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The structure determination of the title compound, [Ni(C4H13N3)2][Ni(CN)4], reveals the presence of a complex [Ni(dien)2]2+ cation (dien is diethyl­enetri­amine) and a pair of crystallographically independent half-complex [Ni(CN)4]2- anions in the asymmetric unit. The Ni atoms of the anions lie on crystallographic inversion centres. In the cationic unit, the ligand geometry around the nickel(II) is distorted octahedral, with the two dien ligands coordinated in mer fashion, whereas in the anionic unit, the geometry of the nickel(II) atom is square planar. The crystal structure shows a three-dimensional hydrogen-bonding network involving alternating anionic and cationic rows placed in the (1\overline 11) plane.

Supporting information

cif

Crystallographic Information File (CIF) https://doi.org/10.1107/S160053680301479X/ci6241sup1.cif
Contains datablocks global, I

hkl

Structure factor file (CIF format) https://doi.org/10.1107/S160053680301479X/ci6241Isup2.hkl
Contains datablock I

CCDC reference: 221621

Key indicators

  • Single-crystal X-ray study
  • T = 293 K
  • Mean [sigma](C-C) = 0.012 Å
  • R factor = 0.042
  • wR factor = 0.078
  • Data-to-parameter ratio = 15.6

checkCIF results

No syntax errors found

ADDSYM reports no extra symmetry


Yellow Alert Alert Level C:
GOODF_01 Alert C The least squares goodness of fit parameter lies outside the range 0.80 <> 2.00 Goodness of fit given = 0.701 RINTA_01 Alert C The value of Rint is greater than 0.10 Rint given 0.121 PLAT_420 Alert C D-H Without Acceptor N24 - H24 ... ?
0 Alert Level A = Potentially serious problem
0 Alert Level B = Potential problem
3 Alert Level C = Please check

Computing details top

Data collection: IPDS (Stoe & Cie, 1996); cell refinement: IPDS; data reduction: X-RED (Stoe & Cie, 1996); program(s) used to solve structure: DIRDIF99.2 (Beurskens et al., 1999); program(s) used to refine structure: SHELXL97 (Sheldrick, 1997); molecular graphics: ORTEP-3 for Windows (Farrugia, 1997) and DIAMOND (Brandenburg, 2002); software used to prepare material for publication: WinGX publication routines (Farrugia, 1999).

(I) top
Crystal data top
[Ni(C4H13N3)2][Ni(CN)4]F(000) = 896
Mr = 427.85Dx = 1.403 Mg m3
Monoclinic, P21/cMo Kα radiation, λ = 0.71073 Å
Hall symbol: -P 2ybcCell parameters from 4000 reflections
a = 15.138 (2) Åθ = 2.7–30°
b = 9.458 (1) ŵ = 1.87 mm1
c = 15.248 (2) ÅT = 293 K
β = 111.884 (16)°Needle, violet
V = 2025.8 (5) Å30.51 × 0.11 × 0.09 mm
Z = 4
Data collection top
Stoe IPDS area-detector
diffractometer
3410 independent reflections
Radiation source: fine-focus sealed tube1449 reflections with I > 2σ(I)
Graphite monochromatorRint = 0.121
φ scansθmax = 25°, θmin = 2.7°
Absorption correction: analytical
(X-RED; Stoe & Cie, 1996)
h = 1818
Tmin = 0.744, Tmax = 0.897k = 1111
11730 measured reflectionsl = 1818
Refinement top
Refinement on F2Secondary atom site location: difference Fourier map
Least-squares matrix: fullH-atom parameters constrained
R[F2 > 2σ(F2)] = 0.042 w = 1/[σ2(Fo2) + (0.013P)2]
where P = (Fo2 + 2Fc2)/3
wR(F2) = 0.078(Δ/σ)max = 0.001
S = 0.70Δρmax = 0.26 e Å3
3410 reflectionsΔρmin = 0.47 e Å3
218 parametersExtinction correction: SHELXL97, Fc*=kFc[1+0.001xFc2λ3/sin(2θ)]-1/4
0 restraintsExtinction coefficient: 0.00329 (18)
Primary atom site location: structure-invariant direct methods
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.

Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top
xyzUiso*/Ueq
Ni10.74212 (6)0.06579 (8)0.20575 (6)0.0411 (2)
Ni20.50000.50000.00000.0434 (3)
Ni31.00000.50000.50000.0561 (4)
C10.4986 (5)0.3125 (8)0.0333 (4)0.0486 (19)
N10.4997 (4)0.1949 (7)0.0539 (4)0.0632 (18)
C20.3961 (5)0.4715 (7)0.0379 (4)0.052 (2)
N20.3341 (5)0.4561 (7)0.0606 (4)0.077 (2)
C30.8843 (6)0.4112 (8)0.4798 (5)0.061 (2)
N30.8140 (5)0.3553 (7)0.4674 (5)0.080 (2)
C41.0105 (5)0.3894 (10)0.4042 (6)0.089 (3)
N41.0171 (5)0.3193 (10)0.3467 (6)0.128 (4)
N110.6833 (3)0.0009 (6)0.0616 (3)0.0498 (13)
H11A0.61980.01000.04280.060*
H11B0.69590.06370.02450.060*
C120.7265 (5)0.1383 (7)0.0537 (5)0.0553 (19)
H12A0.78170.12250.03720.066*
H12B0.68090.19420.00400.066*
C130.7563 (5)0.2185 (7)0.1468 (5)0.059 (2)
H13A0.70060.24750.15920.071*
H13B0.79220.30230.14430.071*
N140.8148 (4)0.1240 (5)0.2209 (4)0.0510 (15)
H140.86990.10750.21170.061*
C150.8392 (6)0.1766 (7)0.3189 (5)0.067 (2)
H15A0.88370.25490.33150.080*
H15B0.78240.20860.32820.080*
C160.8833 (5)0.0548 (9)0.3825 (5)0.073 (2)
H16A0.94200.02780.37530.087*
H16B0.89840.08250.44780.087*
N170.8159 (4)0.0687 (6)0.3588 (3)0.0625 (16)
H17A0.84810.15020.37740.075*
H17B0.77410.06010.38770.075*
N210.6148 (3)0.0065 (6)0.2277 (3)0.0541 (14)
H21A0.58560.07460.18560.065*
H21B0.63100.04270.28620.065*
C220.5505 (5)0.1139 (8)0.2158 (5)0.069 (2)
H22A0.51510.10250.25690.083*
H22B0.50520.11710.15100.083*
C230.6056 (6)0.2499 (8)0.2391 (5)0.071 (2)
H23A0.56230.32970.22220.085*
H23B0.64290.25460.30640.085*
N240.6693 (4)0.2550 (5)0.1853 (4)0.0578 (17)
H240.63190.26090.12290.069*
C250.7366 (7)0.3720 (6)0.2070 (6)0.074 (2)
H25A0.77120.37950.27470.089*
H25B0.70360.46050.18410.089*
C260.8037 (7)0.3390 (9)0.1574 (6)0.086 (3)
H26A0.76940.34300.08960.103*
H26B0.85390.40930.17420.103*
N270.8458 (4)0.1971 (6)0.1842 (4)0.0606 (17)
H27A0.89810.20220.23760.073*
H27B0.86270.16130.13810.073*
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
Ni10.0417 (5)0.0425 (5)0.0377 (4)0.0059 (4)0.0132 (4)0.0038 (4)
Ni20.0446 (7)0.0459 (7)0.0375 (7)0.0034 (6)0.0129 (6)0.0074 (6)
