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In the title complex, [Ni(NCS)2(C10H8N2S)2]·H2O, the NiII ion is coordinated by four pyridine N and two thio­cyanate N atoms in a distorted octa­hedral geometry. The Ni—N(pyridine) bond lengths are significantly longer than the Ni—N(NCS) bond lengths.

Supporting information

cif

Crystallographic Information File (CIF) https://doi.org/10.1107/S1600536806006507/xu6087sup1.cif
Contains datablocks global, I

hkl

Structure factor file (CIF format) https://doi.org/10.1107/S1600536806006507/xu6087Isup2.hkl
Contains datablock I

CCDC reference: 601272

Key indicators

  • Single-crystal X-ray study
  • T = 289 K
  • Mean [sigma](C-C) = 0.004 Å
  • H-atom completeness 89%
  • Disorder in solvent or counterion
  • R factor = 0.039
  • wR factor = 0.105
  • Data-to-parameter ratio = 18.0

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 .... ? PLAT068_ALERT_1_C Reported F000 Differs from Calcd (or Missing)... ? PLAT242_ALERT_2_C Check Low Ueq as Compared to Neighbors for C21 PLAT242_ALERT_2_C Check Low Ueq as Compared to Neighbors for C22 PLAT302_ALERT_4_C Anion/Solvent Disorder ......................... 50.00 Perc. PLAT311_ALERT_2_C Isolated Disordered Oxygen Atom (No H's ?) ..... <O1W' PLAT720_ALERT_4_C Number of Unusual/Non-Standard Label(s) ........ 1
Alert level G FORMU01_ALERT_2_G There is a discrepancy between the atom counts in the _chemical_formula_sum and the formula from the _atom_site* data. Atom count from _chemical_formula_sum:C22 H18 N6 Ni1 O1 S4 Atom count from the _atom_site data: C22 H16 N6 Ni1 O1 S4 CELLZ01_ALERT_1_G Difference between formula and atom_site contents detected. CELLZ01_ALERT_1_G WARNING: H atoms missing from atom site list. Is this intentional? From the CIF: _cell_formula_units_Z 4 From the CIF: _chemical_formula_sum C22 H18 N6 Ni O S4 TEST: Compare cell contents of formula and atom_site data atom Z*formula cif sites diff C 88.00 88.00 0.00 H 72.00 64.00 8.00 N 24.00 24.00 0.00 Ni 4.00 4.00 0.00 O 4.00 4.00 0.00 S 16.00 16.00 0.00
0 ALERT level A = In general: serious problem 0 ALERT level B = Potentially serious problem 8 ALERT level C = Check and explain 3 ALERT level G = General alerts; check 5 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 2 ALERT type 4 Improvement, methodology, query or suggestion

Computing details top

Data collection: SMART (Bruker, 1998); cell refinement: SAINT (Bruker, 1998); 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, 1998); software used to prepare material for publication: SHELXTL.

