Hexaaqua­nickelate(II) bis­(thio­diacetato-κ3O,S,O′)nickel(II) tetra­hydrate

Pan, T.-T.; Su, J.-R.; Xu, D.-J.

doi:10.1107/S1600536805018982

Hexaaquanickelate(II) bis(thiodiacetato-κ³O,S,O′)nickel(II) tetrahydrate

The title compound, [Ni^II(H₂O)₆][Ni^II(C₄H₄O₄S)₂]·4H₂O, consists of [Ni^II(H₂O)₆]²⁺ complex dications, [Ni^II(C₄H₄O₄S)₂]²⁻ complex dianions and non-coordinated water molecules. In the complex dianion, two thiodiacetate dianions coordinate to the Ni^II ion in a fac-SO₂-tridentate chelating mode, resulting in a distorted octahedral trans-NiO₄S₂ coordination geometry. The crystal structure is stabilized by an extensive O—H

O hydrogen-bonding network.

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Supporting information

	Crystallographic Information File (CIF) https://doi.org/10.1107/S1600536805018982/hb6214sup1.cif Contains datablocks I, global
	Structure factor file (CIF format) https://doi.org/10.1107/S1600536805018982/hb6214Isup2.hkl Contains datablock I

CCDC reference: 277263

checkCIF report

Key indicators

Single-crystal X-ray study
T = 295 K
Mean (C-C) = 0.004 Å
Disorder in solvent or counterion
R factor = 0.021
wR factor = 0.061
Data-to-parameter ratio = 17.5

checkCIF/PLATON results

No syntax errors found



Alert level B
PLAT111_ALERT_2_B ADDSYM Detects (Pseudo) Centre of Symmetry .....         96 PerFit
PLAT111_ALERT_2_B ADDSYM Detects (Pseudo) Centre of Symmetry .....         96 PerFit

Alert level C
PLAT042_ALERT_1_C Calc. and Rep. MoietyFormula Strings Differ ....          ?
PLAT302_ALERT_4_C Anion/Solvent Disorder .........................       8.00 Perc.
PLAT417_ALERT_2_C Short Inter D-H..H-D       H1B    ..  H3B     ..       2.13 Ang.
PLAT417_ALERT_2_C Short Inter D-H..H-D       H2A    ..  H4A     ..       2.14 Ang.
PLAT720_ALERT_4_C Number of Unusual/Non-Standard Label(s) ........          2

Alert level G
REFLT03_ALERT_4_G Please check that the estimate of the number of Friedel pairs is
            correct. If it is not, please give the correct count in the
            _publ_section_exptl_refinement section of the submitted CIF.
           From the CIF: _diffrn_reflns_theta_max           27.50
           From the CIF: _reflns_number_total               4886
           Count of symmetry unique reflns         2548
           Completeness (_total/calc)            191.76%
           TEST3: Check Friedels for noncentro structure
           Estimate of Friedel pairs measured      2338
           Fraction of Friedel pairs measured     0.918
           Are heavy atom types Z>Si present        yes

   0 ALERT level A = In general: serious problem
   2 ALERT level B = Potentially serious problem
   5 ALERT level C = Check and explain
   1 ALERT level G = General alerts; check

   1 ALERT type 1 CIF construction/syntax error, inconsistent or missing data
   4 ALERT type 2 Indicator that the structure model may be wrong or deficient
   0 ALERT type 3 Indicator that the structure quality may be low
   3 ALERT type 4 Improvement, methodology, query or suggestion

Computing details top

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, 1997); molecular graphics: ORTEP-3 for Windows (Farrugia, 1997); software used to prepare material for publication: WinGX (Farrugia, 1999).

