[Bis(3-amino-prop-yl)amine-κN,N',N'']bis-(thio-cyanato-κN)cobalt(II).

The asymmetric unit of the title compound, [Co(NCS)(2)(C(6)H(17)N(3))], consists of one Co(2+) cation, two thio-cyanate anions and one bis-(3-amino-prop-yl)amine ligand, all in general positions. The cobalt cation is coordinated by five N atoms of two terminal N-bonded thio-cyanate anions and one bis-(3-amino-prop-yl)amine ligand, defining a slightly distorted square-pyramidal coordination polyhedron. The mol-ecules are held together in the crystal by weak N-H⋯S inter-actions.

Related literature

For isostructural compounds with copper(II) and cadmium(II) but with an alternate setting of the space group, see: Cannas et al. (1974 ▶, 1977 ▶). For background to thermal decomposition reactions and the resulting inter­mediates, see: Boeckmann & Näther (2010 ▶, 2011 ▶); Boeckmann et al. (2011 ▶); Wöhlert et al. (2011 ▶); Wriedt et al. (2009a ▶,b ▶); Wriedt & Näther (2010 ▶).

Experimental

Crystal data

[Co(NCS)2(C6H17N3)]

M = 306.32

Monoclinic,

a = 7.5515 (4) Å

b = 14.2250 (11) Å

c = 12.8825 (8) Å

β = 103.091 (7)°

V = 1347.88 (15) Å3

Z = 4

Mo Kα radiation

μ = 1.57 mm−1

T = 170 K

0.11 × 0.08 × 0.06 mm

Data collection

Stoe IPDS-1 diffractometer

Absorption correction: numerical (X-SHAPE and X-RED32; Stoe & Cie, 2008 ▶) T min = 0.856, T max = 0.905

15883 measured reflections

3234 independent reflections

2832 reflections with I > 2σ(I)

R int = 0.043

Refinement

R[F 2 > 2σ(F 2)] = 0.027

wR(F 2) = 0.070

S = 1.04

3234 reflections

146 parameters

H-atom parameters constrained

Δρmax = 0.33 e Å−3

Δρmin = −0.51 e Å−3

Data collection: X-AREA (Stoe & Cie, 2008 ▶); cell refinement: X-AREA; data reduction: X-AREA; 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 ▶) and DIAMOND (Brandenburg, 2011 ▶); software used to prepare material for publication: SHELXL97.

Crystal structure: contains datablock(s) I, global. DOI: 10.1107/S1600536811025876/bt5568sup1.cif

Structure factors: contains datablock(s) I. DOI: 10.1107/S1600536811025876/bt5568Isup2.hkl

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

[Co(NCS)2(C6H17N3)]	F(000) = 636
Mr = 306.32	Dx = 1.509 Mg m−3
Monoclinic, P21/n	Mo Kα radiation, λ = 0.71073 Å
Hall symbol: -P 2yn	Cell parameters from 8000 reflections
a = 7.5515 (4) Å	θ = 3.2–28.1°
b = 14.2250 (11) Å	µ = 1.57 mm−1
c = 12.8825 (8) Å	T = 170 K
β = 103.091 (7)°	Block, violet
V = 1347.88 (15) Å3	0.11 × 0.08 × 0.06 mm
Z = 4

Stoe IPDS-1 diffractometer	3234 independent reflections
Radiation source: fine-focus sealed tube	2832 reflections with I > 2σ(I)
graphite	Rint = 0.043
φ scans	θmax = 28.1°, θmin = 3.2°
Absorption correction: numerical (X-SHAPE and X-RED32; Stoe & Cie, 2008)	h = −9→9
Tmin = 0.856, Tmax = 0.905	k = −18→18
15883 measured reflections	l = −16→17

Refinement on F2	Secondary atom site location: difference Fourier map
Least-squares matrix: full	Hydrogen site location: inferred from neighbouring sites
R[F2 > 2σ(F2)] = 0.027	H-atom parameters constrained
wR(F2) = 0.070	w = 1/[σ2(Fo2) + (0.0414P)2 + 0.3919P] where P = (Fo2 + 2Fc2)/3
S = 1.04	(Δ/σ)max = 0.002
3234 reflections	Δρmax = 0.33 e Å−3
146 parameters	Δρmin = −0.51 e Å−3
0 restraints	Extinction correction: SHELXL97 (Sheldrick, 2008), Fc*=kFc[1+0.001xFc2λ3/sin(2θ)]-1/4
Primary atom site location: structure-invariant direct methods	Extinction coefficient: 0.0069 (15)

