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The title compound, [Ni(C2H3N)3(C9H23N3)](PF6)2, has the Ni atom in an octa­hedral environment. It is coordinated by the three N atoms of one chelating 1,1,4,7,7-penta­methyl­diethylenetriamine mol­ecule and by three acetonitrile mol­ecules. The charge is balanced by two hexa­fluoridophosphate anions. The ethyl­ene chains and the central methyl group of the 1,1,4,7,7-penta­methyl­diethylenetriamine are disordered over two sites with occupation factors 0.619 (6) and 0.381 (6).

Supporting information

cif

Crystallographic Information File (CIF) https://doi.org/10.1107/S1600536807054360/at2457sup1.cif
Contains datablocks I, global

hkl

Structure factor file (CIF format) https://doi.org/10.1107/S1600536807054360/at2457Isup2.hkl
Contains datablock I

CCDC reference: 674055

Key indicators

  • Single-crystal X-ray study
  • T = 173 K
  • Mean [sigma](C-C) = 0.005 Å
  • Disorder in main residue
  • R factor = 0.048
  • wR factor = 0.130
  • Data-to-parameter ratio = 14.2

checkCIF/PLATON results

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Alert level C PLAT042_ALERT_1_C Calc. and Rep. MoietyFormula Strings Differ .... ? PLAT241_ALERT_2_C Check High Ueq as Compared to Neighbors for C1 PLAT244_ALERT_4_C Low 'Solvent' Ueq as Compared to Neighbors for P1 PLAT244_ALERT_4_C Low 'Solvent' Ueq as Compared to Neighbors for P2 PLAT301_ALERT_3_C Main Residue Disorder ......................... 12.00 Perc. PLAT720_ALERT_4_C Number of Unusual/Non-Standard Label(s) ........ 11
0 ALERT level A = In general: serious problem 0 ALERT level B = Potentially serious problem 6 ALERT level C = Check and explain 0 ALERT level G = General alerts; check 1 ALERT type 1 CIF construction/syntax error, inconsistent or missing data 1 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 3 ALERT type 4 Improvement, methodology, query or suggestion 0 ALERT type 5 Informative message, check

Comment top

We report here the X-ray crystal structure analysis of the nickel salt of 1,1,4,7,7-pentamethyldiethylenetriamine and hexafluoridophosphate, [Ni(PMDTA)(CH3CN)3]2+.2[PF6]- (PMDTA = Me2NHCH2CH2NMeCH2CH2NHMe2). We are interested in the synthesis of transition metal complexes with the PMDTA ligand (Margraf et al., 2005) which are a convenient starting material for novel benzoquinone- and hydroquinone-substituted transition metal derivatives (Margraf et al., 2006). The synthesis of the title compound was achieved by reaction of NiCl2 with AgPF6 in the presence of PMDTA, as shown in the equation below. Blue crystals of the title compound suitable for X-ray diffraction were grown from acetonitrile/diethyl ether solution at ambient temperature.

The title compound has the Ni atom in an octahedral environment. It is coordinated by the three N atoms of one chelating 1,1,4,7,7-pentamethyldiethylenetriamine molecule and three acetonitrile molecules. The charge is balanced by two hexafluoridophosphate anions.

Related literature top

For related literature, see: Margraf et al. (2005, 2006).

Experimental top

AgPF6 (3.2 mmol, 0.799 g) was added to a solution of NiCl2 (1.6 mmol, 0.205 g) and PMDTA (1.6 mmol, 0.274 g) in 20 ml acetonitrile. After filtering the reaction solution blue crystals of the title compound suitable for X-ray diffraction were grown by slow diffusion of diethyl ether (25 ml) to the acetonitrile solution at ambient temperature (Yield 85%).

Refinement top

H atoms were were geometrically positioned and refined with fixed individual displacement parameters [U(H) = 1.2 Ueq(C) or U(H) = 1.5 Ueq(Cmethyl)] using a riding model with C—H = 0.99Å or 0.98Å for CH2 and CH3 groups, respectively. The methyl groups of the acetonitrile molecules were allowed to rotate but not to tip. The ethylene chains and the central methyl group of the 1,1,4,7,7-pentamethyldiethylenetriamine are disordered over two sites with the occupation factors of 0.619 (6) and 0.381 (6).