Hexaaquanickel(II) bis(thiodiacetato-κ³O,S,O')nickel(II) tetrahydrate top

Crystal data top

[Ni(H₂O)₆][Ni(C₄H₄O₄S)₂]·4H₂O	F(000) = 1232
M_r = 593.84	D_x = 1.774 Mg m⁻³
Monoclinic, Cc	Mo Kα radiation, λ = 0.71073 Å
Hall symbol: C -2yc	Cell parameters from 9212 reflections
a = 18.8369 (5) Å	θ = 1.9–27.5°
b = 13.4729 (3) Å	µ = 1.96 mm⁻¹
c = 8.9472 (2) Å	T = 295 K
β = 101.639 (8)°	Block, green
V = 2224.00 (11) Å³	0.46 × 0.40 × 0.31 mm
Z = 4

Data collection top

Rigaku R-AXIS RAPID diffractometer	4886 independent reflections
Radiation source: fine-focus sealed tube	4779 reflections with I > 2σ(I)
Graphite monochromator	R_int = 0.018
Detector resolution: 10.0 pixels mm^-1	θ_max = 27.5°, θ_min = 1.9°
ω scans	h = −24→24
Absorption correction: multi-scan (ABSCOR; Higashi, 1995)	k = −17→17
T_min = 0.408, T_max = 0.543	l = −11→11
10303 measured reflections

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)] = 0.021	H-atom parameters constrained
wR(F²) = 0.061	w = 1/[σ²(F_o²) + (0.0445P)² + 0.5706P] where P = (F_o² + 2F_c²)/3
S = 1.07	(Δ/σ)_max = 0.004
4886 reflections	Δρ_max = 0.24 e Å⁻³
280 parameters	Δρ_min = −0.52 e Å⁻³
2 restraints	Absolute structure: Flack (1983), 2338 Friedel Pairs
Primary atom site location: structure-invariant direct methods	Absolute structure parameter: 0.135 (8)

