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In the crystal structure of the title compound, [Ni(C6H4N2O4S)(H2O)3]·2.5H2O, the NiII atom is six-coordinated by one 2-(6-oxido-4-oxo-3,4-dihydro­pyimidin-2-ylsulfan­yl)­acetate ligand and three water mol­ecules. Hydrogen-bonding inter­actions between the coordinated and uncoordinated water mol­ecules and between the water mol­ecules and the organic ligand result in a three-dimensional network structure.

Supporting information

cif

Crystallographic Information File (CIF) https://doi.org/10.1107/S1600536807006149/is2132sup1.cif
Contains datablocks global, I

hkl

Structure factor file (CIF format) https://doi.org/10.1107/S1600536807006149/is2132Isup2.hkl
Contains datablock I

CCDC reference: 640397

Key indicators

  • Single-crystal X-ray study
  • T = 293 K
  • Mean [sigma](C-C) = 0.004 Å
  • R factor = 0.038
  • wR factor = 0.111
  • Data-to-parameter ratio = 14.4

checkCIF/PLATON results

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Alert level C PLAT041_ALERT_1_C Calc. and Rep. SumFormula Strings Differ .... ? PLAT042_ALERT_1_C Calc. and Rep. MoietyFormula Strings Differ .... ? PLAT045_ALERT_1_C Calculated and Reported Z Differ by ............ 0.50 Ratio
Alert level G PLAT199_ALERT_1_G Check the Reported _cell_measurement_temperature 293 K PLAT200_ALERT_1_G Check the Reported _diffrn_ambient_temperature . 293 K
0 ALERT level A = In general: serious problem 0 ALERT level B = Potentially serious problem 3 ALERT level C = Check and explain 2 ALERT level G = General alerts; check 5 ALERT type 1 CIF construction/syntax error, inconsistent or missing data 0 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: SMART (Bruker, 2000); cell refinement: SAINT (Bruker, 2000); data reduction: SAINT; program(s) used to solve structure: SHELXS97 (Sheldrick, 1997); program(s) used to refine structure: SHELXL97 (Sheldrick, 1997); molecular graphics: SHELXTL (Bruker, 2000); software used to prepare material for publication: SHELXTL.

Triaqua[2-(6-oxido-4-oxo-3,4-dihydropyimidin-2-ylsulfanyl)acetato]nickel(II) 2.5-hydrate top
Crystal data top
[Ni(C6H4N2O4S)(H2O)3]·2.5H2OF(000) = 1480
Mr = 357.97Dx = 1.820 Mg m3
Orthorhombic, PbcnMo Kα radiation, λ = 0.71073 Å
Hall symbol: -P 2n 2abCell parameters from 996 reflections
a = 25.272 (5) Åθ = 4.3–27.6°
b = 7.5122 (16) ŵ = 1.69 mm1
c = 13.764 (3) ÅT = 293 K
V = 2613.1 (9) Å3Block, green
Z = 80.28 × 0.25 × 0.20 mm
Data collection top
Bruker SMART APEX CCD area-detector
diffractometer
2557 independent reflections
Radiation source: fine-focus sealed tube2222 reflections with I > 2σ(I)
Graphite monochromatorRint = 0.089
φ and ω scansθmax = 26.0°, θmin = 2.8°
Absorption correction: multi-scan
(SADABS; Sheldrick, 1996)
h = 3030
Tmin = 0.62, Tmax = 0.71k = 69
12876 measured reflectionsl = 1616
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)] = 0.038Hydrogen site location: inferred from neighbouring sites
wR(F2) = 0.111H-atom parameters constrained
S = 1.00 w = 1/[σ2(Fo2) + (0.0712P)2 + 1.4863P]
where P = (Fo2 + 2Fc2)/3
2557 reflections(Δ/σ)max < 0.001
177 parametersΔρmax = 0.55 e Å3
0 restraintsΔρmin = 0.51 e Å3
Special details top

Experimental. A thermogravimetric analysis gave the loss of all uncoordinated water molecules between 110 and 140 °C (13.2% observed, 12.57% calculated). On further heating, the compound lost weight continuously, corresponding to the preliminary decomposition of the whole framework, and an obvious decomposition was observed at 280 °C, corresponding to the final decomposition of the whole framework.

