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The title compound, catena-poly­[[[2-(2-pyridinyl)-4,4,5,5-tetra­methyl­imidazolin-1-oxyl]­thio­cyanato­nickel(II)]-μ-thiocyanato], [Ni(NCS)2(C12H16N3O)]n, was prepared from the imino nitroxide radical (IM2py), nickel(II) nitrate and potassium thio­cyanate. The crystal structure consists of neutral chains of [Ni(IM2py)(SCN)] units linked by further thio­cyanate as bridges. The Ni—NCS—Ni chains form a zigzag structure. Each NiII ion is located in a distorted square-pyramidal environment. The basal plane positions are occupied by two N atoms from the imino nitroxide radical and two thio­cyanate N atoms, one from the terminal thio­cyanate group and the other from the bridging thio­cyanate group. The apical position is occupied by an S atom from the bridging thio­cyanate group.

Supporting information

cif

Crystallographic Information File (CIF) https://doi.org/10.1107/S1600536804009717/ci6363sup1.cif
Contains datablocks global, I

hkl

Structure factor file (CIF format) https://doi.org/10.1107/S1600536804009717/ci6363Isup2.hkl
Contains datablock I

CCDC reference: 226025

Key indicators

  • Single-crystal X-ray study
  • T = 293 K
  • Mean [sigma](C-C) = 0.009 Å
  • R factor = 0.051
  • wR factor = 0.112
  • Data-to-parameter ratio = 14.7

checkCIF/PLATON results

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Alert level C PLAT094_ALERT_2_C Ratio of Maximum / Minimum Residual Density .... 2.19 PLAT241_ALERT_2_C Check High U(eq) as Compared to Neighbors .... N1 PLAT241_ALERT_2_C Check High U(eq) as Compared to Neighbors .... N2 PLAT242_ALERT_2_C Check Low U(eq) as Compared to Neighbors .... C1 PLAT242_ALERT_2_C Check Low U(eq) as Compared to Neighbors .... C2 PLAT341_ALERT_3_C Low Bond Precision on C-C bonds (x 1000) Ang ... 9
Alert level G REFLT03_ALERT_4_G Please check that the estimate of the number of Friedel pairs is correct. If it is not, please give the correct count in the _publ_section_exptl_refinement section of the submitted CIF. From the CIF: _diffrn_reflns_theta_max 25.03 From the CIF: _reflns_number_total 3118 Count of symmetry unique reflns 1814 Completeness (_total/calc) 171.89% TEST3: Check Friedels for noncentro structure Estimate of Friedel pairs measured 1304 Fraction of Friedel pairs measured 0.719 Are heavy atom types Z>Si present yes
0 ALERT level A = In general: serious problem 0 ALERT level B = Potentially serious problem 6 ALERT level C = Check and explain 1 ALERT level G = General alerts; check 0 ALERT type 1 CIF construction/syntax error, inconsistent or missing data 5 ALERT type 2 Indicator that the structure model may be wrong or deficient 1 ALERT type 3 Indicator that the structure quality may be low 1 ALERT type 4 Improvement, methodology, query or suggestion

Computing details top

Data collection: SMART (Bruker, 1998); cell refinement: SMART; data reduction: SAINT (Bruker, 1998); 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: SHELXL97.