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	Occ. (<1)
Ni1	0.491615 (16)	0.239049 (19)	0.10055 (3)	0.02244 (7)
Ni2	0.235514 (16)	0.194970 (19)	0.35362 (3)	0.02473 (7)
S1	0.47671 (3)	0.07430 (4)	0.19731 (6)	0.02698 (11)
S2	0.50126 (3)	0.40259 (4)	−0.00355 (6)	0.02577 (11)
O1	0.57489 (10)	0.17600 (13)	0.0206 (2)	0.0346 (4)
O2	0.63325 (11)	0.04398 (14)	−0.0376 (3)	0.0428 (4)
O3	0.42167 (10)	0.18858 (12)	−0.08625 (19)	0.0336 (4)
O4	0.33469 (10)	0.08514 (13)	−0.1925 (2)	0.0335 (4)
O5	0.40915 (10)	0.29921 (13)	0.1875 (2)	0.0356 (4)
O6	0.33747 (14)	0.42673 (17)	0.2120 (3)	0.0656 (8)
O7	0.56421 (10)	0.29103 (12)	0.28429 (19)	0.0317 (4)
O8	0.63729 (10)	0.41001 (14)	0.3946 (2)	0.0363 (4)
O11	0.12579 (9)	0.19655 (13)	0.3310 (2)	0.0337 (4)
H11A	0.0983	0.2115	0.2326	0.050*
H11B	0.1076	0.2353	0.4011	0.050*
O12	0.34692 (9)	0.19063 (12)	0.3851 (2)	0.0311 (4)
H12A	0.3625	0.2282	0.3149	0.050*
H12B	0.3779	0.2112	0.4654	0.050*
O13	0.23120 (11)	0.19806 (14)	0.1210 (2)	0.0375 (4)
H13A	0.2269	0.2537	0.0805	0.050*
H13B	0.2046	0.1636	0.0595	0.050*
O14	0.24000 (10)	0.19638 (13)	0.5889 (2)	0.0355 (4)
H14A	0.2699	0.1557	0.6454	0.050*
H14B	0.2511	0.2556	0.6301	0.050*
O15	0.24030 (14)	0.34690 (13)	0.3615 (3)	0.0502 (5)
H15A	0.2690	0.3849	0.3238	0.050*
H15B	0.2077	0.3880	0.3793	0.050*
O16	0.23399 (11)	0.04640 (12)	0.3492 (4)	0.0482 (5)
H16A	0.2690	0.0047	0.3406	0.050*
H16B	0.2023	0.0050	0.3658	0.050*
O1W	0.67651 (13)	0.14693 (16)	0.4203 (3)	0.0528 (5)
H1A	0.6317	0.1486	0.3948	0.050*
H1B	0.6925	0.0922	0.4794	0.050*
O2W	0.40052 (10)	0.29162 (17)	0.6510 (2)	0.0433 (4)
H2A	0.4155	0.2551	0.7331	0.050*
H2B	0.3631	0.3138	0.6693	0.050*
O3W	0.27803 (16)	0.38074 (19)	0.7383 (3)	0.0699 (7)
H3A	0.2836	0.4336	0.6977	0.050*
H3B	0.2524	0.3942	0.8022	0.050*
O4WA	0.0346 (2)	0.2552 (4)	0.0699 (4)	0.0514 (9)	0.64
O4WB	0.0302 (4)	0.1881 (8)	0.0778 (7)	0.059 (2)	0.36
C1	0.58695 (13)	0.08436 (18)	0.0229 (3)	0.0288 (4)
C2	0.54453 (14)	0.01582 (18)	0.1093 (3)	0.0336 (5)
H2C	0.5789	−0.0180	0.1883	0.040*
H2D	0.5208	−0.0344	0.0389	0.040*
C3	0.39369 (14)	0.05031 (19)	0.0615 (3)	0.0336 (5)
H3C	0.3927	−0.0192	0.0332	0.040*
H3D	0.3532	0.0619	0.1113	0.040*
C4	0.38259 (12)	0.11249 (17)	−0.0834 (3)	0.0266 (4)
C5	0.38803 (14)	0.38820 (19)	0.1623 (3)	0.0343 (5)
C6	0.42529 (15)	0.4543 (2)	0.0657 (4)	0.0410 (6)
H6A	0.4421	0.5132	0.1248	0.049*
H6B	0.3894	0.4756	−0.0220	0.049*
C7	0.57839 (15)	0.4381 (2)	0.1390 (3)	0.0371 (6)
H7A	0.6209	0.4359	0.0933	0.045*
H7B	0.5718	0.5065	0.1673	0.045*
C8	0.59400 (11)	0.37589 (16)	0.2848 (3)	0.0260 (4)
H4A	−0.0132	0.2299	0.0766	0.050*
H4B	0.0430	0.2224	−0.0039	0.050*

