Bis(triethyl-ammonium) tetra-chlorido-cobaltate(II).

The crystal structure of the title compound, (C(6)H(16)N)(2)[CoCl(4)], is comprised of a tetrahedral [CoCl(4)](2-) anion and two independent triethyl-ammonium cations. The latter are featureless while the [CoCl(4)](2-) anion exhibits typical Co-Cl bond lengths [2.2428 (15)-2.2847 (16) Å] and a Cl-Co-Cl angular range of 107.58 (6)-112.73 (7)°. In the crystal, N-H⋯Cl hydrogen bonds between the two crystallographically independent cations and the [CoCl(4)](2-) anion generate discrete ion triplets. The two Co-Cl bonds involved in these inter-actions are slightly longer than the remaining two.

Related literature

For the crystal structure of a related complex, see: Clegg & Martin (2007 ▶).

Experimental

Crystal data

(C6H16N)2[CoCl4]

M = 405.13

Orthorhombic,

a = 11.981 (5) Å

b = 13.226 (5) Å

c = 25.946 (10) Å

V = 4112 (3) Å3

Z = 8

Mo Kα radiation

μ = 1.35 mm−1

T = 296 K

0.18 × 0.14 × 0.13 mm

Data collection

Bruker APEXII CCD diffractometer

Absorption correction: multi-scan (SADABS; Bruker, 2007 ▶) T min = 0.661, T max = 0.745

42005 measured reflections

4090 independent reflections

2078 reflections with I > 2σ(I)

R int = 0.117

Refinement

R[F 2 > 2σ(F 2)] = 0.052

wR(F 2) = 0.119

S = 1.00

4090 reflections

180 parameters

1 restraint

H atoms treated by a mixture of independent and constrained refinement

Δρmax = 0.45 e Å−3

Δρmin = −0.51 e Å−3

Data collection: APEX2 (Bruker, 2007 ▶); cell refinement: SAINT (Bruker, 2007 ▶); data reduction: SAINT; program(s) used to solve structure: SHELXS97 (Sheldrick, 2008 ▶); program(s) used to refine structure: SHELXL97 (Sheldrick, 2008 ▶); molecular graphics: XP in SHELXTL (Sheldrick, 2008 ▶); software used to prepare material for publication: SHELXTL.

Crystal structure: contains datablock(s) I, global. DOI: 10.1107/S1600536812022441/bg2461sup1.cif

Structure factors: contains datablock(s) I. DOI: 10.1107/S1600536812022441/bg2461Isup2.hkl

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

(C6H16N)2[CoCl4]	F(000) = 1704
Mr = 405.13	Dx = 1.309 Mg m−3
Orthorhombic, Pbca	Mo Kα radiation, λ = 0.71073 Å
Hall symbol: -P 2ac 2ab	Cell parameters from 3697 reflections
a = 11.981 (5) Å	θ = 2.3–19.2°
b = 13.226 (5) Å	µ = 1.35 mm−1
c = 25.946 (10) Å	T = 296 K
V = 4112 (3) Å3	Irregular, green
Z = 8	0.18 × 0.14 × 0.13 mm

Bruker APEXII CCD diffractometer	4090 independent reflections
Radiation source: fine-focus sealed tube	2078 reflections with I > 2σ(I)
Graphite monochromator	Rint = 0.117
φ and ω scans	θmax = 26.1°, θmin = 1.6°
Absorption correction: multi-scan (SADABS; Bruker, 2007)	h = −14→12
Tmin = 0.661, Tmax = 0.745	k = −16→16
42005 measured reflections	l = −32→32

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)] = 0.052	Hydrogen site location: inferred from neighbouring sites
wR(F2) = 0.119	H atoms treated by a mixture of independent and constrained refinement
S = 1.00	w = 1/[σ2(Fo2) + (0.0298P)2 + 6.2054P] where P = (Fo2 + 2Fc2)/3
4090 reflections	(Δ/σ)max < 0.001
180 parameters	Δρmax = 0.45 e Å−3
1 restraint	Δρmin = −0.51 e Å−3