Bis(thiocyanato-κN)bis(2,2'-thiodipyridine-κ2N,N')nickel(II) monohydrate top
Crystal data top
[Ni(NCS)2(C10H8N2S)2]·H2OF(000) = 1168
Mr = 569.38Dx = 1.517 Mg m3
Monoclinic, P21/cMo Kα radiation, λ = 0.71073 Å
Hall symbol: -P 2ybcCell parameters from 4506 reflections
a = 8.3379 (5) Åθ = 2.4–25.4°
b = 29.3927 (19) ŵ = 1.14 mm1
c = 10.2119 (7) ÅT = 289 K
β = 95.147 (1)°Block, blue
V = 2492.6 (3) Å30.38 × 0.26 × 0.14 mm
Z = 4
Data collection top
Bruker APEXII CCD area-detector
diffractometer
5708 independent reflections
Radiation source: fine-focus sealed tube4345 reflections with I > 2σ(I)
Graphite monochromatorRint = 0.023
φ and ω scansθmax = 27.5°, θmin = 2.1°
Absorption correction: multi-scan
(SADABS; Bruker, 1998)
h = 1010
Tmin = 0.705, Tmax = 0.850k = 3836
16243 measured reflectionsl = 139
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)] = 0.039Hydrogen site location: inferred from neighbouring sites
wR(F2) = 0.105H-atom parameters constrained
S = 1.04 w = 1/[σ2(Fo2) + (0.0512P)2 + 1.153P]
where P = (Fo2 + 2Fc2)/3
5708 reflections(Δ/σ)max = 0.002
317 parametersΔρmax = 0.50 e Å3
12 restraintsΔρmin = 0.60 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*/UeqOcc. (<1)
Ni10.58750 (4)0.362796 (10)0.42512 (3)0.03727 (10)
S10.45073 (8)0.40363 (3)0.71818 (7)0.05304 (19)
S20.17063 (7)0.34870 (2)0.36259 (7)0.04650 (17)
S30.92553 (15)0.45186 (5)0.16661 (11)0.1048 (4)
S40.85797 (10)0.22061 (3)0.36455 (11)0.0775 (3)
O1W0.491 (3)0.4858 (5)0.0404 (14)0.221 (7)0.54 (2)
O1W'0.331 (4)0.4744 (5)0.0091 (15)0.235 (14)0.46 (2)
N10.7208 (2)0.38152 (7)0.6046 (2)0.0402 (5)
N20.4444 (2)0.42109 (7)0.4568 (2)0.0436 (5)
N30.4332 (2)0.31900 (7)0.51759 (19)0.0361 (4)
N40.4506 (2)0.34625 (7)0.2458 (2)0.0402 (5)
N50.7350 (3)0.40343 (8)0.3252 (2)0.0540 (6)
N60.7323 (2)0.30683 (8)0.4031 (2)0.0477 (5)
C10.7569 (4)0.40738 (10)0.8278 (3)0.0529 (7)
H10.71120.41740.90250.063*
C20.9217 (4)0.40255 (10)0.8277 (3)0.0595 (8)
H20.98900.40880.90310.071*
C30.9847 (3)0.38859 (10)0.7158 (3)0.0560 (7)
H31.09550.38600.71300.067*
C40.8814 (3)0.37833 (10)0.6069 (3)0.0481 (6)
H40.92530.36870.53100.058*
C50.6615 (3)0.39685 (8)0.7137 (3)0.0410 (6)
C60.3929 (3)0.43393 (9)0.5717 (3)0.0456 (6)
C70.3965 (4)0.44630 (9)0.3515 (3)0.0578 (7)
H70.43650.43940.27160.069*
C80.2896 (4)0.48228 (10)0.3566 (4)0.0687 (9)
H80.25570.49840.28080.082*
C90.2349 (4)0.49365 (11)0.4739 (5)0.0769 (11)
H90.16240.51750.47880.092*
C100.2871 (3)0.46984 (10)0.5840 (4)0.0635 (9)
H100.25280.47750.66540.076*
C110.1749 (3)0.29267 (9)0.5704 (3)0.0449 (6)
H110.06410.29170.54960.054*
C120.2438 (3)0.27032 (9)0.6788 (3)0.0482 (6)
H120.18000.25530.73520.058*
C130.4085 (3)0.27041 (8)0.7034 (3)0.0453 (6)
H130.45820.25480.77500.054*
C140.4983 (3)0.29411 (8)0.6197 (3)0.0418 (6)