Atomic displacement parameters (Å²) top

	U¹¹	U²²	U³³	U¹²	U¹³	U²³
Ni1	0.02538 (11)	0.02138 (13)	0.02099 (11)	−0.00519 (11)	0.00569 (8)	−0.00098 (10)
Ni2	0.02300 (11)	0.02334 (13)	0.02821 (12)	0.00013 (11)	0.00604 (9)	−0.00001 (11)
S1	0.0319 (3)	0.0286 (2)	0.0204 (2)	−0.0056 (2)	0.0050 (2)	0.00309 (19)
S2	0.0275 (2)	0.0274 (2)	0.0228 (2)	−0.0044 (2)	0.00617 (19)	0.00221 (19)
O1	0.0388 (9)	0.0278 (8)	0.0425 (9)	−0.0005 (7)	0.0209 (7)	0.0031 (7)
O2	0.0429 (10)	0.0332 (9)	0.0586 (12)	−0.0009 (8)	0.0250 (9)	−0.0042 (8)
O3	0.0421 (9)	0.0317 (8)	0.0242 (8)	−0.0141 (7)	0.0003 (7)	0.0046 (6)
O4	0.0347 (8)	0.0313 (8)	0.0304 (9)	−0.0085 (7)	−0.0032 (7)	0.0001 (7)
O5	0.0379 (9)	0.0297 (8)	0.0452 (10)	−0.0009 (7)	0.0231 (8)	0.0060 (7)
O6	0.0678 (15)	0.0416 (11)	0.107 (2)	0.0098 (10)	0.0636 (16)	0.0104 (12)
O7	0.0392 (9)	0.0268 (7)	0.0272 (8)	−0.0115 (7)	0.0021 (7)	0.0029 (6)
O8	0.0389 (9)	0.0348 (9)	0.0313 (9)	−0.0137 (7)	−0.0017 (7)	0.0003 (7)
O11	0.0252 (8)	0.0393 (10)	0.0371 (10)	0.0050 (6)	0.0073 (7)	−0.0038 (7)
O12	0.0248 (8)	0.0345 (9)	0.0339 (9)	−0.0037 (6)	0.0055 (7)	0.0020 (6)
O13	0.0436 (10)	0.0382 (10)	0.0294 (9)	−0.0001 (8)	0.0043 (8)	−0.0009 (7)
O14	0.0372 (9)	0.0406 (10)	0.0280 (9)	0.0004 (7)	0.0050 (7)	0.0034 (7)
O15	0.0592 (11)	0.0236 (8)	0.0800 (13)	0.0015 (9)	0.0430 (10)	0.0009 (10)
O16	0.0290 (7)	0.0193 (7)	0.1001 (14)	−0.0011 (8)	0.0220 (8)	−0.0001 (10)
O1W	0.0522 (12)	0.0393 (11)	0.0641 (14)	−0.0011 (9)	0.0050 (10)	0.0035 (9)
O2W	0.0416 (10)	0.0575 (12)	0.0301 (9)	−0.0051 (9)	0.0056 (8)	0.0097 (8)
O3W	0.095 (2)	0.0489 (13)	0.0726 (17)	0.0076 (13)	0.0335 (15)	−0.0114 (12)
O4WA	0.0427 (18)	0.078 (3)	0.0338 (17)	0.004 (2)	0.0082 (13)	−0.0131 (19)
O4WB	0.036 (3)	0.110 (7)	0.029 (3)	0.014 (4)	0.006 (2)	−0.001 (4)
C1	0.0304 (10)	0.0281 (10)	0.0275 (11)	−0.0038 (9)	0.0048 (9)	−0.0028 (8)
C2	0.0424 (13)	0.0254 (11)	0.0344 (12)	−0.0007 (9)	0.0114 (10)	0.0022 (9)
C3	0.0327 (11)	0.0341 (12)	0.0305 (12)	−0.0126 (10)	−0.0020 (9)	0.0068 (9)
C4	0.0282 (10)	0.0255 (10)	0.0264 (11)	−0.0029 (8)	0.0065 (9)	0.0016 (8)
C5	0.0332 (12)	0.0318 (12)	0.0423 (14)	−0.0005 (10)	0.0178 (11)	0.0005 (10)
C6	0.0393 (13)	0.0318 (12)	0.0573 (17)	0.0054 (11)	0.0226 (12)	0.0117 (12)
C7	0.0390 (13)	0.0324 (12)	0.0370 (13)	−0.0153 (10)	0.0007 (11)	0.0065 (10)
C8	0.0249 (10)	0.0275 (10)	0.0251 (10)	−0.0041 (8)	0.0041 (8)	−0.0010 (8)

