Butane-1,4-di-ammonium hexa-fluoro-silicate.

The title compound, [NH3(CH2)4NH3](2+)·SiF6 (2-), is a hybrid built from an organic butane-1,4-di-ammonium dication linked to a hexa-fluoro-silicate mineral anion. Both ions posses inversion symmetry. In the anion the Si atom is located on an inversion center, while in the cation the center of inversion is situated at the mid-point of the central -CH2-CH2- bond. The Si atom is surrounded by six F atoms, forming a slightly distorted SiF6 (2-) octa-hedron. These octa-hedra are linked to the organic cations through N-H⋯F hydrogen bonds, forming a three-dimensional network.

Related literature

For background to potential physical properties, see: Ouasri et al. (2003 ▶); Elyoubi et al. (2004 ▶). For similar compounds, see: Jeghnou et al. (2005 ▶); Rhandour et al. (2011 ▶); Ouasri et al. (2012 ▶, 2013a ▶,b ▶, 2014 ▶).

Experimental

Crystal data

C4H14N2 2+·SiF6 2−

M = 232.26

Triclinic,

a = 5.796 (1) Å

b = 5.889 (1) Å

c = 7.774 (2) Å

α = 87.02 (1)°

β = 82.15 (1)°

γ = 61.87 (1)°

V = 231.79 (8) Å3

Z = 1

Mo Kα radiation

μ = 0.31 mm−1

T = 296 K

0.36 × 0.32 × 0.27 mm

Data collection

Bruker X8 APEX diffractometer

Absorption correction: multi-scan (SADABS; Bruker, 2009 ▶) T min = 0.512, T max = 0.640

5351 measured reflections

1285 independent reflections

1185 reflections with I > 2σ(I)

R int = 0.025

Refinement

R[F 2 > 2σ(F 2)] = 0.038

wR(F 2) = 0.108

S = 1.05

1285 reflections

61 parameters

H-atom parameters constrained

Δρmax = 0.74 e Å−3

Δρmin = −0.33 e Å−3

Data collection: APEX2 (Bruker, 2009 ▶); cell refinement: SAINT-Plus (Bruker, 2009 ▶); data reduction: SAINT-Plus; program(s) used to solve structure: SHELXS97 (Sheldrick, 2008 ▶); program(s) used to refine structure: SHELXL97 (Sheldrick, 2008 ▶); molecular graphics: ORTEP-3 for Windows (Farrugia, 2012 ▶); software used to prepare material for publication: PLATON (Spek, 2009 ▶) and publCIF (Westrip, 2010 ▶).

Crystal structure: contains datablock(s) I. DOI: 10.1107/S1600536814001068/im2447sup1.cif

Structure factors: contains datablock(s) I. DOI: 10.1107/S1600536814001068/im2447Isup2.hkl

CCDC reference:

Additional supporting information: crystallographic information; 3D view; checkCIF report

C4H14N22+·SiF62−	Z = 1
Mr = 232.26	F(000) = 120
Triclinic, p1	Dx = 1.664 Mg m−3
Hall symbol: -p 1	Mo Kα radiation, λ = 0.71073 Å
a = 5.796 (1) Å	Cell parameters from 1285 reflections
b = 5.889 (1) Å	θ = 3.9–29.6°
c = 7.774 (2) Å	µ = 0.31 mm−1
α = 87.02 (1)°	T = 296 K
β = 82.15 (1)°	Block, colourless
γ = 61.87 (1)°	0.36 × 0.32 × 0.27 mm
V = 231.79 (8) Å3

Bruker X8 APEX diffractometer	1285 independent reflections
Radiation source: fine-focus sealed tube	1185 reflections with I > 2σ(I)
Graphite monochromator	Rint = 0.025
φ and ω scans	θmax = 29.6°, θmin = 3.9°
Absorption correction: multi-scan (SADABS; Bruker, 2009)	h = −7→8
Tmin = 0.512, Tmax = 0.640	k = −8→8
5351 measured reflections	l = −10→10

