catena-Poly[[[diaqua­(tetra­methyl­ethylenediamine-κ2N,N′)nickel(II)]-μ-sulfato-κ2O:O′] monohydrate]

Schmidt, G.; Merzweiler, K.

doi:10.1107/S1600536813006557

metal-organic compounds

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ISSN: 2056-9890

Volume 69| Part 4| April 2013| Page m197

doi:10.1107/S1600536813006557

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catena-Poly[[[diaqua(tetramethylethylenediamine-κ²N,N′)nickel(II)]-μ-sulfato-κ²O:O′] monohydrate]

Guntram Schmidt ^a and Kurt Merzweiler ^a ^*

^aInstitut für Chemie, Naturwissenschaftliche Fakultät II, Martin-Luther-Universität Halle-Wittenberg, Kurt-Mothes-Strasse 2, 06120 Halle (Saale), Germany
^*Correspondence e-mail: kurt.merzweiler@chemie.uni-halle.de

(Received 25 January 2013; accepted 7 March 2013; online 13 March 2013)

The title compound, {[Ni(SO₄)(C₆H₁₆N₂)(H₂O)₂]·H₂O}_n, contains a Ni^II atom that is coordinated nearly octahedrally by a chelating tetraethylenediamine (tmeda) ligand, two water molecules in a cis arrangement and two O atoms of two sulfate anions in a trans arrangement. The sulfate anions act as μ₂-bridging ligands leading to a chain structure of alternating NiO₄N₂ octahedra and SO₄ tetrahedra parallel to [001]. The polymeric chains are linked by O—H⋯O hydrogen bonds between coordinating water molecules and sulfate anions to give double strands. There is a lattice water molecule which is also involved in O—H⋯O hydrogen bonding between adjacent [Ni(SO₄)(tmeda)(H₂O)₂] chains.

Related literature

For crystal structures of oligo- and polymeric nickel(II) tmeda complexes, see: Anderson et al. (2009 ); Erer et al. (2010 ). For related literature on one-dimensional metal sulfates, see: Behera & Rao (2006 ).

Experimental

Crystal data

[Ni(SO₄)(C₆H₁₆N₂)(H₂O)₂]·H₂O
M_r = 325.03
Orthorhombic, P n a 2₁
a = 21.108 (4) Å
b = 9.9335 (19) Å
c = 6.3879 (13) Å
V = 1339.4 (5) Å³
Z = 4
Mo Kα radiation
μ = 1.63 mm⁻¹
T = 223 K
0.48 × 0.11 × 0.11 mm

Data collection

Stoe IPDS diffractometer
Absorption correction: numerical (IPDS; Stoe & Cie, 1999 ) T_min = 0.648, T_max = 0.841
10054 measured reflections
2585 independent reflections
2291 reflections with I > 2σ(I)
R_int = 0.054

Refinement

R[F² > 2σ(F²)] = 0.023
wR(F²) = 0.052
S = 1.04
2585 reflections
176 parameters
7 restraints
H atoms treated by a mixture of independent and constrained refinement
Δρ_max = 0.37 e Å⁻³
Δρ_min = −0.31 e Å⁻³
Absolute structure: Flack (1983 ), 1167 Friedel pairs
Flack parameter: −0.005 (13)

Table 1
Hydrogen-bond geometry (Å, °)

D—H⋯A	D—H	H⋯A	D⋯A	D—H⋯A
O5—H2⋯O4ⁱ	0.84 (2)	1.84 (2)	2.672 (2)	171 (3)
O5—H1⋯O7	0.83 (2)	1.93 (2)	2.765 (3)	176 (3)
O6—H4⋯O3	0.83 (2)	1.89 (2)	2.687 (3)	160 (3)
O6—H3⋯O3ⁱⁱ	0.83 (2)	2.03 (2)	2.829 (3)	162 (3)
O7—H5⋯O4	0.83 (2)	2.12 (2)	2.899 (3)	157 (3)
O7—H6⋯O3ⁱⁱ	0.83 (2)	2.18 (2)	2.934 (3)	151 (3)
Symmetry codes: (i) x, y, z-1; (ii) $[-x, -y+1, z-{\script{1\over 2}}]$ .