Geometric parameters (Å, º) top

Ni1—O1	2.0365 (18)	O14—H14A	0.8710
Ni1—O3	2.0257 (17)	O14—H14B	0.8864
Ni1—O5	2.0404 (18)	O15—H15A	0.8603
Ni1—O7	2.0386 (17)	O15—H15B	0.8656
Ni1—S1	2.4194 (6)	O16—H16A	0.8813
Ni1—S2	2.4132 (6)	O16—H16B	0.8519
Ni2—O11	2.0359 (17)	O1W—H1A	0.8281
Ni2—O12	2.0611 (16)	O1W—H1B	0.9221
Ni2—O13	2.0664 (19)	O2W—H2A	0.8817
Ni2—O14	2.0899 (18)	O2W—H2B	0.8123
Ni2—O15	2.0495 (18)	O3W—H3A	0.8160
Ni2—O16	2.0022 (16)	O3W—H3B	0.8385
S1—C3	1.805 (2)	O4WA—O4WB	0.912 (9)
S1—C2	1.811 (3)	O4WA—H4A	0.976 (4)
S2—C7	1.794 (3)	O4WA—H4B	0.836 (4)
S2—C6	1.809 (3)	O4WB—H4A	0.991 (7)
O1—C1	1.255 (3)	O4WB—H4B	0.937 (8)
O2—C1	1.241 (3)	C1—C2	1.529 (3)
O3—C4	1.265 (3)	C2—H2C	0.9700
O4—C4	1.244 (3)	C2—H2D	0.9700
O5—C5	1.269 (3)	C3—C4	1.522 (3)
O6—C5	1.243 (3)	C3—H3C	0.9700
O7—C8	1.273 (3)	C3—H3D	0.9700
O8—C8	1.232 (3)	C5—C6	1.509 (3)
O11—H11A	0.9491	C6—H6A	0.9700
O11—H11B	0.9319	C6—H6B	0.9700
O12—H12A	0.9004	C7—C8	1.528 (3)
O12—H12B	0.8738	C7—H7A	0.9700
O13—H13A	0.8302	C7—H7B	0.9700
O13—H13B	0.8114

O1—Ni1—O3	89.37 (8)	Ni2—O15—H15A	127.4
O1—Ni1—O5	177.97 (9)	Ni2—O15—H15B	128.1
O1—Ni1—O7	89.30 (8)	H15A—O15—H15B	102.6
O1—Ni1—S1	84.05 (5)	Ni2—O16—H16A	129.1
O1—Ni1—S2	97.00 (5)	Ni2—O16—H16B	131.2
O3—Ni1—O5	91.69 (8)	H16A—O16—H16B	99.3
O3—Ni1—O7	178.21 (8)	H1A—O1W—H1B	112.0
O3—Ni1—S1	83.35 (5)	H2A—O2W—H2B	100.5
O3—Ni1—S2	94.31 (5)	H3A—O3W—H3B	105.0
O5—Ni1—O7	89.68 (8)	O4WB—O4WA—H4A	63.2 (6)
O5—Ni1—S1	94.35 (5)	O4WB—O4WA—H4B	64.7 (5)
O5—Ni1—S2	84.65 (5)	H4A—O4WA—H4B	100.8 (4)
O7—Ni1—S1	97.70 (5)	O4WA—O4WB—H4A	61.6 (7)
O7—Ni1—S2	84.67 (5)	O4WA—O4WB—H4B	53.7 (6)
S1—Ni1—S2	177.43 (2)	H4A—O4WB—H4B	93.0 (7)
O11—Ni2—O12	177.65 (8)	O2—C1—O1	124.4 (2)
O11—Ni2—O15	91.70 (9)	O2—C1—C2	116.1 (2)
O11—Ni2—O16	89.90 (8)	O1—C1—C2	119.4 (2)
O11—Ni2—O13	93.85 (8)	C1—C2—S1	116.34 (17)
O11—Ni2—O14	86.20 (8)	C1—C2—H2C	108.2
O12—Ni2—O13	88.29 (8)	S1—C2—H2C	108.2
O12—Ni2—O14	91.69 (7)	C1—C2—H2D	108.2
O12—Ni2—O15	89.26 (9)	S1—C2—H2D	108.2
O12—Ni2—O16	89.12 (8)	H2C—C2—H2D	107.4
O13—Ni2—O14	178.32 (7)	C4—C3—S1	115.22 (16)
O13—Ni2—O15	90.39 (10)	C4—C3—H3C	108.5
O13—Ni2—O16	90.17 (10)	S1—C3—H3C	108.5
O14—Ni2—O15	87.93 (9)	C4—C3—H3D	108.5
O14—Ni2—O16	91.51 (10)	S1—C3—H3D	108.5
O15—Ni2—O16	178.26 (11)	H3C—C3—H3D	107.5
C3—S1—C2	102.75 (13)	O4—C4—O3	123.9 (2)
C3—S1—Ni1	94.06 (8)	O4—C4—C3	117.3 (2)
C2—S1—Ni1	95.77 (8)	O3—C4—C3	118.9 (2)
C7—S2—C6	103.71 (15)	O6—C5—O5	124.5 (2)
C7—S2—Ni1	94.71 (9)	O6—C5—C6	115.9 (2)
C6—S2—Ni1	95.34 (8)	O5—C5—C6	119.6 (2)
C1—O1—Ni1	123.67 (16)	C5—C6—S2	117.40 (19)
C4—O3—Ni1	122.66 (15)	C5—C6—H6A	108.0
C5—O5—Ni1	122.89 (16)	S2—C6—H6A	108.0
C8—O7—Ni1	122.35 (15)	C5—C6—H6B	108.0
Ni2—O11—H11A	116.6	S2—C6—H6B	108.0
Ni2—O11—H11B	116.3	H6A—C6—H6B	107.2
H11A—O11—H11B	107.5	C8—C7—S2	116.72 (16)
Ni2—O12—H12A	110.7	C8—C7—H7A	108.1
Ni2—O12—H12B	126.5	S2—C7—H7A	108.1
H12A—O12—H12B	98.0	C8—C7—H7B	108.1
Ni2—O13—H13A	116.0	S2—C7—H7B	108.1
Ni2—O13—H13B	124.4	H7A—C7—H7B	107.3
H13A—O13—H13B	103.1	O8—C8—O7	123.9 (2)
Ni2—O14—H14A	118.0	O8—C8—C7	117.3 (2)
Ni2—O14—H14B	112.7	O7—C8—C7	118.7 (2)
H14A—O14—H14B	104.7

