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The title compound, [Ni(NCS)2(C6H7NO)2(H2O)2]·H2O, consists of a mononuclear complex and an uncoordinated water mol­ecule. The nickel(II) ion has a distorted octahedral coordination, formed by two N atoms from two thio­cyanate anions and four O atoms from two water mol­ecules and two 4-methyl­pyridine N-oxide mol­ecules. The uncoordinated water mol­ecules and the complex are connected by O—H...O and O—H...S hydrogen bonds.

Supporting information

cif

Crystallographic Information File (CIF) https://doi.org/10.1107/S1600536805010937/hb6177sup1.cif
Contains datablocks I, 1

hkl

Structure factor file (CIF format) https://doi.org/10.1107/S1600536805010937/hb6177Isup2.hkl
Contains datablock I

CCDC reference: 261032

Key indicators

  • Single-crystal X-ray study
  • T = 293 K
  • Mean [sigma](C-C) = 0.005 Å
  • R factor = 0.035
  • wR factor = 0.094
  • Data-to-parameter ratio = 14.1

checkCIF/PLATON results

No syntax errors found



Alert level C PLAT220_ALERT_2_C Large Non-Solvent C Ueq(max)/Ueq(min) ... 2.85 Ratio PLAT230_ALERT_2_C Hirshfeld Test Diff for S1 - C13 .. 5.70 su PLAT230_ALERT_2_C Hirshfeld Test Diff for S2 - C14 .. 6.44 su PLAT242_ALERT_2_C Check Low Ueq as Compared to Neighbors for C3 PLAT710_ALERT_4_C Delete 1-2-3 or 2-3-4 Linear Torsion Angle ... # 1 N4 -NI1 -N3 -C13 22.60 1.30 1.555 1.555 1.555 1.555 PLAT710_ALERT_4_C Delete 1-2-3 or 2-3-4 Linear Torsion Angle ... # 6 N3 -NI1 -N4 -C14 22.70 1.40 1.555 1.555 1.555 1.555 PLAT710_ALERT_4_C Delete 1-2-3 or 2-3-4 Linear Torsion Angle ... # 37 O2 -NI1 -O1 -N1 104.00 0.80 1.555 1.555 1.555 1.555 PLAT710_ALERT_4_C Delete 1-2-3 or 2-3-4 Linear Torsion Angle ... # 44 O1 -NI1 -O2 -N2 83.70 0.90 1.555 1.555 1.555 1.555 PLAT720_ALERT_4_C Number of Unusual/Non-Standard Label(s) ........ 4
0 ALERT level A = In general: serious problem 0 ALERT level B = Potentially serious problem 9 ALERT level C = Check and explain 0 ALERT level G = General alerts; check 0 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 5 ALERT type 4 Improvement, methodology, query or suggestion

Computing details top

Data collection: SMART (Bruker, 1997); cell refinement: SMART; data reduction: SAINT (Bruker, 1997); program(s) used to solve structure: SHELXS97 (Sheldrick, 1997); program(s) used to refine structure: SHELXL97 (Sheldrick, 1997); molecular graphics: SHELXTL (Bruker, 2001); software used to prepare material for publication: SHELXTL.

