trans-Chloridobis-(ethane-1,2-di-amine-κ(2) N,N')(thio-cyanato-κN)cobalt(III) diammine-tetra-kis-(thio-cyanato-κN)cromate(III).

The title ionic complex [CoCl(NCS)(C2H8N2)2][Cr(NCS)4(NH3)2], which crystallizes as a non-merohedral twin, is build up of a complex cation [CoCl(NCS)(en)2](+) (en is ethane-1,2-di-amine) and the Reinecke's salt anion [Cr(NCS)4(NH3)2](-) as complex counter-ion. A network of N-H⋯S and N-H⋯Cl hydrogen bonds, as well as short S⋯S contacts [3.538 (2) and 3.489 (3) Å], between the NCS groups of the complex anions link the mol-ecules into a three-dimentional supra-molecular network. Intensity statistic indicated twinning by non-mero-hedry with refined weighs of twin components are 0.5662:0.4338.

Related literature

For background to the ammonium salt route for direct synthesis of coordination compounds, see: Kovbasyuk et al. (1997 ▶); Pryma et al. (2003 ▶); Buvaylo et al. (2005 ▶). For the salt route for direct synthesis of coordination compounds, see: Vassilyeva et al. (1997 ▶); Makhankova et al. (2002 ▶). For direct synthesis of heterometallic complexes with ethyl­enedi­amine, see: Nesterova (Pryma) et al. (2004 ▶); Nesterova et al. (2005 ▶, 2008 ▶). For the application of Reinecke’s salt in the direct synthesis of heterometallic complexes, see: Nikitina et al. (2008 ▶, 2009 ▶). For the structures of related complexes, see: Schubert et al. (1981 ▶); Tang et al. (1993 ▶); Foust & Janickis (1980 ▶); Anbalagan et al. (2009 ▶).

Experimental

Crystal data

[CoCl(NCS)(C2H8N2)2][Cr(NCS)4(NH3)2]

M = 591.05

Triclinic,

a = 8.8290 (15) Å

b = 10.745 (3) Å

c = 13.275 (3) Å

α = 106.98 (2)°

β = 93.131 (17)°

γ = 90.646 (17)°

V = 1202.1 (5) Å3

Z = 2

Mo Kα radiation

μ = 1.71 mm−1

T = 293 K

0.27 × 0.24 × 0.08 mm

Data collection

Oxford Diffraction Xcalibur Sapphire3 diffractometer

Absorption correction: multi-scan (CrysAlis PRO; Oxford Diffraction, 2010 ▶) T min = 0.855, T max = 0.883

8238 measured reflections

8238 independent reflections

6185 reflections with I > 2σ(I)

Refinement

R[F 2 > 2σ(F 2)] = 0.052

wR(F 2) = 0.141

S = 1.03

8238 reflections

256 parameters

H-atom parameters constrained

Δρmax = 1.19 e Å−3

Δρmin = −0.72 e Å−3

Data collection: CrysAlis PRO (Oxford Diffraction, 2010 ▶); cell refinement: CrysAlis PRO; data reduction: CrysAlis PRO; program(s) used to solve structure: SHELXTL (Sheldrick, 2008 ▶); program(s) used to refine structure: SHELXTL; molecular graphics: SHELXTL; software used to prepare material for publication: publCIF (Westrip, 2010 ▶).

Crystal structure: contains datablock(s) I. DOI: 10.1107/S1600536814003869/br2236sup1.cif

Structure factors: contains datablock(s) I. DOI: 10.1107/S1600536814003869/br2236Isup2.hkl

CCDC reference:

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

[CoCl(NCS)(C2H8N2)2][Cr(NCS)4(NH3)2]	Z = 2
Mr = 591.05	F(000) = 602
Triclinic, P1	Dx = 1.633 Mg m−3
Hall symbol: -P 1	Mo Kα radiation, λ = 0.7107 Å
a = 8.8290 (15) Å	Cell parameters from 3528 reflections
b = 10.745 (3) Å	θ = 3.1–27.3°
c = 13.275 (3) Å	µ = 1.71 mm−1
α = 106.98 (2)°	T = 293 K
β = 93.131 (17)°	Block, light brown
γ = 90.646 (17)°	0.27 × 0.24 × 0.08 mm
V = 1202.1 (5) Å3

