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In the title compound, [Ni(H2O)6](C8H6NO4S)2, the NiII 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.

Supporting information

cif

Crystallographic Information File (CIF) https://doi.org/10.1107/S1600536806049725/dn2089sup1.cif
Contains datablocks global, I

hkl

Structure factor file (CIF format) https://doi.org/10.1107/S1600536806049725/dn2089Isup2.hkl
Contains datablock I

CCDC reference: 629648

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

Computing details top

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] top
Crystal data top
[Ni(H2O)6](C8H6NO4S)2Z = 1
Mr = 591.20F(000) = 306
Triclinic, P1Dx = 1.693 Mg m3
Hall symbol: -P 1Mo Kα radiation, λ = 0.71073 Å
a = 7.365 (6) ÅCell parameters from 4871 reflections
b = 7.368 (7) Åθ = 6.0–55.1°
c = 11.755 (10) ŵ = 1.09 mm1
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) Å3
Data collection top
Rigaku R-AXIS RAPID
diffractometer
2634 independent reflections
Radiation source: fine-focus sealed tube2208 reflections with I > 2σ(I)
Graphite monochromatorRint = 0.021
ω scansθmax = 27.5°, θmin = 3.0°
Absorption correction: multi-scan
(ABSCOR; Higashi, 1995)
h = 89
Tmin = 0.625, Tmax = 0.925k = 99
5748 measured reflectionsl = 1515
Refinement top
Refinement on F2Primary atom site location: structure-invariant direct methods
Least-squares matrix: fullSecondary atom site location: difference Fourier map
R[F2 > 2σ(F2)] = 0.032Hydrogen site location: inferred from neighbouring sites
wR(F2) = 0.116H-atom parameters constrained
S = 1.16 w = 1/[σ2(Fo2) + (0.065P)2 + 0.196P]
where P = (Fo2 + 2Fc2)/3
2634 reflections(Δ/σ)max < 0.001
160 parametersΔρmax = 0.47 e Å3
0 restraintsΔρmin = 0.44 e Å3
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
xyzUiso*/Ueq
Ni11.00000.50000.50000.02290 (15)
O60.8719 (3)0.2515 (3)0.55782 (17)0.0322 (4)
H610.94170.23440.61810.048*
H620.80710.13910.51120.048*
O50.8554 (3)0.6380 (3)0.59702 (16)0.0290 (4)
H510.81660.72010.56480.044*
H520.75750.55900.61600.044*
O70.7636 (3)0.4093 (3)0.35363 (17)0.0325 (4)
H710.75670.36290.28130.049*
H720.68260.46850.35750.049*
S10.32407 (11)0.27518 (10)0.17512 (6)0.03321 (19)
O30.0692 (4)0.1335 (4)0.25650 (19)0.0567 (7)
O40.2331 (4)0.4010 (4)0.1270 (2)0.0497 (6)
O10.4994 (3)0.4139 (3)0.35430 (18)0.0333 (4)
O20.7057 (3)0.1326 (3)0.47445 (18)0.0410 (5)
N10.1688 (4)0.2216 (4)0.1571 (2)0.0345 (5)
C40.2101 (4)0.1056 (4)0.0730 (2)0.0284 (5)
C20.3633 (4)0.0890 (4)0.1177 (2)0.0326 (6)
H20.44120.15100.19320.039*
C10.2845 (4)0.1153 (4)0.0853 (2)0.0273 (5)
C60.1645 (4)0.2063 (4)0.0278 (2)0.0313 (6)
H60.10890.34300.04920.038*
C30.3264 (4)0.2005 (4)0.0380 (3)0.0323 (6)
H30.37920.33730.05910.039*
C70.4946 (4)0.1102 (4)0.3075 (2)0.0283 (5)
H7A0.60390.01510.28670.034*
H7B0.42810.03910.35010.034*
C50.1274 (4)0.0972 (4)0.1078 (2)0.0304 (6)
H50.04890.15800.18330.036*
C80.5716 (4)0.2293 (4)0.3848 (2)0.0273 (5)
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
Ni10.0239 (2)0.0192 (2)0.0248 (2)0.00804 (18)0.00066 (18)0.00755 (17)
