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In the title compound, [Ni(C8H9N2O3S)(H2O)3)]ClO4·H2O, the NiII atom is coordinated by the two N atoms [Ni—N = 2.054 (3) and 2.077 (3) Å] and one O atom [Ni—O = 2.070 (2) Å] from a tridentate 2-(2-pyridylmethyl­ene)­amino­ethanesulfonate [or N-(2-pyridylmethyl­idene)­taurine] ligand and three water mol­ecules [Ni—O = 2.025 (3)–2.081 (3) Å] in a distorted octa­hedral geometry. An extensive three-dimensional network of O—H...O hydrogen bonds, involving perchlorate anions, and coordinating and non-coordinating water mol­ecules, stabilizes the crystal packing.

Supporting information

cif

Crystallographic Information File (CIF) https://doi.org/10.1107/S1600536806055929/cv2165sup1.cif
Contains datablocks global, I

hkl

Structure factor file (CIF format) https://doi.org/10.1107/S1600536806055929/cv2165Isup2.hkl
Contains datablock I

CCDC reference: 636226

Key indicators

  • Single-crystal X-ray study
  • T = 293 K
  • Mean [sigma](C-C) = 0.006 Å
  • R factor = 0.044
  • wR factor = 0.109
  • Data-to-parameter ratio = 13.2

checkCIF/PLATON results

No syntax errors found



Alert level C PLAT094_ALERT_2_C Ratio of Maximum / Minimum Residual Density .... 2.94 PLAT242_ALERT_2_C Check Low Ueq as Compared to Neighbors for S1 PLAT244_ALERT_4_C Low 'Solvent' Ueq as Compared to Neighbors for Cl1 PLAT736_ALERT_1_C H...A Calc 1.937(19), Rep 1.93(4) ...... 2.11 su-Ra H6B -O3 1.555 1.655
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 4 ALERT level C = Check and explain 2 ALERT level G = General alerts; check 3 ALERT type 1 CIF construction/syntax error, inconsistent or missing data 2 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 1 ALERT type 4 Improvement, methodology, query or suggestion 0 ALERT type 5 Informative message, check

Computing details top

Data collection: SMART (Siemens, 1996); cell refinement: SAINT (Siemens, 1996); data reduction: SHELXTL (Sheldrick, 1997b); program(s) used to solve structure: SHELXS97 (Sheldrick, 1997a); program(s) used to refine structure: SHELXL97 (Sheldrick, 1997a); molecular graphics: SHELXTL; software used to prepare material for publication: SHELXL97.

Triaqua[2-(2-pyridylmethylene)aminoethanesulfonato-κ3N,N',O]nickel(II) perchlorate monohydrate top
Crystal data top
[Ni(C8H9N2O3S)(H2O)3)]ClO4·H2OF(000) = 1824
Mr = 443.46Dx = 1.782 Mg m3
Orthorhombic, PbcaMo Kα radiation, λ = 0.71073 Å
Hall symbol: -P 2ac 2abCell parameters from 2160 reflections
a = 7.818 (2) Åθ = 1.5–26.0°
b = 15.019 (4) ŵ = 1.52 mm1
c = 28.156 (7) ÅT = 293 K
V = 3305.7 (15) Å3Prism, green
Z = 80.25 × 0.10 × 0.10 mm
Data collection top
Siemens SMART CCD area-detector
diffractometer
3253 independent reflections
Radiation source: fine-focus sealed tube2616 reflections with I > 2σ(I)
Graphite monochromatorRint = 0.032
φ and ω scansθmax = 26.0°, θmin = 1.5°
Absorption correction: multi-scan
(SADABS; Sheldrick, 1996)
h = 99
Tmin = 0.703, Tmax = 0.863k = 1618
14207 measured reflectionsl = 3430
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)] = 0.044Hydrogen site location: inferred from neighbouring sites
wR(F2) = 0.110H atoms treated by a mixture of independent and constrained refinement
S = 1.06 w = 1/[σ2(Fo2) + (0.0511P)2 + 3.2755P]
where P = (Fo2 + 2Fc2)/3
3253 reflections(Δ/σ)max < 0.001
246 parametersΔρmax = 0.81 e Å3
12 restraintsΔρmin = 0.28 e Å3
Special details top