Oxford Diffraction Xcalibur Sapphire3 diffractometer	8238 measured reflections
Radiation source: Enhance (Mo) X-ray Source	8238 independent reflections
Graphite monochromator	6185 reflections with I > 2σ(I)
Detector resolution: 16.1827 pixels mm-1	θmax = 28.6°, θmin = 2.9°
ω scans	h = −11→11
Absorption correction: multi-scan (CrysAlis PRO; Oxford Diffraction, 2010)	k = −13→13
Tmin = 0.855, Tmax = 0.883	l = −17→17

Refinement on F2	Primary atom site location: structure-invariant direct methods
Least-squares matrix: full	Hydrogen site location: inferred from neighbouring sites
R[F2 > 2σ(F2)] = 0.052	H-atom parameters constrained
wR(F2) = 0.141	w = 1/[σ2(Fo2) + (0.080P)2 + 0.5674P] where P = (Fo2 + 2Fc2)/3
S = 1.03	(Δ/σ)max = 0.001
8238 reflections	Δρmax = 1.19 e Å−3
256 parameters	Δρmin = −0.72 e Å−3
0 restraints

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.

	x	y	z	Uiso*/Ueq
Co1	0.54186 (7)	0.40606 (6)	0.75563 (4)	0.02775 (16)
Cr1	0.08452 (9)	−0.07796 (8)	0.76057 (7)	0.0385 (2)
Cl1	0.40444 (16)	0.35647 (13)	0.87609 (9)	0.0438 (3)
S1	0.78440 (16)	0.49754 (14)	0.48138 (10)	0.0452 (3)
S2	0.0503 (3)	−0.3524 (2)	0.9791 (2)	0.1063 (9)
S3	0.0184 (2)	0.2947 (2)	0.6471 (2)	0.0984 (8)
S4	0.55652 (16)	−0.22096 (14)	0.61991 (10)	0.0442 (3)
S5	−0.38612 (16)	0.04575 (16)	0.91039 (11)	0.0518 (4)
N1	0.6708 (5)	0.2569 (4)	0.7487 (3)	0.0370 (9)
H1A	0.7764	0.2817	0.7471	0.044*
H1B	0.6599	0.2272	0.8104	0.044*
N2	0.4114 (4)	0.2859 (4)	0.6452 (3)	0.0343 (9)
H2A	0.3061	0.2971	0.6623	0.041*
H2B	0.4225	0.3036	0.5783	0.041*
N3	0.4130 (5)	0.5558 (4)	0.7636 (3)	0.0371 (9)
H3A	0.4180	0.5815	0.6996	0.045*
H3B	0.3084	0.5323	0.7701	0.045*
N4	0.6745 (5)	0.5263 (4)	0.8661 (3)	0.0367 (9)
H4A	0.6582	0.5137	0.9342	0.044*
H4B	0.7801	0.5104	0.8513	0.044*
N5	0.6529 (5)	0.4460 (4)	0.6499 (3)	0.0362 (9)
N6	0.0981 (6)	−0.2081 (5)	0.8404 (4)	0.0603 (14)
N7	0.0637 (6)	0.0593 (5)	0.6873 (4)	0.0561 (13)
N8	0.2839 (5)	−0.1270 (4)	0.6994 (4)	0.0461 (11)
N9	−0.1149 (5)	−0.0282 (5)	0.8214 (4)	0.0515 (12)
N10	−0.0200 (6)	−0.2146 (5)	0.6325 (4)	0.0695 (15)
H10A	−0.1087	−0.2397	0.6501	0.104*
H10B	0.0388	−0.2832	0.6125	0.104*
H10C	−0.0353	−0.1801	0.5796	0.104*
N11	0.1914 (5)	0.0620 (4)	0.8881 (3)	0.0472 (11)
H11A	0.1242	0.1198	0.9190	0.071*
H11B	0.2652	0.1023	0.8656	0.071*
H11C	0.2306	0.0238	0.9344	0.071*
C1	0.6231 (7)	0.1510 (5)	0.6512 (4)	0.0502 (14)
H1C	0.6687	0.1659	0.5908	0.060*
H1D	0.6558	0.0677	0.6578	0.060*
C2	0.4560 (7)	0.1507 (5)	0.6370 (4)	0.0482 (13)
H2C	0.4101	0.1210	0.6910	0.058*
H2D	0.4220	0.0926	0.5685	0.058*
C3	0.4661 (6)	0.6663 (5)	0.8567 (4)	0.0444 (13)
H3C	0.4223	0.6579	0.9200	0.053*
H3D	0.4360	0.7484	0.8463	0.053*
C4	0.6367 (7)	0.6613 (5)	0.8674 (4)	0.0459 (13)
H4C	0.6814	0.6831	0.8093	0.055*
H4D	0.6757	0.7230	0.9330	0.055*
C5	0.7041 (5)	0.4652 (4)	0.5783 (4)	0.0323 (10)
C6	0.0819 (7)	−0.2700 (6)	0.8967 (6)	0.0664 (19)
C7	0.0454 (6)	0.1544 (7)	0.6701 (5)	0.0591 (17)
C8	0.3977 (5)	−0.1639 (4)	0.6657 (4)	0.0334 (10)
C9	−0.2279 (6)	0.0020 (5)	0.8567 (4)	0.0374 (11)