(I) top
Crystal data top
[Ni(C6H7NO)2(NCS)2(H2O)2]·H2OZ = 2
Mr = 447.17F(000) = 464
Triclinic, P1Dx = 1.496 Mg m3
Hall symbol: -P 1Mo Kα radiation, λ = 0.71073 Å
a = 7.5665 (16) ÅCell parameters from 2545 reflections
b = 9.701 (2) Åθ = 2.3–27.1°
c = 14.129 (3) ŵ = 1.22 mm1
α = 103.820 (3)°T = 293 K
β = 98.958 (3)°Prism, blue
γ = 91.721 (3)°0.14 × 0.09 × 0.08 mm
V = 992.4 (4) Å3
Data collection top
Bruker SMART CCD
diffractometer
3426 independent reflections
Radiation source: fine-focus sealed tube3069 reflections with I > 2σ(I)
Graphite monochromatorRint = 0.018
φ and ω scansθmax = 25.0°, θmin = 2.2°
Absorption correction: multi-scan
(SADABS; Sheldrick, 1996)
h = 88
Tmin = 0.848, Tmax = 0.909k = 1111
5120 measured reflectionsl = 1016
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)] = 0.035Hydrogen site location: inferred from neighbouring sites
wR(F2) = 0.094H-atom parameters constrained
S = 1.06 w = 1/[σ2(Fo2) + (0.0493P)2 + 0.2162P]
where P = (Fo2 + 2Fc2)/3
3426 reflections(Δ/σ)max = 0.001
243 parametersΔρmax = 0.31 e Å3
0 restraintsΔρmin = 0.30 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
Ni10.72854 (4)0.78816 (3)0.96374 (2)0.02952 (12)
N10.4422 (3)0.7770 (2)0.79274 (15)0.0371 (5)
N21.0013 (3)0.8015 (2)1.13636 (14)0.0347 (5)
N30.8328 (3)0.7651 (2)0.83858 (16)0.0408 (5)
N40.6168 (3)0.7886 (2)1.08468 (15)0.0378 (5)
C10.4779 (4)0.8912 (3)0.7603 (2)0.0523 (8)
H10.50950.97890.80520.063*
C20.4683 (5)0.8799 (4)0.6612 (2)0.0628 (9)
H20.49380.96020.63930.075*
C30.4216 (4)0.7521 (4)0.5938 (2)0.0589 (8)
C40.4238 (6)0.7372 (6)0.4851 (3)0.0963 (15)
H4A0.54260.71940.47150.144*
H4B0.38850.82340.46780.144*
H4C0.34170.65920.44680.144*
C50.3816 (5)0.6373 (4)0.6303 (2)0.0663 (9)
H50.34650.54920.58670.080*
C60.3928 (4)0.6511 (3)0.7296 (2)0.0521 (7)
H60.36590.57260.75310.063*
C70.9994 (4)0.9239 (3)1.2041 (2)0.0503 (7)
H71.00381.01011.18630.060*
C80.9910 (5)0.9217 (4)1.2996 (2)0.0606 (9)
H80.99151.00721.34670.073*
C90.9819 (4)0.7952 (4)1.3277 (2)0.0539 (8)
C100.9557 (6)0.7893 (5)1.4297 (3)0.0921 (14)
H10A0.97550.69561.43840.138*
H10B0.83550.81141.43830.138*
H10C1.03930.85731.47760.138*
C110.9904 (4)0.6727 (3)1.2560 (2)0.0506 (7)
H110.98910.58551.27240.061*
C121.0007 (4)0.6769 (3)1.1612 (2)0.0400 (6)
H121.00730.59311.11380.048*
C130.8636 (4)0.7224 (3)0.7597 (2)0.0383 (6)
C140.5605 (3)0.7571 (3)1.14885 (18)0.0342 (6)
O10.4630 (2)0.78897 (19)0.89102 (12)0.0399 (4)
O20.9936 (2)0.80314 (18)1.04032 (12)0.0370 (4)
O30.7109 (3)0.56658 (19)0.93464 (15)0.0518 (5)
H3WA0.65460.53310.87890.078*
H3WB0.71130.53180.97720.048 (9)*
O40.7445 (3)1.01096 (18)0.99352 (15)0.0484 (5)
H4WA0.84091.03910.98260.073*