Refinement on F2	Primary atom site location: structure-invariant direct methods
Least-squares matrix: full	Secondary atom site location: difference Fourier map
R[F2 > 2σ(F2)] = 0.038	Hydrogen site location: inferred from neighbouring sites
wR(F2) = 0.108	H-atom parameters constrained
S = 1.05	w = 1/[σ2(Fo2) + (0.0549P)2 + 0.127P] where P = (Fo2 + 2Fc2)/3
1285 reflections	(Δ/σ)max < 0.001
61 parameters	Δρmax = 0.74 e Å−3
0 restraints	Δρmin = −0.33 e Å−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 > 2σ(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
C1	−0.1629 (3)	0.2744 (4)	0.3650 (2)	0.0394 (4)
H1A	0.0138	0.2407	0.3801	0.047*
H1B	−0.1739	0.1160	0.3876	0.047*
C2	−0.3593 (4)	0.4783 (4)	0.4953 (2)	0.0435 (4)
H2A	−0.3573	0.6396	0.4663	0.052*
H2B	−0.3024	0.4297	0.6094	0.052*
N1	−0.2086 (2)	0.3508 (2)	0.18267 (15)	0.0269 (3)
H1NA	−0.0891	0.2252	0.1110	0.040*
H1NB	−0.1946	0.4939	0.1603	0.040*
H1NC	−0.3695	0.3792	0.1675	0.040*
Si1	0.5000	0.0000	0.0000	0.02400 (16)
F1	0.35813 (19)	0.26912 (18)	0.12542 (14)	0.0381 (3)
F2	0.3234 (2)	−0.1206 (2)	0.12259 (14)	0.0426 (3)
F3	0.2526 (2)	0.1424 (2)	−0.12459 (15)	0.0445 (3)

	U11	U22	U33	U12	U13	U23
C1	0.0304 (7)	0.0470 (9)	0.0266 (7)	−0.0069 (7)	−0.0029 (5)	0.0022 (6)
C2	0.0368 (9)	0.0649 (12)	0.0278 (7)	−0.0233 (8)	0.0014 (6)	−0.0109 (7)
N1	0.0262 (6)	0.0287 (6)	0.0236 (5)	−0.0117 (5)	0.0007 (4)	−0.0032 (4)
Si1	0.0193 (3)	0.0203 (3)	0.0312 (3)	−0.00873 (19)	0.00039 (18)	−0.00429 (18)
F1	0.0318 (5)	0.0310 (5)	0.0487 (6)	−0.0135 (4)	0.0061 (4)	−0.0182 (4)
F2	0.0412 (6)	0.0386 (5)	0.0505 (6)	−0.0251 (5)	0.0122 (4)	−0.0037 (4)
F3	0.0405 (6)	0.0350 (5)	0.0593 (7)	−0.0143 (4)	−0.0245 (5)	0.0034 (5)

C1—N1	1.4853 (19)	N1—H1NB	0.8900
C1—C2	1.512 (2)	N1—H1NC	0.8900
C1—H1A	0.9700	Si1—F2ii	1.6757 (10)
C1—H1B	0.9700	Si1—F2	1.6757 (10)
C2—C2i	1.519 (4)	Si1—F1	1.6886 (9)
C2—H2A	0.9700	Si1—F1ii	1.6886 (9)
C2—H2B	0.9700	Si1—F3	1.6908 (10)
N1—H1NA	0.8900	Si1—F3ii	1.6908 (10)
N1—C1—C2	112.70 (13)	H1NB—N1—H1NC	109.5
N1—C1—H1A	109.1	F2ii—Si1—F2	180.0
C2—C1—H1A	109.1	F2ii—Si1—F1	89.09 (5)
N1—C1—H1B	109.1	F2—Si1—F1	90.91 (5)
C2—C1—H1B	109.1	F2ii—Si1—F1ii	90.91 (5)
H1A—C1—H1B	107.8	F2—Si1—F1ii	89.09 (5)
C1—C2—C2i	114.65 (19)	F1—Si1—F1ii	180.0
C1—C2—H2A	108.6	F2ii—Si1—F3	91.03 (6)
C2i—C2—H2A	108.6	F2—Si1—F3	88.98 (6)
C1—C2—H2B	108.6	F1—Si1—F3	89.04 (6)
C2i—C2—H2B	108.6	F1ii—Si1—F3	90.96 (6)
H2A—C2—H2B	107.6	F2ii—Si1—F3ii	88.97 (6)
C1—N1—H1NA	109.5	F2—Si1—F3ii	91.02 (6)
C1—N1—H1NB	109.5	F1—Si1—F3ii	90.96 (6)
H1NA—N1—H1NB	109.5	F1ii—Si1—F3ii	89.04 (6)
C1—N1—H1NC	109.5	F3—Si1—F3ii	180.0
H1NA—N1—H1NC	109.5

D—H···A	D—H	H···A	D···A	D—H···A
N1—H1NA···F2	0.89	2.31	3.017 (2)	137
N1—H1NA···F3	0.89	2.39	3.134 (2)	142
N1—H1NB···F3iii	0.89	2.02	2.890 (2)	167
N1—H1NC···F1iv	0.89	2.04	2.864 (2)	154

Table 1

Hydrogen-bond geometry (Å, °)

D—H⋯A	D—H	H⋯A	D⋯A	D—H⋯A
N1—H1NA⋯F2	0.89	2.31	3.017 (2)	137
N1—H1NA⋯F3	0.89	2.39	3.134 (2)	142
N1—H1NB⋯F3i	0.89	2.02	2.890 (2)	167
N1—H1NC⋯F1ii	0.89	2.04	2.864 (2)	154

Symmetry codes: (i) ; (ii) .