Computing details top

Data collection: X-AREA (Stoe & Cie, 2001); cell refinement: X-AREA (Stoe & Cie, 2001); data reduction: X-AREA (Stoe & Cie, 2001); program(s) used to solve structure: SHELXS97 (Sheldrick, 1990); program(s) used to refine structure: SHELXL97 (Sheldrick, 1997); molecular graphics: XP in SHELXTL-Plus (Sheldrick, 1991); software used to prepare material for publication: SHELXL97 and PLATON (Spek, 2003).

Figures top
[Figure 1] Fig. 1. Perspective view of the title compound with the atom numbering; displacement ellipsoids are at the 50% probability level; hydrogen atoms and the minor occupied sites of the disordered atoms are omitted for clarity.
[Figure 2] Fig. 2. Preparation of the title compound.
Triacetonitrile(1,1,4,7,7-pentamethyldiethylenetriamine)nickel(II) bis(hexafluoridophosphate) top
Crystal data top
[Ni(C2H3N)3(C9H23N3)](PF6)2F(000) = 1320
Mr = 645.12Dx = 1.578 Mg m3
Monoclinic, P21/cMo Kα radiation, λ = 0.71073 Å
Hall symbol: -P 2ybcCell parameters from 31260 reflections
a = 17.4418 (8) Åθ = 3.6–25.7°
b = 10.5913 (6) ŵ = 0.93 mm1
c = 15.7326 (8) ÅT = 173 K
β = 110.921 (4)°Rod, light blue
V = 2714.7 (3) Å30.38 × 0.17 × 0.14 mm
Z = 4
Data collection top
STOE IPDS II two-circle-
diffractometer
5076 independent reflections
Radiation source: fine-focus sealed tube4263 reflections with I > 2σ(I)
Graphite monochromatorRint = 0.081
ω scansθmax = 25.7°, θmin = 3.6°
Absorption correction: multi-scan
(MULABS; Spek, 2003; Blessing, 1995)
h = 2120
Tmin = 0.719, Tmax = 0.881k = 1212
33712 measured reflectionsl = 1919
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)] = 0.048H-atom parameters constrained
wR(F2) = 0.130 w = 1/[σ2(Fo2) + (0.0753P)2 + 3.1233P]
where P = (Fo2 + 2Fc2)/3
S = 1.04(Δ/σ)max < 0.001
5076 reflectionsΔρmax = 0.83 e Å3
357 parametersΔρmin = 0.46 e Å3
0 restraintsExtinction correction: SHELXL, Fc*=kFc[1+0.001xFc2λ3/sin(2θ)]-1/4
Primary atom site location: structure-invariant direct methodsExtinction coefficient: 0.0019 (5)
Crystal data top
[Ni(C2H3N)3(C9H23N3)](PF6)2V = 2714.7 (3) Å3
Mr = 645.12Z = 4
Monoclinic, P21/cMo Kα radiation
a = 17.4418 (8) ŵ = 0.93 mm1
b = 10.5913 (6) ÅT = 173 K
c = 15.7326 (8) Å0.38 × 0.17 × 0.14 mm
β = 110.921 (4)°
Data collection top
STOE IPDS II two-circle-
diffractometer
5076 independent reflections
Absorption correction: multi-scan
(MULABS; Spek, 2003; Blessing, 1995)
4263 reflections with I > 2σ(I)
Tmin = 0.719, Tmax = 0.881Rint = 0.081
33712 measured reflections
Refinement top
R[F2 > 2σ(F2)] = 0.0480 restraints
wR(F2) = 0.130H-atom parameters constrained
S = 1.04Δρmax = 0.83 e Å3