Geometry. All s.u.'s (except the s.u. in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell s.u.'s are taken into account individually in the estimation of s.u.'s in distances, angles and torsion angles; correlations between s.u.'s in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell s.u.'s is used for estimating s.u.'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
Co	0.05270 (5)	0.21711 (5)	0.12639 (2)	0.0501 (2)
Cl1	−0.02174 (14)	0.34750 (11)	0.08048 (6)	0.0963 (6)
Cl2	−0.06848 (12)	0.08799 (10)	0.12358 (5)	0.0758 (4)
Cl4	0.08198 (12)	0.25981 (12)	0.21063 (5)	0.0840 (5)
Cl3	0.21929 (11)	0.17851 (12)	0.09060 (5)	0.0786 (4)
N1	0.2550 (4)	0.4391 (4)	0.23571 (17)	0.0634 (12)
N2	0.1187 (4)	0.3092 (3)	−0.02326 (17)	0.0593 (12)
C2	0.3882 (5)	0.3716 (5)	0.1714 (2)	0.106 (2)
H2A	0.4369	0.3915	0.1438	0.159*
H2B	0.3332	0.3252	0.1585	0.159*
H2C	0.4310	0.3393	0.1980	0.159*
C1	0.3327 (6)	0.4609 (5)	0.1925 (2)	0.098 (2)
H1A	0.2913	0.4938	0.1651	0.118*
H1B	0.3891	0.5080	0.2044	0.118*
C3	0.3132 (5)	0.4070 (6)	0.2830 (2)	0.106 (2)
H3A	0.3725	0.3609	0.2734	0.127*
H3B	0.3478	0.4660	0.2985	0.127*
C4	0.2438 (5)	0.3579 (5)	0.3221 (2)	0.099 (2)
H4A	0.2892	0.3396	0.3511	0.149*
H4B	0.2104	0.2982	0.3078	0.149*
H4C	0.1862	0.4036	0.3331	0.149*
C6	0.1254 (8)	0.5774 (8)	0.2169 (4)	0.207 (6)
H6A	0.0886	0.6314	0.2349	0.311*
H6B	0.0705	0.5342	0.2013	0.311*
H6C	0.1727	0.6051	0.1906	0.311*
C5	0.1830 (8)	0.5274 (7)	0.2479 (4)	0.188 (5)
H5A	0.1314	0.5041	0.2742	0.225*
H5B	0.2315	0.5760	0.2647	0.225*
C10	0.2315 (6)	0.4566 (4)	0.0047 (3)	0.121 (3)
H10A	0.3066	0.4816	0.0066	0.182*
H10B	0.2003	0.4532	0.0387	0.182*
H10C	0.1874	0.5013	−0.0161	0.182*
C9	0.2319 (5)	0.3537 (5)	−0.0188 (2)	0.0868 (18)
H9A	0.2651	0.3575	−0.0528	0.104*
H9B	0.2780	0.3093	0.0020	0.104*
C7	0.1263 (5)	0.2003 (4)	−0.0402 (2)	0.0769 (17)
H7A	0.1468	0.1980	−0.0764	0.092*
H7B	0.1847	0.1669	−0.0207	0.092*
C8	0.0190 (5)	0.1446 (4)	−0.0327 (2)	0.095 (2)
H8A	0.0279	0.0758	−0.0437	0.143*
H8B	−0.0386	0.1763	−0.0527	0.143*
H8C	−0.0011	0.1460	0.0031	0.143*
C12	0.0734 (7)	0.3786 (5)	−0.1106 (2)	0.137 (3)
H12A	0.0194	0.4182	−0.1291	0.206*
H12B	0.0776	0.3122	−0.1254	0.206*
H12C	0.1451	0.4107	−0.1128	0.206*
C11	0.0390 (5)	0.3705 (4)	−0.0550 (2)	0.0858 (18)
H11A	0.0336	0.4379	−0.0405	0.103*
H11B	−0.0344	0.3398	−0.0532	0.103*
H2	0.089 (3)	0.310 (3)	0.0084 (17)	0.052 (14)*
H1	0.212 (4)	0.394 (4)	0.2253 (18)	0.055 (17)*