Ni30.0487 (8)0.0756 (9)0.0462 (8)0.0137 (7)0.0202 (7)0.0184 (7)
C10.033 (4)0.059 (5)0.048 (4)0.013 (3)0.009 (4)0.011 (3)
N10.045 (4)0.061 (4)0.076 (4)0.009 (3)0.014 (3)0.021 (3)
C20.054 (4)0.051 (5)0.054 (4)0.015 (3)0.023 (4)0.019 (3)
N20.071 (4)0.092 (6)0.082 (4)0.020 (4)0.043 (4)0.028 (4)
C30.064 (5)0.080 (6)0.044 (4)0.019 (5)0.025 (4)0.021 (4)
N30.076 (5)0.101 (5)0.077 (5)0.037 (4)0.042 (4)0.040 (4)
C40.041 (4)0.146 (9)0.085 (6)0.038 (5)0.028 (5)0.066 (6)
N40.066 (5)0.216 (9)0.116 (6)0.052 (5)0.052 (5)0.109 (7)
N110.046 (3)0.057 (3)0.045 (3)0.012 (3)0.016 (2)0.012 (3)
C120.051 (4)0.054 (4)0.060 (5)0.007 (3)0.020 (4)0.022 (3)
C130.051 (5)0.043 (4)0.078 (5)0.001 (3)0.017 (4)0.007 (4)
N140.049 (4)0.055 (4)0.049 (3)0.006 (3)0.018 (3)0.007 (3)
C150.076 (6)0.058 (5)0.068 (5)0.016 (4)0.029 (5)0.010 (4)
C160.071 (5)0.090 (6)0.046 (4)0.012 (5)0.010 (4)0.016 (4)
N170.075 (4)0.064 (4)0.049 (3)0.015 (4)0.025 (3)0.005 (3)
N210.053 (3)0.060 (4)0.049 (3)0.011 (3)0.020 (3)0.007 (3)
C220.054 (5)0.082 (6)0.070 (5)0.018 (4)0.023 (4)0.001 (4)
C230.090 (6)0.057 (5)0.065 (5)0.021 (4)0.028 (5)0.007 (4)
N240.077 (4)0.043 (4)0.048 (3)0.000 (3)0.018 (3)0.001 (3)
C250.111 (7)0.041 (4)0.062 (4)0.004 (5)0.023 (5)0.001 (4)
C260.103 (7)0.071 (6)0.070 (5)0.033 (5)0.016 (6)0.005 (4)
N270.068 (4)0.059 (4)0.049 (3)0.019 (3)0.014 (3)0.001 (3)
Geometric parameters (Å, º) top
Ni1—N242.063 (5)N14—H140.91
Ni1—N142.072 (5)C15—C161.494 (9)
Ni1—N272.120 (5)C15—H15A0.97
Ni1—N112.136 (4)C15—H15B0.97
Ni1—N172.179 (5)C16—N171.504 (8)
Ni1—N212.185 (5)C16—H16A0.97
Ni2—C1i1.843 (7)C16—H16B0.97
Ni2—C11.843 (7)N17—H17A0.90
Ni2—C2i1.887 (8)N17—H17B0.90
Ni2—C21.887 (8)N21—C221.466 (8)
Ni3—C4ii1.851 (9)N21—H21A0.90
Ni3—C41.851 (9)N21—H21B0.90
Ni3—C3ii1.862 (8)C22—C231.502 (9)
Ni3—C31.862 (8)C22—H22A0.97
C1—N11.157 (7)C22—H22B0.97
C2—N21.124 (8)C23—N241.481 (9)
C3—N31.139 (8)C23—H23A0.97
C4—N41.133 (9)C23—H23B0.97
N11—C121.479 (7)N24—C251.456 (9)
N11—H11A0.90N24—H240.91
N11—H11B0.90C25—C261.507 (12)
C12—C131.522 (9)C25—H25A0.97
C12—H12A0.97C25—H25B0.97