5076 reflectionsΔρmin = 0.46 e Å3
357 parameters
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)
Ni10.25753 (2)0.72144 (3)0.39571 (2)0.01573 (14)
N10.36863 (17)0.6842 (3)0.36422 (19)0.0275 (6)
C110.3512 (3)0.6273 (4)0.2723 (3)0.0421 (9)
H11A0.31880.68660.22540.063*
H11B0.32040.54860.26760.063*
H11C0.40310.60940.26370.063*
C120.4179 (3)0.8012 (4)0.3684 (3)0.0502 (11)
H12A0.43060.84150.42790.075*
H12B0.38630.85970.32040.075*
H12C0.46910.77890.35950.075*
C10.4183 (2)0.5922 (4)0.4352 (3)0.0474 (11)
H1A0.47750.60600.44820.057*0.619 (6)
H1B0.40450.50480.41280.057*0.619 (6)
H1A'0.45270.63790.49060.057*0.381 (6)
H1B'0.45470.54260.41200.057*0.381 (6)
C20.3981 (3)0.6126 (6)0.5261 (4)0.0303 (13)0.619 (6)
H2A0.42970.55250.57400.036*0.619 (6)
H2B0.41190.69970.54940.036*0.619 (6)
C2'0.3532 (5)0.4976 (8)0.4591 (5)0.0240 (19)0.381 (6)
H2A'0.31490.45680.40350.029*0.381 (6)
H2B'0.38240.43180.50350.029*0.381 (6)
N20.30893 (16)0.5893 (2)0.49946 (16)0.0213 (5)
C210.2897 (4)0.4536 (5)0.4767 (4)0.0311 (14)0.619 (6)
H2C0.23050.44010.45880.047*0.619 (6)
H2D0.31870.40160.53000.047*0.619 (6)
H2E0.30730.42990.42630.047*0.619 (6)
C21'0.3699 (6)0.6356 (9)0.5892 (5)0.031 (2)0.381 (6)
H2C'0.38360.72400.58310.047*0.381 (6)
H2D'0.41980.58410.60620.047*0.381 (6)
H2E'0.34560.62860.63640.047*0.381 (6)
C30.2762 (4)0.6294 (5)0.5703 (3)0.0291 (13)0.619 (6)
H3A0.29930.71260.59500.035*0.619 (6)
H3B0.29250.56760.62090.035*0.619 (6)
C3'0.2374 (6)0.5281 (8)0.5133 (6)0.029 (2)0.381 (6)
H3A'0.25620.47120.56670.035*0.381 (6)
H3B'0.20550.47810.45910.035*0.381 (6)
C40.1832 (2)0.6380 (3)0.5295 (2)0.0320 (7)
H4A0.15980.55410.50690.038*0.619 (6)
H4B0.16140.66550.57660.038*0.619 (6)
H4A'0.13330.60180.53590.038*0.381 (6)
H4B'0.21440.68240.58680.038*0.381 (6)
N30.15869 (16)0.7311 (2)0.45229 (18)0.0228 (5)
C310.1484 (2)0.8585 (3)0.4872 (3)0.0374 (8)
H31A0.20080.88660.53190.056*
H31B0.10710.85420.51610.056*
H31C0.13030.91860.43650.056*
C320.0773 (2)0.6948 (4)0.3851 (3)0.0337 (8)
H32A0.08120.61120.36020.051*
H32B0.06020.75690.33570.051*
H32C0.03680.69230.41510.051*
N40.31638 (17)0.8772 (3)0.47852 (19)0.0270 (6)
C410.3362 (2)0.9746 (3)0.5098 (2)0.0296 (7)
C420.3589 (3)1.0992 (4)0.5502 (3)0.0555 (12)
H42A0.31221.13650.56210.083*
H42B0.37401.15350.50820.083*
H42C0.40571.09160.60750.083*
N50.19225 (16)0.5870 (2)0.29991 (17)0.0236 (6)
C510.1556 (2)0.5185 (3)0.2436 (2)0.0255 (7)
C520.1096 (3)0.4311 (4)0.1724 (2)0.0412 (9)
H52A0.06840.47780.12330.062*
H52B0.08230.36840.19750.062*
H52C0.14730.38810.14820.062*
N60.20712 (17)0.8590 (2)0.29706 (17)0.0246 (6)
C610.1785 (2)0.9455 (3)0.2550 (2)0.0248 (7)
C620.1419 (3)1.0573 (3)0.2014 (3)0.0402 (9)
