Hexaaqua­nickel(II) bis­[(4-nitro­phenyl­sulfan­yl)acetate]

In the title compound, [Ni(H₂O)₆](C₈H₆NO₄S)₂, the Ni^II atom lies on an inversion center and is six-coordinated in an octa­hedral environment. Cations and anions are linked by O—H...O hydrogen bonds into a three-dimensional network.

Key indicators

• Single-crystal X-ray study
• T = 291 K
• Mean [sigma](C-C) = 0.004 Å
• R factor = 0.032
• wR factor = 0.116
• Data-to-parameter ratio = 16.5

checkCIF/PLATON results

No syntax errors found



Alert level B
PLAT420_ALERT_2_B D-H Without Acceptor       O7     -   H71    ...          ?

Alert level C
PLAT042_ALERT_1_C Calc. and Rep. MoietyFormula Strings Differ ....          ?

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

   1 ALERT type 1 CIF construction/syntax error, inconsistent or missing data
   1 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
   0 ALERT type 4 Improvement, methodology, query or suggestion
   0 ALERT type 5 Informative message, check

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Computing details

Data collection: RAPID-AUTO (Rigaku, 1998); cell refinement: RAPID-AUTO; data reduction: CrystalStructure (Rigaku/MSC, 2002); program(s) used to solve structure: SHELXS97 (Sheldrick, 1997); program(s) used to refine structure: SHELXL97 (Sheldrick, 1997); molecular graphics: SHELXTL (Bruker, 1997); software used to prepare material for publication: SHELXL97.

Hexaaquanicklel(II) bis[(4-nitrophenylsulfanyl)acetate]

Crystal data

[Ni(H2O)6](C8H6NO4S)2	Z = 1
Mr = 591.20	F(000) = 306
Triclinic, P1	Dx = 1.693 Mg m^−3
Hall symbol: -P 1	Mo Kα radiation, λ = 0.71073 Å
a = 7.365 (6) Å	Cell parameters from 4871 reflections
b = 7.368 (7) Å	θ = 6.0–55.1°
c = 11.755 (10) Å	µ = 1.09 mm^−1
α = 98.33 (3)°	T = 291 K
β = 99.61 (3)°	Block, yellow
γ = 109.29 (3)°	0.48 × 0.18 × 0.07 mm
V = 579.8 (9) Å^3

Data collection

Rigaku R-AXIS RAPID diffractometer	2634 independent reflections
Radiation source: fine-focus sealed tube	2208 reflections with I > 2σ(I)
Graphite monochromator	Rint = 0.021
ω scans	θmax = 27.5°, θmin = 3.0°
Absorption correction: multi-scan (ABSCOR; Higashi, 1995)	h = −8→9
Tmin = 0.625, Tmax = 0.925	k = −9→9
5748 measured reflections	l = −15→15

Refinement

Refinement on F^2	Primary atom site location: structure-invariant direct methods
Least-squares matrix: full	Secondary atom site location: difference Fourier map
R[F^2 > 2σ(F^2)] = 0.032	Hydrogen site location: inferred from neighbouring sites
wR(F^2) = 0.116	H-atom parameters constrained
S = 1.16	w = 1/[σ^2(Fo^2) + (0.065P)^2 + 0.196P] where P = (Fo^2 + 2Fc^2)/3
2634 reflections	(Δ/σ)max < 0.001
160 parameters	Δρmax = 0.47 e Å^−3
0 restraints	Δρmin = −0.44 e Å^−3

Special details

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 (Ų)