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*/UeqOcc. (<1)
C10.19767 (10)0.2131 (3)0.79562 (19)0.0232 (5)
C20.25131 (10)0.2292 (4)0.80848 (19)0.0269 (6)
H20.26450.28000.86510.032*
C30.28603 (11)0.1697 (3)0.7373 (2)0.0240 (6)
C40.21006 (10)0.0838 (3)0.64389 (18)0.0224 (5)
C50.12182 (10)0.0726 (3)0.5623 (2)0.0254 (6)
H5A0.10920.15550.51350.030*
H5B0.12220.13500.62400.030*
C60.08260 (11)0.0801 (4)0.57045 (19)0.0262 (6)
N10.17726 (9)0.1375 (3)0.71028 (16)0.0233 (5)
N20.26281 (8)0.0965 (3)0.65380 (15)0.0245 (5)
H2A0.28480.08220.60620.029*
Ni10.100163 (13)0.17208 (4)0.76578 (3)0.02264 (15)
O10.16111 (7)0.2609 (3)0.85411 (13)0.0286 (4)
O20.33560 (8)0.1748 (2)0.73959 (15)0.0311 (5)
O30.05587 (7)0.0872 (3)0.64912 (13)0.0288 (4)
O40.07691 (10)0.1831 (3)0.50215 (16)0.0472 (6)
O50.10126 (8)0.0831 (3)0.81986 (14)0.0318 (5)
H5D0.12240.14600.78620.038*
H5C0.11160.08160.87860.038*
O60.09224 (8)0.4218 (3)0.70658 (17)0.0388 (5)
H6B0.10120.49930.74840.047*
H6A0.11210.43060.65700.047*
O70.04217 (7)0.2261 (3)0.86169 (15)0.0334 (5)
H7A0.01230.20240.83630.040*
H7B0.04330.33570.87690.040*
O80.17025 (11)0.5103 (3)1.00349 (17)0.0510 (7)
H8A0.17650.42520.96450.061*
H8B0.14260.56540.98520.061*
H9B0.02810.55520.90450.061*
H9A0.01780.62950.94200.061*
O90.00541 (12)0.5571 (4)0.9003 (2)0.0692 (8)
O100.00000.7844 (5)0.75000.0524 (9)
H10A0.03120.80880.73110.063*0.50
H10B0.01550.87940.76760.063*0.50
S10.18896 (3)0.01007 (10)0.53348 (5)0.0290 (2)
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
C10.0283 (14)0.0219 (12)0.0193 (12)0.0017 (10)0.0013 (10)0.0016 (10)
C20.0284 (13)0.0274 (14)0.0251 (13)0.0006 (11)0.0040 (11)0.0036 (11)
C30.0240 (15)0.0191 (14)0.0290 (15)0.0027 (10)0.0013 (10)0.0030 (10)
C40.0253 (13)0.0220 (13)0.0200 (12)0.0012 (10)0.0000 (10)0.0030 (10)
C50.0251 (13)0.0259 (14)0.0252 (13)0.0005 (11)0.0004 (10)0.0020 (11)
C60.0277 (14)0.0293 (14)0.0215 (13)0.0013 (11)0.0018 (11)0.0017 (11)
N10.0229 (11)0.0257 (11)0.0212 (11)0.0015 (9)0.0008 (9)0.0017 (9)
N20.0226 (11)0.0285 (12)0.0224 (11)0.0012 (9)0.0032 (8)0.0010 (9)
Ni10.0213 (2)0.0260 (2)0.0207 (2)0.00033 (12)0.00101 (12)0.00109 (13)
O10.0263 (9)0.0368 (11)0.0226 (9)0.0016 (8)0.0010 (7)0.0076 (8)
O20.0241 (11)0.0294 (11)0.0398 (12)0.0018 (8)0.0007 (8)0.0035 (8)
O30.0248 (9)0.0385 (11)0.0231 (10)0.0002 (8)0.0004 (7)0.0035 (8)
O40.0655 (16)0.0465 (14)0.0297 (12)0.0239 (12)0.0088 (11)0.0101 (10)
O50.0414 (12)0.0314 (11)0.0227 (10)0.0072 (8)0.0048 (8)0.0017 (9)
O60.0402 (12)0.0298 (11)0.0464 (13)0.0066 (9)0.0068 (9)0.0047 (10)