Data collection: IPDS (Stoe & Cie, 1999); cell refinement: IPDS; data reduction: IPDS; program(s) used to solve structure: SHELXS97 (Sheldrick, 2008 ); program(s) used to refine structure: SHELXL97 (Sheldrick, 2008); molecular graphics: DIAMOND (Brandenburg, 2009 ); software used to prepare material for publication: SHELXL97.

Supporting information

Crystal structure: contains datablocks I, global. DOI: 10.1107/S1600536813006557/wm2722sup1.cif

Structure factors: contains datablock I. DOI: 10.1107/S1600536813006557/wm2722Isup2.hkl

checkCIF report

Comment top

The title compound, {[Ni(H₂O)₂(C₆H₁₆N₂)(SO₄)]^.H₂O}_n, (I), forms a coordination polymer which consists of an alternating arrangement of [Ni(H₂O)₂(tmeda)]²⁺ (tmeda is tetraethylenediamine) cations and SO₄^2- anions. The coordination around nickel(II) is roughly octahedral with a chelating tmeda ligand, two water molecules in cis positions and two oxygen atoms of the SO₄^2- anions in a trans arrangement (Fig. 1). In a polyhedral description the chain consists of corner sharing NiN₂O₄ octahedra and SO₄ tetrahedra (Fig. 2). The observed Ni—N (2.141 (2), 2.1453 (19) Å) and Ni—O(aqua) distances (2.0639 (17), 2.084 (2) Å) agree well with the values reported for other nickel(II) complexes containing tmeda and aqua ligands, e.g. [Ni₆(CO₃)₄(tmeda)₆]Cl₄^.CH₂Cl₂ (Anderson et al., 2009) and [Ni(C₄O₄)(tmeda)(H₂O)₂]^.H₂O (Erer et al., 2010). A related chain structure consisting of corner-sharing NiO₄(H₂O)₂ octahedra and SO₄ tetrahedra has been observed in the compound [C₂N₂H₁₀][Ni(SO₄)₂(H₂O)₂] (Behera & Rao, 2006). However, in contrast to compound (I) each NiO₄(H₂O)₂ octahedron of the chain is connected to four SO₄ tetrahedra.

The crystal packing of the [Ni(H₂O)₂(tmeda)]SO₄ chains is supported by a network of hydrogen bridges (Figs. 2 and 3). Each of the water molecules attached to nickel forms an intrachain hydrogen bond of the type R¹₁(6) or R¹₁(6) to a sulfate oxygen atom. The lattice water molecule, which acts as a linker between the chains, forms two hydrogen bonds of the type R¹₁(2) to sulfate oxygen atoms and a D¹₁(2) hydrogen bond to a coordinating water molecule. Additonally, there are hydrogen bond motifs of the type R²₂(12) which are formed between coordinating water molecules and sulfate oxygen atoms of neighbouring chains. As a result of these interchain hydrogen bridges, double strands are formed which propagate parallel to [001]. The arrangement of the double strands corresponds to a distorted hexagonal rod packing.

Related literature top

For crystal structures of oligo- and polymeric nickel(II) tmeda complexes, see: Anderson et al. (2009); Erer et al. (2010). For related literature on one-dimensional metal sulfates, see: Behera & Rao (2006).

Experimental top

3.7 ml (46 mmol) of pyridine were added to a solution of 2.0 g (7.6 mmol) of nickel sulfate hexahydrate in 50 ml of water. 1.2 ml (8.0 mmol) of tmeda were added and all volatile compounds removed under reduced pressure at 333 K. The resulting solid was recrystallized from water and washed with ether to obtain the title compound in a yield of 85% (2.1 g).

Computing details top

Data collection: IPDS (Stoe & Cie, 1999); cell refinement: IPDS (Stoe & Cie, 1999); data reduction: IPDS (Stoe & Cie, 1999); program(s) used to solve structure: SHELXS97 (Sheldrick, 2008); program(s) used to refine structure: SHELXL97 (Sheldrick, 2008); molecular graphics: DIAMOND (Brandenburg, 2009); software used to prepare material for publication: SHELXL97 (Sheldrick, 2008).