H62A0.11841.11140.23640.060*
H62B0.09861.03130.14480.060*
H62C0.18421.10420.18710.060*
P10.06223 (6)0.25769 (8)0.91132 (6)0.0285 (2)
F110.0825 (3)0.1545 (4)0.8516 (3)0.1208 (17)
F120.0812 (3)0.1592 (4)0.9895 (3)0.1160 (17)
F130.0419 (2)0.3586 (3)0.8304 (2)0.0832 (11)
F140.1530 (2)0.3044 (5)0.9479 (4)0.1351 (19)
F150.0322 (2)0.2210 (4)0.8730 (3)0.1009 (13)
F160.0399 (2)0.3628 (3)0.97109 (18)0.0702 (9)
P20.60650 (6)0.79625 (9)0.70684 (7)0.0366 (2)
F210.6226 (4)0.8502 (5)0.8033 (3)0.154 (2)
F220.6603 (2)0.9020 (3)0.6859 (3)0.1093 (16)
F230.5515 (2)0.6870 (4)0.7266 (2)0.0805 (10)
F240.6838 (2)0.7085 (3)0.7493 (3)0.1051 (15)
F250.5273 (2)0.8800 (3)0.6621 (3)0.1024 (13)
F260.5853 (3)0.7330 (4)0.6089 (2)0.0873 (11)
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
Ni10.0157 (2)0.0130 (2)0.0168 (2)0.00060 (13)0.00374 (14)0.00083 (13)
N10.0241 (14)0.0277 (14)0.0349 (15)0.0070 (11)0.0155 (12)0.0090 (12)
C110.053 (2)0.045 (2)0.043 (2)0.0073 (18)0.0347 (19)0.0026 (17)
C120.034 (2)0.050 (2)0.078 (3)0.0101 (18)0.033 (2)0.005 (2)
C10.032 (2)0.062 (3)0.055 (2)0.0274 (19)0.0240 (19)0.030 (2)
C20.023 (3)0.036 (3)0.028 (3)0.011 (2)0.003 (2)0.005 (2)
C2'0.024 (4)0.022 (4)0.023 (4)0.007 (3)0.006 (3)0.003 (3)
N20.0240 (13)0.0201 (12)0.0176 (12)0.0036 (10)0.0050 (10)0.0023 (10)
C210.047 (4)0.014 (2)0.031 (3)0.009 (2)0.011 (2)0.007 (2)
C21'0.033 (5)0.036 (5)0.016 (4)0.005 (4)0.003 (3)0.001 (3)
C30.039 (3)0.028 (3)0.020 (2)0.010 (2)0.010 (2)0.007 (2)
C3'0.032 (5)0.027 (4)0.029 (4)0.001 (4)0.013 (4)0.010 (3)
C40.0335 (19)0.0374 (19)0.0314 (17)0.0028 (15)0.0193 (15)0.0078 (14)
N30.0201 (13)0.0229 (13)0.0263 (13)0.0020 (10)0.0093 (11)0.0010 (10)
C310.037 (2)0.0314 (19)0.053 (2)0.0029 (15)0.0269 (18)0.0076 (16)
C320.0155 (15)0.044 (2)0.0408 (19)0.0008 (14)0.0096 (14)0.0038 (16)
N40.0266 (14)0.0229 (14)0.0292 (14)0.0036 (11)0.0072 (11)0.0008 (11)
C410.0315 (18)0.0292 (18)0.0291 (16)0.0090 (14)0.0121 (14)0.0062 (14)
C420.072 (3)0.039 (2)0.061 (3)0.029 (2)0.030 (2)0.025 (2)
N50.0247 (14)0.0220 (13)0.0208 (13)0.0011 (11)0.0040 (11)0.0007 (11)
C510.0306 (17)0.0212 (15)0.0239 (15)0.0000 (13)0.0086 (13)0.0012 (13)
C520.054 (2)0.0325 (19)0.0303 (18)0.0126 (17)0.0063 (17)0.0101 (15)
N60.0264 (14)0.0220 (13)0.0230 (13)0.0022 (11)0.0059 (11)0.0043 (11)
C610.0272 (16)0.0255 (16)0.0215 (15)0.0039 (13)0.0085 (13)0.0012 (13)
C620.055 (2)0.0307 (19)0.0362 (19)0.0201 (17)0.0184 (18)0.0142 (15)
P10.0328 (5)0.0281 (4)0.0257 (4)0.0039 (4)0.0118 (4)0.0009 (3)
F110.194 (5)0.094 (3)0.097 (3)0.061 (3)0.079 (3)0.023 (2)
F120.187 (5)0.092 (3)0.084 (3)0.062 (3)0.066 (3)0.063 (2)