O70.0256 (10)0.0365 (11)0.0381 (11)0.0019 (8)0.0058 (8)0.0084 (9)
O80.0648 (16)0.0505 (15)0.0377 (13)0.0167 (12)0.0196 (11)0.0114 (11)
O90.092 (2)0.0450 (15)0.0703 (19)0.0004 (14)0.0144 (16)0.0092 (14)
O100.040 (2)0.0419 (19)0.075 (2)0.0000.0025 (16)0.000
S10.0279 (4)0.0392 (4)0.0200 (3)0.0010 (3)0.0017 (2)0.0057 (3)
Geometric parameters (Å, º) top
C1—O11.277 (3)Ni1—O72.0136 (19)
C1—C21.373 (4)Ni1—O62.055 (2)
C1—N11.403 (3)Ni1—O52.057 (2)
C2—C31.389 (4)Ni1—O32.0585 (19)
C2—H20.93Ni1—O12.0725 (19)
C3—O21.254 (4)O5—H5D0.85
C3—N21.403 (3)O5—H5C0.85
C4—N11.298 (3)O6—H6B0.85
C4—N21.344 (3)O6—H6A0.85
C4—S11.758 (3)O7—H7A0.85
C5—C61.520 (4)O7—H7B0.85
C5—S11.805 (3)O8—H8A0.85
C5—H5A0.97O8—H8B0.85
C5—H5B0.97O9—H9B0.85
C6—O41.226 (3)O9—H9A0.85
C6—O31.277 (3)O10—H10A0.85
N1—Ni12.109 (2)O10—H10B0.85
N2—H2A0.87
O1—C1—C2127.5 (2)O6—Ni1—O5174.68 (8)
O1—C1—N1112.1 (2)O7—Ni1—O3100.25 (8)
C2—C1—N1120.4 (2)O6—Ni1—O385.45 (8)
C1—C2—C3120.3 (2)O5—Ni1—O390.05 (8)
C1—C2—H2119.9O7—Ni1—O195.26 (8)
C3—C2—H2119.8O6—Ni1—O190.64 (8)
O2—C3—C2127.1 (3)O5—Ni1—O194.45 (8)
O2—C3—N2116.8 (2)O3—Ni1—O1164.01 (7)
C2—C3—N2116.1 (2)O7—Ni1—N1159.18 (8)
N1—C4—N2122.7 (2)O6—Ni1—N193.37 (9)
N1—C4—S1122.6 (2)O5—Ni1—N190.22 (8)
N2—C4—S1114.65 (19)O3—Ni1—N1100.47 (8)
C6—C5—S1115.65 (19)O1—Ni1—N164.24 (8)
C6—C5—H5A108.8C1—O1—Ni194.45 (15)
S1—C5—H5A108.8C6—O3—Ni1112.75 (16)
C6—C5—H5B107.9Ni1—O5—H5D109.2
S1—C5—H5B108.0Ni1—O5—H5C109.6
H5A—C5—H5B107.4H5D—O5—H5C109.5
O4—C6—O3124.2 (3)Ni1—O6—H6B109.3
O4—C6—C5119.8 (2)Ni1—O6—H6A109.4
O3—C6—C5116.0 (2)H6B—O6—H6A109.5
C4—N1—C1118.7 (2)Ni1—O7—H7A109.5
C4—N1—Ni1152.05 (19)Ni1—O7—H7B109.4
C1—N1—Ni189.22 (15)H7A—O7—H7B109.5
C4—N2—C3121.7 (2)H8A—O8—H8B109.5
C4—N2—H2A123.4H9B—O9—H9A109.4
C3—N2—H2A113.6H10A—O10—H10B109.5
O7—Ni1—O690.30 (9)C4—S1—C5101.50 (12)
O7—Ni1—O587.73 (8)
Hydrogen-bond geometry (Å, º) top
D—H···AD—HH···AD···AD—H···A
O10—H10B···O5i0.852.502.909 (2)111
O10—H10B···O3i0.852.193.016 (3)165
O10—H10A···O3ii0.852.463.016 (3)124
O10—H10A···O5ii0.852.302.909 (2)129
O8—H8B···O4iii0.852.533.297 (4)151
O8—H8A···O10.852.002.791 (3)156
O7—H7A···O3iv0.851.942.693 (3)147
O6—H6B···O2v0.852.072.673 (3)127
O5—H5C···O4vi0.852.062.690 (3)131
O5—H5D···O2vii0.851.832.660 (3)165
N2—H2A···O8viii0.871.942.790 (3)166
Symmetry codes: (i) x, y+1, z+3/2; (ii) x, y+1, z; (iii) x, y+1, z+1/2; (iv) x, y, z+3/2; (v) x+1/2, y+1/2, z; (vi) x, y, z+1/2; (vii) x+1/2, y1/2, z; (viii) x+1/2, y+1/2, z1/2.
 

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