C12—H12B0.97C26—N271.477 (9)
C13—N141.453 (7)C26—H26A0.97
C13—H13A0.97C26—H26B0.97
C13—H13B0.97N27—H27A0.90
N14—C151.485 (8)N27—H27B0.90
N24—Ni1—N14177.8 (2)N14—C15—H15B110.5
N24—Ni1—N2781.6 (3)C16—C15—H15B110.5
N14—Ni1—N2797.6 (2)H15A—C15—H15B108.7
N24—Ni1—N1196.1 (2)C15—C16—N17110.1 (5)
N14—Ni1—N1181.9 (2)C15—C16—H16A109.6
N27—Ni1—N1193.6 (2)N17—C16—H16A109.6
N24—Ni1—N17100.5 (2)C15—C16—H16B109.6
N14—Ni1—N1781.5 (2)N17—C16—H16B109.6
N27—Ni1—N1792.6 (2)H16A—C16—H16B108.1
N11—Ni1—N17163.0 (2)C16—N17—Ni1106.2 (4)
N24—Ni1—N2181.0 (2)C16—N17—H17A110.5
N14—Ni1—N21100.0 (2)Ni1—N17—H17A110.5
N27—Ni1—N21162.3 (2)C16—N17—H17B110.5
N11—Ni1—N2190.70 (19)Ni1—N17—H17B110.5
N17—Ni1—N2188.2 (2)H17A—N17—H17B108.7
C1i—Ni2—C1180.0C22—N21—Ni1108.7 (4)
C1i—Ni2—C2i91.2 (3)C22—N21—H21A109.9
C1—Ni2—C2i88.8 (3)Ni1—N21—H21A109.9
C1i—Ni2—C288.8 (3)C22—N21—H21B109.9
C1—Ni2—C291.2 (3)Ni1—N21—H21B109.9
C2i—Ni2—C2180.0 (3)H21A—N21—H21B108.3
C4ii—Ni3—C4180.000 (1)N21—C22—C23110.6 (6)
C4ii—Ni3—C3ii88.1 (3)N21—C22—H22A109.5
C4—Ni3—C3ii91.9 (3)C23—C22—H22A109.5
C4ii—Ni3—C391.9 (3)N21—C22—H22B109.5
C4—Ni3—C388.1 (3)C23—C22—H22B109.5
C3ii—Ni3—C3180.0 (4)H22A—C22—H22B108.1
N1—C1—Ni2178.6 (6)N24—C23—C22108.4 (6)
N2—C2—Ni2179.2 (7)N24—C23—H23A110.0
N3—C3—Ni3179.2 (8)C22—C23—H23A110.0
N4—C4—Ni3178.6 (11)N24—C23—H23B110.0
C12—N11—Ni1108.4 (4)C22—C23—H23B110.0
C12—N11—H11A110.0H23A—C23—H23B108.4
Ni1—N11—H11A110.0C25—N24—C23116.3 (6)
C12—N11—H11B110.0C25—N24—Ni1109.6 (5)
Ni1—N11—H11B110.0C23—N24—Ni1108.0 (4)
H11A—N11—H11B108.4C25—N24—H24107.5
N11—C12—C13110.4 (6)C23—N24—H24107.5
N11—C12—H12A109.6Ni1—N24—H24107.5
C13—C12—H12A109.6N24—C25—C26105.9 (6)
N11—C12—H12B109.6N24—C25—H25A110.6
C13—C12—H12B109.6C26—C25—H25A110.6
H12A—C12—H12B108.1N24—C25—H25B110.6
N14—C13—C12107.5 (5)C26—C25—H25B110.6
N14—C13—H13A110.2H25A—C25—H25B108.7
C12—C13—H13A110.2N27—C26—C25110.6 (6)
N14—C13—H13B110.2N27—C26—H26A109.5
C12—C13—H13B110.2C25—C26—H26A109.5
H13A—C13—H13B108.5N27—C26—H26B109.5
C13—N14—C15115.3 (5)C25—C26—H26B109.5
C13—N14—Ni1107.6 (4)H26A—C26—H26B108.1