F130.113 (3)0.089 (2)0.0639 (18)0.032 (2)0.0519 (19)0.0411 (17)
F140.0301 (17)0.150 (4)0.206 (5)0.009 (2)0.019 (2)0.003 (4)
F150.057 (2)0.098 (3)0.132 (3)0.0344 (19)0.015 (2)0.023 (2)
F160.087 (2)0.0728 (19)0.0465 (15)0.0167 (16)0.0193 (14)0.0234 (13)
P20.0420 (6)0.0273 (5)0.0373 (5)0.0052 (4)0.0102 (4)0.0038 (4)
F210.240 (6)0.132 (4)0.066 (2)0.021 (4)0.024 (3)0.064 (3)
F220.063 (2)0.064 (2)0.173 (4)0.0286 (17)0.008 (2)0.052 (2)
F230.075 (2)0.099 (2)0.0649 (18)0.0377 (19)0.0205 (16)0.0212 (17)
F240.0484 (18)0.063 (2)0.177 (4)0.0078 (15)0.008 (2)0.045 (2)
F250.065 (2)0.066 (2)0.151 (4)0.0231 (17)0.009 (2)0.007 (2)
F260.117 (3)0.096 (3)0.065 (2)0.018 (2)0.052 (2)0.0248 (18)
Geometric parameters (Å, º) top
Ni1—N62.081 (3)C3'—H3B'0.9900
Ni1—N52.090 (3)C4—N31.503 (4)
Ni1—N22.093 (2)C4—H4A0.9900
Ni1—N42.125 (3)C4—H4B0.9900
Ni1—N12.200 (3)C4—H4A'0.9900
Ni1—N32.207 (3)C4—H4B'0.9900
N1—C111.494 (5)N3—C321.486 (4)
N1—C121.496 (5)N3—C311.492 (4)
N1—C11.502 (4)C31—H31A0.9800
C11—H11A0.9800C31—H31B0.9800
C11—H11B0.9800C31—H31C0.9800
C11—H11C0.9800C32—H32A0.9800
C12—H12A0.9800C32—H32B0.9800
C12—H12B0.9800C32—H32C0.9800
C12—H12C0.9800N4—C411.142 (4)
C1—C21.605 (7)C41—C421.458 (5)
C1—C2'1.655 (9)C42—H42A0.9800
C1—H1A0.9900C42—H42B0.9800
C1—H1B0.9900C42—H42C0.9800
C1—H1A'0.9900N5—C511.146 (4)
C1—H1B'0.9900C51—C521.455 (4)
C2—N21.480 (6)C52—H52A0.9800
C2—H2A0.9900C52—H52B0.9800
C2—H2B0.9900C52—H52C0.9800
C2'—N21.515 (8)N6—C611.137 (4)
C2'—H2A'0.9900C61—C621.461 (4)
C2'—H2B'0.9900C62—H62A0.9800
N2—C31.484 (6)C62—H62B0.9800
N2—C3'1.489 (9)C62—H62C0.9800
N2—C211.490 (6)P1—F121.556 (3)
N2—C21'1.514 (8)P1—F141.559 (4)
C21—H2C0.9800P1—F111.562 (3)
C21—H2D0.9800P1—F151.586 (3)
C21—H2E0.9800P1—F161.593 (3)
C21'—H2C'0.9800P1—F131.602 (3)
C21'—H2D'0.9800P2—F211.551 (4)
C21'—H2E'0.9800P2—F221.570 (3)
C3—C41.518 (7)P2—F241.577 (3)
C3—H3A0.9900P2—F251.580 (3)
C3—H3B0.9900P2—F261.598 (3)
C3'—C41.576 (10)P2—F231.602 (3)
C3'—H3A'0.9900
N6—Ni1—N587.88 (10)N2—C3—H3B109.7
N6—Ni1—N2177.41 (10)C4—C3—H3B109.7
N5—Ni1—N294.48 (10)H3A—C3—H3B108.2
N6—Ni1—N484.08 (11)N2—C3'—C4106.5 (5)
N5—Ni1—N4171.95 (10)N2—C3'—H3A'110.4
N2—Ni1—N493.56 (10)C4—C3'—H3A'110.4
N6—Ni1—N197.41 (10)N2—C3'—H3B'110.4
N5—Ni1—N190.71 (11)C4—C3'—H3B'110.4
N2—Ni1—N183.66 (10)H3A'—C3'—H3B'108.6
N4—Ni1—N190.32 (11)N3—C4—C3109.5 (3)
N6—Ni1—N394.90 (10)N3—C4—C3'111.6 (4)
N5—Ni1—N391.12 (10)C3—C4—C3'54.0 (4)
N2—Ni1—N383.99 (10)N3—C4—H4A109.8
N4—Ni1—N389.57 (10)C3—C4—H4A109.8
N1—Ni1—N3167.61 (10)C3'—C4—H4A58.2
C11—N1—C12106.9 (3)N3—C4—H4B109.8
C11—N1—C1108.8 (3)C3—C4—H4B109.8
C12—N1—C1109.6 (3)C3'—C4—H4B138.6
C11—N1—Ni1113.5 (2)H4A—C4—H4B108.2
