catena-Poly[[[bis-[aqua-nickel(II)]bis-(μ-pyridine-2,6-dicarboxyl-ato N-oxide)]-μ-1,2-di-4-pyridylethane] tetra-hydrate].

In the title compound, {[Ni(2)(C(7)H(3)NO(5))(2)(C(12)H(12)N(2))(H(2)O)(2)]·4H(2)O}(n), two Ni(II) ions, two tridentate pyridine-2,6-dicarboxyl-ate N-oxide ligands and two coordinated water mol-ecules form centrosymmetric dinuclear units, which are further bridged by centrosymmetric 1,2-di-4-pyridylethane ligands into polymeric chains along [210]. Each Ni(II) ion has a distorted square-pyramidal environment, with the basal plane formed by three O [Ni-O = 1.9290 (16)-1.9588 (10) Å] and one N [Ni-N = 1.9828 (18) Å] atoms and the apical position occupied by the water mol-ecule [Ni-O = 2.2643 (11) Å]. The water mol-ecules are involved in the formation of O-H⋯O hydrogen bonds.

Related literature

For related literature, see: Laine et al. (1995a ▶,b ▶); Lin et al. (2006 ▶); Nathan et al. (1985 ▶). For a related structure, see: Wen et al. (2005 ▶).

Experimental

Crystal data

[Ni2(C7H3NO5)2(C12H12N2)(H2O)2]·4H2O

M = 771.96

Triclinic,

a = 8.2803 (16) Å

b = 10.3542 (15) Å

c = 11.1326 (16) Å

α = 113.727 (2)°

β = 104.282 (2)°

γ = 100.255 (2)°

V = 804.4 (2) Å3

Z = 1

Mo Kα radiation

μ = 1.25 mm−1

T = 298 (2) K

0.25 × 0.19 × 0.16 mm

Data collection

Bruker APEXII area-detector diffractometer

Absorption correction: multi-scan (SADABS; Sheldrick, 1996 ▶) T min = 0.745, T max = 0.825

4146 measured reflections

2850 independent reflections

2180 reflections with I > 2σ(I)

R int = 0.033

Refinement

R[F 2 > 2σ(F 2)] = 0.028

wR(F 2) = 0.063

S = 0.83

2850 reflections

199 parameters

H-atom parameters constrained

Δρmax = 0.35 e Å−3

Δρmin = −0.29 e Å−3

Data collection: APEX2 (Bruker, 2004 ▶); cell refinement: APEX2; data reduction: APEX2; program(s) used to solve structure: SHELXS97 (Sheldrick, 2008 ▶); program(s) used to refine structure: SHELXL97 (Sheldrick, 2008 ▶); molecular graphics: ORTEPIII (Burnett & Johnson, 1996 ▶), ORTEP-3 for Windows (Farrugia, 1997 ▶) and PLATON (Spek, 2003 ▶); software used to prepare material for publication: SHELXL97.

Crystal structure: contains datablocks I, global. DOI: 10.1107/S1600536808031619/cv2458sup1.cif

Structure factors: contains datablocks I. DOI: 10.1107/S1600536808031619/cv2458Isup2.hkl

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

[Ni2(C7H3NO5)2(C12H12N2)(H2O)2]·4H2O	Z = 1
Mr = 771.96	F(000) = 398
Triclinic, P1	Dx = 1.594 Mg m−3
Hall symbol: -P 1	Mo Kα radiation, λ = 0.71073 Å
a = 8.2803 (16) Å	Cell parameters from 2850 reflections
b = 10.3542 (15) Å	θ = 2.1–25.2°
c = 11.1326 (16) Å	µ = 1.25 mm−1
α = 113.727 (2)°	T = 298 K
β = 104.282 (2)°	Block, green
γ = 100.255 (2)°	0.25 × 0.19 × 0.16 mm
V = 804.4 (2) Å3

Bruker APEXII area-detector diffractometer	2850 independent reflections
Radiation source: fine-focus sealed tube	2180 reflections with I > 2σ(I)
graphite	Rint = 0.033
φ and ω scans	θmax = 25.2°, θmin = 2.1°
Absorption correction: multi-scan (SADABS; Sheldrick, 1996)	h = −9→9
Tmin = 0.745, Tmax = 0.825	k = −12→12
4146 measured reflections	l = −13→12