	U11	U22	U33	U12	U13	U23
Co	0.0547 (4)	0.0482 (4)	0.0476 (3)	−0.0002 (3)	0.0041 (3)	−0.0008 (3)
Cl1	0.1149 (13)	0.0708 (10)	0.1032 (12)	0.0411 (9)	0.0525 (10)	0.0382 (9)
Cl2	0.0832 (10)	0.0699 (9)	0.0741 (9)	−0.0231 (8)	−0.0188 (8)	0.0107 (7)
Cl4	0.0758 (9)	0.1138 (12)	0.0623 (8)	−0.0229 (9)	0.0088 (7)	−0.0328 (8)
Cl3	0.0671 (9)	0.0994 (11)	0.0693 (9)	0.0168 (8)	0.0126 (7)	−0.0066 (8)
N1	0.064 (3)	0.067 (3)	0.059 (3)	0.001 (3)	0.015 (3)	0.003 (2)
N2	0.067 (3)	0.057 (3)	0.053 (3)	0.008 (2)	0.020 (2)	0.005 (2)
C2	0.116 (5)	0.098 (5)	0.104 (5)	−0.016 (4)	0.050 (4)	−0.020 (4)
C1	0.116 (5)	0.089 (5)	0.091 (4)	−0.009 (4)	0.053 (4)	0.002 (4)
C3	0.079 (4)	0.166 (7)	0.072 (4)	−0.027 (5)	−0.013 (4)	−0.005 (4)
C4	0.088 (4)	0.143 (6)	0.066 (4)	−0.001 (4)	−0.009 (4)	0.022 (4)
C6	0.188 (10)	0.214 (11)	0.220 (11)	0.125 (9)	0.093 (8)	0.125 (9)
C5	0.222 (11)	0.164 (8)	0.178 (9)	0.113 (8)	0.118 (8)	0.064 (7)
C10	0.103 (5)	0.063 (4)	0.199 (8)	−0.020 (4)	0.031 (5)	−0.003 (5)
C9	0.067 (4)	0.084 (5)	0.109 (5)	0.001 (3)	0.027 (4)	0.026 (4)
C7	0.099 (5)	0.067 (4)	0.065 (3)	0.029 (3)	0.012 (3)	0.001 (3)
C8	0.118 (5)	0.077 (4)	0.091 (4)	−0.010 (4)	−0.013 (4)	−0.013 (4)
C12	0.220 (9)	0.112 (6)	0.080 (5)	0.032 (6)	−0.019 (5)	0.036 (4)
C11	0.088 (4)	0.062 (4)	0.107 (5)	0.023 (3)	0.003 (4)	0.017 (3)