C12—N1—Ni1112.4 (2)N3—C4—H4A'109.3
C1—N1—Ni1105.6 (2)C3—C4—H4A'141.2
N1—C11—H11A109.5C3'—C4—H4A'109.3
N1—C11—H11B109.5H4A—C4—H4A'54.8
H11A—C11—H11B109.5H4B—C4—H4A'56.6
N1—C11—H11C109.5N3—C4—H4B'109.3
H11A—C11—H11C109.5C3—C4—H4B'59.1
H11B—C11—H11C109.5C3'—C4—H4B'109.3
N1—C12—H12A109.5H4A—C4—H4B'140.8
N1—C12—H12B109.5H4B—C4—H4B'54.0
H12A—C12—H12B109.5H4A'—C4—H4B'108.0
N1—C12—H12C109.5C32—N3—C31106.6 (3)
H12A—C12—H12C109.5C32—N3—C4109.2 (3)
H12B—C12—H12C109.5C31—N3—C4109.5 (3)
N1—C1—C2108.9 (3)C32—N3—Ni1112.7 (2)
N1—C1—C2'107.6 (4)C31—N3—Ni1113.9 (2)
C2—C1—C2'59.5 (4)C4—N3—Ni1104.91 (19)
N1—C1—H1A109.9N3—C31—H31A109.5
C2—C1—H1A109.9N3—C31—H31B109.5
C2'—C1—H1A142.4H31A—C31—H31B109.5
N1—C1—H1B109.9N3—C31—H31C109.5
C2—C1—H1B109.9H31A—C31—H31C109.5
C2'—C1—H1B54.2H31B—C31—H31C109.5
H1A—C1—H1B108.3N3—C32—H32A109.5
N1—C1—H1A'110.2N3—C32—H32B109.5
C2—C1—H1A'53.6H32A—C32—H32B109.5
C2'—C1—H1A'110.2N3—C32—H32C109.5
H1A—C1—H1A'59.1H32A—C32—H32C109.5
H1B—C1—H1A'139.8H32B—C32—H32C109.5
N1—C1—H1B'110.2C41—N4—Ni1166.1 (3)
C2—C1—H1B'140.8N4—C41—C42178.0 (4)
C2'—C1—H1B'110.2C41—C42—H42A109.5
H1A—C1—H1B'52.7C41—C42—H42B109.5
H1B—C1—H1B'58.5H42A—C42—H42B109.5
H1A'—C1—H1B'108.5C41—C42—H42C109.5
N2—C2—C1105.5 (4)H42A—C42—H42C109.5
N2—C2—H2A110.6H42B—C42—H42C109.5
C1—C2—H2A110.6C51—N5—Ni1176.1 (3)
N2—C2—H2B110.6N5—C51—C52179.6 (4)
C1—C2—H2B110.6C51—C52—H52A109.5
H2A—C2—H2B108.8C51—C52—H52B109.5
N2—C2'—C1101.6 (5)H52A—C52—H52B109.5
N2—C2'—H2A'111.5C51—C52—H52C109.5
C1—C2'—H2A'111.5H52A—C52—H52C109.5
N2—C2'—H2B'111.5H52B—C52—H52C109.5
C1—C2'—H2B'111.5C61—N6—Ni1168.5 (3)
H2A'—C2'—H2B'109.3N6—C61—C62179.6 (4)
C2—N2—C3112.8 (4)C61—C62—H62A109.5
C2—N2—C3'151.8 (4)C61—C62—H62B109.5
C3—N2—C3'56.4 (4)H62A—C62—H62B109.5
C2—N2—C21110.6 (4)C61—C62—H62C109.5
C3—N2—C21110.0 (4)H62A—C62—H62C109.5
C3'—N2—C2159.2 (4)H62B—C62—H62C109.5
C2—N2—C21'50.6 (4)F12—P1—F1491.1 (3)
C3—N2—C21'62.5 (4)F12—P1—F1188.7 (2)
C3'—N2—C21'110.5 (5)F14—P1—F1191.5 (3)
C21—N2—C21'124.0 (4)F12—P1—F1592.0 (3)
C2—N2—C2'65.4 (4)F14—P1—F15175.7 (3)
C3—N2—C2'152.8 (4)F11—P1—F1591.6 (3)
C3'—N2—C2'111.2 (5)F12—P1—F1691.7 (2)
C21—N2—C2'52.1 (4)F14—P1—F1689.4 (2)
C21'—N2—C2'107.8 (5)F11—P1—F16179.0 (2)
C2—N2—Ni1102.9 (3)F15—P1—F1687.5 (2)
C3—N2—Ni1102.8 (2)F12—P1—F13179.5 (3)
C3'—N2—Ni1104.9 (4)F14—P1—F1389.4 (3)
C21—N2—Ni1117.4 (2)F11—P1—F1391.3 (2)
C21'—N2—Ni1118.3 (4)F15—P1—F1387.5 (2)
C2'—N2—Ni1104.0 (3)F16—P1—F1388.34 (18)
N2—C21—H2C109.5F21—P2—F2291.7 (3)
N2—C21—H2D109.5F21—P2—F2488.5 (3)
H2C—C21—H2D109.5F22—P2—F2491.44 (19)
N2—C21—H2E109.5F21—P2—F2593.0 (3)
H2C—C21—H2E109.5F22—P2—F2589.9 (2)
H2D—C21—H2E109.5F24—P2—F25177.9 (2)