Figures top

	Fig. 1. The coordination sphere around the nickel(II) atom in the structure of compound (I). The asymmetric unit is marked by solid lines of corresponding bonds. Displacement ellipsoids are drawn at the 50% probability level. [Symmetry code: ii) x, y, z-1].
	Fig. 2. Polyhedral representation of the structure of compound (I). NiN₂O₄ octahedra are blue, SO₄ tetrahedra are yellow.
	Fig. 3. Part of the hydrogen-bonding network (dashed lines) in the structure of compound (I). [Symmetry codes: i) x, y, -z+1; iii) -x, -y+1, z-0.5; iv) -x, -y + 1, z + 0.5.]

catena-Poly[[[diaqua(tetramethylethylenediamine-κ²N,N')nickel(II)]-µ-sulfato-κ²O:O'] monohydrate] top

Crystal data top

[Ni(SO₄)(C₆H₁₆N₂)(H₂O)₂]·H₂O	F(000) = 688
M_r = 325.03	D_x = 1.612 Mg m⁻³
Orthorhombic, Pna2₁	Mo Kα radiation, λ = 0.71073 Å
Hall symbol: P 2c -2n	Cell parameters from 8000 reflections
a = 21.108 (4) Å	θ = 2.2–25.8°
b = 9.9335 (19) Å	µ = 1.63 mm⁻¹
c = 6.3879 (13) Å	T = 223 K
V = 1339.4 (5) Å³	Block, green
Z = 4	0.48 × 0.11 × 0.11 mm

Data collection top

Stoe IPDS diffractometer	2585 independent reflections
Radiation source: fine-focus sealed tube	2291 reflections with I > 2σ(I)
Graphite monochromator	R_int = 0.054
area detector scans	θ_max = 25.9°, θ_min = 2.3°
Absorption correction: numerical (IPDS; Stoe & Cie, 1999)	h = −25→25
T_min = 0.648, T_max = 0.841	k = −12→12
10054 measured reflections	l = −7→7

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)] = 0.023	H atoms treated by a mixture of independent and constrained refinement
wR(F²) = 0.052	w = 1/[σ²(F_o²) + (0.0286P)²] where P = (F_o² + 2F_c²)/3
S = 1.04	(Δ/σ)_max = 0.001
2585 reflections	Δρ_max = 0.37 e Å⁻³
176 parameters	Δρ_min = −0.31 e Å⁻³
7 restraints	Absolute structure: Flack (1983), 1167 Friedel pairs
Primary atom site location: structure-invariant direct methods	Absolute structure parameter: −0.005 (13)

Crystal data top

[Ni(SO₄)(C₆H₁₆N₂)(H₂O)₂]·H₂O	V = 1339.4 (5) Å³
M_r = 325.03	Z = 4
Orthorhombic, Pna2₁	Mo Kα radiation
a = 21.108 (4) Å	µ = 1.63 mm⁻¹
b = 9.9335 (19) Å	T = 223 K
c = 6.3879 (13) Å	0.48 × 0.11 × 0.11 mm

Data collection top

Stoe IPDS diffractometer	2585 independent reflections
Absorption correction: numerical (IPDS; Stoe & Cie, 1999)	2291 reflections with I > 2σ(I)
T_min = 0.648, T_max = 0.841	R_int = 0.054
10054 measured reflections

Refinement top

R[F² > 2σ(F²)] = 0.023	H atoms treated by a mixture of independent and constrained refinement
wR(F²) = 0.052	Δρ_max = 0.37 e Å⁻³
S = 1.04	Δρ_min = −0.31 e Å⁻³
2585 reflections	Absolute structure: Flack (1983), 1167 Friedel pairs
176 parameters	Absolute structure parameter: −0.005 (13)
7 restraints