catena-Poly[[[2-(2-pyridinyl)-4,4,5,5-tetramethylimidazoline-1- oxyl]thiocyanatonickel(II)]-µ-thiocyanato] top
Crystal data top
[Ni(NCS)2(C12H16N3O)]F(000) = 812
Mr = 393.15Dx = 1.472 Mg m3
Orthorhombic, P212121Mo Kα radiation, λ = 0.71073 Å
Hall symbol: P 2ac 2abCell parameters from 695 reflections
a = 8.364 (4) Åθ = 3.0–20.8°
b = 9.463 (5) ŵ = 1.34 mm1
c = 22.411 (12) ÅT = 293 K
V = 1773.9 (16) Å3Block, green
Z = 40.40 × 0.36 × 0.15 mm
Data collection top
Bruker SMART CCD area-detector
diffractometer
3118 independent reflections
Radiation source: fine-focus sealed tube2353 reflections with I > 2σ(I)
Graphite monochromatorRint = 0.044
φ and ω scansθmax = 25.0°, θmin = 1.8°
Absorption correction: multi-scan
(SADABS; Sheldrick, 1996)
h = 98
Tmin = 0.645, Tmax = 0.818k = 116
6085 measured reflectionsl = 2026
Refinement top
Refinement on F2Secondary atom site location: difference Fourier map
Least-squares matrix: fullHydrogen site location: inferred from neighbouring sites
R[F2 > 2σ(F2)] = 0.051H-atom parameters constrained
wR(F2) = 0.112 w = 1/[σ2(Fo2) + (0.0456P)2]
where P = (Fo2 + 2Fc2)/3
S = 1.08(Δ/σ)max = 0.001
3118 reflectionsΔρmax = 0.88 e Å3
212 parametersΔρmin = 0.40 e Å3
0 restraintsAbsolute structure: Flack (1983); 1305 Friedel pairs
Primary atom site location: structure-invariant direct methodsAbsolute structure parameter: 0.03 (3)
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
Ni10.15427 (9)1.05133 (7)0.04285 (3)0.0396 (2)
O10.1729 (6)0.7680 (5)0.23888 (18)0.0605 (12)
N10.2774 (8)1.1720 (7)0.0115 (2)0.0692 (18)
C10.3610 (8)1.2080 (6)0.0494 (3)0.0524 (16)
S10.4775 (3)1.2596 (2)0.10256 (8)0.0680 (6)
N20.0244 (7)0.9884 (6)0.0239 (2)0.0611 (16)
C20.0171 (7)0.9556 (7)0.0711 (3)0.0494 (15)
S20.0745 (3)0.9064 (3)0.13603 (9)0.0874 (7)
N30.0796 (5)0.9020 (5)0.1008 (2)0.0376 (11)
N40.1093 (5)0.7992 (5)0.1893 (2)0.0440 (12)
N50.3227 (5)1.0720 (5)0.10788 (19)0.0412 (11)
C30.4414 (8)1.1700 (7)0.1088 (3)0.0568 (17)
H30.45481.22970.07630.068*
C40.5425 (8)1.1826 (7)0.1572 (3)0.0580 (18)
H40.62361.24990.15680.070*
C50.5237 (7)1.0967 (7)0.2053 (3)0.0545 (18)
H50.59071.10580.23820.065*
C60.4045 (7)0.9961 (7)0.2050 (3)0.0475 (16)
H60.39120.93510.23710.057*
C70.3049 (6)0.9880 (6)0.1555 (2)0.0397 (14)
C80.1647 (7)0.8931 (5)0.1480 (2)0.0365 (12)
C90.0544 (7)0.7508 (6)0.1706 (3)0.0438 (14)
C100.1709 (9)0.8325 (8)0.2099 (3)0.0680 (19)
H10A0.14830.81320.25110.102*
H10B0.27830.80380.20080.102*
H10C0.15950.93190.20240.102*
C110.0699 (9)0.5917 (7)0.1829 (3)0.074 (2)
H11A0.01920.54280.16550.110*
H11B0.16750.55710.16580.110*
H11C0.07100.57570.22520.110*
C120.0541 (7)0.7943 (6)0.1035 (3)0.0469 (16)