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)] = 0.028	Hydrogen site location: inferred from neighbouring sites
wR(F2) = 0.063	H-atom parameters constrained
S = 0.83	w = 1/[σ2(Fo2) + (0.0269P)2 + 0.19P] where P = (Fo2 + 2Fc2)/3
2850 reflections	(Δ/σ)max < 0.001
199 parameters	Δρmax = 0.35 e Å−3
0 restraints	Δρmin = −0.29 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	0.19610 (4)	0.10188 (3)	0.85792 (3)	0.03124 (11)
O1	0.0912 (2)	0.1451 (2)	0.70832 (19)	0.0473 (5)
O2	−0.1257 (2)	0.1548 (2)	0.5550 (2)	0.0600 (6)
O3	−0.03449 (19)	0.0177 (2)	0.85274 (17)	0.0433 (4)
N1	0.4335 (2)	0.2138 (2)	0.8837 (2)	0.0376 (5)
N2	−0.1753 (2)	−0.0555 (2)	0.7358 (2)	0.0354 (5)
C1	−0.0673 (3)	0.1028 (3)	0.6318 (3)	0.0401 (6)
C2	−0.2011 (3)	−0.0227 (3)	0.6272 (3)	0.0368 (6)
C3	−0.3544 (3)	−0.1043 (3)	0.5128 (3)	0.0489 (7)
H3	−0.3736	−0.0847	0.4369	0.059*
C4	−0.4795 (4)	−0.2144 (3)	0.5092 (3)	0.0570 (8)
H4	−0.5824	−0.2686	0.4315	0.068*
C5	−0.4508 (3)	−0.2433 (3)	0.6215 (3)	0.0492 (7)
H5	−0.5343	−0.3172	0.6205	0.059*
C6	−0.2980 (3)	−0.1624 (3)	0.7350 (3)	0.0366 (6)
C8	0.5711 (3)	0.1727 (3)	0.9306 (3)	0.0490 (7)
H8	0.5514	0.0953	0.9529	0.059*
C9	0.7394 (3)	0.2397 (3)	0.9470 (3)	0.0507 (7)
H9	0.8307	0.2077	0.9798	0.061*
C10	0.7726 (3)	0.3553 (3)	0.9144 (3)	0.0436 (6)
C11	0.9551 (3)	0.4316 (3)	0.9304 (3)	0.0518 (7)
H11A	1.0234	0.3635	0.9215	0.062*
H11B	0.9488	0.4587	0.8559	0.062*
C12	0.6307 (3)	0.3995 (3)	0.8690 (3)	0.0479 (7)
H12	0.6474	0.4782	0.8482	0.058*
C13	0.46548 (10)	0.32671 (9)	0.85477 (8)	0.0442 (7)
H13	0.3722	0.3577	0.8236	0.053*
O1W	0.22201 (10)	−0.11885 (9)	0.72089 (8)	0.0584 (5)
H1W	0.1610	−0.1939	0.7212	0.088*
H2W	0.2045	−0.1367	0.6357	0.088*
O2W	0.15515 (10)	0.41900 (9)	0.61420 (8)	0.0944 (8)
H3W	0.0828	0.3364	0.5887	0.142*
H4W	0.1122	0.489	0.6354	0.142*
O3W	0.03080 (10)	0.37588 (9)	0.33371 (8)	0.0875 (7)
H6W	0.0820	0.3592	0.2741	0.131*
H5W	0.1116	0.4510	0.4044	0.131*
C7	−0.25478 (10)	−0.18425 (9)	0.86469 (8)	0.0374 (6)
O4	−0.28538 (10)	−0.09359 (9)	0.96606 (8)	0.0401 (4)
O5	−0.19822 (10)	−0.28825 (9)	0.85957 (8)	0.0540 (5)

