Tri-chlorido-(1-ethyl-piperazin-1-ium)cobalt(II).

In the title complex, [Co(C6H15N2)Cl3], the Co(2+) ion is coordinated in a distorted tetra-hedral fashion by three chloride ions and one N atom of the piperazine ring; the ring adopts a chair conformation with the N-Co and N-CEt bonds in equatorial orientations. In the crystal, mol-ecules are connected by N-H⋯Cl hydrogen bonds, generating (10-1) sheets.

Related literature

For related structures, see: Ciccarese et al. (1998 ▶); Clemente et al. (1999 ▶); Marzotto et al. (2000 ▶).

Experimental

Crystal data

[Co(C6H15N2)Cl3]

M = 280.49

Monoclinic,

a = 7.421 (3) Å

b = 18.160 (7) Å

c = 8.691 (4) Å

β = 90.524 (7)°

V = 1171.1 (8) Å3

Z = 4

Mo Kα radiation

μ = 2.10 mm−1

T = 173 K

0.32 × 0.13 × 0.13 mm

Data collection

Rigaku XtaLAB mini diffractometer

Absorption correction: multi-scan (REQAB; Rigaku, 1998 ▶) T min = 0.529, T max = 0.761

11015 measured reflections

2399 independent reflections

2099 reflections with F 2 > 2σ(F 2)

R int = 0.025

Refinement

R[F 2 > 2σ(F 2)] = 0.022

wR(F 2) = 0.050

S = 1.08

2399 reflections

118 parameters

H atoms treated by a mixture of independent and constrained refinement

Δρmax = 0.27 e Å−3

Δρmin = −0.27 e Å−3

Data collection: CrystalClear-SM Expert (Rigaku, 2011 ▶); cell refinement: CrystalClear-SM Expert; data reduction: CrystalClear-SM Expert; program(s) used to solve structure: SIR2004 (Burla et al., 2005 ▶); program(s) used to refine structure: SHELXL97 (Sheldrick, 2008 ▶); molecular graphics: ORTEP-3 for Windows (Farrugia, 2012 ▶); software used to prepare material for publication: CrystalStructure (Rigaku, 2010 ▶).

Crystal structure: contains datablock(s) General, I. DOI: 10.1107/S1600536814006989/hb7215sup1.cif

Structure factors: contains datablock(s) I. DOI: 10.1107/S1600536814006989/hb7215Isup2.hkl

CCDC reference: 994292

Additional supporting information: crystallographic information; 3D view; checkCIF report

[Co(C6H15N2)Cl3]	F(000) = 572.00
Mr = 280.49	Dx = 1.591 Mg m−3
Monoclinic, P21/n	Mo Kα radiation, λ = 0.71075 Å
Hall symbol: -P 2yn	Cell parameters from 7042 reflections
a = 7.421 (3) Å	θ = 3.3–26.5°
b = 18.160 (7) Å	µ = 2.10 mm−1
c = 8.691 (4) Å	T = 173 K
β = 90.524 (7)°	Prism, blue
V = 1171.1 (8) Å3	0.32 × 0.13 × 0.13 mm
Z = 4

Rigaku XtaLAB mini diffractometer	2099 reflections with F2 > 2σ(F2)
Detector resolution: 6.849 pixels mm-1	Rint = 0.025
ω scans	θmax = 26.4°
Absorption correction: multi-scan (REQAB; Rigaku, 1998)	h = −9→9
Tmin = 0.529, Tmax = 0.761	k = −22→22
11015 measured reflections	l = −10→10
2399 independent reflections

Refinement on F2	Secondary atom site location: difference Fourier map
R[F2 > 2σ(F2)] = 0.022	Hydrogen site location: inferred from neighbouring sites
wR(F2) = 0.050	H atoms treated by a mixture of independent and constrained refinement
S = 1.08	w = 1/[σ2(Fo2) + (0.0195P)2 + 0.4P] where P = (Fo2 + 2Fc2)/3
2399 reflections	(Δ/σ)max = 0.001
118 parameters	Δρmax = 0.27 e Å−3
0 restraints	Δρmin = −0.27 e Å−3
Primary atom site location: structure-invariant direct methods

Geometry. ENTER SPECIAL DETAILS OF THE MOLECULAR GEOMETRY

Refinement. Refinement was performed using all reflections. The weighted R-factor (wR) and goodness of fit (S) are based on F2. R-factor (gt) are based on F. The threshold expression of F2 > 2.0 σ(F2) is used only for calculating R-factor (gt).