C130.0052 (10)0.6773 (7)0.0610 (3)0.068 (2)
H13A0.01500.71670.02220.103*
H13B0.08980.60900.05820.103*
H13C0.08990.63230.07550.103*
C140.2102 (7)0.8622 (8)0.0830 (3)0.068 (2)
H14A0.20810.87400.04040.102*
H14B0.22230.95270.10180.102*
H14C0.29840.80250.09380.102*
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
Ni10.0398 (4)0.0394 (4)0.0397 (4)0.0084 (3)0.0066 (4)0.0061 (4)
O10.054 (3)0.078 (3)0.050 (3)0.002 (3)0.003 (2)0.022 (2)
N10.078 (5)0.081 (5)0.049 (3)0.029 (4)0.007 (3)0.018 (3)
C10.063 (4)0.052 (4)0.042 (4)0.007 (3)0.009 (4)0.007 (3)
S10.0779 (14)0.0612 (12)0.0648 (12)0.0247 (10)0.0168 (10)0.0061 (9)
N20.070 (4)0.064 (4)0.049 (3)0.017 (3)0.011 (3)0.008 (3)
C20.042 (3)0.058 (4)0.048 (4)0.005 (3)0.000 (3)0.010 (3)
S20.0890 (16)0.1137 (19)0.0594 (12)0.0160 (14)0.0176 (11)0.0180 (11)
N30.033 (2)0.033 (3)0.047 (3)0.005 (2)0.007 (2)0.001 (2)
N40.037 (3)0.052 (3)0.043 (3)0.004 (2)0.001 (2)0.008 (2)
N50.032 (3)0.041 (3)0.051 (3)0.003 (2)0.005 (2)0.003 (2)
C30.052 (4)0.062 (4)0.057 (4)0.012 (3)0.000 (4)0.000 (3)
C40.040 (4)0.070 (5)0.064 (5)0.008 (3)0.004 (3)0.014 (4)
C50.035 (4)0.079 (5)0.049 (4)0.000 (3)0.011 (3)0.012 (3)
C60.038 (3)0.061 (4)0.044 (4)0.002 (3)0.001 (3)0.001 (3)
C70.031 (3)0.051 (4)0.037 (3)0.006 (2)0.000 (2)0.001 (3)
C80.030 (3)0.035 (3)0.044 (3)0.006 (3)0.001 (3)0.005 (2)
C90.032 (3)0.042 (3)0.057 (4)0.001 (3)0.001 (3)0.008 (3)
C100.044 (4)0.084 (5)0.076 (5)0.007 (4)0.007 (4)0.000 (4)
C110.073 (5)0.055 (5)0.093 (5)0.019 (4)0.001 (4)0.017 (4)
C120.036 (4)0.037 (4)0.067 (4)0.014 (3)0.008 (3)0.002 (3)
C130.084 (6)0.049 (4)0.072 (5)0.018 (4)0.002 (4)0.001 (3)
C140.031 (4)0.073 (5)0.100 (6)0.015 (3)0.014 (4)0.023 (4)
Geometric parameters (Å, º) top
Ni1—N21.942 (6)C5—H50.93
Ni1—N11.961 (6)C6—C71.389 (7)
Ni1—N32.018 (4)C6—H60.93
Ni1—N52.036 (4)C7—C81.487 (8)
Ni1—S1i2.680 (2)C9—C101.524 (9)
O1—N41.267 (5)C9—C111.537 (8)
N1—C11.153 (8)C9—C121.559 (8)
C1—S11.614 (7)C10—H10A0.96
S1—Ni1ii2.680 (2)C10—H10B0.96
N2—C21.156 (7)C10—H10C0.96
C2—S21.601 (7)C11—H11A0.96
N3—C81.279 (7)C11—H11B0.96
N3—C121.514 (7)C11—H11C0.96
N4—C81.363 (7)C12—C131.517 (9)
N4—C91.503 (7)C12—C141.526 (9)
N5—C71.339 (7)C13—H13A0.96
N5—C31.359 (7)C13—H13B0.96
C3—C41.379 (9)C13—H13C0.96
C3—H30.93C14—H14A0.96
C4—C51.359 (9)C14—H14B0.96
C4—H40.93C14—H14C0.96
C5—C61.378 (9)
N2—Ni1—N189.7 (2)N3—C8—N4114.5 (5)
N2—Ni1—N396.2 (2)N3—C8—C7119.5 (5)
N1—Ni1—N3165.8 (2)N4—C8—C7125.9 (5)
N2—Ni1—N5165.4 (2)N4—C9—C10105.5 (5)
N1—Ni1—N591.4 (2)N4—C9—C11109.0 (5)
N3—Ni1—N579.69 (18)C10—C9—C11109.8 (5)
N2—Ni1—S1i106.30 (19)N4—C9—C12100.8 (4)
N1—Ni1—S1i102.2 (2)C10—C9—C12115.1 (5)