C15—N14—Ni1109.0 (4)C26—N27—Ni1107.9 (5)
C13—N14—H14108.3C26—N27—H27A110.1
C15—N14—H14108.3Ni1—N27—H27A110.1
Ni1—N14—H14108.3C26—N27—H27B110.1
N14—C15—C16106.2 (5)Ni1—N27—H27B110.1
N14—C15—H15A110.5H27A—N27—H27B108.4
C16—C15—H15A110.5
N24—Ni1—N11—C12178.4 (4)N24—Ni1—N21—C220.3 (4)
N14—Ni1—N11—C120.6 (4)N14—Ni1—N21—C22177.7 (4)
N27—Ni1—N11—C1296.5 (4)N27—Ni1—N21—C228.3 (8)
N17—Ni1—N11—C1214.4 (10)N11—Ni1—N21—C2295.8 (4)
N21—Ni1—N11—C12100.6 (4)N17—Ni1—N21—C22101.2 (4)
Ni1—N11—C12—C1327.7 (6)Ni1—N21—C22—C2327.2 (7)
N11—C12—C13—N1452.1 (7)N21—C22—C23—N2451.2 (8)
C12—C13—N14—C15171.6 (6)C22—C23—N24—C25173.2 (6)
C12—C13—N14—Ni149.8 (6)C22—C23—N24—Ni149.5 (6)
N27—Ni1—N14—C13119.9 (4)N27—Ni1—N24—C2523.3 (5)
N11—Ni1—N14—C1327.4 (4)N11—Ni1—N24—C25116.0 (5)
N17—Ni1—N14—C13148.6 (5)N17—Ni1—N24—C2567.8 (5)
N21—Ni1—N14—C1361.9 (5)N21—Ni1—N24—C25154.3 (5)
N27—Ni1—N14—C15114.5 (5)N27—Ni1—N24—C23150.9 (5)
N11—Ni1—N14—C15153.0 (5)N11—Ni1—N24—C23116.4 (4)
N17—Ni1—N14—C1523.0 (5)N17—Ni1—N24—C2359.9 (5)
N21—Ni1—N14—C1563.7 (5)N21—Ni1—N24—C2326.6 (4)
C13—N14—C15—C16170.0 (6)C23—N24—C25—C26169.9 (6)
Ni1—N14—C15—C1649.0 (7)Ni1—N24—C25—C2647.0 (7)
N14—C15—C16—N1757.0 (8)N24—C25—C26—N2753.9 (8)
C15—C16—N17—Ni136.2 (7)C25—C26—N27—Ni133.9 (7)
N24—Ni1—N17—C16172.2 (4)N24—Ni1—N27—C266.1 (4)
N14—Ni1—N17—C167.0 (5)N14—Ni1—N27—C26171.9 (4)
N27—Ni1—N17—C1690.3 (5)N11—Ni1—N27—C2689.6 (5)
N11—Ni1—N17—C1620.7 (11)N17—Ni1—N27—C26106.3 (5)
N21—Ni1—N17—C16107.4 (5)N21—Ni1—N27—C2614.1 (9)
Symmetry codes: (i) x+1, y+1, z; (ii) x+2, y+1, z+1.
Hydrogen-bond geometry (Å, º) top
D—H···AD—HH···AD···AD—H···A
N11—H11A···N1iii0.902.573.288 (8)138
N11—H11A···N10.902.693.258 (8)122
N11—H11B···N3iv0.902.393.161 (9)144
N14—H14···N4v0.912.313.128 (10)150
N17—H17A···N30.902.543.183 (9)129
N17—H17B···N2vi0.902.293.143 (9)159
N21—H21A···N1iii0.902.253.127 (7)165
N21—H21B···N2vi0.902.193.046 (8)158
N27—H27A···N40.902.243.067 (8)153
Symmetry codes: (iii) x+1, y, z; (iv) x, y+1/2, z1/2; (v) x+2, y1/2, z+1/2; (vi) x+1, y1/2, z+1/2.
 

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