cis-Chlorido(ethyl-amine)-bis-(propane-1,3-diamine)-cobalt(III) dichloride.

In the title compound, [CoCl(C2H7N)(C3H10N2)2]Cl2, the Co(III) ion has a distorted octa-hedral coordination environment and is surrounded by four N atoms in the equatorial plane, with the other N and Cl atoms occupying the axial positions. The crystal packing is stabilized by N-H⋯Cl hydrogen bonds, forming a layered arrangement parallel to (1-10).

Related literature

For supramolecular structures, see: Desiraju (1995 ▶); Khlobystov et al. (2001 ▶); Lehn (1995 ▶); Seo et al. (2000 ▶). For CoIII complexes, see: Chang et al. (2010 ▶). For related and comparable structures, see: Anbalagan et al. (2009 ▶); Lee et al. (2007 ▶); Ramesh et al. (2008 ▶); Ravichandran et al. (2009 ▶). For the preparation of (1,3-diamino­propane)­cobalt(III), see: Bailar & Work (1946 ▶).

Experimental

Crystal data

[CoCl(C2H7N)(C3H10N2)2]Cl2

M = 358.63

Triclinic,

a = 7.8847 (4) Å

b = 8.0627 (4) Å

c = 12.6526 (5) Å

α = 102.780 (3)°

β = 99.936 (4)°

γ = 92.580 (4)°

V = 769.76 (6) Å3

Z = 2

Mo Kα radiation

μ = 1.62 mm−1

T = 293 K

0.45 × 0.35 × 0.35 mm

Data collection

Oxford Diffraction Xcalibur Eos diffractometer

Absorption correction: multi-scan (CrysAlis PRO; Oxford Diffraction, 2009 ▶) T min = 0.600, T max = 1.000

4965 measured reflections

2711 independent reflections

2299 reflections with I > 2σ(I)

R int = 0.018

Refinement

R[F 2 > 2σ(F 2)] = 0.025

wR(F 2) = 0.060

S = 0.99

2711 reflections

194 parameters

H atoms treated by a mixture of independent and constrained refinement

Δρmax = 0.30 e Å−3

Δρmin = −0.35 e Å−3

Data collection: CrysAlis CCD (Oxford Diffraction, 2009 ▶); cell refinement: CrysAlis RED (Oxford Diffraction, 2009 ▶); data reduction: CrysAlis RED; 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 ▶) and PLATON (Spek, 2009 ▶); software used to prepare material for publication: PLATON.

Click here for additional data file.

Crystal structure: contains datablock(s) global, I. DOI: 10.1107/S1600536813004650/bt6888sup1.cif

Click here for additional data file.

Structure factors: contains datablock(s) I. DOI: 10.1107/S1600536813004650/bt6888Isup2.hkl

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

[CoCl(C2H7N)(C3H10N2)2]Cl2	Z = 2
Mr = 358.63	F(000) = 376
Triclinic, P1	Dx = 1.547 Mg m−3
Hall symbol: -P 1	Mo Kα radiation, λ = 0.71073 Å
a = 7.8847 (4) Å	Cell parameters from 2784 reflections
b = 8.0627 (4) Å	θ = 3.4–29.0°
c = 12.6526 (5) Å	µ = 1.62 mm−1
α = 102.780 (3)°	T = 293 K
β = 99.936 (4)°	Block, yellow
γ = 92.580 (4)°	0.45 × 0.35 × 0.35 mm
V = 769.76 (6) Å3

Oxford Diffraction Xcalibur Eos diffractometer	2711 independent reflections
Radiation source: fine-focus sealed tube	2299 reflections with I > 2σ(I)
Graphite monochromator	Rint = 0.018
ω scans	θmax = 25.0°, θmin = 2.8°
Absorption correction: multi-scan (CrysAlis PRO; Oxford Diffraction, 2009)	h = −9→9
Tmin = 0.600, Tmax = 1.000	k = −9→9
4965 measured reflections	l = −15→12