N2—C21'—H2C'109.5F21—P2—F26175.6 (3)
N2—C21'—H2D'109.5F22—P2—F2692.7 (2)
H2C'—C21'—H2D'109.5F24—P2—F2691.7 (3)
N2—C21'—H2E'109.5F25—P2—F2686.6 (2)
H2C'—C21'—H2E'109.5F21—P2—F2389.3 (3)
H2D'—C21'—H2E'109.5F22—P2—F23179.0 (2)
N2—C3—C4109.8 (4)F24—P2—F2388.42 (19)
N2—C3—H3A109.7F25—P2—F2390.2 (2)
C4—C3—H3A109.7F26—P2—F2386.32 (19)
N6—Ni1—N1—C1165.5 (2)N5—Ni1—N2—C21'176.2 (5)
N5—Ni1—N1—C1122.4 (2)N4—Ni1—N2—C21'3.9 (5)
N2—Ni1—N1—C11116.8 (2)N1—Ni1—N2—C21'86.0 (5)
N4—Ni1—N1—C11149.6 (2)N3—Ni1—N2—C21'93.1 (5)
N3—Ni1—N1—C11120.9 (5)N5—Ni1—N2—C2'56.8 (4)
N6—Ni1—N1—C1256.0 (3)N4—Ni1—N2—C2'123.4 (4)
N5—Ni1—N1—C12143.9 (3)N1—Ni1—N2—C2'33.5 (4)
N2—Ni1—N1—C12121.6 (3)N3—Ni1—N2—C2'147.4 (4)
N4—Ni1—N1—C1228.1 (3)C2—N2—C3—C4164.0 (4)
N3—Ni1—N1—C12117.6 (5)C3'—N2—C3—C445.7 (5)
N6—Ni1—N1—C1175.4 (3)C21—N2—C3—C471.9 (4)
N5—Ni1—N1—C196.7 (3)C21'—N2—C3—C4169.3 (6)
N2—Ni1—N1—C12.2 (3)C2'—N2—C3—C4115.8 (9)
N4—Ni1—N1—C191.3 (3)Ni1—N2—C3—C453.9 (4)
N3—Ni1—N1—C11.9 (6)C2—N2—C3'—C4117.8 (9)
C11—N1—C1—C2150.4 (4)C3—N2—C3'—C442.5 (4)
C12—N1—C1—C293.0 (4)C21—N2—C3'—C4166.5 (7)
Ni1—N1—C1—C228.2 (4)C21'—N2—C3'—C475.4 (6)
C11—N1—C1—C2'87.4 (4)C2'—N2—C3'—C4165.0 (5)
C12—N1—C1—C2'156.0 (4)Ni1—N2—C3'—C453.1 (5)
Ni1—N1—C1—C2'34.8 (4)N2—C3—C4—N358.9 (4)
N1—C1—C2—N259.8 (5)N2—C3—C4—C3'44.1 (4)
C2'—C1—C2—N239.9 (4)N2—C3'—C4—N356.1 (6)
N1—C1—C2'—N264.0 (5)N2—C3'—C4—C342.9 (4)
C2—C1—C2'—N238.0 (4)C3—C4—N3—C32151.1 (3)
C1—C2—N2—C3168.2 (3)C3'—C4—N3—C3293.2 (5)
C1—C2—N2—C3'130.9 (9)C3—C4—N3—C3192.5 (4)
C1—C2—N2—C2168.1 (4)C3'—C4—N3—C31150.5 (4)
C1—C2—N2—C21'174.2 (7)C3—C4—N3—Ni130.1 (3)
C1—C2—N2—C2'41.6 (4)C3'—C4—N3—Ni127.9 (5)
C1—C2—N2—Ni158.1 (4)N6—Ni1—N3—C3262.5 (2)
C1—C2'—N2—C239.3 (4)N5—Ni1—N3—C3225.4 (2)
C1—C2'—N2—C3131.7 (8)N2—Ni1—N3—C32119.8 (2)
C1—C2'—N2—C3'171.2 (5)N4—Ni1—N3—C32146.5 (2)
C1—C2'—N2—C21172.8 (6)N1—Ni1—N3—C32123.9 (5)
C1—C2'—N2—C21'67.6 (6)N6—Ni1—N3—C3159.1 (2)
C1—C2'—N2—Ni158.8 (4)N5—Ni1—N3—C31147.1 (2)
N5—Ni1—N2—C2124.3 (3)N2—Ni1—N3—C31118.6 (2)
N4—Ni1—N2—C255.9 (3)N4—Ni1—N3—C3124.9 (2)
N1—Ni1—N2—C234.0 (3)N1—Ni1—N3—C31114.5 (5)
N3—Ni1—N2—C2145.1 (3)N6—Ni1—N3—C4178.8 (2)
N5—Ni1—N2—C3118.4 (3)N5—Ni1—N3—C493.3 (2)
N4—Ni1—N2—C361.5 (3)N2—Ni1—N3—C41.1 (2)
N1—Ni1—N2—C3151.4 (3)N4—Ni1—N3—C494.7 (2)
N3—Ni1—N2—C327.7 (3)N1—Ni1—N3—C45.2 (6)
N5—Ni1—N2—C3'60.1 (4)N6—Ni1—N4—C4116.6 (12)
N4—Ni1—N2—C3'119.7 (4)N2—Ni1—N4—C41162.4 (12)
N1—Ni1—N2—C3'150.3 (4)N1—Ni1—N4—C41114.0 (12)
N3—Ni1—N2—C3'30.5 (4)N3—Ni1—N4—C4178.4 (12)
N5—Ni1—N2—C212.5 (3)N5—Ni1—N6—C61139.9 (14)
N4—Ni1—N2—C21177.6 (3)N4—Ni1—N6—C6140.1 (14)
N1—Ni1—N2—C2187.7 (3)N1—Ni1—N6—C61129.7 (14)
N3—Ni1—N2—C2193.2 (3)N3—Ni1—N6—C6148.9 (14)