	U11	U22	U33	U12	U13	U23
Ni1	0.02697 (17)	0.0386 (2)	0.03728 (19)	0.00914 (13)	0.01384 (14)	0.02526 (16)
O1	0.0408 (10)	0.0605 (12)	0.0545 (12)	0.0133 (9)	0.0172 (9)	0.0406 (11)
O2	0.0654 (13)	0.0709 (14)	0.0579 (13)	0.0196 (11)	0.0122 (10)	0.0495 (12)
O3	0.0302 (9)	0.0632 (12)	0.0351 (10)	0.0041 (8)	0.0070 (8)	0.0286 (9)
N1	0.0335 (11)	0.0434 (13)	0.0472 (13)	0.0122 (10)	0.0175 (10)	0.0297 (11)
N2	0.0296 (11)	0.0454 (13)	0.0341 (12)	0.0114 (10)	0.0107 (10)	0.0218 (11)
C1	0.0484 (16)	0.0430 (16)	0.0361 (15)	0.0176 (13)	0.0183 (13)	0.0219 (13)
C2	0.0388 (14)	0.0456 (16)	0.0335 (14)	0.0180 (12)	0.0152 (12)	0.0221 (13)
C3	0.0471 (16)	0.0630 (19)	0.0386 (16)	0.0170 (15)	0.0102 (14)	0.0285 (15)
C4	0.0403 (16)	0.073 (2)	0.0413 (17)	0.0064 (15)	0.0009 (14)	0.0243 (16)
C5	0.0403 (15)	0.0570 (19)	0.0440 (17)	0.0067 (13)	0.0102 (13)	0.0241 (15)
C6	0.0319 (13)	0.0431 (16)	0.0374 (15)	0.0096 (12)	0.0129 (12)	0.0219 (13)
C8	0.0419 (15)	0.0528 (18)	0.070 (2)	0.0182 (13)	0.0246 (15)	0.0413 (16)
C9	0.0376 (15)	0.0531 (18)	0.070 (2)	0.0172 (13)	0.0220 (14)	0.0340 (16)
C10	0.0384 (14)	0.0430 (16)	0.0456 (16)	0.0072 (12)	0.0191 (13)	0.0172 (14)
C11	0.0420 (16)	0.0497 (18)	0.0549 (18)	0.0048 (13)	0.0224 (14)	0.0172 (14)
C12	0.0497 (16)	0.0403 (16)	0.0560 (18)	0.0061 (13)	0.0202 (14)	0.0270 (15)
C13	0.0400 (15)	0.0445 (16)	0.0553 (17)	0.0127 (13)	0.0167 (13)	0.0305 (15)
O1W	0.0732 (13)	0.0580 (13)	0.0531 (12)	0.0221 (11)	0.0286 (11)	0.0301 (11)
O2W	0.1038 (19)	0.0682 (16)	0.113 (2)	0.0268 (14)	0.0349 (16)	0.0454 (15)
O3W	0.127 (2)	0.0742 (16)	0.0925 (17)	0.0440 (15)	0.0679 (16)	0.0463 (14)
C7	0.0256 (13)	0.0449 (17)	0.0418 (16)	0.0028 (12)	0.0102 (12)	0.0249 (14)
O4	0.0350 (9)	0.0520 (11)	0.0420 (10)	0.0147 (8)	0.0165 (8)	0.0278 (9)
O5	0.0675 (13)	0.0502 (12)	0.0608 (13)	0.0252 (10)	0.0269 (11)	0.0360 (11)