H4WB0.67881.05901.01430.051 (10)*
O50.2223 (3)0.6051 (2)0.94194 (15)0.0497 (5)
H5B0.31270.64570.93130.072 (12)*
H5A0.15010.66750.96770.083 (12)*
S10.90757 (14)0.66716 (10)0.64821 (6)0.0665 (3)
S20.48009 (11)0.71646 (8)1.24005 (5)0.0525 (2)
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
Ni10.0346 (2)0.02782 (18)0.0292 (2)0.00189 (13)0.01142 (13)0.00910 (13)
N10.0356 (12)0.0419 (12)0.0369 (12)0.0065 (9)0.0082 (9)0.0138 (10)
N20.0353 (12)0.0364 (11)0.0328 (12)0.0033 (9)0.0072 (9)0.0090 (9)
N30.0479 (14)0.0425 (12)0.0382 (13)0.0055 (10)0.0176 (11)0.0152 (10)
N40.0425 (13)0.0388 (12)0.0345 (12)0.0004 (9)0.0139 (10)0.0092 (9)
C10.079 (2)0.0391 (15)0.0432 (16)0.0088 (14)0.0143 (15)0.0155 (13)
C20.084 (3)0.064 (2)0.053 (2)0.0163 (18)0.0215 (17)0.0311 (17)
C30.0500 (19)0.090 (3)0.0392 (17)0.0150 (17)0.0116 (14)0.0161 (17)
C40.087 (3)0.159 (5)0.044 (2)0.016 (3)0.019 (2)0.020 (2)
C50.062 (2)0.076 (2)0.0486 (19)0.0055 (18)0.0048 (16)0.0056 (17)
C60.0515 (18)0.0484 (17)0.0524 (18)0.0095 (14)0.0059 (14)0.0081 (14)
C70.069 (2)0.0354 (15)0.0436 (17)0.0049 (13)0.0062 (14)0.0065 (12)
C80.083 (2)0.0567 (19)0.0339 (16)0.0041 (17)0.0132 (15)0.0049 (14)
C90.0506 (18)0.075 (2)0.0384 (16)0.0025 (15)0.0093 (13)0.0179 (15)
C100.105 (3)0.135 (4)0.047 (2)0.000 (3)0.024 (2)0.038 (2)
C110.0486 (17)0.0579 (18)0.0531 (18)0.0038 (14)0.0070 (14)0.0307 (15)
C120.0408 (15)0.0352 (14)0.0454 (16)0.0023 (11)0.0102 (12)0.0110 (12)
C130.0390 (15)0.0380 (14)0.0445 (16)0.0060 (11)0.0153 (12)0.0170 (12)
C140.0343 (14)0.0326 (13)0.0337 (14)0.0008 (10)0.0075 (11)0.0040 (10)
O10.0396 (10)0.0523 (11)0.0327 (10)0.0043 (8)0.0100 (8)0.0173 (8)
O20.0392 (10)0.0445 (10)0.0293 (9)0.0015 (8)0.0103 (7)0.0105 (7)
O30.0858 (16)0.0306 (9)0.0397 (11)0.0004 (9)0.0094 (11)0.0114 (9)
O40.0523 (13)0.0288 (9)0.0719 (14)0.0050 (9)0.0348 (11)0.0114 (9)
O50.0553 (13)0.0368 (10)0.0625 (13)0.0001 (10)0.0208 (10)0.0165 (9)
S10.0865 (7)0.0797 (6)0.0442 (5)0.0240 (5)0.0359 (4)0.0183 (4)
S20.0652 (5)0.0580 (5)0.0389 (4)0.0092 (4)0.0230 (4)0.0136 (3)
Geometric parameters (Å, º) top
Ni1—N32.014 (2)C5—C61.365 (4)
Ni1—N42.020 (2)C5—H50.9300
Ni1—O32.0859 (18)C6—H60.9300
Ni1—O42.0970 (18)C7—C81.366 (4)
Ni1—O22.1082 (18)C7—H70.9300
Ni1—O12.1109 (18)C8—C91.380 (5)
N1—C11.331 (3)C8—H80.9300
N1—C61.332 (4)C9—C111.375 (4)
N1—O11.349 (3)C9—C101.499 (4)
N2—C121.337 (3)C10—H10A0.9600
N2—C71.338 (3)C10—H10B0.9600
N2—O21.353 (2)C10—H10C0.9600
N3—C131.155 (3)C11—C121.364 (4)
N4—C141.159 (3)C11—H110.9300
C1—C21.370 (4)C12—H120.9300
C1—H10.9300C13—S11.628 (3)
C2—C31.368 (5)C14—S21.630 (3)
C2—H20.9300O3—H3WA0.8200
C3—C51.379 (5)O3—H3WB0.7556
C3—C41.511 (4)O4—H4WA0.8200
C4—H4A0.9600O4—H4WB0.7382
