Tris(1,2-diamino-ethane)-nickel(II) hexa-fluoridosilicate.

The ionic title complex, [Ni(C(2)H(8)N(2))(3)](SiF(6)), is built up of [Ni(en)(3)](2+) complex cations (en = 1,2-diamino-ethane) and hexa-fluoridosilicate anions. Single crystals of the title complex were isolated from an aqueous-ethano-lic Ni(2+)-en-SiF(6) (2-) system. The Ni(II) and Si atoms are each located on a special position with site symmetry 3.2. The Ni(II) atom coordination sphere is octa-hedrally deformed, being coordinated by three chelating diamine ligands with an Ni-N distance of 2.1233 (18) Å. The crystal packing of the respective ions corresponds to the structure type of the hexa-gonal form of BN. Beside ionic forces, the packing is governed by N-H⋯F hydrogen bonds, which lead to the formation of hydro-phobic channels running along the 6(3) screw axis. The structure was refined as an inversion twin [0.49 (3): 0.51 (3)].

Related literature

For the hexa­fluoridosilicate anion acting as simple counter-ion, see: Li et al. (2009 ▶). For two nickel(II) complexes containing the hexa­fluoridosilicate anion as counter-ion, see: Spek et al. (1988 ▶); Wu et al. (2008 ▶). For complexes containing the [Ni(en)3]2+ complex cation and hexa­fluorido-type anions, see: Pan et al. (2005 ▶); Ribas et al. (1998 ▶); James et al. (1998 ▶); Contakes et al. (2000 ▶).

Experimental

Crystal data

[Ni(C2H8N2)3](SiF6)

M = 381.11

Hexagonal,

a = 9.1670 (9) Å

c = 9.763 (1) Å

V = 710.51 (12) Å3

Z = 2

Mo Kα radiation

μ = 1.52 mm−1

T = 291 K

0.42 × 0.21 × 0.15 mm

Data collection

Oxford Diffraction Xcalibur diffractometer with Sapphire2 detector

Absorption correction: numerical [Clark & Reid (1995 ▶) in CrysAlis PRO (Oxford Diffraction, 2009 ▶)] T min = 0.834, T max = 0.859

8628 measured reflections

554 independent reflections

489 reflections with I > 2σ(I)

R int = 0.050

Refinement

R[F 2 > 2σ(F 2)] = 0.027

wR(F 2) = 0.064

S = 1.07

554 reflections

33 parameters

H-atom parameters constrained

Δρmax = 0.68 e Å−3

Δρmin = −0.19 e Å−3

Absolute structure: Flack (1983 ▶), 89 Friedel pairs

Flack parameter: 0.49 (3)

Data collection: CrysAlis PRO (Oxford Diffraction, 2009 ▶); cell refinement: CrysAlis PRO; data reduction: CrysAlis PRO; program(s) used to solve structure: SHELXS97 (Sheldrick, 2008 ▶); program(s) used to refine structure: SHELXL97 (Sheldrick, 2008 ▶); molecular graphics: DIAMOND (Crystal Impact, 2007 ▶); software used to prepare material for publication: SHELXL97.

Crystal structure: contains datablocks I, Global. DOI: 10.1107/S1600536810041553/su2212sup1.cif

Structure factors: contains datablocks I. DOI: 10.1107/S1600536810041553/su2212Isup2.hkl

Additional supplementary materials: crystallographic information; 3D view; checkCIF report

[Ni(C2H8N2)3](SiF6)	Dx = 1.781 Mg m−3
Mr = 381.11	Mo Kα radiation, λ = 0.71069 Å
Hexagonal, P6322	Cell parameters from 8628 reflections
Hall symbol: P 6c 2c	θ = 2.6–27.4°
a = 9.1670 (9) Å	µ = 1.52 mm−1
c = 9.763 (1) Å	T = 291 K
V = 710.51 (12) Å3	Prism, pink
Z = 2	0.42 × 0.21 × 0.15 mm
F(000) = 396

Oxford Diffraction Xcalibur diffractometer with Sapphire2 detector	554 independent reflections
Radiation source: fine-focus sealed tube	489 reflections with I > 2σ(I)
graphite	Rint = 0.050
Detector resolution: 8.3438 pixels mm-1	θmax = 27.4°, θmin = 2.6°
ω scans	h = −11→11
Absorption correction: numerical [Clark & Reid (1995) in CrysAlis PRO (Oxford Diffraction, 2009)]	k = −11→11
Tmin = 0.834, Tmax = 0.859	l = −12→12
8628 measured reflections

Refinement on F2	Secondary atom site location: difference Fourier map
Least-squares matrix: full	Hydrogen site location: inferred from neighbouring sites
R[F2 > 2σ(F2)] = 0.027	H-atom parameters constrained
wR(F2) = 0.064	w = 1/[σ2(Fo2) + (0.0413P)2] where P = (Fo2 + 2Fc2)/3
S = 1.07	(Δ/σ)max < 0.001
554 reflections	Δρmax = 0.68 e Å−3
33 parameters	Δρmin = −0.19 e Å−3
0 restraints	Absolute structure: Flack (1983), 89 Friedel pairs
Primary atom site location: structure-invariant direct methods	Flack parameter: 0.49 (3)

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.