Experimental. Analysis found (%): C 22.31, H 3.60, N 5.87, S 8.03. required (%): C 21.65, H 3.83, N 6.31, S 7.22; IR (KBr, ν, cm-1): 1041.9, 1152.8, 1187.7 (–SO32-); 1089.2 (ClO4-); 1600, 1646.3 (CN + CC); 3508.8 (O—H).

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
Ni10.18679 (6)0.36701 (3)0.167160 (15)0.03238 (15)
S10.15767 (11)0.25244 (6)0.18167 (3)0.0362 (2)
O10.0139 (3)0.30221 (17)0.20044 (8)0.0435 (6)
O20.1449 (5)0.1595 (2)0.18940 (13)0.0747 (10)
O30.3155 (3)0.2903 (3)0.20017 (12)0.0727 (10)
O40.0260 (4)0.47576 (19)0.16012 (10)0.0524 (7)
H4A0.045 (6)0.5136 (19)0.1386 (9)0.079*
H4B0.019 (6)0.509 (2)0.1843 (8)0.062 (14)*
O50.2536 (4)0.41813 (19)0.23109 (9)0.0518 (7)
H5A0.315 (5)0.462 (2)0.2385 (16)0.078*
H5B0.269 (9)0.385 (3)0.2549 (14)0.14 (3)*
O60.3404 (3)0.25750 (19)0.18236 (10)0.0464 (6)
H6A0.348 (5)0.224 (3)0.1583 (11)0.070*
H6B0.445 (2)0.266 (3)0.1883 (16)0.087 (18)*
N10.3768 (4)0.42301 (19)0.12516 (11)0.0378 (7)
N20.1223 (4)0.3151 (2)0.10208 (10)0.0405 (7)
C10.5056 (5)0.4762 (2)0.13734 (15)0.0468 (9)
H10.51270.49640.16850.056*
C20.6291 (5)0.5025 (3)0.10513 (15)0.0476 (10)
H20.71530.54150.11440.057*
C30.6243 (5)0.4714 (3)0.05980 (15)0.0494 (10)
H30.70910.48660.03810.059*
C40.4907 (5)0.4167 (3)0.04687 (14)0.0461 (9)
H40.48340.39460.01610.055*
C50.3684 (5)0.3949 (2)0.07997 (13)0.0378 (8)
C60.2218 (5)0.3378 (3)0.06882 (13)0.0435 (9)
H60.20230.31870.03790.052*
C70.0188 (5)0.2531 (3)0.09204 (14)0.0569 (11)
H7A0.01750.19290.09930.068*
H7B0.04650.25560.05850.068*
C80.1730 (5)0.2746 (3)0.12008 (14)0.0534 (11)
H8A0.26850.24100.10730.064*
H8B0.19880.33730.11590.064*
Cl10.07783 (15)0.61866 (7)0.05759 (4)0.0546 (3)
O70.1029 (7)0.6375 (3)0.10622 (14)0.1186 (18)
O80.0450 (6)0.5269 (2)0.05387 (15)0.0991 (13)
O90.0650 (9)0.6637 (4)0.0428 (2)0.177 (3)
O100.2171 (8)0.6416 (4)0.0310 (2)0.156 (3)
O110.0819 (4)0.07420 (19)0.25912 (12)0.0556 (8)
H11A0.149 (5)0.112 (2)0.2715 (16)0.074 (17)*
H11B0.023 (6)0.108 (2)0.2415 (17)0.10 (2)*
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