H140.60990.29290.63450.050*
C150.2723 (3)0.31683 (8)0.4918 (2)0.0367 (5)
C160.2894 (3)0.34376 (8)0.2288 (3)0.0413 (6)
C170.5319 (4)0.33964 (9)0.1395 (3)0.0500 (6)
H170.64380.33960.15060.060*
C180.4581 (4)0.33291 (10)0.0151 (3)0.0577 (7)
H180.51870.32840.05600.069*
C190.2922 (4)0.33303 (11)0.0018 (3)0.0631 (8)
H190.23880.32980.08520.076*
C200.2072 (4)0.33787 (10)0.1055 (3)0.0550 (7)
H200.09520.33720.09620.066*
C210.8143 (3)0.42330 (10)0.2591 (3)0.0503 (7)
C220.7849 (3)0.27134 (10)0.3869 (3)0.0451 (6)
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
Ni10.03273 (17)0.03821 (18)0.04085 (19)0.00160 (12)0.00319 (13)0.00344 (13)
S10.0430 (4)0.0645 (5)0.0528 (4)0.0047 (3)0.0113 (3)0.0090 (3)
S20.0341 (3)0.0595 (4)0.0452 (4)0.0084 (3)0.0006 (3)0.0024 (3)
S30.1066 (8)0.1416 (11)0.0707 (7)0.0638 (8)0.0338 (6)0.0070 (6)
S40.0564 (5)0.0585 (5)0.1135 (8)0.0182 (4)0.0161 (5)0.0299 (5)
O1W0.225 (10)0.233 (9)0.211 (9)0.004 (6)0.049 (6)0.010 (6)
O1W'0.35 (4)0.212 (14)0.155 (12)0.046 (16)0.108 (16)0.067 (10)
N10.0345 (10)0.0400 (11)0.0460 (12)0.0004 (9)0.0032 (9)0.0032 (9)
N20.0390 (11)0.0376 (11)0.0529 (13)0.0013 (9)0.0024 (10)0.0006 (10)
N30.0332 (10)0.0379 (10)0.0367 (11)0.0015 (8)0.0000 (8)0.0011 (8)
N40.0428 (11)0.0416 (11)0.0363 (11)0.0012 (9)0.0038 (9)0.0025 (9)
N50.0505 (13)0.0545 (14)0.0583 (15)0.0070 (11)0.0119 (12)0.0025 (11)
N60.0368 (11)0.0498 (13)0.0564 (14)0.0071 (10)0.0035 (10)0.0095 (11)
C10.0597 (17)0.0533 (16)0.0446 (16)0.0035 (13)0.0010 (13)0.0072 (12)
C20.0559 (18)0.0593 (18)0.0593 (19)0.0017 (14)0.0183 (15)0.0042 (15)
C30.0361 (14)0.0592 (18)0.071 (2)0.0038 (13)0.0075 (13)0.0019 (15)
C40.0384 (14)0.0521 (15)0.0536 (16)0.0006 (11)0.0037 (12)0.0016 (12)
C50.0392 (13)0.0380 (13)0.0457 (15)0.0003 (10)0.0025 (11)0.0024 (11)
C60.0328 (12)0.0383 (13)0.0652 (18)0.0012 (10)0.0020 (12)0.0118 (12)
C70.0600 (18)0.0414 (15)0.069 (2)0.0016 (13)0.0081 (15)0.0053 (14)
C80.0609 (19)0.0423 (16)0.099 (3)0.0026 (14)0.0171 (19)0.0121 (17)
C90.0546 (19)0.0432 (17)0.130 (3)0.0147 (14)0.006 (2)0.009 (2)
C100.0457 (16)0.0494 (17)0.095 (3)0.0072 (13)0.0032 (16)0.0179 (17)
C110.0355 (12)0.0451 (14)0.0541 (16)0.0036 (11)0.0039 (11)0.0034 (12)
C120.0520 (16)0.0435 (14)0.0507 (16)0.0034 (12)0.0127 (13)0.0024 (12)
C130.0557 (16)0.0383 (13)0.0411 (14)0.0022 (11)0.0001 (12)0.0025 (11)
C140.0378 (13)0.0398 (13)0.0463 (15)0.0035 (10)0.0036 (11)0.0034 (11)
C150.0348 (12)0.0352 (12)0.0394 (13)0.0035 (9)0.0002 (10)0.0074 (10)
C160.0434 (13)0.0390 (13)0.0405 (14)0.0039 (11)0.0021 (11)0.0004 (10)
C170.0542 (16)0.0498 (16)0.0469 (16)0.0006 (13)0.0086 (13)0.0028 (12)
C180.078 (2)0.0574 (18)0.0388 (16)0.0024 (15)0.0106 (14)0.0000 (13)
C190.082 (2)0.068 (2)0.0366 (16)0.0036 (17)0.0084 (15)0.0006 (14)
C200.0565 (17)0.0585 (17)0.0473 (17)0.0056 (14)0.0101 (13)0.0032 (13)