Ni1—O3	1.9290 (16)	C8—C9	1.373 (3)
Ni1—O1	1.9373 (16)	C8—H8	0.9300
Ni1—O4i	1.9588 (10)	C9—C10	1.386 (3)
Ni1—N1	1.9828 (18)	C9—H9	0.9300
Ni1—O1W	2.2643 (11)	C10—C12	1.390 (3)
O1—C1	1.258 (3)	C10—C11	1.506 (3)
O2—C1	1.230 (3)	C11—C11ii	1.501 (5)
O3—N2	1.331 (2)	C11—H11A	0.9700
N1—C13	1.3332 (19)	C11—H11B	0.9700
N1—C8	1.345 (3)	C12—C13	1.376 (3)
N2—C6	1.358 (3)	C12—H12	0.9300
N2—C2	1.361 (3)	C13—H13	0.9300
C1—C2	1.525 (3)	O1W—H1W	0.85
C2—C3	1.379 (3)	O1W—H2W	0.86
C3—C4	1.377 (4)	O2W—H3W	0.84
C3—H3	0.9300	O2W—H4W	0.84
C4—C5	1.375 (3)	O3W—H6W	0.85
C4—H4	0.9300	O3W—H5W	0.86
C5—C6	1.371 (3)	C7—O5	1.2351 (14)
C5—H5	0.9300	C7—O4	1.2618 (12)
C6—C7	1.517 (3)	O4—Ni1i	1.9588 (10)
O3—Ni1—O1	89.83 (7)	N2—C6—C5	120.3 (2)
O3—Ni1—O4i	86.14 (5)	N2—C6—C7	116.2 (2)
O1—Ni1—O4i	167.38 (6)	C5—C6—C7	123.6 (3)
O3—Ni1—N1	172.23 (8)	N1—C8—C9	123.1 (2)
O1—Ni1—N1	90.76 (7)	N1—C8—H8	118.5
O4i—Ni1—N1	91.65 (6)	C9—C8—H8	118.5
O3—Ni1—O1W	94.95 (6)	C8—C9—C10	119.7 (2)
O1—Ni1—O1W	97.00 (6)	C8—C9—H9	120.2
O4i—Ni1—O1W	95.30 (6)	C10—C9—H9	120.2
N1—Ni1—O1W	92.67 (6)	C9—C10—C12	117.0 (2)
C1—O1—Ni1	129.11 (16)	C9—C10—C11	121.5 (2)
N2—O3—Ni1	123.58 (13)	C12—C10—C11	121.5 (2)
C13—N1—C8	117.39 (17)	C11ii—C11—C10	111.5 (3)
C13—N1—Ni1	123.82 (12)	C11ii—C11—H11A	109.3
C8—N1—Ni1	118.78 (15)	C10—C11—H11A	109.3
O3—N2—C6	114.80 (18)	C11ii—C11—H11B	109.3
O3—N2—C2	123.49 (19)	C10—C11—H11B	109.3
C6—N2—C2	121.6 (2)	H11A—C11—H11B	108.0
O2—C1—O1	124.3 (2)	C13—C12—C10	120.0 (2)
O2—C1—C2	115.3 (2)	C13—C12—H12	120.0
O1—C1—C2	120.5 (2)	C10—C12—H12	120.0
N2—C2—C3	118.2 (2)	N1—C13—C12	122.78 (15)
N2—C2—C1	121.5 (2)	N1—C13—H13	118.6
C3—C2—C1	120.3 (2)	C12—C13—H13	118.6
C4—C3—C2	121.1 (2)	Ni1—O1W—H1W	115.3
C4—C3—H3	119.5	Ni1—O1W—H2W	114.2
C2—C3—H3	119.5	H1W—O1W—H2W	108.3
C5—C4—C3	119.4 (3)	H3W—O2W—H4W	113.1
C5—C4—H4	120.3	H6W—O3W—H5W	99.6
C3—C4—H4	120.3	O5—C7—O4	127.3 (1)
C6—C5—C4	119.5 (2)	O5—C7—C6	117.9 (2)
C6—C5—H5	120.3	O4—C7—C6	114.9 (2)
C4—C5—H5	120.3	C7—O4—Ni1i	114.7 (1)

D—H···A	D—H	H···A	D···A	D—H···A
O1W—H1W···O3Wiii	0.85	1.99	2.8144 (15)	162
O1W—H2W···O2iii	0.86	1.98	2.824 (2)	168
O3W—H6W···O5iii	0.85	1.94	2.7791 (13)	170
O3W—H5W···O2W	0.86	2.44	2.8527 (13)	110
O2W—H3W···O2	0.84	2.15	2.976 (2)	167
O2W—H4W···O3Wiv	0.84	1.97	2.7985 (14)	169

Table 1

Hydrogen-bond geometry (Å, °)

D—H⋯A	D—H	H⋯A	D⋯A	D—H⋯A
O1W—H1W⋯O3Wi	0.85	1.99	2.8144 (15)	162
O1W—H2W⋯O2i	0.86	1.98	2.824 (2)	168
O3W—H6W⋯O5i	0.85	1.94	2.7791 (13)	170
O3W—H5W⋯O2W	0.86	2.44	2.8527 (13)	110
O2W—H3W⋯O2	0.84	2.15	2.976 (2)	167
O2W—H4W⋯O3Wii	0.84	1.97	2.7985 (14)	169

Symmetry codes: (i) ; (ii) .