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	U_iso*/U_eq
C1	0.24703 (13)	0.7260 (3)	0.0085 (5)	0.0305 (6)
H1C	0.2232	0.7845	−0.0842	0.037*
H1B	0.2424	0.6334	−0.0371	0.037*
H1A	0.2914	0.7511	0.0051	0.037*
C4	0.16332 (11)	0.9525 (2)	0.2039 (4)	0.0224 (6)
H4B	0.1637	1.0473	0.2462	0.027*
H4A	0.1625	0.9489	0.0507	0.027*
C2	0.26524 (13)	0.6637 (3)	0.3636 (5)	0.0329 (7)
H2C	0.2506	0.6717	0.5070	0.039*
H2B	0.3079	0.6996	0.3527	0.039*
H2A	0.2653	0.5696	0.3229	0.039*
C3	0.22243 (11)	0.8836 (3)	0.2836 (5)	0.0244 (6)
H3B	0.2599	0.9279	0.2250	0.029*
H3A	0.2244	0.8915	0.4364	0.029*
C5	0.05032 (14)	0.9321 (3)	0.1665 (5)	0.0332 (7)
H5C	0.0121	0.8923	0.2238	0.040*
H5B	0.0552	0.9048	0.0216	0.040*
H5A	0.0473	1.0294	0.1742	0.040*
C6	0.09619 (15)	0.9283 (3)	0.5084 (5)	0.0316 (7)
H6C	0.0580	0.8867	0.5626	0.038*
H6B	0.0920	1.0254	0.5143	0.038*
H6A	0.1322	0.9005	0.5922	0.038*
N1	0.22264 (8)	0.7398 (2)	0.2241 (4)	0.0197 (5)
N2	0.10595 (9)	0.8859 (2)	0.2890 (3)	0.0190 (5)
Ni	0.125910 (11)	0.67593 (3)	0.25156 (6)	0.01456 (8)
O1	0.11212 (10)	0.69565 (19)	0.9294 (3)	0.0245 (5)
O2	0.13632 (9)	0.6444 (2)	0.5737 (3)	0.0232 (5)
O3	0.02891 (8)	0.6195 (2)	0.7004 (3)	0.0262 (4)
O4	0.10994 (9)	0.46409 (19)	0.8110 (3)	0.0265 (4)
O5	0.15204 (9)	0.47588 (19)	0.2051 (3)	0.0240 (4)
H1	0.1316 (12)	0.424 (3)	0.283 (4)	0.029*
H2	0.1375 (14)	0.463 (3)	0.084 (3)	0.029*
O6	0.03092 (8)	0.6302 (2)	0.2801 (3)	0.0234 (4)
H3	0.0187 (12)	0.557 (2)	0.234 (6)	0.028*
H4	0.0213 (14)	0.634 (3)	0.406 (3)	0.028*
O7	0.08191 (10)	0.2998 (2)	0.4475 (3)	0.0305 (5)
H5	0.0789 (16)	0.343 (3)	0.558 (4)	0.037*
H6	0.0442 (10)	0.309 (3)	0.414 (5)	0.037*
S	0.09690 (2)	0.60503 (5)	0.75426 (13)	0.01806 (12)

Atomic displacement parameters (Å²) top

	U¹¹	U²²	U³³	U¹²	U¹³	U²³
C1	0.0277 (15)	0.0361 (17)	0.0278 (15)	−0.0013 (12)	0.0109 (12)	−0.0029 (14)
C4	0.0255 (13)	0.0152 (11)	0.0265 (17)	−0.0026 (9)	0.0032 (10)	0.0009 (11)
C2	0.0187 (13)	0.0386 (18)	0.0413 (17)	0.0035 (12)	−0.0036 (12)	0.0087 (16)
C3	0.0203 (11)	0.0238 (12)	0.0290 (17)	−0.0054 (9)	0.0000 (11)	−0.0024 (14)
C5	0.0262 (14)	0.0265 (15)	0.0470 (18)	0.0070 (12)	−0.0093 (12)	0.0022 (14)
C6	0.0396 (17)	0.0267 (16)	0.0284 (15)	0.0031 (12)	0.0099 (13)	−0.0099 (13)
N1	0.0173 (9)	0.0215 (10)	0.0202 (13)	0.0008 (7)	0.0012 (10)	−0.0005 (11)
N2	0.0178 (9)	0.0203 (10)	0.0188 (14)	−0.0005 (8)	0.0008 (8)	−0.0001 (10)
Ni	0.01562 (12)	0.01675 (14)	0.01132 (12)	−0.00151 (11)	−0.00008 (17)	0.00004 (18)
O1	0.0349 (11)	0.0235 (12)	0.0151 (10)	−0.0064 (8)	−0.0011 (9)	−0.0023 (9)
O2	0.0215 (10)	0.0346 (12)	0.0135 (9)	−0.0053 (8)	0.0024 (7)	0.0030 (9)
O3	0.0192 (8)	0.0360 (10)	0.0235 (11)	−0.0042 (7)	0.0023 (7)	0.0020 (8)
O4	0.0342 (10)	0.0240 (10)	0.0215 (11)	−0.0027 (8)	−0.0042 (7)	−0.0013 (8)
O5	0.0335 (10)	0.0216 (10)	0.0170 (11)	−0.0004 (8)	−0.0007 (7)	0.0005 (8)
O6	0.0223 (8)	0.0286 (9)	0.0193 (11)	−0.0084 (6)	0.0004 (9)	0.0028 (11)
O7	0.0331 (11)	0.0285 (12)	0.0298 (11)	0.0014 (9)	0.0020 (9)	−0.0013 (10)
S	0.0190 (2)	0.0221 (3)	0.0131 (2)	−0.00424 (19)	0.0019 (4)	−0.0007 (4)