	x	y	z	Uiso*/Ueq
Ni1	0.3333	0.6667	0.2500	0.02783 (19)
N1	0.3156 (2)	0.4642 (2)	0.13146 (17)	0.0368 (4)
H1	0.3098	0.4839	0.0419	0.044*
H2	0.4076	0.4547	0.1449	0.044*
C1	0.1634 (3)	0.3071 (2)	0.1729 (2)	0.0432 (5)
H5	0.1732	0.2107	0.1455	0.052*
H6	0.0651	0.2992	0.1284	0.052*
Si1	0.6667	0.3333	0.2500	0.0267 (3)
F1	0.51790 (19)	0.18375 (19)	0.14983 (14)	0.0550 (4)

	U11	U22	U33	U12	U13	U23
Ni1	0.0286 (2)	0.0286 (2)	0.0262 (3)	0.01432 (11)	0.000	0.000
N1	0.0401 (10)	0.0429 (11)	0.0319 (9)	0.0241 (9)	0.0020 (8)	−0.0013 (8)
C1	0.0428 (16)	0.0339 (10)	0.0489 (12)	0.0162 (13)	−0.0016 (11)	−0.0079 (8)
Si1	0.0270 (3)	0.0270 (3)	0.0262 (5)	0.01349 (17)	0.000	0.000
F1	0.0521 (8)	0.0495 (8)	0.0489 (8)	0.0145 (6)	−0.0110 (7)	−0.0086 (7)

Ni1—N1i	2.1233 (18)	C1—C1iv	1.515 (4)
Ni1—N1ii	2.1233 (18)	C1—H5	0.9700
Ni1—N1iii	2.1233 (18)	C1—H6	0.9700
Ni1—N1iv	2.1233 (18)	Si1—F1vi	1.6812 (14)
Ni1—N1	2.1233 (18)	Si1—F1vii	1.6812 (14)
Ni1—N1v	2.1233 (18)	Si1—F1	1.6812 (14)
N1—C1	1.475 (2)	Si1—F1v	1.6812 (14)
N1—H1	0.9000	Si1—F1viii	1.6812 (14)
N1—H2	0.9000	Si1—F1ix	1.6812 (14)
N1i—Ni1—N1ii	81.62 (9)	N1—C1—C1iv	109.08 (16)
N1i—Ni1—N1iii	93.12 (7)	N1—C1—H5	109.9
N1ii—Ni1—N1iii	92.62 (10)	C1iv—C1—H5	109.9
N1i—Ni1—N1iv	92.62 (10)	N1—C1—H6	109.9
N1ii—Ni1—N1iv	93.12 (7)	C1iv—C1—H6	109.9
N1iii—Ni1—N1iv	172.42 (9)	H5—C1—H6	108.3
N1i—Ni1—N1	93.12 (7)	F1vi—Si1—F1vii	90.75 (10)
N1ii—Ni1—N1	172.42 (9)	F1vi—Si1—F1	90.12 (10)
N1iii—Ni1—N1	93.12 (6)	F1vii—Si1—F1	89.57 (7)
N1iv—Ni1—N1	81.62 (9)	F1vi—Si1—F1v	89.57 (7)
N1i—Ni1—N1v	172.42 (9)	F1vii—Si1—F1v	90.12 (10)
N1ii—Ni1—N1v	93.12 (7)	F1—Si1—F1v	179.56 (10)
N1iii—Ni1—N1v	81.62 (9)	F1vi—Si1—F1viii	89.57 (7)
N1iv—Ni1—N1v	93.12 (6)	F1vii—Si1—F1viii	179.56 (10)
N1—Ni1—N1v	92.62 (10)	F1—Si1—F1viii	90.75 (10)
C1—N1—Ni1	108.97 (13)	F1v—Si1—F1viii	89.57 (7)
C1—N1—H1	109.9	F1vi—Si1—F1ix	179.56 (10)
Ni1—N1—H1	109.9	F1vii—Si1—F1ix	89.57 (7)
C1—N1—H2	109.9	F1—Si1—F1ix	89.57 (7)
Ni1—N1—H2	109.9	F1v—Si1—F1ix	90.75 (10)
H1—N1—H2	108.3	F1viii—Si1—F1ix	90.12 (10)
N1i—Ni1—N1—C1	−78.08 (18)	N1v—Ni1—N1—C1	106.88 (16)
N1iii—Ni1—N1—C1	−171.38 (15)	Ni1—N1—C1—C1iv	−39.4 (3)
N1iv—Ni1—N1—C1	14.11 (12)

D—H···A	D—H	H···A	D···A	D—H···A
N1—H1···F1x	0.90	2.30	3.137 (2)	154
N1—H1···F1xi	0.90	2.48	3.235 (2)	142
N1—H2···F1ix	0.90	2.25	3.137 (2)	167

Table 1

Hydrogen-bond geometry (Å, °)

D—H⋯A	D—H	H⋯A	D⋯A	D—H⋯A
N1—H1⋯F1i	0.90	2.30	3.137 (2)	154
N1—H1⋯F1ii	0.90	2.48	3.235 (2)	142
N1—H2⋯F1iii	0.90	2.25	3.137 (2)	167

Symmetry codes: (i) ; (ii) ; (iii) .