Geometry. All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds 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 > 2sigma(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
Co1	0.56529 (3)	0.529621 (13)	0.677913 (16)	0.01799 (9)
N1	0.70311 (18)	0.40562 (9)	0.66179 (10)	0.0210 (3)
H1A	0.6229	0.3651	0.6195	0.025*
H1B	0.7930	0.4192	0.6264	0.025*
N2	0.42397 (18)	0.45541 (10)	0.78508 (11)	0.0231 (3)
H2	0.3396	0.4158	0.7426	0.028*
N3	0.32593 (19)	0.60251 (10)	0.61765 (11)	0.0260 (3)
H3A	0.3495	0.6483	0.5722	0.031*
H3B	0.2434	0.5615	0.5779	0.031*
C1	0.7876 (2)	0.35590 (11)	0.76221 (14)	0.0265 (3)
H1C	0.8689	0.3995	0.8108	0.032*
H1D	0.8619	0.3028	0.7463	0.032*
C2	0.6429 (3)	0.31937 (12)	0.81595 (14)	0.0300 (4)
H2A	0.7001	0.2748	0.8727	0.036*
H2B	0.5521	0.2839	0.7629	0.036*
C3	0.5447 (3)	0.39473 (13)	0.86483 (13)	0.0301 (4)
H3C	0.4711	0.3640	0.9097	0.036*
H3D	0.6362	0.4348	0.9119	0.036*
C4	0.3199 (3)	0.51944 (14)	0.84044 (15)	0.0349 (4)
H4A	0.4057	0.5638	0.8851	0.042*
H4B	0.2627	0.4817	0.8886	0.042*
C5	0.1732 (3)	0.57537 (16)	0.76589 (18)	0.0420 (5)
H5A	0.0926	0.5308	0.7182	0.050*
H5B	0.0987	0.6078	0.8090	0.050*
C6	0.2402 (3)	0.64767 (13)	0.69795 (16)	0.0355 (4)
H6A	0.1368	0.6870	0.6611	0.043*
H6B	0.3298	0.6892	0.7442	0.043*
N11	0.6789 (2)	0.58506 (10)	0.55469 (12)	0.0293 (3)
C11	0.7699 (2)	0.61541 (10)	0.50112 (12)	0.0199 (3)
S11	0.89760 (6)	0.65832 (3)	0.42551 (3)	0.03094 (12)
N21	0.70829 (19)	0.60345 (10)	0.80127 (12)	0.0274 (3)
C21	0.7925 (2)	0.63897 (11)	0.87783 (13)	0.0225 (3)
S21	0.91711 (7)	0.68852 (4)	0.98333 (4)	0.03999 (14)

	U11	U22	U33	U12	U13	U23
Co1	0.01799 (12)	0.01756 (12)	0.01939 (12)	0.00138 (7)	0.00625 (8)	0.00026 (7)
N1	0.0237 (6)	0.0202 (6)	0.0208 (6)	0.0026 (5)	0.0087 (5)	0.0013 (5)
N2	0.0225 (6)	0.0295 (7)	0.0195 (6)	−0.0052 (5)	0.0092 (5)	−0.0009 (5)
N3	0.0243 (7)	0.0301 (7)	0.0233 (7)	0.0076 (5)	0.0046 (5)	−0.0032 (5)
C1	0.0242 (8)	0.0232 (7)	0.0312 (9)	0.0032 (6)	0.0045 (6)	0.0086 (6)
C2	0.0363 (9)	0.0226 (8)	0.0311 (9)	−0.0039 (6)	0.0074 (7)	0.0103 (6)
C3	0.0369 (9)	0.0345 (9)	0.0202 (8)	−0.0070 (7)	0.0096 (7)	0.0065 (6)
C4	0.0370 (10)	0.0456 (10)	0.0297 (9)	−0.0021 (8)	0.0235 (8)	−0.0041 (7)
C5	0.0280 (9)	0.0571 (13)	0.0476 (12)	0.0059 (8)	0.0227 (8)	−0.0088 (9)
C6	0.0339 (9)	0.0371 (9)	0.0370 (10)	0.0144 (7)	0.0111 (8)	−0.0093 (8)
N11	0.0329 (8)	0.0246 (7)	0.0344 (8)	0.0023 (5)	0.0163 (6)	0.0078 (6)
C11	0.0211 (7)	0.0172 (6)	0.0210 (7)	0.0004 (5)	0.0039 (6)	−0.0016 (5)
S11	0.0279 (2)	0.0411 (2)	0.0277 (2)	−0.00521 (17)	0.01443 (17)	0.00238 (17)
N21	0.0255 (7)	0.0272 (7)	0.0292 (7)	−0.0064 (5)	0.0053 (6)	−0.0037 (6)
C21	0.0211 (7)	0.0203 (7)	0.0275 (8)	−0.0004 (5)	0.0081 (6)	0.0015 (6)
S21	0.0455 (3)	0.0373 (3)	0.0297 (2)	0.0007 (2)	−0.0071 (2)	−0.00828 (18)