Geometric parameters (Å, º) top

C1—N1	1.477 (4)	C6—H6C	0.9700
C1—H1C	0.9700	C6—H6B	0.9700
C1—H1B	0.9700	C6—H6A	0.9700
C1—H1A	0.9700	N1—Ni	2.1453 (19)
C4—N2	1.483 (3)	N2—Ni	2.141 (2)
C4—C3	1.511 (4)	Ni—O6	2.0639 (17)
C4—H4B	0.9800	Ni—O5	2.084 (2)
C4—H4A	0.9800	Ni—O1ⁱ	2.088 (2)
C2—N1	1.475 (4)	Ni—O2	2.0931 (19)
C2—H2C	0.9700	O1—S	1.471 (2)
C2—H2B	0.9700	O1—Niⁱⁱ	2.088 (2)
C2—H2A	0.9700	O2—S	1.4751 (19)
C3—N1	1.478 (3)	O3—S	1.4828 (18)
C3—H3B	0.9800	O4—S	1.472 (2)
C3—H3A	0.9800	O5—H1	0.834 (18)
C5—N2	1.484 (3)	O5—H2	0.841 (18)
C5—H5C	0.9700	O6—H3	0.825 (17)
C5—H5B	0.9700	O6—H4	0.830 (17)
C5—H5A	0.9700	O7—H5	0.832 (18)
C6—N2	1.477 (4)	O7—H6	0.829 (18)