C4—H4B0.9600O5—H5B0.8301
C4—H4C0.9600O5—H5A0.8791
N3—Ni1—N4173.85 (8)C6—C5—C3121.0 (3)
N3—Ni1—O386.78 (8)C6—C5—H5119.5
N4—Ni1—O387.20 (8)C3—C5—H5119.5
N3—Ni1—O493.60 (8)N1—C6—C5120.1 (3)
N4—Ni1—O492.41 (8)N1—C6—H6120.0
O3—Ni1—O4179.56 (8)C5—C6—H6120.0
N3—Ni1—O287.51 (8)N2—C7—C8119.7 (3)
N4—Ni1—O293.96 (8)N2—C7—H7120.2
O3—Ni1—O292.28 (8)C8—C7—H7120.2
O4—Ni1—O287.97 (8)C7—C8—C9121.3 (3)
N3—Ni1—O193.53 (8)C7—C8—H8119.4
N4—Ni1—O185.42 (8)C9—C8—H8119.4
O3—Ni1—O191.72 (8)C11—C9—C8116.7 (3)
O4—Ni1—O188.03 (8)C11—C9—C10121.0 (3)
O2—Ni1—O1175.92 (7)C8—C9—C10122.2 (3)
C1—N1—C6120.8 (2)C9—C10—H10A109.5
C1—N1—O1119.1 (2)C9—C10—H10B109.5
C6—N1—O1120.1 (2)H10A—C10—H10B109.5
C12—N2—C7121.0 (2)C9—C10—H10C109.5
C12—N2—O2119.4 (2)H10A—C10—H10C109.5
C7—N2—O2119.5 (2)H10B—C10—H10C109.5
C13—N3—Ni1163.1 (2)C12—C11—C9121.2 (3)
C14—N4—Ni1164.7 (2)C12—C11—H11119.4
N1—C1—C2120.2 (3)C9—C11—H11119.4
N1—C1—H1119.9N2—C12—C11120.0 (3)
C2—C1—H1119.9N2—C12—H12120.0
C3—C2—C1121.0 (3)C11—C12—H12120.0
C3—C2—H2119.5N3—C13—S1178.3 (2)
C1—C2—H2119.5N4—C14—S2178.7 (2)
C2—C3—C5117.0 (3)N1—O1—Ni1116.01 (14)
C2—C3—C4121.0 (4)N2—O2—Ni1112.85 (13)
C5—C3—C4121.9 (4)Ni1—O3—H3WA109.5
C3—C4—H4A109.5Ni1—O3—H3WB119.0
C3—C4—H4B109.5H3WA—O3—H3WB124.0
H4A—C4—H4B109.5Ni1—O4—H4WA109.5
C3—C4—H4C109.5Ni1—O4—H4WB126.9
H4A—C4—H4C109.5H4WA—O4—H4WB123.5
H4B—C4—H4C109.5H5B—O5—H5A110.9
N4—Ni1—N3—C1322.6 (13)N2—C7—C8—C90.9 (5)
O3—Ni1—N3—C1334.2 (7)C7—C8—C9—C113.0 (5)
O4—Ni1—N3—C13145.6 (7)C7—C8—C9—C10174.3 (3)
O2—Ni1—N3—C13126.6 (7)C8—C9—C11—C122.3 (5)
O1—Ni1—N3—C1357.4 (7)C10—C9—C11—C12175.0 (3)
N3—Ni1—N4—C1422.7 (14)C7—N2—C12—C112.8 (4)
O3—Ni1—N4—C1411.1 (8)O2—N2—C12—C11173.5 (2)
O4—Ni1—N4—C14169.1 (8)C9—C11—C12—N20.5 (4)
O2—Ni1—N4—C1481.0 (8)C1—N1—O1—Ni179.0 (3)
O1—Ni1—N4—C14103.0 (8)C6—N1—O1—Ni198.7 (2)
C6—N1—C1—C21.5 (5)N3—Ni1—O1—N10.75 (16)
O1—N1—C1—C2176.1 (3)N4—Ni1—O1—N1174.68 (16)
N1—C1—C2—C30.2 (5)O3—Ni1—O1—N187.62 (16)
C1—C2—C3—C51.3 (5)O4—Ni1—O1—N192.74 (15)
C1—C2—C3—C4175.6 (3)O2—Ni1—O1—N1104.0 (8)
C2—C3—C5—C61.5 (5)C12—N2—O2—Ni188.0 (2)
C4—C3—C5—C6175.3 (3)C7—N2—O2—Ni188.3 (2)
C1—N1—C6—C51.3 (4)N3—Ni1—O2—N2171.32 (15)
O1—N1—C6—C5176.3 (3)N4—Ni1—O2—N22.71 (15)
C3—C5—C6—N10.3 (5)O3—Ni1—O2—N284.65 (15)
C12—N2—C7—C82.1 (4)O4—Ni1—O2—N294.99 (14)
O2—N2—C7—C8174.2 (3)O1—Ni1—O2—N283.7 (9)
Hydrogen-bond geometry (Å, º) top
D—H···AD—HH···AD···AD—H···A
O3—H3WA···S2i0.822.663.337 (2)140
O3—H3WB···O5i0.761.982.690 (3)157
O4—H4WA···O2ii0.822.072.811 (2)151
O4—H4WB···O1iii0.742.172.892 (3)165
O5—H5A···O2iv0.882.002.879 (3)174
Symmetry codes: (i) x+1, y+1, z+2; (ii) x+2, y+2, z+2; (iii) x+1, y+2, z+2; (iv) x1, y, z.
 

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