	x	y	z	Uiso*/Ueq
Ni1	1.0000	0.5000	0.5000	0.02290 (15)
O6	0.8719 (3)	0.2515 (3)	0.55782 (17)	0.0322 (4)
H61	0.9417	0.2344	0.6181	0.048*
H62	0.8071	0.1391	0.5112	0.048*
O5	0.8554 (3)	0.6380 (3)	0.59702 (16)	0.0290 (4)
H51	0.8166	0.7201	0.5648	0.044*
H52	0.7575	0.5590	0.6160	0.044*
O7	0.7636 (3)	0.4093 (3)	0.35363 (17)	0.0325 (4)
H71	0.7567	0.3629	0.2813	0.049*
H72	0.6826	0.4685	0.3575	0.049*
S1	0.32407 (11)	−0.27518 (10)	0.17512 (6)	0.03321 (19)
O3	0.0692 (4)	0.1335 (4)	−0.25650 (19)	0.0567 (7)
O4	0.2331 (4)	0.4010 (4)	−0.1270 (2)	0.0497 (6)
O1	0.4994 (3)	−0.4139 (3)	0.35430 (18)	0.0333 (4)
O2	0.7057 (3)	−0.1326 (3)	0.47445 (18)	0.0410 (5)
N1	0.1688 (4)	0.2216 (4)	−0.1571 (2)	0.0345 (5)
C4	0.2101 (4)	0.1056 (4)	−0.0730 (2)	0.0284 (5)
C2	0.3633 (4)	0.0890 (4)	0.1177 (2)	0.0326 (6)
H2	0.4412	0.1510	0.1932	0.039*
C1	0.2845 (4)	−0.1153 (4)	0.0853 (2)	0.0273 (5)
C6	0.1645 (4)	−0.2063 (4)	−0.0278 (2)	0.0313 (6)
H6	0.1089	−0.3430	−0.0492	0.038*
C3	0.3264 (4)	0.2005 (4)	0.0380 (3)	0.0323 (6)
H3	0.3792	0.3373	0.0591	0.039*
C7	0.4946 (4)	−0.1102 (4)	0.3075 (2)	0.0283 (5)
H7A	0.6039	−0.0151	0.2867	0.034*
H7B	0.4281	−0.0391	0.3501	0.034*
C5	0.1274 (4)	−0.0972 (4)	−0.1078 (2)	0.0304 (6)
H5	0.0489	−0.1580	−0.1833	0.036*
C8	0.5716 (4)	−0.2293 (4)	0.3848 (2)	0.0273 (5)

Atomic displacement parameters (Ų)

	U^11	U^22	U^33	U^12	U^13	U^23
Ni1	0.0239 (2)	0.0192 (2)	0.0248 (2)	0.00804 (18)	0.00066 (18)	0.00755 (17)
O6	0.0385 (11)	0.0237 (9)	0.0309 (9)	0.0078 (8)	0.0004 (8)	0.0118 (7)
O5	0.0311 (9)	0.0256 (9)	0.0325 (9)	0.0128 (8)	0.0041 (8)	0.0105 (7)
O7	0.0318 (10)	0.0318 (10)	0.0306 (9)	0.0137 (8)	−0.0032 (8)	0.0030 (8)
S1	0.0383 (4)	0.0274 (4)	0.0318 (3)	0.0121 (3)	−0.0013 (3)	0.0102 (3)
O3	0.086 (2)	0.0572 (16)	0.0310 (11)	0.0356 (15)	−0.0015 (12)	0.0156 (11)
O4	0.0646 (16)	0.0403 (13)	0.0523 (13)	0.0258 (12)	0.0108 (12)	0.0219 (11)
O1	0.0312 (10)	0.0255 (10)	0.0420 (11)	0.0106 (8)	0.0022 (9)	0.0106 (8)
O2	0.0498 (13)	0.0268 (10)	0.0370 (11)	0.0105 (9)	−0.0091 (10)	0.0087 (8)
N1	0.0393 (13)	0.0439 (15)	0.0333 (12)	0.0264 (12)	0.0119 (11)	0.0174 (11)
C4	0.0289 (13)	0.0343 (14)	0.0310 (13)	0.0179 (11)	0.0104 (11)	0.0148 (11)
C2	0.0299 (13)	0.0321 (15)	0.0307 (13)	0.0098 (11)	−0.0031 (11)	0.0062 (11)
C1	0.0243 (12)	0.0341 (14)	0.0284 (12)	0.0147 (11)	0.0055 (10)	0.0120 (11)
C6	0.0336 (14)	0.0269 (13)	0.0319 (13)	0.0117 (11)	0.0040 (11)	0.0039 (11)
C3	0.0304 (13)	0.0285 (14)	0.0377 (14)	0.0120 (11)	0.0015 (12)	0.0103 (11)
C7	0.0290 (13)	0.0283 (13)	0.0288 (12)	0.0130 (11)	0.0019 (11)	0.0092 (10)
C5	0.0324 (13)	0.0360 (15)	0.0240 (12)	0.0167 (12)	0.0023 (11)	0.0051 (11)
C8	0.0284 (13)	0.0273 (13)	0.0309 (13)	0.0130 (11)	0.0071 (11)	0.0131 (10)