Ni10.0308 (2)0.0367 (3)0.0297 (2)0.00311 (19)0.00015 (17)0.00045 (18)
S10.0334 (5)0.0400 (5)0.0352 (5)0.0070 (4)0.0017 (3)0.0019 (4)
O10.0362 (14)0.0598 (17)0.0345 (14)0.0158 (13)0.0024 (11)0.0032 (11)
O20.107 (3)0.0387 (16)0.078 (2)0.0072 (18)0.001 (2)0.0004 (16)
O30.0308 (16)0.107 (3)0.080 (2)0.0016 (16)0.0022 (15)0.026 (2)
O40.0580 (19)0.0521 (17)0.0470 (17)0.0138 (15)0.0023 (14)0.0103 (14)
O50.078 (2)0.0409 (15)0.0361 (15)0.0136 (15)0.0147 (14)0.0013 (12)
O60.0389 (16)0.0454 (16)0.0550 (18)0.0026 (13)0.0058 (12)0.0044 (13)
N10.0353 (16)0.0388 (16)0.0393 (17)0.0020 (13)0.0032 (13)0.0004 (13)
N20.0380 (17)0.0510 (19)0.0324 (16)0.0073 (15)0.0012 (13)0.0026 (13)
C10.043 (2)0.043 (2)0.054 (2)0.0044 (18)0.0044 (18)0.0064 (18)
C20.036 (2)0.043 (2)0.064 (3)0.0085 (17)0.0051 (19)0.0017 (19)
C30.041 (2)0.049 (2)0.058 (3)0.0017 (19)0.0142 (19)0.011 (2)
C40.048 (2)0.051 (2)0.039 (2)0.0011 (19)0.0095 (18)0.0036 (17)
C50.039 (2)0.0381 (19)0.0362 (19)0.0009 (16)0.0042 (15)0.0050 (15)
C60.045 (2)0.055 (2)0.0306 (19)0.0036 (18)0.0005 (16)0.0003 (16)
C70.054 (3)0.080 (3)0.037 (2)0.022 (2)0.0017 (18)0.015 (2)
C80.049 (2)0.067 (3)0.044 (2)0.012 (2)0.0094 (19)0.004 (2)
Cl10.0680 (7)0.0514 (6)0.0443 (5)0.0014 (5)0.0102 (5)0.0021 (4)
O70.193 (5)0.109 (3)0.054 (2)0.060 (3)0.000 (3)0.018 (2)
O80.117 (3)0.066 (2)0.115 (3)0.018 (2)0.009 (3)0.013 (2)
O90.217 (7)0.196 (6)0.117 (4)0.141 (5)0.015 (4)0.007 (4)
O100.165 (5)0.151 (5)0.153 (5)0.084 (4)0.108 (4)0.058 (4)
O110.057 (2)0.0427 (16)0.067 (2)0.0026 (15)0.0077 (16)0.0060 (15)
Geometric parameters (Å, º) top
Ni1—O52.025 (3)C1—H10.9300
Ni1—N22.054 (3)C2—C31.360 (6)
Ni1—O12.070 (2)C2—H20.9300
Ni1—O42.070 (3)C3—C41.378 (6)
Ni1—N12.077 (3)C3—H30.9300
Ni1—O62.081 (3)C4—C51.375 (5)
S1—O21.417 (3)C4—H40.9300
S1—O11.450 (3)C5—C61.465 (5)
S1—O31.455 (3)C6—H60.9300
S1—C81.770 (4)C7—C81.477 (6)
O4—H4A0.84 (4)C7—H7A0.9700
O4—H4B0.84 (4)C7—H7B0.9700
O5—H5A0.84 (4)C8—H8A0.9700
O5—H5B0.84 (4)C8—H8B0.9700
O6—H6A0.84 (4)Cl1—O101.366 (4)
O6—H6B0.84 (4)Cl1—O91.370 (5)
