Bis(diethyl-enetriamine)-cobalt(III) hexa-chloridoindate(III).

The title compound, [Co(C(4)H(13)N(3))(2)][InCl(6)], was synthesized under hydro-thermal conditions. In the cation, the Co-N bond lengths lie in the range 1.967 (2)-1.9684 (15) Å. In the anion, the In(III) atom is coordinated by six Cl atoms resulting in a slightly distorted octa-hedral geometry. Both metal atoms are located on special positions of site symmetry 2/m. Furthermore, one Cl atom and one N atom are located on a mirror plane. N-H⋯Cl hydrogen bonds between cations and anions consolidate the crystal packing.

Related literature

For the use of chiral metal complexes as templates in the synthesis of open-framework metal phosphates and germanates, see: Stalder & Wilkinson (1997 ▶); Wang et al. (2003a ▶,b ▶); Pan et al. (2005 ▶, 2008 ▶). For the introduction of chiral metal complexes into coordination polymers, see: Pan et al. (2010a ▶,b ▶, 2011 ▶); Tong & Pan (2011 ▶). For In—Cl bond lengths in other hexa­chloridoindium compounds, see: Rothammel et al. (1998 ▶).

Experimental

Crystal data

[Co(C4H13N3)2][InCl6]

M = 592.80

Orthorhombic,

a = 10.8925 (5) Å

b = 14.7291 (7) Å

c = 12.2205 (6) Å

V = 1960.62 (16) Å3

Z = 4

Mo Kα radiation

μ = 2.84 mm−1

T = 296 K

0.20 × 0.18 × 0.15 mm

Data collection

Bruker SMART APEX CCD area-detector diffractometer

Absorption correction: multi-scan (SADABS; Bruker, 2002 ▶) T min = 0.572, T max = 0.653

6910 measured reflections

1282 independent reflections

1139 reflections with I > 2σ(I)

R int = 0.021

Refinement

R[F 2 > 2σ(F 2)] = 0.018

wR(F 2) = 0.046

S = 1.06

1282 reflections

57 parameters

H-atom parameters constrained

Δρmax = 0.34 e Å−3

Δρmin = −0.37 e Å−3

Data collection: APEX2 (Bruker, 2002 ▶); cell refinement: SAINT (Bruker, 2002 ▶); data reduction: SAINT; program(s) used to solve structure: SHELXS97 (Sheldrick, 2008 ▶); program(s) used to refine structure: SHELXL97 (Sheldrick, 2008 ▶); molecular graphics: SHELXTL (Sheldrick, 2008 ▶); software used to prepare material for publication: SHELXTL.

Crystal structure: contains datablocks I, global. DOI: 10.1107/S1600536811016758/vm2092sup1.cif

Structure factors: contains datablocks I. DOI: 10.1107/S1600536811016758/vm2092Isup2.hkl

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

[Co(C4H13N3)2][InCl6]	F(000) = 1176
Mr = 592.80	Dx = 2.008 Mg m−3
Orthorhombic, Cccm	Mo Kα radiation, λ = 0.71073 Å
Hall symbol: -C 2 2c	θ = 2.3–28.3°
a = 10.8925 (5) Å	µ = 2.84 mm−1
b = 14.7291 (7) Å	T = 296 K
c = 12.2205 (6) Å	Block, yellow
V = 1960.62 (16) Å3	0.2 × 0.18 × 0.15 mm
Z = 4

Bruker SMART APEX CCD area-detector diffractometer	1282 independent reflections
Radiation source: fine-focus sealed tube	1139 reflections with I > 2σ(I)
graphite	Rint = 0.021
Detector resolution: 5.00cm pixels mm-1	θmax = 28.3°, θmin = 2.3°
φ and ω scans	h = −14→11
Absorption correction: multi-scan (SADABS; Bruker, 2002)	k = −19→18
Tmin = 0.572, Tmax = 0.653	l = −12→16
6910 measured reflections

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)] = 0.018	Hydrogen site location: inferred from neighbouring sites
wR(F2) = 0.046	H-atom parameters constrained
S = 1.06	w = 1/[σ2(Fo2) + (0.0179P)2 + 3.2797P] where P = (Fo2 + 2Fc2)/3
1282 reflections	(Δ/σ)max < 0.001
57 parameters	Δρmax = 0.34 e Å−3
0 restraints	Δρmin = −0.37 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 > 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
In1	−0.2500	−0.2500	0.0000	0.02018 (8)
Co1	−0.2500	0.2500	0.0000	0.01769 (10)
Cl1	−0.38483 (5)	−0.31981 (4)	0.14285 (4)	0.03547 (12)
Cl2	−0.38713 (6)	−0.11293 (4)	0.0000	0.03569 (17)
N1	−0.35382 (15)	0.19629 (10)	0.11486 (13)	0.0265 (3)
H1A	−0.3447	0.2282	0.1772	0.080*
H1B	−0.4331	0.1999	0.0945	0.080*
N2	−0.1606 (2)	0.13392 (14)	0.0000	0.0228 (4)
H2	−0.0789	0.1466	0.0000	0.080*
C1	−0.18921 (19)	0.08352 (13)	0.10310 (16)	0.0289 (4)
H1C	−0.1353	0.1041	0.1612	0.080*
H1D	−0.1753	0.0191	0.0921	0.080*
C2	−0.32142 (19)	0.09943 (13)	0.13544 (17)	0.0295 (4)
H2A	−0.3748	0.0601	0.0931	0.080*
H2B	−0.3326	0.0853	0.2123	0.080*