Hydrogen-bond geometry (Å, º) top

D—H···A	D—H	H···A	D···A	D—H···A
O1W—H1A···O7	0.83	2.40	2.947 (3)	124
O1W—H1B···O2ⁱ	0.92	2.14	2.747 (3)	123
O2W—H2A···O3ⁱⁱ	0.88	1.83	2.690 (3)	164
O2W—H2B···O3W	0.81	2.04	2.847 (4)	172
O3W—H3A···O6ⁱⁱⁱ	0.82	2.13	2.854 (4)	148
O3W—H3B···O1W^iv	0.84	2.02	2.774 (4)	150
O4WA—H4A···O2W^v	0.98	1.90	2.836 (4)	160
O4WA—H4B···O7^v	0.84	2.02	2.795 (4)	153
O11—H11A···O4WA	0.95	1.79	2.722 (4)	167
O11—H11B···O1^iv	0.93	1.79	2.721 (3)	172
O12—H12A···O5	0.90	1.84	2.734 (2)	171
O12—H12B···O2W	0.87	1.96	2.750 (3)	150
O13—H13A···O1W^v	0.83	2.05	2.811 (3)	152
O13—H13B···O8^v	0.81	2.00	2.812 (3)	175
O14—H14A···O4ⁱⁱ	0.87	1.94	2.801 (3)	167
O14—H14B···O3W	0.89	1.96	2.843 (3)	175
O15—H15A···O6	0.86	1.87	2.699 (4)	161
O15—H15B···O2^iv	0.87	1.94	2.789 (3)	165
O16—H16A···O4ⁱ	0.88	1.80	2.677 (3)	175
O16—H16B···O8^vi	0.85	1.83	2.675 (3)	176

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

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Hexaaqua­nickelate(II) bis­(thio­diacetato-κ3O,S,O′)nickel(II) tetra­hydrate

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Key indicators

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Hexaaquanickelate(II) bis(thiodiacetato-κ³O,S,O′)nickel(II) tetrahydrate