	U11	U22	U33	U12	U13	U23
Co1	0.0309 (3)	0.0296 (3)	0.0247 (3)	0.0017 (2)	0.0031 (3)	0.0106 (3)
Cr1	0.0263 (4)	0.0419 (5)	0.0462 (5)	0.0008 (3)	0.0036 (4)	0.0108 (4)
Cl1	0.0507 (8)	0.0489 (7)	0.0341 (7)	−0.0010 (6)	0.0105 (6)	0.0143 (6)
S1	0.0434 (8)	0.0541 (8)	0.0429 (7)	−0.0030 (6)	0.0120 (6)	0.0201 (6)
S2	0.0773 (14)	0.1127 (18)	0.167 (2)	−0.0156 (12)	−0.0050 (15)	0.1033 (18)
S3	0.0516 (11)	0.1282 (18)	0.163 (2)	0.0142 (11)	0.0175 (12)	0.1146 (18)
S4	0.0379 (7)	0.0539 (8)	0.0404 (7)	0.0099 (6)	0.0089 (6)	0.0116 (6)
S5	0.0381 (8)	0.0682 (10)	0.0514 (8)	0.0099 (7)	0.0136 (6)	0.0190 (7)
N1	0.040 (2)	0.037 (2)	0.040 (2)	0.0086 (18)	0.0094 (19)	0.0181 (19)
N2	0.034 (2)	0.037 (2)	0.030 (2)	−0.0024 (17)	0.0018 (17)	0.0074 (17)
N3	0.043 (2)	0.038 (2)	0.032 (2)	0.0060 (18)	0.0011 (19)	0.0116 (18)
N4	0.040 (2)	0.038 (2)	0.033 (2)	−0.0029 (18)	−0.0041 (18)	0.0126 (17)
N5	0.042 (2)	0.035 (2)	0.033 (2)	0.0034 (18)	0.0054 (19)	0.0111 (18)
N6	0.051 (3)	0.056 (3)	0.083 (4)	0.000 (2)	0.013 (3)	0.033 (3)
N7	0.047 (3)	0.068 (3)	0.057 (3)	0.005 (3)	0.003 (2)	0.024 (3)
N8	0.033 (2)	0.050 (3)	0.055 (3)	0.005 (2)	0.008 (2)	0.014 (2)
N9	0.034 (3)	0.062 (3)	0.059 (3)	0.004 (2)	0.013 (2)	0.016 (2)
N10	0.049 (3)	0.073 (4)	0.073 (4)	−0.004 (3)	−0.002 (3)	0.002 (3)
N11	0.041 (3)	0.049 (3)	0.048 (3)	−0.010 (2)	−0.003 (2)	0.012 (2)
C1	0.068 (4)	0.032 (3)	0.051 (3)	0.011 (3)	0.021 (3)	0.009 (2)
C2	0.065 (4)	0.034 (3)	0.042 (3)	−0.011 (3)	0.004 (3)	0.007 (2)
C3	0.060 (4)	0.037 (3)	0.036 (3)	0.012 (2)	0.004 (2)	0.008 (2)
C4	0.064 (4)	0.031 (3)	0.041 (3)	−0.011 (2)	−0.003 (3)	0.008 (2)
C5	0.032 (3)	0.030 (2)	0.033 (3)	−0.0010 (19)	−0.001 (2)	0.007 (2)
C6	0.035 (3)	0.049 (4)	0.122 (6)	0.001 (3)	0.004 (4)	0.038 (4)
C7	0.029 (3)	0.105 (5)	0.063 (4)	0.003 (3)	0.008 (3)	0.053 (4)
C8	0.034 (3)	0.030 (2)	0.039 (3)	−0.001 (2)	0.000 (2)	0.014 (2)
C9	0.038 (3)	0.039 (3)	0.039 (3)	0.000 (2)	−0.003 (2)	0.017 (2)