Co—Cl2	2.2428 (15)	C6—C5	1.250 (9)
Co—Cl3	2.2597 (16)	C6—H6A	0.9600
Co—Cl1	2.2778 (16)	C6—H6B	0.9600
Co—Cl4	2.2847 (16)	C6—H6C	0.9600
N1—C3	1.474 (7)	C5—H5A	0.9700
N1—C1	1.486 (6)	C5—H5B	0.9700
N1—C5	1.486 (8)	C10—C9	1.492 (8)
N1—H1	0.84 (4)	C10—H10A	0.9600
N2—C9	1.483 (7)	C10—H10B	0.9600
N2—C11	1.498 (6)	C10—H10C	0.9600
N2—C7	1.508 (6)	C9—H9A	0.9700
N2—H2	0.90 (4)	C9—H9B	0.9700
C2—C1	1.462 (7)	C7—C8	1.494 (7)
C2—H2A	0.9600	C7—H7A	0.9700
C2—H2B	0.9600	C7—H7B	0.9700
C2—H2C	0.9600	C8—H8A	0.9600
C1—H1A	0.9700	C8—H8B	0.9600
C1—H1B	0.9700	C8—H8C	0.9600
C3—C4	1.464 (7)	C12—C11	1.503 (8)
C3—H3A	0.9700	C12—H12A	0.9600
C3—H3B	0.9700	C12—H12B	0.9600
C4—H4A	0.9600	C12—H12C	0.9600
C4—H4B	0.9600	C11—H11A	0.9700
C4—H4C	0.9600	C11—H11B	0.9700
Cl2—Co—Cl3	112.73 (7)	C5—C6—H6C	109.5
Cl2—Co—Cl1	107.82 (7)	H6A—C6—H6C	109.5
Cl3—Co—Cl1	107.58 (6)	H6B—C6—H6C	109.5
Cl2—Co—Cl4	108.58 (6)	C6—C5—N1	126.8 (9)
Cl3—Co—Cl4	108.26 (6)	C6—C5—H5A	105.6
Cl1—Co—Cl4	111.92 (7)	N1—C5—H5A	105.6
C3—N1—C1	112.8 (5)	C6—C5—H5B	105.6
C3—N1—C5	108.9 (6)	N1—C5—H5B	105.6
C1—N1—C5	111.8 (5)	H5A—C5—H5B	106.1
C3—N1—H1	111 (3)	C9—C10—H10A	109.5
C1—N1—H1	106 (3)	C9—C10—H10B	109.5
C5—N1—H1	106 (3)	H10A—C10—H10B	109.5
C9—N2—C11	114.3 (4)	C9—C10—H10C	109.5
C9—N2—C7	110.2 (4)	H10A—C10—H10C	109.5
C11—N2—C7	113.2 (4)	H10B—C10—H10C	109.5
C9—N2—H2	107 (3)	N2—C9—C10	113.0 (5)
C11—N2—H2	104 (3)	N2—C9—H9A	109.0
C7—N2—H2	107 (3)	C10—C9—H9A	109.0
C1—C2—H2A	109.5	N2—C9—H9B	109.0
C1—C2—H2B	109.5	C10—C9—H9B	109.0
H2A—C2—H2B	109.5	H9A—C9—H9B	107.8
C1—C2—H2C	109.5	C8—C7—N2	112.4 (4)
H2A—C2—H2C	109.5	C8—C7—H7A	109.1
H2B—C2—H2C	109.5	N2—C7—H7A	109.1
C2—C1—N1	114.3 (5)	C8—C7—H7B	109.1
C2—C1—H1A	108.7	N2—C7—H7B	109.1
N1—C1—H1A	108.7	H7A—C7—H7B	107.9
C2—C1—H1B	108.7	C7—C8—H8A	109.5
N1—C1—H1B	108.7	C7—C8—H8B	109.5
H1A—C1—H1B	107.6	H8A—C8—H8B	109.5
C4—C3—N1	115.8 (5)	C7—C8—H8C	109.5
C4—C3—H3A	108.3	H8A—C8—H8C	109.5
N1—C3—H3A	108.3	H8B—C8—H8C	109.5
C4—C3—H3B	108.3	C11—C12—H12A	109.5
N1—C3—H3B	108.3	C11—C12—H12B	109.5
H3A—C3—H3B	107.4	H12A—C12—H12B	109.5
C3—C4—H4A	109.5	C11—C12—H12C	109.5
C3—C4—H4B	109.5	H12A—C12—H12C	109.5
H4A—C4—H4B	109.5	H12B—C12—H12C	109.5
C3—C4—H4C	109.5	N2—C11—C12	113.1 (5)
H4A—C4—H4C	109.5	N2—C11—H11A	109.0
H4B—C4—H4C	109.5	C12—C11—H11A	109.0
C5—C6—H6A	109.5	N2—C11—H11B	109.0
C5—C6—H6B	109.5	C12—C11—H11B	109.0
H6A—C6—H6B	109.5	H11A—C11—H11B	107.8
C3—N1—C1—C2	69.4 (8)	C11—N2—C9—C10	59.1 (7)
C5—N1—C1—C2	−167.5 (7)	C7—N2—C9—C10	−172.1 (5)
C1—N1—C3—C4	−163.6 (6)	C9—N2—C7—C8	165.6 (5)
C5—N1—C3—C4	71.6 (8)	C11—N2—C7—C8	−65.0 (6)
C3—N1—C5—C6	176.5 (11)	C9—N2—C11—C12	64.2 (7)
C1—N1—C5—C6	51.2 (14)	C7—N2—C11—C12	−63.1 (6)

D—H···A	D—H	H···A	D···A	D—H···A
N1—H1···Cl4	0.84 (4)	2.39 (5)	3.216 (6)	170 (4)
N2—H2···Cl1	0.90 (4)	2.34 (4)	3.214 (5)	163 (4)

Table 1

Hydrogen-bond geometry (Å, °)

D—H⋯A	D—H	H⋯A	D⋯A	D—H⋯A
N1—H1⋯Cl4	0.84 (4)	2.39 (5)	3.216 (6)	170 (4)
N2—H2⋯Cl1	0.90 (4)	2.34 (4)	3.214 (5)	163 (4)