2—C3	1.380 (6)
S1—O2	1.488 (2)	C2—H2	0.9500
S1—O1	1.491 (2)	C3—C4	1.372 (6)
O2—Ni1ii	2.110 (2)	C3—H3	0.9500
O5—H5A	0.82 (3)	C4—C5	1.379 (6)
O5—H5B	0.818 (10)	C4—H4	0.9500
O6—H6A	0.821 (10)	C5—H5C	0.9500
O7—Ni1—N1	91.13 (11)	H5A—O5—H5B	108 (4)
O7—Ni1—O6	177.36 (10)	Ni1—O6—H6A	117 (3)
N1—Ni1—O6	89.97 (11)	Ni1—O6—H6B	118 (3)
O7—Ni1—O5	89.45 (9)	H6A—O6—H6B	94 (4)
N1—Ni1—O5	92.04 (11)	Ni1—O7—H7A	131 (3)
O6—Ni1—O5	92.91 (10)	Ni1—O7—H7B	113 (3)
O7—Ni1—O1	86.80 (10)	H7A—O7—H7B	115 (4)
N1—Ni1—O1	177.81 (10)	C1—N1—C5	117.1 (3)
O6—Ni1—O1	92.13 (9)	C1—N1—Ni1	121.8 (2)
O5—Ni1—O1	87.23 (9)	C5—N1—Ni1	121.1 (3)
O7—Ni1—O2i	92.22 (9)	N1—C1—C2	123.1 (4)
N1—Ni1—O2i	91.89 (10)	N1—C1—H1	118.5
O6—Ni1—O2i	85.33 (9)	C2—C1—H1	118.5
O5—Ni1—O2i	175.69 (9)	C3—C2—C1	118.9 (4)
O1—Ni1—O2i	88.90 (9)	C3—C2—H2	120.5
O3—S1—O4	111.21 (14)	C1—C2—H2	120.5
O3—S1—O2	111.13 (13)	C4—C3—C2	118.8 (4)
O4—S1—O2	109.26 (13)	C4—C3—H3	120.6
O3—S1—O1	108.13 (14)	C2—C3—H3	120.6
O4—S1—O1	108.95 (13)	C3—C4—C5	118.9 (4)
O2—S1—O1	108.08 (12)	C3—C4—H4	120.6
S1—O1—Ni1	132.76 (14)	C5—C4—H4	120.6
S1—O2—Ni1ii	134.32 (13)	N1—C5—C4	123.2 (4)
Ni1—O5—H5A	116 (3)	N1—C5—H5C	118.4
Ni1—O5—H5B	118 (3)	C4—C5—H5C	118.4
O3—S1—O1—Ni1	150.13 (18)	O2i—Ni1—N1—C1	37.9 (3)
O4—S1—O1—Ni1	29.1 (2)	O7—Ni1—N1—C5	−52.1 (3)
O2—S1—O1—Ni1	−89.5 (2)	O6—Ni1—N1—C5	130.3 (3)
O7—Ni1—O1—S1	−167.8 (2)	O5—Ni1—N1—C5	37.4 (3)
O6—Ni1—O1—S1	9.8 (2)	O2i—Ni1—N1—C5	−144.4 (3)
O5—Ni1—O1—S1	102.64 (19)	C5—N1—C1—C2	−0.3 (5)
O2i—Ni1—O1—S1	−75.47 (19)	Ni1—N1—C1—C2	177.5 (3)
O3—S1—O2—Ni1ii	−103.2 (2)	N1—C1—C2—C3	0.2 (6)
O4—S1—O2—Ni1ii	19.9 (2)	C1—C2—C3—C4	−0.1 (6)
O1—S1—O2—Ni1ii	138.29 (18)	C2—C3—C4—C5	0.1 (6)
O7—Ni1—N1—C1	130.2 (3)	C1—N1—C5—C4	0.3 (5)
O6—Ni1—N1—C1	−47.4 (3)	Ni1—N1—C5—C4	−177.5 (3)
O5—Ni1—N1—C1	−140.3 (3)	C3—C4—C5—N1	−0.3 (6)

D—H···A	D—H	H···A	D···A	D—H···A
O5—H5A···O4ii	0.82 (3)	2.04 (3)	2.849 (3)	170 (4)
O5—H5A···S1ii	0.82 (3)	2.81 (2)	3.571 (3)	157 (3)
O5—H5B···O1iii	0.82 (1)	1.94 (1)	2.753 (3)	173 (4)
O5—H5B···S1iii	0.82 (1)	2.85 (2)	3.584 (3)	151 (4)
O6—H6A···O3ii	0.82 (1)	1.95 (1)	2.764 (3)	172 (4)
O6—H6A···S1ii	0.82 (1)	2.71 (2)	3.458 (3)	152 (4)
O6—H6B···O4	0.82 (3)	2.15 (3)	2.821 (3)	139 (4)
O6—H6B···S1	0.82 (3)	2.85 (4)	3.336 (3)	120 (3)
O7—H7A···O2iii	0.82 (3)	2.00 (3)	2.817 (3)	176 (4)
O7—H7A···S1iii	0.82 (3)	2.82 (2)	3.571 (3)	154 (4)
O7—H7B···O4i	0.82 (1)	1.94 (2)	2.690 (3)	153 (4)
O7—H7B···S1i	0.82 (1)	2.84 (4)	3.372 (3)	125 (4)
C4—H4···O3iv	0.95	2.57	3.304 (5)	135

Table 1

Hydrogen-bond geometry (Å, °)

D—H⋯A	D—H	H⋯A	D⋯A	D—H⋯A
O5—H5A⋯O4i	0.82 (3)	2.04 (3)	2.849 (3)	170 (4)
O5—H5B⋯O1ii	0.818 (10)	1.939 (12)	2.753 (3)	173 (4)
O6—H6A⋯O3i	0.821 (10)	1.949 (12)	2.764 (3)	172 (4)
O6—H6B⋯O4	0.82 (3)	2.15 (3)	2.821 (3)	139 (4)
O7—H7A⋯O2ii	0.82 (3)	2.00 (3)	2.817 (3)	176 (4)
O7—H7B⋯O4iii	0.815 (10)	1.94 (2)	2.690 (3)	153 (4)
C4—H4⋯O3iv	0.95	2.57	3.304 (5)	135

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