	U11	U22	U33	U12	U13	U23
In1	0.01848 (12)	0.02348 (13)	0.01860 (12)	0.00027 (9)	0.000	0.000
Co1	0.0176 (2)	0.0165 (2)	0.0190 (2)	−0.00096 (17)	0.000	0.000
Cl1	0.0303 (2)	0.0454 (3)	0.0307 (2)	−0.0003 (2)	0.0080 (2)	0.0119 (2)
Cl2	0.0245 (3)	0.0231 (3)	0.0595 (5)	0.0016 (2)	0.000	0.000
N1	0.0266 (8)	0.0242 (7)	0.0286 (8)	−0.0011 (6)	0.0058 (6)	0.0023 (6)
N2	0.0220 (10)	0.0210 (10)	0.0255 (11)	0.0000 (8)	0.000	0.000
C1	0.0342 (10)	0.0247 (9)	0.0277 (9)	0.0031 (8)	−0.0027 (8)	0.0049 (7)
C2	0.0352 (11)	0.0234 (9)	0.0298 (10)	−0.0029 (8)	0.0031 (8)	0.0056 (7)

In1—Cl1i	2.5024 (5)	N1—C2	1.491 (2)
In1—Cl1ii	2.5024 (5)	N1—H1A	0.9000
In1—Cl1	2.5024 (5)	N1—H1B	0.9000
In1—Cl1iii	2.5024 (5)	N2—C1i	1.495 (2)
In1—Cl2iii	2.5114 (7)	N2—C1	1.495 (2)
In1—Cl2	2.5114 (7)	N2—H2	0.9100
Co1—N2	1.967 (2)	C1—C2	1.512 (3)
Co1—N2iv	1.967 (2)	C1—H1C	0.9700
Co1—N1i	1.9684 (15)	C1—H1D	0.9700
Co1—N1v	1.9684 (15)	C2—H2A	0.9700
Co1—N1iv	1.9684 (15)	C2—H2B	0.9700
Co1—N1	1.9684 (15)
Cl1i—In1—Cl1ii	180.0	N1i—Co1—N1	90.97 (10)
Cl1i—In1—Cl1	88.48 (3)	N1v—Co1—N1	89.03 (10)
Cl1ii—In1—Cl1	91.52 (3)	N1iv—Co1—N1	180.00 (8)
Cl1i—In1—Cl1iii	91.52 (3)	C2—N1—Co1	111.65 (12)
Cl1ii—In1—Cl1iii	88.48 (3)	C2—N1—H1A	109.3
Cl1—In1—Cl1iii	180.0	Co1—N1—H1A	109.3
Cl1i—In1—Cl2iii	91.076 (16)	C2—N1—H1B	109.3
Cl1ii—In1—Cl2iii	88.924 (17)	Co1—N1—H1B	109.3
Cl1—In1—Cl2iii	91.076 (16)	H1A—N1—H1B	108.0
Cl1iii—In1—Cl2iii	88.924 (17)	C1i—N2—C1	114.8 (2)
Cl1i—In1—Cl2	88.924 (17)	C1i—N2—Co1	109.18 (12)
Cl1ii—In1—Cl2	91.076 (16)	C1—N2—Co1	109.18 (12)
Cl1—In1—Cl2	88.924 (17)	C1i—N2—H2	107.8
Cl1iii—In1—Cl2	91.076 (16)	C1—N2—H2	107.8
Cl2iii—In1—Cl2	180.0	Co1—N2—H2	107.8
N2—Co1—N2iv	180.0	N2—C1—C2	109.98 (16)
N2—Co1—N1i	86.27 (6)	N2—C1—H1C	109.7
N2iv—Co1—N1i	93.73 (6)	C2—C1—H1C	109.7
N2—Co1—N1v	93.73 (6)	N2—C1—H1D	109.7
N2iv—Co1—N1v	86.27 (6)	C2—C1—H1D	109.7
N1i—Co1—N1v	180.00 (10)	H1C—C1—H1D	108.2
N2—Co1—N1iv	93.73 (6)	N1—C2—C1	109.24 (15)
N2iv—Co1—N1iv	86.27 (6)	N1—C2—H2A	109.8
N1i—Co1—N1iv	89.03 (10)	C1—C2—H2A	109.8
N1v—Co1—N1iv	90.97 (10)	N1—C2—H2B	109.8
N2—Co1—N1	86.27 (6)	C1—C2—H2B	109.8
N2iv—Co1—N1	93.73 (6)	H2A—C2—H2B	108.3

D—H···A	D—H	H···A	D···A	D—H···A
N1—H1A···Cl1vi	0.90	2.62	3.4915 (17)	164
N1—H1B···Cl2vii	0.90	2.61	3.3823 (18)	144
N1—H1B···Cl1viii	0.90	2.72	3.3957 (17)	133
N2—H2···Cl1ix	0.91	2.79	3.5407 (19)	141
N2—H2···Cl1x	0.91	2.79	3.5407 (19)	141

Table 1

Hydrogen-bond geometry (Å, °)

D—H⋯A	D—H	H⋯A	D⋯A	D—H⋯A
N1—H1A⋯Cl1i	0.90	2.62	3.4915 (17)	164
N1—H1B⋯Cl2ii	0.90	2.61	3.3823 (18)	144
N1—H1B⋯Cl1iii	0.90	2.72	3.3957 (17)	133
N2—H2⋯Cl1iv	0.91	2.79	3.5407 (19)	141
N2—H2⋯Cl1v	0.91	2.79	3.5407 (19)	141

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