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)] = 0.025	Hydrogen site location: inferred from neighbouring sites
wR(F2) = 0.060	H atoms treated by a mixture of independent and constrained refinement
S = 0.99	w = 1/[σ2(Fo2) + (0.036P)2] where P = (Fo2 + 2Fc2)/3
2711 reflections	(Δ/σ)max = 0.001
194 parameters	Δρmax = 0.30 e Å−3
0 restraints	Δρmin = −0.35 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
C1	0.7176 (3)	0.6154 (3)	0.98937 (17)	0.0278 (5)
H1A	0.7705	0.6146	1.0644	0.033*
H1B	0.6287	0.5210	0.9632	0.033*
C2	0.6360 (3)	0.7792 (3)	0.98931 (16)	0.0289 (5)
H2A	0.7265	0.8717	1.0056	0.035*
H2B	0.5691	0.8005	1.0477	0.035*
C3	0.5193 (3)	0.7803 (3)	0.88121 (16)	0.0253 (5)
H3A	0.4308	0.6858	0.8637	0.030*
H3B	0.4622	0.8853	0.8896	0.030*
C4	1.0645 (3)	0.9053 (3)	0.74479 (16)	0.0364 (6)
H4A	1.1607	0.8388	0.7295	0.044*
H4B	1.1112	1.0209	0.7820	0.044*
C5	0.9486 (4)	0.9081 (3)	0.63747 (19)	0.0460 (7)
H5A	0.8456	0.9630	0.6526	0.055*
H5B	1.0082	0.9744	0.5975	0.055*
C6	0.8976 (3)	0.7309 (3)	0.56745 (17)	0.0359 (6)
H6A	0.8494	0.7373	0.4927	0.043*
H6B	0.9996	0.6683	0.5650	0.043*
C7	0.4777 (3)	0.3755 (3)	0.7108 (2)	0.0333 (5)
H7A	0.4207	0.4316	0.6557	0.040*
H7B	0.4483	0.4289	0.7811	0.040*
C8	0.4119 (3)	0.1879 (3)	0.6799 (2)	0.0432 (7)
H8A	0.2888	0.1776	0.6750	0.065*
H8B	0.4656	0.1326	0.7353	0.065*
H8C	0.4396	0.1349	0.6100	0.065*
N1	0.8505 (2)	0.5908 (2)	0.91895 (14)	0.0205 (4)
N2	0.6139 (2)	0.7664 (2)	0.78807 (14)	0.0202 (4)
N3	0.9726 (3)	0.8316 (2)	0.81887 (14)	0.0210 (4)
N4	0.7690 (3)	0.6375 (3)	0.61050 (14)	0.0223 (4)
N5	0.6662 (2)	0.3992 (2)	0.71863 (16)	0.0222 (4)
Cl1	1.03872 (7)	0.47044 (7)	0.74016 (4)	0.03006 (14)
Cl2	0.79985 (7)	0.17837 (6)	0.92229 (4)	0.02905 (14)
Cl3	0.36383 (7)	0.73553 (7)	0.55285 (4)	0.03125 (14)
Co1	0.80944 (3)	0.62246 (3)	0.766006 (19)	0.01506 (9)
H2C	0.543 (3)	0.741 (3)	0.7294 (17)	0.024 (6)*
H3C	0.926 (3)	0.908 (3)	0.8502 (17)	0.020 (7)*
H3D	1.052 (3)	0.797 (3)	0.8632 (17)	0.022 (6)*
H4D	0.685 (3)	0.678 (3)	0.5978 (17)	0.019 (7)*
H1C	0.882 (3)	0.490 (3)	0.9103 (16)	0.020 (6)*
H4C	0.756 (3)	0.532 (3)	0.5693 (16)	0.020 (6)*
H2D	0.652 (3)	0.867 (3)	0.7894 (17)	0.030 (7)*
H5D	0.693 (3)	0.360 (3)	0.659 (2)	0.037 (7)*
H1D	0.937 (3)	0.652 (3)	0.9535 (17)	0.024 (6)*
H5C	0.717 (3)	0.339 (3)	0.763 (2)	0.042 (8)*

	U11	U22	U33	U12	U13	U23
C1	0.0319 (13)	0.0330 (12)	0.0235 (11)	0.0038 (10)	0.0115 (10)	0.0120 (10)
C2	0.0376 (14)	0.0307 (12)	0.0203 (11)	0.0054 (10)	0.0138 (10)	0.0030 (9)
C3	0.0241 (12)	0.0242 (11)	0.0291 (11)	0.0077 (9)	0.0117 (9)	0.0033 (9)
C4	0.0341 (14)	0.0469 (15)	0.0264 (12)	−0.0202 (12)	0.0066 (11)	0.0086 (11)
C5	0.0562 (17)	0.0496 (16)	0.0346 (13)	−0.0224 (14)	0.0048 (12)	0.0233 (12)
C6	0.0319 (13)	0.0576 (16)	0.0186 (11)	−0.0099 (12)	0.0059 (10)	0.0113 (11)
C7	0.0252 (12)	0.0287 (12)	0.0428 (13)	−0.0039 (10)	0.0049 (11)	0.0037 (10)
C8	0.0386 (15)	0.0320 (14)	0.0556 (16)	−0.0137 (11)	0.0004 (13)	0.0130 (12)
N1	0.0189 (10)	0.0188 (10)	0.0230 (9)	0.0011 (8)	0.0022 (8)	0.0047 (8)
N2	0.0198 (10)	0.0212 (10)	0.0184 (9)	0.0030 (8)	0.0005 (8)	0.0039 (8)
N3	0.0210 (10)	0.0211 (10)	0.0206 (9)	−0.0018 (8)	0.0032 (8)	0.0051 (8)
N4	0.0196 (11)	0.0259 (11)	0.0188 (9)	−0.0004 (9)	0.0013 (8)	0.0021 (8)
N5	0.0224 (10)	0.0205 (9)	0.0213 (10)	−0.0017 (8)	0.0027 (8)	0.0016 (8)
Cl1	0.0230 (3)	0.0349 (3)	0.0332 (3)	0.0107 (2)	0.0084 (2)	0.0057 (2)
Cl2	0.0321 (3)	0.0204 (3)	0.0321 (3)	−0.0007 (2)	0.0000 (2)	0.0061 (2)
Cl3	0.0277 (3)	0.0351 (3)	0.0248 (3)	0.0028 (2)	0.0000 (2)	−0.0022 (2)
Co1	0.01382 (15)	0.01541 (15)	0.01497 (15)	0.00020 (10)	0.00225 (10)	0.00205 (10)