Co1—N21	2.0043 (14)	C2—C3	1.519 (3)
Co1—N3	2.0758 (13)	C2—H2A	0.9900
Co1—N1	2.0822 (13)	C2—H2B	0.9900
Co1—N11	2.1201 (14)	C3—H3C	0.9900
Co1—N2	2.1970 (13)	C3—H3D	0.9900
N1—C1	1.486 (2)	C4—C5	1.517 (3)
N1—H1A	0.9200	C4—H4A	0.9900
N1—H1B	0.9200	C4—H4B	0.9900
N2—C3	1.486 (2)	C5—C6	1.510 (3)
N2—C4	1.487 (2)	C5—H5A	0.9900
N2—H2	0.9300	C5—H5B	0.9900
N3—C6	1.485 (2)	C6—H6A	0.9900
N3—H3A	0.9200	C6—H6B	0.9900
N3—H3B	0.9200	N11—C11	1.162 (2)
C1—C2	1.512 (2)	C11—S11	1.6362 (16)
C1—H1C	0.9900	N21—C21	1.161 (2)
C1—H1D	0.9900	C21—S21	1.6280 (17)
N21—Co1—N3	107.58 (6)	C1—C2—C3	114.74 (14)
N21—Co1—N1	109.34 (6)	C1—C2—H2A	108.6
N3—Co1—N1	142.97 (5)	C3—C2—H2A	108.6
N21—Co1—N11	99.33 (6)	C1—C2—H2B	108.6
N3—Co1—N11	89.99 (6)	C3—C2—H2B	108.6
N1—Co1—N11	86.80 (5)	H2A—C2—H2B	107.6
N21—Co1—N2	90.27 (6)	N2—C3—C2	113.84 (13)
N3—Co1—N2	88.24 (6)	N2—C3—H3C	108.8
N1—Co1—N2	88.88 (5)	C2—C3—H3C	108.8
N11—Co1—N2	170.33 (6)	N2—C3—H3D	108.8
C1—N1—Co1	116.24 (10)	C2—C3—H3D	108.8
C1—N1—H1A	108.2	H3C—C3—H3D	107.7
Co1—N1—H1A	108.2	N2—C4—C5	114.03 (15)
C1—N1—H1B	108.2	N2—C4—H4A	108.7
Co1—N1—H1B	108.2	C5—C4—H4A	108.7
H1A—N1—H1B	107.4	N2—C4—H4B	108.7
C3—N2—C4	109.42 (13)	C5—C4—H4B	108.7
C3—N2—Co1	113.85 (10)	H4A—C4—H4B	107.6
C4—N2—Co1	113.08 (10)	C6—C5—C4	115.58 (16)
C3—N2—H2	106.7	C6—C5—H5A	108.4
C4—N2—H2	106.7	C4—C5—H5A	108.4
Co1—N2—H2	106.7	C6—C5—H5B	108.4
C6—N3—Co1	115.82 (11)	C4—C5—H5B	108.4
C6—N3—H3A	108.3	H5A—C5—H5B	107.4
Co1—N3—H3A	108.3	N3—C6—C5	111.42 (15)
C6—N3—H3B	108.3	N3—C6—H6A	109.3
Co1—N3—H3B	108.3	C5—C6—H6A	109.3
H3A—N3—H3B	107.4	N3—C6—H6B	109.3
N1—C1—C2	110.50 (13)	C5—C6—H6B	109.3
N1—C1—H1C	109.5	H6A—C6—H6B	108.0
C2—C1—H1C	109.6	C11—N11—Co1	167.72 (14)
N1—C1—H1D	109.5	N11—C11—S11	179.86 (18)
C2—C1—H1D	109.5	C21—N21—Co1	174.01 (14)
H1C—C1—H1D	108.1	N21—C21—S21	177.91 (15)

D—H···A	D—H	H···A	D···A	D—H···A
N1—H1A···S21i	0.92	2.82	3.6177 (14)	145
N1—H1B···S11ii	0.92	2.80	3.5665 (14)	142
N2—H2···S11iii	0.93	2.69	3.5903 (15)	162
N3—H3A···S21iv	0.92	2.69	3.5839 (16)	165

Table 1

Hydrogen-bond geometry (Å, °)

D—H⋯A	D—H	H⋯A	D⋯A	D—H⋯A
N1—H1A⋯S21i	0.92	2.82	3.6177 (14)	145
N1—H1B⋯S11ii	0.92	2.80	3.5665 (14)	142
N2—H2⋯S11iii	0.93	2.69	3.5903 (15)	162
N3—H3A⋯S21iv	0.92	2.69	3.5839 (16)	165

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