Tetra-methyl-ammonium borohydride from powder data.

In the crystal structure of the title compound, C(4)H(12)N(+)·BH(4) (-), the tetra-methyl-ammonium cations are situated on special positions with site symmetry [Formula: see text]m2. The borohydride anions are situated on special positions with 4mm site symmetry and show rotational disorder around the fourfold axis.

Related literature

For details of the synthesis, see: Banus et al. (1952 ▶); King et al. (1956 ▶). For previous studies of the title compound, see: Harmon et al. (1974 ▶); Eckert et al. (2004 ▶). The isostructural compounds (CH3)4NClO4 and (CH3)4NBF4 were reported by McCullough (1964 ▶) and Giuseppetti et al. (1992 ▶), respectively. For applications of the title compound, see: Evans et al. (1988 ▶).

Experimental

Crystal data

C4H12N+·BH4 −

M = 88.99

Tetragonal,

a = 7.9133 (2) Å

c = 5.65696 (17) Å

V = 354.24 (2) Å3

Z = 2

Cu Kα radiation, λ = 1.54051, 1.54433 Å

μ = 0.33 mm−1

T = 298 K

cylinder, 18 × 1 mm

Data collection

Bruker D8 Discover diffractometer

Specimen mounting: quartz capillary

Data collection mode: transmission

Scan method: continuous

2θmin = 8°, 2θmax = 121°, 2θstep = 0.012°

Refinement

R p = 0.014

R wp = 0.020

R exp = 0.007

R Bragg = 0.053

χ2 = 7.673

9220 data points

56 parameters

14 restraints

H atoms treated by a mixture of independent and constrained refinement

Data collection: DIFFRACplus (Bruker, 2006 ▶); cell refinement: X-CELL (Neumann, 2003 ▶) and JANA2006 (Petricek et al., 2006 ▶); data reduction: DIFFRACplus; program(s) used to solve structure: JANA2006; program(s) used to refine structure: JANA2006; molecular graphics: CrystalMaker (Palmer, 2005 ▶); software used to prepare material for publication: publCIF (Westrip, 2010 ▶).

Crystal structure: contains datablock(s) global, I. DOI: 10.1107/S1600536811029291/cv5120sup1.cif

Supplementary material file. DOI: 10.1107/S1600536811029291/cv5120Isup2.cml

Rietveld powder data: contains datablock(s) I. DOI: 10.1107/S1600536811029291/cv5120Isup2.rtv

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

Enhanced figure: interactive version of Fig. 1

C4H12N+·BH4−	F(000) = 104
Mr = 88.99	Dx = 0.834 Mg m−3Dm = 0.813 Mg m−3Dm measured by helium pycnometry (Banus et al., 1952)
Tetragonal, P4/nmm	Cu Kα radiation, λ = 1.54051, 1.54433 Å
Hall symbol: -P 4a 2a	µ = 0.33 mm−1
a = 7.9133 (2) Å	T = 298 K
c = 5.65696 (17) Å	white
V = 354.24 (2) Å3	cylinder, 18 × 1 mm
Z = 2	Specimen preparation: Prepared at 298 K

Bruker D8 Discover diffractometer	Data collection mode: transmission
none	Scan method: continuous
Specimen mounting: quartz capillary	2θmin = 8°, 2θmax = 120.999°, 2θstep = 0.012°

Rp = 0.014	14 restraints
Rwp = 0.020	2 constraints
Rexp = 0.007	All H-atom parameters refined
RBragg = 0.053	Weighting scheme based on measured s.u.'s w = 1/[σ2(I) + 0.0016I2]
χ2 = 7.673	(Δ/σ)max = 0.009
9220 data points	Background function: 25 Legendre polynoms
Profile function: Pseudo-Voigt	Preferred orientation correction: none
56 parameters

	x	y	z	Uiso*/Ueq	Occ. (<1)
H4	0.315 (2)	0.363 (4)	0.957 (3)	0.14971 (4)*	0.25
H2	0.1457 (17)	0.5963 (4)	0.2429 (17)	0.10060 (2)*
B1	0.25	0.25	0.8925 (14)	0.084 (5)
H3	0.25	0.25	0.702 (4)	0.14971 (4)*
C1	0.25	0.5959 (3)	0.3460 (5)	0.065 (2)
H1	0.25	0.492 (2)	0.4477 (19)	0.10060 (2)*
H5	0.25	0.119 (5)	0.957 (3)	0.14971 (4)*	0.25
N1	0.25	0.75	0.5	0.045 (3)

	U11	U22	U33	U12	U13	U23
B1	0.100 (7)	0.100 (7)	0.053 (9)	0	0	0
C1	0.084 (4)	0.036 (3)	0.075 (4)	0	0	−0.013 (3)
N1	0.045 (4)	0.045 (4)	0.045 (7)	0	0	0

B1—H3	1.08 (2)	C1—H1	1.004 (15)
B1—H4	1.10 (3)	C1—H2	1.010 (12)
B1—H5	1.10 (4)	C1—N1	1.498 (3)
H1—C1—H2	109.5 (5)	H4—B1—H4ii	109.5 (16)
H2—C1—N1	109.5 (4)	H4—B1—H5iii	109.5 (12)
H2—C1—H2i	109.5 (9)	C1—N1—C1iv	108.91 (14)
H3—B1—H5	109.5 (12)	C1—N1—C1v	109.75 (7)
H4—B1—H3	109.5 (10)