O60.0385 (11)0.0237 (9)0.0309 (9)0.0078 (8)0.0004 (8)0.0118 (7)
O50.0311 (9)0.0256 (9)0.0325 (9)0.0128 (8)0.0041 (8)0.0105 (7)
O70.0318 (10)0.0318 (10)0.0306 (9)0.0137 (8)0.0032 (8)0.0030 (8)
S10.0383 (4)0.0274 (4)0.0318 (3)0.0121 (3)0.0013 (3)0.0102 (3)
O30.086 (2)0.0572 (16)0.0310 (11)0.0356 (15)0.0015 (12)0.0156 (11)
O40.0646 (16)0.0403 (13)0.0523 (13)0.0258 (12)0.0108 (12)0.0219 (11)
O10.0312 (10)0.0255 (10)0.0420 (11)0.0106 (8)0.0022 (9)0.0106 (8)
O20.0498 (13)0.0268 (10)0.0370 (11)0.0105 (9)0.0091 (10)0.0087 (8)
N10.0393 (13)0.0439 (15)0.0333 (12)0.0264 (12)0.0119 (11)0.0174 (11)
C40.0289 (13)0.0343 (14)0.0310 (13)0.0179 (11)0.0104 (11)0.0148 (11)
C20.0299 (13)0.0321 (15)0.0307 (13)0.0098 (11)0.0031 (11)0.0062 (11)
C10.0243 (12)0.0341 (14)0.0284 (12)0.0147 (11)0.0055 (10)0.0120 (11)
C60.0336 (14)0.0269 (13)0.0319 (13)0.0117 (11)0.0040 (11)0.0039 (11)
C30.0304 (13)0.0285 (14)0.0377 (14)0.0120 (11)0.0015 (12)0.0103 (11)
C70.0290 (13)0.0283 (13)0.0288 (12)0.0130 (11)0.0019 (11)0.0092 (10)
C50.0324 (13)0.0360 (15)0.0240 (12)0.0167 (12)0.0023 (11)0.0051 (11)
C80.0284 (13)0.0273 (13)0.0309 (13)0.0130 (11)0.0071 (11)0.0131 (10)
Geometric parameters (Å, º) top
Ni1—O62.034 (2)O1—C81.256 (3)
Ni1—O6i2.034 (2)O2—C81.250 (3)
Ni1—O5i2.062 (2)N1—C41.455 (3)
Ni1—O52.062 (2)C4—C31.375 (4)
Ni1—O72.082 (2)C4—C51.382 (4)
Ni1—O7i2.082 (2)C2—C31.383 (4)
O6—H610.8540C2—C11.389 (4)
O6—H620.8567C2—H20.9300
O5—H510.8576C1—C61.399 (4)
O5—H520.8500C6—C51.372 (4)
O7—H710.8557C6—H60.9300
O7—H720.8506C3—H30.9300
S1—C11.752 (3)C7—C81.518 (4)
S1—C71.807 (3)C7—H7A0.9700
O3—N11.227 (4)C7—H7B0.9700
O4—N11.221 (4)C5—H50.9300
O6—Ni1—O6i180.0C3—C4—C5122.5 (3)
O6—Ni1—O5i91.28 (10)C3—C4—N1119.3 (3)
O6i—Ni1—O5i88.72 (10)C5—C4—N1118.2 (3)
O6—Ni1—O588.72 (10)C3—C2—C1120.2 (3)
O6i—Ni1—O591.28 (10)C3—C2—H2119.9
O5i—Ni1—O5180.00 (9)C1—C2—H2119.9
O6—Ni1—O790.38 (9)C2—C1—C6119.2 (2)
O6i—Ni1—O789.62 (9)C2—C1—S1125.3 (2)
O5i—Ni1—O789.35 (10)C6—C1—S1115.5 (2)
O5—Ni1—O790.65 (10)C5—C6—C1121.1 (3)
O6—Ni1—O7i89.62 (9)C5—C6—H6119.5
O6i—Ni1—O7i90.38 (9)C1—C6—H6119.5
O5i—Ni1—O7i90.65 (10)C4—C3—C2118.8 (3)
O5—Ni1—O7i89.35 (10)C4—C3—H3120.6
O7—Ni1—O7i180.000 (1)C2—C3—H3120.6
Ni1—O6—H61115.7C8—C7—S1109.07 (19)
Ni1—O6—H62123.1C8—C7—H7A109.9
H61—O6—H62108.3S1—C7—H7A109.9
Ni1—O5—H51114.7C8—C7—H7B109.9
Ni1—O5—H52113.8S1—C7—H7B109.9
H51—O5—H52108.2H7A—C7—H7B108.3
Ni1—O7—H71129.9C6—C5—C4118.1 (3)
Ni1—O7—H72114.8C6—C5—H5121.0
H71—O7—H72109.7C4—C5—H5121.0
C1—S1—C7103.34 (14)O2—C8—O1125.2 (2)
O4—N1—O3122.5 (3)O2—C8—C7116.1 (2)
O4—N1—C4119.6 (2)O1—C8—C7118.6 (2)
O3—N1—C4118.0 (3)
C1—S1—C7—C8169.76 (17)
Symmetry code: (i) x+2, y+1, z+1.
Hydrogen-bond geometry (Å, º) top
D—H···AD—HH···AD···AD—H···A
O6—H61···O3ii0.851.982.821 (3)168
O6—H62···O20.861.852.641 (4)154
O5—H51···O2iii0.861.902.749 (3)171
O5—H52···O1iv0.851.962.794 (3)167
O7—H72···O1iii0.851.832.676 (3)176
Symmetry codes: (ii) x+1, y, z+1; (iii) x, y+1, z; (iv) x+1, y, z+1.
 

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