N1—C1—H1C	109.5	C2—N1—Ni	112.29 (17)
N1—C1—H1B	109.5	C1—N1—Ni	112.36 (18)
H1C—C1—H1B	109.5	C3—N1—Ni	105.19 (13)
N1—C1—H1A	109.5	C6—N2—C4	109.5 (2)
H1C—C1—H1A	109.5	C6—N2—C5	107.6 (2)
H1B—C1—H1A	109.5	C4—N2—C5	108.4 (2)
N2—C4—C3	110.4 (2)	C6—N2—Ni	114.27 (17)
N2—C4—H4B	109.6	C4—N2—Ni	103.46 (15)
C3—C4—H4B	109.6	C5—N2—Ni	113.46 (16)
N2—C4—H4A	109.6	O6—Ni—O5	93.42 (8)
C3—C4—H4A	109.6	O6—Ni—O1ⁱ	88.42 (8)
H4B—C4—H4A	108.1	O5—Ni—O1ⁱ	89.20 (7)
N1—C2—H2C	109.5	O6—Ni—O2	88.97 (8)
N1—C2—H2B	109.5	O5—Ni—O2	88.25 (8)
H2C—C2—H2B	109.5	O1ⁱ—Ni—O2	176.24 (7)
N1—C2—H2A	109.5	O6—Ni—N2	90.77 (8)
H2C—C2—H2A	109.5	O5—Ni—N2	175.58 (8)
H2B—C2—H2A	109.5	O1ⁱ—Ni—N2	89.51 (8)
N1—C3—C4	110.7 (2)	O2—Ni—N2	93.23 (8)
N1—C3—H3B	109.5	O6—Ni—N1	175.51 (8)
C4—C3—H3B	109.5	O5—Ni—N1	91.06 (8)
N1—C3—H3A	109.5	O1ⁱ—Ni—N1	91.40 (9)
C4—C3—H3A	109.5	O2—Ni—N1	91.41 (8)
H3B—C3—H3A	108.1	N2—Ni—N1	84.74 (8)
N2—C5—H5C	109.5	S—O1—Niⁱⁱ	136.26 (12)
N2—C5—H5B	109.5	S—O2—Ni	138.52 (11)
H5C—C5—H5B	109.5	Ni—O5—H1	111 (2)
N2—C5—H5A	109.5	Ni—O5—H2	100 (2)
H5C—C5—H5A	109.5	H1—O5—H2	105 (3)
H5B—C5—H5A	109.5	Ni—O6—H3	117.8 (19)
N2—C6—H6C	109.5	Ni—O6—H4	108 (2)
N2—C6—H6B	109.5	H3—O6—H4	108 (3)
H6C—C6—H6B	109.5	H5—O7—H6	95 (3)
N2—C6—H6A	109.5	O1—S—O4	110.72 (12)
H6C—C6—H6A	109.5	O1—S—O2	108.00 (10)
H6B—C6—H6A	109.5	O4—S—O2	109.83 (12)
C2—N1—C1	107.7 (2)	O1—S—O3	109.19 (12)
C2—N1—C3	110.0 (2)	O4—S—O3	109.28 (11)
C1—N1—C3	109.3 (2)	O2—S—O3	109.80 (11)

N2—C4—C3—N1	58.5 (3)	C3—N1—Ni—O5	−171.47 (18)
C4—C3—N1—C2	−158.6 (2)	C2—N1—Ni—O1ⁱ	−141.1 (2)
C4—C3—N1—C1	83.4 (2)	C1—N1—Ni—O1ⁱ	−19.51 (19)
C4—C3—N1—Ni	−37.4 (3)	C3—N1—Ni—O1ⁱ	99.30 (18)
C3—C4—N2—C6	77.5 (3)	C2—N1—Ni—O2	36.4 (2)
C3—C4—N2—C5	−165.5 (2)	C1—N1—Ni—O2	158.00 (19)
C3—C4—N2—Ni	−44.8 (2)	C3—N1—Ni—O2	−83.19 (19)
C6—N2—Ni—O6	79.76 (18)	C2—N1—Ni—N2	129.6 (2)
C4—N2—Ni—O6	−161.23 (16)	C1—N1—Ni—N2	−108.89 (19)
C5—N2—Ni—O6	−44.05 (19)	C3—N1—Ni—N2	9.93 (18)
C6—N2—Ni—O1ⁱ	168.18 (18)	O6—Ni—O2—S	0.8 (2)
C4—N2—Ni—O1ⁱ	−72.82 (15)	O5—Ni—O2—S	−92.6 (2)
C5—N2—Ni—O1ⁱ	44.37 (19)	N2—Ni—O2—S	91.5 (2)
C6—N2—Ni—O2	−9.25 (18)	N1—Ni—O2—S	176.3 (2)
C4—N2—Ni—O2	109.75 (15)	Niⁱⁱ—O1—S—O4	−18.4 (2)
C5—N2—Ni—O2	−133.06 (19)	Niⁱⁱ—O1—S—O2	−138.68 (15)
C6—N2—Ni—N1	−100.37 (18)	Niⁱⁱ—O1—S—O3	102.0 (2)
C4—N2—Ni—N1	18.63 (15)	Ni—O2—S—O1	−135.26 (17)
C5—N2—Ni—N1	135.8 (2)	Ni—O2—S—O4	103.9 (2)
C2—N1—Ni—O5	−51.8 (2)	Ni—O2—S—O3	−16.3 (2)
C1—N1—Ni—O5	69.72 (19)