Experimental details

Crystal data
Chemical formula[Ni(C2H3N)3(C9H23N3)](PF6)2
Mr645.12
Crystal system, space groupMonoclinic, P21/c
Temperature (K)173
a, b, c (Å)17.4418 (8), 10.5913 (6), 15.7326 (8)
β (°) 110.921 (4)
V3)2714.7 (3)
Z4
Radiation typeMo Kα
µ (mm1)0.93
Crystal size (mm)0.38 × 0.17 × 0.14
Data collection
DiffractometerSTOE IPDS II two-circle-
diffractometer
Absorption correctionMulti-scan
(MULABS; Spek, 2003; Blessing, 1995)
Tmin, Tmax0.719, 0.881
No. of measured, independent and
observed [I > 2σ(I)] reflections
33712, 5076, 4263
Rint0.081
(sin θ/λ)max1)0.609
Refinement
R[F2 > 2σ(F2)], wR(F2), S 0.048, 0.130, 1.04
No. of reflections5076
No. of parameters357
H-atom treatmentH-atom parameters constrained
Δρmax, Δρmin (e Å3)0.83, 0.46

Computer programs: X-AREA (Stoe & Cie, 2001), SHELXS97 (Sheldrick, 1990), SHELXL97 (Sheldrick, 1997), XP in SHELXTL-Plus (Sheldrick, 1991), SHELXL97 and PLATON (Spek, 2003).

 

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