	x	y	z	Uiso*/Ueq
Co1	0.50887 (3)	0.124866 (12)	−0.13052 (2)	0.02446 (7)
Cl1	0.62618 (6)	0.22726 (2)	−0.24155 (5)	0.03456 (11)
Cl2	0.21414 (6)	0.13426 (3)	−0.07964 (6)	0.04714 (13)
Cl3	0.58634 (6)	0.02448 (2)	−0.27061 (5)	0.03491 (11)
N1	0.62169 (18)	0.11055 (8)	0.08596 (15)	0.0237 (3)
N2	0.87397 (18)	0.13728 (7)	0.34217 (15)	0.0235 (3)
C1	0.6034 (3)	0.17490 (9)	0.19013 (19)	0.0301 (4)
C2	0.6795 (3)	0.15991 (10)	0.34991 (19)	0.0306 (4)
C3	0.8943 (3)	0.07188 (9)	0.23786 (19)	0.0306 (4)
C4	0.8130 (3)	0.08778 (10)	0.07959 (19)	0.0318 (4)
C5	0.9516 (3)	0.12430 (10)	0.50161 (19)	0.0324 (4)
C6	1.1522 (3)	0.10910 (10)	0.5011 (3)	0.0393 (5)
H1A	0.4743	0.1880	0.1985	0.0361*
H1B	0.6670	0.2176	0.1450	0.0361*
H2A	0.6688	0.2048	0.4137	0.0367*
H2B	0.6089	0.1203	0.3993	0.0367*
H2	0.932 (3)	0.1733 (10)	0.3034 (19)	0.022 (5)*
H3A	0.8333	0.0288	0.2837	0.0367*
H3B	1.0237	0.0598	0.2272	0.0367*
H4A	0.8835	0.1273	0.0298	0.0381*
H4B	0.8227	0.0430	0.0151	0.0381*
H5A	0.9283	0.1682	0.5660	0.0389*
H5B	0.8890	0.0820	0.5490	0.0389*
H6A	1.2141	0.1487	0.4461	0.0472*
H6B	1.1749	0.0620	0.4497	0.0472*
H6C	1.1974	0.1068	0.6073	0.0472*
H1	0.566 (3)	0.0763 (11)	0.128 (3)	0.032 (6)*

	U11	U22	U33	U12	U13	U23
Co1	0.02308 (12)	0.02612 (12)	0.02421 (12)	−0.00175 (8)	0.00169 (8)	−0.00177 (9)
Cl1	0.0399 (3)	0.0238 (2)	0.0403 (3)	0.00338 (17)	0.01486 (18)	0.00187 (17)
Cl2	0.0227 (3)	0.0724 (4)	0.0464 (3)	−0.0018 (2)	0.00471 (18)	−0.0063 (3)
Cl3	0.0445 (3)	0.0260 (3)	0.0344 (3)	−0.00757 (17)	0.01151 (18)	−0.00670 (17)
N1	0.0221 (7)	0.0234 (8)	0.0257 (7)	−0.0032 (6)	0.0028 (6)	−0.0002 (6)
N2	0.0259 (7)	0.0209 (7)	0.0238 (7)	−0.0035 (6)	0.0013 (6)	0.0001 (6)
C1	0.0299 (9)	0.0289 (9)	0.0314 (9)	0.0056 (7)	−0.0011 (7)	−0.0051 (7)
C2	0.0278 (9)	0.0347 (10)	0.0294 (9)	0.0044 (7)	0.0039 (7)	−0.0085 (8)
C3	0.0312 (9)	0.0294 (9)	0.0312 (9)	0.0065 (7)	−0.0023 (7)	−0.0069 (7)
C4	0.0263 (9)	0.0406 (11)	0.0285 (9)	0.0069 (8)	0.0012 (7)	−0.0075 (8)
C5	0.0405 (10)	0.0347 (10)	0.0220 (9)	−0.0017 (8)	−0.0027 (7)	−0.0003 (7)
C6	0.0424 (11)	0.0400 (11)	0.0354 (10)	0.0069 (8)	−0.0107 (8)	0.0022 (8)