C1—N1	1.481 (3)	C7—H7A	0.9700
C1—C2	1.495 (3)	C7—H7B	0.9700
C1—H1A	0.9700	C8—H8A	0.9600
C1—H1B	0.9700	C8—H8B	0.9600
C2—C3	1.513 (3)	C8—H8C	0.9600
C2—H2A	0.9700	N1—Co1	1.9811 (17)
C2—H2B	0.9700	N1—H1C	0.85 (2)
C3—N2	1.486 (2)	N1—H1D	0.82 (2)
C3—H3A	0.9700	N2—Co1	1.9921 (18)
C3—H3B	0.9700	N2—H2C	0.83 (2)
C4—N3	1.483 (2)	N2—H2D	0.84 (2)
C4—C5	1.506 (3)	N3—Co1	1.9887 (17)
C4—H4A	0.9700	N3—H3C	0.79 (2)
C4—H4B	0.9700	N3—H3D	0.87 (2)
C5—C6	1.502 (3)	N4—Co1	1.9698 (18)
C5—H5A	0.9700	N4—H4D	0.76 (2)
C5—H5B	0.9700	N4—H4C	0.88 (2)
C6—N4	1.482 (3)	N5—Co1	1.9953 (16)
C6—H6A	0.9700	N5—H5D	0.82 (2)
C6—H6B	0.9700	N5—H5C	0.88 (3)
C7—N5	1.474 (3)	Cl1—Co1	2.2591 (6)
C7—C8	1.519 (3)
N1—C1—C2	112.37 (17)	H8B—C8—H8C	109.5
N1—C1—H1A	109.1	C1—N1—Co1	122.70 (14)
C2—C1—H1A	109.1	C1—N1—H1C	111.0 (14)
N1—C1—H1B	109.1	Co1—N1—H1C	102.2 (13)
C2—C1—H1B	109.1	C1—N1—H1D	106.7 (15)
H1A—C1—H1B	107.9	Co1—N1—H1D	108.1 (14)
C1—C2—C3	113.66 (17)	H1C—N1—H1D	105 (2)
C1—C2—H2A	108.8	C3—N2—Co1	124.93 (14)
C3—C2—H2A	108.8	C3—N2—H2C	108.5 (15)
C1—C2—H2B	108.8	Co1—N2—H2C	106.5 (15)
C3—C2—H2B	108.8	C3—N2—H2D	106.4 (15)
H2A—C2—H2B	107.7	Co1—N2—H2D	105.9 (16)
N2—C3—C2	112.96 (17)	H2C—N2—H2D	102 (2)
N2—C3—H3A	109.0	C4—N3—Co1	122.95 (13)
C2—C3—H3A	109.0	C4—N3—H3C	105.6 (15)
N2—C3—H3B	109.0	Co1—N3—H3C	109.9 (15)
C2—C3—H3B	109.0	C4—N3—H3D	105.5 (14)
H3A—C3—H3B	107.8	Co1—N3—H3D	100.6 (14)
N3—C4—C5	112.45 (18)	H3C—N3—H3D	112 (2)
N3—C4—H4A	109.1	C6—N4—Co1	120.95 (14)
C5—C4—H4A	109.1	C6—N4—H4D	105.3 (16)
N3—C4—H4B	109.1	Co1—N4—H4D	109.1 (16)
C5—C4—H4B	109.1	C6—N4—H4C	105.5 (13)
H4A—C4—H4B	107.8	Co1—N4—H4C	107.6 (13)
C6—C5—C4	111.3 (2)	H4D—N4—H4C	108 (2)
C6—C5—H5A	109.4	C7—N5—Co1	125.65 (15)
C4—C5—H5A	109.4	C7—N5—H5D	110.9 (17)
C6—C5—H5B	109.4	Co1—N5—H5D	100.9 (16)
C4—C5—H5B	109.4	C7—N5—H5C	109.0 (16)
H5A—C5—H5B	108.0	Co1—N5—H5C	103.4 (16)
N4—C6—C5	111.91 (19)	H5D—N5—H5C	105 (2)
N4—C6—H6A	109.2	N4—Co1—N1	176.20 (8)
C5—C6—H6A	109.2	N4—Co1—N3	94.63 (7)
N4—C6—H6B	109.2	N1—Co1—N3	88.27 (8)
C5—C6—H6B	109.2	N4—Co1—N2	88.57 (8)
H6A—C6—H6B	107.9	N1—Co1—N2	93.94 (7)
N5—C7—C8	111.9 (2)	N3—Co1—N2	89.27 (9)
N5—C7—H7A	109.2	N4—Co1—N5	88.27 (8)
C8—C7—H7A	109.2	N1—Co1—N5	88.62 (8)
N5—C7—H7B	109.2	N3—Co1—N5	173.98 (9)
C8—C7—H7B	109.2	N2—Co1—N5	96.09 (8)
H7A—C7—H7B	107.9	N4—Co1—Cl1	90.49 (7)
C7—C8—H8A	109.5	N1—Co1—Cl1	87.13 (6)
C7—C8—H8B	109.5	N3—Co1—Cl1	88.21 (7)
H8A—C8—H8B	109.5	N2—Co1—Cl1	177.23 (6)
C7—C8—H8C	109.5	N5—Co1—Cl1	86.49 (6)
H8A—C8—H8C	109.5
N1—C1—C2—C3	70.5 (2)	C1—N1—Co1—N5	−75.46 (17)
C1—C2—C3—N2	−64.4 (2)	C1—N1—Co1—Cl1	−162.02 (16)
N3—C4—C5—C6	−68.7 (3)	C4—N3—Co1—N4	−20.0 (2)
C4—C5—C6—N4	73.7 (3)	C4—N3—Co1—N1	157.5 (2)
C2—C1—N1—Co1	−48.3 (2)	C4—N3—Co1—N2	−108.52 (19)
C2—C3—N2—Co1	37.7 (2)	C4—N3—Co1—Cl1	70.34 (19)
C5—C4—N3—Co1	43.3 (3)	C3—N2—Co1—N4	161.39 (17)
C5—C6—N4—Co1	−51.5 (3)	C3—N2—Co1—N1	−15.75 (17)
C8—C7—N5—Co1	−175.91 (15)	C3—N2—Co1—N3	−103.96 (17)
C6—N4—Co1—N3	23.7 (2)	C3—N2—Co1—N5	73.28 (17)
C6—N4—Co1—N2	112.81 (19)	C7—N5—Co1—N4	−89.73 (19)
C6—N4—Co1—N5	−151.1 (2)	C7—N5—Co1—N1	92.47 (19)
C6—N4—Co1—Cl1	−64.58 (19)	C7—N5—Co1—N2	−1.35 (19)
C1—N1—Co1—N3	109.69 (17)	C7—N5—Co1—Cl1	179.67 (18)
C1—N1—Co1—N2	20.54 (17)

