catena-Poly[[[diaqua-(tetra-methyl-ethylenediamine-κ(2) N,N')nickel(II)]-μ-sulfato-κ(2) O:O'] monohydrate].

The title compound, {[Ni(SO4)(C6H16N2)(H2O)2]·H2O} n , contains a Ni(II) atom that is coordinated nearly octa-hedrally by a chelating tetra-ethyl-enediamine (tmeda) ligand, two water mol-ecules 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 octa-hedra and SO4 tetra-hedra parallel to [001]. The polymeric chains are linked by O-H⋯O hydrogen bonds between coordinating water mol-ecules and sulfate anions to give double strands. There is a lattice water mol-ecule 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 = 325.03

Orthorhombic,

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[F 2 > 2σ(F 2)] = 0.023

wR(F 2) = 0.052

S = 1.04

2585 reflections

176 parameters

7 restraints

H atoms treated by a mixture of independent and constrained refinement

Δρmax = 0.37 e Å−3

Δρmin = −0.31 e Å−3

Absolute structure: Flack (1983 ▶), 1167 Friedel pairs

Flack parameter: −0.005 (13)

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.

Click here for additional data file.

Crystal structure: contains datablock(s) I, global. DOI: 10.1107/S1600536813006557/wm2722sup1.cif

Click here for additional data file.

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

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

[Ni(SO4)(C6H16N2)(H2O)2]·H2O	F(000) = 688
Mr = 325.03	Dx = 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

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

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(Fo2) + (0.0286P)2] where P = (Fo2 + 2Fc2)/3
S = 1.04	(Δ/σ)max = 0.001
2585 reflections	Δρmax = 0.37 e Å−3
176 parameters	Δρmin = −0.31 e Å−3
7 restraints	Absolute structure: Flack (1983), 1167 Friedel pairs
Primary atom site location: structure-invariant direct methods	Flack parameter: −0.005 (13)

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
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)

	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)

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)

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)

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) ; (ii) .