Co1—Cl1	2.2720 (8)	C1—H1A	0.990
Co1—Cl2	2.2419 (10)	C1—H1B	0.990
Co1—Cl3	2.2691 (8)	C2—H2A	0.990
Co1—N1	2.0686 (15)	C2—H2B	0.990
N1—C1	1.485 (3)	C3—H3A	0.990
N1—C4	1.480 (3)	C3—H3B	0.990
N2—C2	1.502 (3)	C4—H4A	0.990
N2—C3	1.503 (3)	C4—H4B	0.990
N2—C5	1.514 (3)	C5—H5A	0.990
C1—C2	1.519 (3)	C5—H5B	0.990
C3—C4	1.525 (3)	C6—H6A	0.980
C5—C6	1.514 (3)	C6—H6B	0.980
N1—H1	0.83 (2)	C6—H6C	0.980
N2—H2	0.853 (18)
Cl1—Co1—Cl2	113.57 (3)	H1A—C1—H1B	107.846
Cl1—Co1—Cl3	109.25 (4)	N2—C2—H2A	109.442
Cl1—Co1—N1	109.61 (5)	N2—C2—H2B	109.452
Cl2—Co1—Cl3	114.80 (2)	C1—C2—H2A	109.445
Cl2—Co1—N1	102.57 (5)	C1—C2—H2B	109.448
Cl3—Co1—N1	106.53 (5)	H2A—C2—H2B	108.051
Co1—N1—C1	114.64 (11)	N2—C3—H3A	109.507
Co1—N1—C4	112.42 (10)	N2—C3—H3B	109.508
C1—N1—C4	109.62 (13)	C4—C3—H3A	109.504
C2—N2—C3	110.19 (13)	C4—C3—H3B	109.503
C2—N2—C5	111.05 (13)	H3A—C3—H3B	108.076
C3—N2—C5	112.93 (13)	N1—C4—H4A	108.972
N1—C1—C2	112.39 (14)	N1—C4—H4B	108.974
N2—C2—C1	110.95 (14)	C3—C4—H4A	108.977
N2—C3—C4	110.70 (14)	C3—C4—H4B	108.982
N1—C4—C3	113.02 (14)	H4A—C4—H4B	107.779
N2—C5—C6	113.06 (14)	N2—C5—H5A	108.969
Co1—N1—H1	107.3 (13)	N2—C5—H5B	108.974
C1—N1—H1	105.7 (14)	C6—C5—H5A	108.963
C4—N1—H1	106.6 (14)	C6—C5—H5B	108.971
C2—N2—H2	107.2 (12)	H5A—C5—H5B	107.768
C3—N2—H2	108.2 (12)	C5—C6—H6A	109.474
C5—N2—H2	107.0 (11)	C5—C6—H6B	109.466
N1—C1—H1A	109.127	C5—C6—H6C	109.477
N1—C1—H1B	109.120	H6A—C6—H6B	109.472
C2—C1—H1A	109.128	H6A—C6—H6C	109.470
C2—C1—H1B	109.129	H6B—C6—H6C	109.468
Cl1—Co1—N1—C1	55.30 (9)	C4—N1—C1—C2	−55.55 (16)
Cl1—Co1—N1—C4	−70.78 (9)	C2—N2—C3—C4	54.82 (16)
Cl2—Co1—N1—C1	−65.66 (8)	C3—N2—C2—C1	−55.64 (16)
Cl2—Co1—N1—C4	168.27 (7)	C2—N2—C5—C6	−174.02 (12)
Cl3—Co1—N1—C1	173.39 (7)	C5—N2—C2—C1	178.47 (12)
Cl3—Co1—N1—C4	47.31 (9)	C3—N2—C5—C6	61.63 (17)
Co1—N1—C1—C2	176.93 (8)	C5—N2—C3—C4	179.64 (12)
Co1—N1—C4—C3	−176.03 (9)	N1—C1—C2—N2	56.87 (17)
C1—N1—C4—C3	55.22 (17)	N2—C3—C4—N1	−55.84 (18)

D—H···A	D—H	H···A	D···A	D—H···A
N2—H2···Cl1i	0.854 (19)	2.347 (18)	3.1794 (16)	165.4 (15)
N1—H1···Cl3ii	0.83 (2)	2.49 (2)	3.3192 (17)	176.0 (17)

Table 1

Selected bond lengths (Å)

Co1—Cl1	2.2720 (8)
Co1—Cl2	2.2419 (10)
Co1—Cl3	2.2691 (8)
Co1—N1	2.0686 (15)

Table 2

Hydrogen-bond geometry (Å, °)

D—H⋯A	D—H	H⋯A	D⋯A	D—H⋯A
N2—H2⋯Cl1i	0.854 (19)	2.347 (18)	3.1794 (16)	165.4 (15)
N1—H1⋯Cl3ii	0.83 (2)	2.49 (2)	3.3192 (17)	176.0 (17)

Symmetry codes: (i) ; (ii) .