Geometric parameters (Å, º)

Ni1—O6	2.034 (2)	O1—C8	1.256 (3)
Ni1—O6^i	2.034 (2)	O2—C8	1.250 (3)
Ni1—O5^i	2.062 (2)	N1—C4	1.455 (3)
Ni1—O5	2.062 (2)	C4—C3	1.375 (4)
Ni1—O7	2.082 (2)	C4—C5	1.382 (4)
Ni1—O7^i	2.082 (2)	C2—C3	1.383 (4)
O6—H61	0.8540	C2—C1	1.389 (4)
O6—H62	0.8567	C2—H2	0.9300
O5—H51	0.8576	C1—C6	1.399 (4)
O5—H52	0.8500	C6—C5	1.372 (4)
O7—H71	0.8557	C6—H6	0.9300
O7—H72	0.8506	C3—H3	0.9300
S1—C1	1.752 (3)	C7—C8	1.518 (4)
S1—C7	1.807 (3)	C7—H7A	0.9700
O3—N1	1.227 (4)	C7—H7B	0.9700
O4—N1	1.221 (4)	C5—H5	0.9300
O6—Ni1—O6^i	180.0	C3—C4—C5	122.5 (3)
O6—Ni1—O5^i	91.28 (10)	C3—C4—N1	119.3 (3)
O6^i—Ni1—O5^i	88.72 (10)	C5—C4—N1	118.2 (3)
O6—Ni1—O5	88.72 (10)	C3—C2—C1	120.2 (3)
O6^i—Ni1—O5	91.28 (10)	C3—C2—H2	119.9
O5^i—Ni1—O5	180.00 (9)	C1—C2—H2	119.9
O6—Ni1—O7	90.38 (9)	C2—C1—C6	119.2 (2)
O6^i—Ni1—O7	89.62 (9)	C2—C1—S1	125.3 (2)
O5^i—Ni1—O7	89.35 (10)	C6—C1—S1	115.5 (2)
O5—Ni1—O7	90.65 (10)	C5—C6—C1	121.1 (3)
O6—Ni1—O7^i	89.62 (9)	C5—C6—H6	119.5
O6^i—Ni1—O7^i	90.38 (9)	C1—C6—H6	119.5
O5^i—Ni1—O7^i	90.65 (10)	C4—C3—C2	118.8 (3)
O5—Ni1—O7^i	89.35 (10)	C4—C3—H3	120.6
O7—Ni1—O7^i	180.000 (1)	C2—C3—H3	120.6
Ni1—O6—H61	115.7	C8—C7—S1	109.07 (19)
Ni1—O6—H62	123.1	C8—C7—H7A	109.9
H61—O6—H62	108.3	S1—C7—H7A	109.9
Ni1—O5—H51	114.7	C8—C7—H7B	109.9
Ni1—O5—H52	113.8	S1—C7—H7B	109.9
H51—O5—H52	108.2	H7A—C7—H7B	108.3
Ni1—O7—H71	129.9	C6—C5—C4	118.1 (3)
Ni1—O7—H72	114.8	C6—C5—H5	121.0
H71—O7—H72	109.7	C4—C5—H5	121.0
C1—S1—C7	103.34 (14)	O2—C8—O1	125.2 (2)
O4—N1—O3	122.5 (3)	O2—C8—C7	116.1 (2)
O4—N1—C4	119.6 (2)	O1—C8—C7	118.6 (2)
O3—N1—C4	118.0 (3)
C1—S1—C7—C8	−169.76 (17)

Symmetry code: (i) −x+2, −y+1, −z+1.

Hydrogen-bond geometry (Å, º)

D—H···A	D—H	H···A	D···A	D—H···A
O6—H61···O3^ii	0.85	1.98	2.821 (3)	168
O6—H62···O2	0.86	1.85	2.641 (4)	154
O5—H51···O2^iii	0.86	1.90	2.749 (3)	171
O5—H52···O1^iv	0.85	1.96	2.794 (3)	167
O7—H72···O1^iii	0.85	1.83	2.676 (3)	176

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