C210.0459 (15)0.0604 (17)0.0439 (15)0.0093 (13)0.0003 (12)0.0115 (13)
C220.0276 (12)0.0569 (17)0.0493 (15)0.0007 (11)0.0047 (11)0.0111 (12)
Geometric parameters (Å, º) top
Ni1—N12.129 (2)C3—C41.378 (4)
Ni1—N22.129 (2)C3—H30.9300
Ni1—N32.103 (2)C4—H40.9300
Ni1—N42.126 (2)C6—C101.388 (4)
Ni1—N52.050 (2)C7—C81.387 (4)
Ni1—N62.065 (2)C7—H70.9300
S1—C61.770 (3)C8—C91.361 (5)
S1—C51.774 (3)C8—H80.9300
S2—C161.763 (3)C9—C101.363 (5)
S2—C151.771 (2)C9—H90.9300
S3—C211.617 (3)C10—H100.9300
S4—C221.634 (3)C11—C121.369 (4)
N1—C41.340 (3)C11—C151.387 (4)
N1—C51.337 (3)C11—H110.9300
N2—C71.337 (4)C12—C131.373 (4)
N2—C61.340 (3)C12—H120.9300
N3—C151.346 (3)C13—C141.375 (4)
N3—C141.348 (3)C13—H130.9300
N4—C171.345 (3)C14—H140.9300
N4—C161.342 (3)C16—C201.390 (4)
N5—C211.147 (4)C17—C181.375 (4)
N6—C221.149 (3)C17—H170.9300
C1—C51.386 (4)C18—C191.379 (4)
C1—C21.382 (4)C18—H180.9300
C1—H10.9300C19—C201.364 (4)
C2—C31.363 (4)C19—H190.9300
C2—H20.9300C20—H200.9300
N5—Ni1—N691.57 (10)N2—C6—C10123.3 (3)
N5—Ni1—N3176.72 (9)N2—C6—S1120.92 (19)
N6—Ni1—N387.04 (8)C10—C6—S1115.7 (2)
N5—Ni1—N490.24 (9)N2—C7—C8122.6 (3)
N6—Ni1—N489.89 (8)N2—C7—H7118.7
N3—Ni1—N486.79 (8)C8—C7—H7118.7
N5—Ni1—N189.29 (9)C9—C8—C7119.2 (3)
N6—Ni1—N191.95 (8)C9—C8—H8120.4
N3—Ni1—N193.73 (8)C7—C8—H8120.4
N4—Ni1—N1178.10 (8)C10—C9—C8119.5 (3)
N5—Ni1—N288.62 (9)C10—C9—H9120.2
N6—Ni1—N2177.23 (9)C8—C9—H9120.2
N3—Ni1—N292.91 (8)C9—C10—C6118.3 (3)
N4—Ni1—N292.87 (8)C9—C10—H10120.8
N1—Ni1—N285.29 (8)C6—C10—H10120.8
C6—S1—C5103.31 (12)C12—C11—C15119.3 (2)
C16—S2—C15105.62 (11)C12—C11—H11120.4
O1Wi—O1W—O1W'101 (3)C15—C11—H11120.4
C4—N1—C5116.9 (2)C11—C12—C13119.1 (2)
C4—N1—Ni1116.16 (18)C11—C12—H12120.4
C5—N1—Ni1126.93 (16)C13—C12—H12120.4
C7—N2—C6116.9 (2)C12—C13—C14118.6 (2)
C7—N2—Ni1117.1 (2)C12—C13—H13120.7
C6—N2—Ni1126.00 (18)C14—C13—H13120.7
C15—N3—C14116.8 (2)N3—C14—C13123.5 (2)
C15—N3—Ni1125.50 (16)N3—C14—H14118.2
C14—N3—Ni1117.38 (16)C13—C14—H14118.2
C17—N4—C16117.4 (2)N3—C15—C11122.4 (2)
C17—N4—Ni1117.27 (18)N3—C15—S2121.52 (18)
C16—N4—Ni1125.30 (17)C11—C15—S2115.86 (18)
C21—N5—Ni1173.3 (2)N4—C16—C20122.0 (3)
C22—N6—Ni1166.7 (2)N4—C16—S2121.41 (19)
C5—C1—C2118.1 (3)C20—C16—S2116.5 (2)
C5—C1—H1120.9N4—C17—C18123.4 (3)
C2—C1—H1120.9N4—C17—H17118.3
C3—C2—C1119.4 (3)C18—C17—H17118.3
C3—C2—H2120.3C17—C18—C19118.4 (3)
C1—C2—H2120.3C17—C18—H18120.8
C2—C3—C4118.8 (3)C19—C18—H18120.8
C2—C3—H3120.6C20—C19—C18119.2 (3)
C4—C3—H3120.6C20—C19—H19120.4
N1—C4—C3123.4 (3)C18—C19—H19120.4
N1—C4—H4118.3C19—C20—C16119.4 (3)
C3—C4—H4118.3C19—C20—H20120.3
N1—C5—C1123.3 (2)C16—C20—H20120.3
N1—C5—S1120.06 (18)N5—C21—S3179.3 (3)
C1—C5—S1116.6 (2)N6—C22—S4179.4 (3)
Symmetry code: (i) x+1, y+1, z.
 

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