N1—C11.330 (5)Cl1—O81.405 (4)
N1—C51.342 (5)Cl1—O71.412 (4)
N2—C61.264 (5)O11—H11A0.85 (4)
N2—C71.471 (5)O11—H11B0.85 (4)
C1—C21.382 (5)
O5—Ni1—N2179.26 (14)N1—C1—C2122.1 (4)
O5—Ni1—O188.35 (11)N1—C1—H1119.0
N2—Ni1—O192.26 (11)C2—C1—H1119.0
O5—Ni1—O486.71 (13)C3—C2—C1119.9 (4)
N2—Ni1—O493.73 (12)C3—C2—H2120.0
O1—Ni1—O487.37 (12)C1—C2—H2120.0
O5—Ni1—N199.68 (12)C2—C3—C4118.3 (4)
N2—Ni1—N179.70 (12)C2—C3—H3120.9
O1—Ni1—N1171.96 (11)C4—C3—H3120.9
O4—Ni1—N193.45 (12)C5—C4—C3119.3 (4)
O5—Ni1—O688.17 (12)C5—C4—H4120.3
N2—Ni1—O691.44 (12)C3—C4—H4120.3
O1—Ni1—O688.42 (11)N1—C5—C4122.3 (4)
O4—Ni1—O6173.46 (12)N1—C5—C6115.2 (3)
N1—Ni1—O691.41 (12)C4—C5—C6122.5 (3)
O2—S1—O1113.4 (2)N2—C6—C5118.7 (3)
O2—S1—O3112.9 (2)N2—C6—H6120.6
O1—S1—O3109.00 (17)C5—C6—H6120.6
O2—S1—C8109.9 (2)N2—C7—C8111.8 (3)
O1—S1—C8108.23 (17)N2—C7—H7A109.3
O3—S1—C8102.7 (2)C8—C7—H7A109.3
S1—O1—Ni1131.68 (15)N2—C7—H7B109.3
Ni1—O4—H4A120 (3)C8—C7—H7B109.3
Ni1—O4—H4B115 (3)H7A—C7—H7B107.9
H4A—O4—H4B101 (4)C7—C8—S1115.3 (3)
Ni1—O5—H5A132 (3)C7—C8—H8A108.4
Ni1—O5—H5B121 (4)S1—C8—H8A108.4
H5A—O5—H5B101 (4)C7—C8—H8B108.4
Ni1—O6—H6A110 (3)S1—C8—H8B108.4
Ni1—O6—H6B119 (3)H8A—C8—H8B107.5
H6A—O6—H6B100 (4)O10—Cl1—O9111.0 (4)
C1—N1—C5118.1 (3)O10—Cl1—O8110.6 (3)
C1—N1—Ni1129.6 (3)O9—Cl1—O8108.2 (4)
C5—N1—Ni1112.2 (2)O10—Cl1—O7111.8 (3)
C6—N2—C7119.3 (3)O9—Cl1—O7108.0 (3)
C6—N2—Ni1114.0 (3)O8—Cl1—O7107.1 (3)
C7—N2—Ni1126.6 (2)H11A—O11—H11B100 (4)
Hydrogen-bond geometry (Å, º) top
D—H···AD—HH···AD···AD—H···A
O4—H4A···O70.84 (4)2.12 (4)2.927 (5)160 (3)
O4—H4B···O11i0.84 (4)2.03 (4)2.840 (4)161 (4)
O5—H5A···O11ii0.84 (4)1.95 (4)2.788 (4)170 (5)
O5—H5B···O3iii0.85 (4)2.01 (4)2.779 (4)150 (5)
O6—H6A···O7iv0.85 (4)2.00 (4)2.836 (5)172 (4)
O6—H6B···O3v0.85 (4)1.93 (4)2.780 (4)177 (5)
O11—H11A···O2iii0.85 (4)2.09 (4)2.882 (5)159 (4)
O11—H11B···O20.85 (4)2.12 (4)2.939 (5)164 (4)
Symmetry codes: (i) x, y+1/2, z+1/2; (ii) x+1/2, y+1/2, z; (iii) x+1/2, y, z+1/2; (iv) x+1/2, y1/2, z; (v) x+1, y, z.
 

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