D—H···A	D—H	H···A	D···A	D—H···A
N2—H2D···Cl2i	0.84 (2)	2.77 (2)	3.5033 (19)	145.6 (18)
N3—H3C···Cl2i	0.79 (2)	2.49 (2)	3.275 (2)	168 (2)
N1—H1D···Cl2ii	0.82 (2)	2.52 (2)	3.3278 (19)	173.2 (18)
N3—H3D···Cl2ii	0.87 (2)	2.72 (2)	3.472 (2)	145.6 (18)
N4—H4C···Cl3iii	0.88 (2)	2.40 (2)	3.261 (2)	163.7 (19)
N5—H5D···Cl3iii	0.82 (2)	2.57 (2)	3.329 (2)	154 (2)

Table 1

Hydrogen-bond geometry (Å, °)

D—H⋯A	D—H	H⋯A	D⋯A	D—H⋯A
N2—H2D⋯Cl2i	0.84 (2)	2.77 (2)	3.5033 (19)	145.6 (18)
N3—H3C⋯Cl2i	0.79 (2)	2.49 (2)	3.275 (2)	168 (2)
N1—H1D⋯Cl2ii	0.82 (2)	2.52 (2)	3.3278 (19)	173.2 (18)
N3—H3D⋯Cl2ii	0.87 (2)	2.72 (2)	3.472 (2)	145.6 (18)
N4—H4C⋯Cl3iii	0.88 (2)	2.40 (2)	3.261 (2)	163.7 (19)
N5—H5D⋯Cl3iii	0.82 (2)	2.57 (2)	3.329 (2)	154 (2)

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