N3—Ni1—S1i88.60 (14)C11—C9—C12115.6 (5)
N5—Ni1—S1i87.70 (14)C9—C10—H10A109.5
C1—N1—Ni1161.6 (6)C9—C10—H10B109.5
N1—C1—S1179.6 (7)H10A—C10—H10B109.5
C1—S1—Ni1ii99.6 (2)C9—C10—H10C109.5
C2—N2—Ni1162.8 (5)H10A—C10—H10C109.5
N2—C2—S2178.7 (7)H10B—C10—H10C109.5
C8—N3—C12109.5 (5)C9—C11—H11A109.5
C8—N3—Ni1114.0 (4)C9—C11—H11B109.5
C12—N3—Ni1136.5 (4)H11A—C11—H11B109.5
O1—N4—C8127.1 (5)C9—C11—H11C109.5
O1—N4—C9123.8 (5)H11A—C11—H11C109.5
C8—N4—C9108.6 (4)H11B—C11—H11C109.5
C7—N5—C3118.3 (5)N3—C12—C13105.5 (5)
C7—N5—Ni1115.9 (4)N3—C12—C14109.7 (4)
C3—N5—Ni1125.6 (4)C13—C12—C14110.4 (6)
N5—C3—C4121.3 (6)N3—C12—C9102.6 (4)
N5—C3—H3119.3C13—C12—C9114.5 (5)
C4—C3—H3119.3C14—C12—C9113.6 (5)
C5—C4—C3120.0 (6)C12—C13—H13A109.5
C5—C4—H4120.0C12—C13—H13B109.5
C3—C4—H4120.0H13A—C13—H13B109.5
C4—C5—C6119.5 (6)C12—C13—H13C109.5
C4—C5—H5120.2H13A—C13—H13C109.5
C6—C5—H5120.2H13B—C13—H13C109.5
C5—C6—C7118.4 (5)C12—C14—H14A109.5
C5—C6—H6120.8C12—C14—H14B109.5
C7—C6—H6120.8H14A—C14—H14B109.5
N5—C7—C6122.5 (5)C12—C14—H14C109.5
N5—C7—C8110.9 (5)H14A—C14—H14C109.5
C6—C7—C8126.6 (5)H14B—C14—H14C109.5
N2—Ni1—N1—C165.1 (18)C5—C6—C7—C8176.3 (6)
N3—Ni1—N1—C150 (2)C12—N3—C8—N44.2 (7)
N5—Ni1—N1—C1100.3 (18)Ni1—N3—C8—N4175.9 (4)
S1i—Ni1—N1—C1171.7 (18)C12—N3—C8—C7179.5 (5)
N1—Ni1—N2—C233 (2)Ni1—N3—C8—C70.5 (6)
N3—Ni1—N2—C2134 (2)O1—N4—C8—N3178.2 (5)
N5—Ni1—N2—C261 (2)C9—N4—C8—N39.6 (7)
S1i—Ni1—N2—C2135.6 (19)O1—N4—C8—C75.8 (9)
N2—Ni1—N3—C8167.1 (4)C9—N4—C8—C7166.5 (5)
N1—Ni1—N3—C853.2 (10)N5—C7—C8—N31.1 (7)
N5—Ni1—N3—C81.2 (4)C6—C7—C8—N3176.9 (5)
S1i—Ni1—N3—C886.7 (4)N5—C7—C8—N4177.0 (5)
N2—Ni1—N3—C1212.9 (6)C6—C7—C8—N41.0 (9)
N1—Ni1—N3—C12126.8 (9)O1—N4—C9—C1070.4 (6)
N5—Ni1—N3—C12178.8 (6)C8—N4—C9—C10102.2 (5)
S1i—Ni1—N3—C1293.3 (5)O1—N4—C9—C1147.5 (7)
N2—Ni1—N5—C776.6 (9)C8—N4—C9—C11139.9 (5)
N1—Ni1—N5—C7170.8 (4)O1—N4—C9—C12169.5 (5)
N3—Ni1—N5—C71.9 (4)C8—N4—C9—C1217.9 (6)
S1i—Ni1—N5—C787.1 (4)C8—N3—C12—C13104.9 (6)
N2—Ni1—N5—C3108.9 (9)Ni1—N3—C12—C1375.1 (7)
N1—Ni1—N5—C314.7 (5)C8—N3—C12—C14136.3 (6)
N3—Ni1—N5—C3176.4 (5)Ni1—N3—C12—C1443.7 (8)
S1i—Ni1—N5—C387.4 (5)C8—N3—C12—C915.2 (6)
C7—N5—C3—C40.5 (9)Ni1—N3—C12—C9164.8 (4)
Ni1—N5—C3—C4174.9 (5)N4—C9—C12—N318.9 (5)
N5—C3—C4—C50.5 (10)C10—C9—C12—N394.0 (6)
C3—C4—C5—C60.9 (10)C11—C9—C12—N3136.2 (5)
C4—C5—C6—C71.3 (9)N4—C9—C12—C1394.8 (6)
C3—N5—C7—C61.1 (8)C10—C9—C12—C13152.3 (6)
Ni1—N5—C7—C6176.0 (4)C11—C9—C12—C1322.5 (8)
C3—N5—C7—C8177.0 (5)N4—C9—C12—C14137.2 (5)
Ni1—N5—C7—C82.1 (6)C10—C9—C12—C1424.3 (7)
C5—C6—C7—N51.5 (8)C11—C9—C12—C14105.5 (6)
Symmetry codes: (i) x1/2, y+5/2, z; (ii) x+1/2, y+5/2, z.
 

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