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

Hydrogen-bond geometry (Å, º) top

D—H···A	D—H	H···A	D···A	D—H···A
O5—H2···O4ⁱ	0.84 (2)	1.84 (2)	2.672 (2)	171 (3)
O5—H1···O7	0.83 (2)	1.93 (2)	2.765 (3)	176 (3)
O6—H4···O3	0.83 (2)	1.89 (2)	2.687 (3)	160 (3)
O6—H3···O3ⁱⁱⁱ	0.83 (2)	2.03 (2)	2.829 (3)	162 (3)
O7—H5···O4	0.83 (2)	2.12 (2)	2.899 (3)	157 (3)
O7—H6···O3ⁱⁱⁱ	0.83 (2)	2.18 (2)	2.934 (3)	151 (3)

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

Experimental details

Crystal data
Chemical formula	[Ni(SO₄)(C₆H₁₆N₂)(H₂O)₂]·H₂O
M_r	325.03
Crystal system, space group	Orthorhombic, Pna2₁
Temperature (K)	223
a, b, c (Å)	21.108 (4), 9.9335 (19), 6.3879 (13)
V (Å³)	1339.4 (5)
Z	4
Radiation type	Mo Kα
µ (mm⁻¹)	1.63
Crystal size (mm)	0.48 × 0.11 × 0.11

Data collection
Diffractometer	Stoe IPDS diffractometer
Absorption correction	Numerical (IPDS; Stoe & Cie, 1999)
T_min, T_max	0.648, 0.841
No. of measured, independent and observed [I > 2σ(I)] reflections	10054, 2585, 2291
R_int	0.054
(sin θ/λ)_max (Å⁻¹)	0.615

Refinement
R[F² > 2σ(F²)], wR(F²), S	0.023, 0.052, 1.04
No. of reflections	2585
No. of parameters	176
No. of restraints	7
H-atom treatment	H atoms treated by a mixture of independent and constrained refinement
Δρ_max, Δρ_min (e Å⁻³)	0.37, −0.31
Absolute structure	Flack (1983), 1167 Friedel pairs
Absolute structure parameter	−0.005 (13)

Computer programs: IPDS (Stoe & Cie, 1999), SHELXS97 (Sheldrick, 2008), SHELXL97 (Sheldrick, 2008), DIAMOND (Brandenburg, 2009).

Hydrogen-bond geometry (Å, º) top

D—H···A	D—H	H···A	D···A	D—H···A
O5—H2···O4ⁱ	0.841 (18)	1.839 (19)	2.672 (2)	171 (3)
O5—H1···O7	0.834 (18)	1.933 (18)	2.765 (3)	176 (3)
O6—H4···O3	0.830 (17)	1.89 (2)	2.687 (3)	160 (3)
O6—H3···O3ⁱⁱ	0.825 (17)	2.033 (18)	2.829 (3)	162 (3)
O7—H5···O4	0.832 (18)	2.12 (2)	2.899 (3)	157 (3)
O7—H6···O3ⁱⁱ	0.829 (18)	2.18 (2)	2.934 (3)	151 (3)

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

References

Anderson, J. C., Blake, A. J., Moreno, R. B., Raynel, G. & van Slageren, J. (2009). Dalton Trans. pp. 9153–9156. Web of Science CSD CrossRef Google Scholar
Behera, J. N. & Rao, C. N. R. (2006). Chem. Asian J. 1, 742–750. Web of Science CSD CrossRef PubMed CAS Google Scholar
Brandenburg, K. (2009). DIAMOND. Crystal Impact GbR, Bonn, Germany. Google Scholar
Erer, H., Yeşilel, O. Z., Dege, N. & Alpaslan, Y. B. (2010). J. Inorg. Organomet. Polym. 20, 411–415. Web of Science CSD CrossRef CAS Google Scholar
Flack, H. D. (1983). Acta Cryst. A39, 876–881. CrossRef CAS Web of Science IUCr Journals Google Scholar
Sheldrick, G. M. (2008). Acta Cryst. A64, 112–122. Web of Science CrossRef CAS IUCr Journals Google Scholar
Stoe & Cie (1999). IPDS Program Package. Stoe & Cie, Darmstadt, Germany. Google Scholar

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