Co1—Cl1	2.2378 (14)	N3—H3B	0.9700
Co1—N1	1.960 (4)	N3—C3	1.492 (6)
Co1—N2	1.954 (4)	N4—H4A	0.9700
Co1—N3	1.962 (4)	N4—H4B	0.9700
Co1—N4	1.965 (4)	N4—C4	1.488 (6)
Co1—N5	1.900 (4)	N5—C5	1.144 (6)
Cr1—N6	1.987 (5)	N6—C6	1.149 (8)
Cr1—N7	1.995 (5)	N7—C7	1.122 (8)
Cr1—N8	1.990 (4)	N8—C8	1.150 (6)
Cr1—N9	1.990 (5)	N9—C9	1.135 (6)
Cr1—N10	2.058 (5)	N10—H10A	0.8900
Cr1—N11	2.080 (4)	N10—H10B	0.8900
S1—C5	1.623 (5)	N10—H10C	0.8900
S2—C6	1.629 (7)	N11—H11A	0.8900
S3—C7	1.640 (7)	N11—H11B	0.8900
S4—C8	1.615 (5)	N11—H11C	0.8900
S5—C9	1.616 (5)	C1—H1C	0.9700
S2—S2i	3.489 (3)	C1—H1D	0.9700
S5—S5ii	3.538 (2)	C1—C2	1.477 (8)
N1—H1A	0.9700	C2—H2C	0.9700
N1—H1B	0.9700	C2—H2D	0.9700
N1—C1	1.489 (7)	C3—H3C	0.9700
N2—H2A	0.9700	C3—H3D	0.9700
N2—H2B	0.9700	C3—C4	1.508 (8)
N2—C2	1.485 (6)	C4—H4C	0.9700
N3—H3A	0.9700	C4—H4D	0.9700
N1—Co1—Cl1	90.78 (12)	H4A—N4—H4B	108.5
N1—Co1—N3	179.61 (17)	C4—N4—Co1	107.7 (3)
N1—Co1—N4	93.44 (17)	C4—N4—H4A	110.2
N2—Co1—Cl1	88.77 (12)	C4—N4—H4B	110.2
N2—Co1—N1	86.23 (17)	C5—N5—Co1	171.6 (4)
N2—Co1—N3	94.07 (17)	C6—N6—Cr1	166.2 (5)
N2—Co1—N4	179.54 (17)	C7—N7—Cr1	163.2 (5)
N3—Co1—Cl1	88.98 (13)	C8—N8—Cr1	175.0 (4)
N3—Co1—N4	86.27 (17)	C9—N9—Cr1	179.0 (5)
N4—Co1—Cl1	91.54 (12)	Cr1—N10—H10A	109.5
N5—Co1—Cl1	178.03 (13)	Cr1—N10—H10B	109.5
N5—Co1—N1	89.78 (17)	Cr1—N10—H10C	109.5
N5—Co1—N2	89.38 (17)	H10A—N10—H10B	109.5
N5—Co1—N3	90.47 (17)	H10A—N10—H10C	109.5
N5—Co1—N4	90.31 (17)	H10B—N10—H10C	109.5
N6—Cr1—N7	176.5 (2)	Cr1—N11—H11A	109.5
N6—Cr1—N8	92.1 (2)	Cr1—N11—H11B	109.5
N6—Cr1—N9	88.1 (2)	Cr1—N11—H11C	109.5
N6—Cr1—N10	90.7 (2)	H11A—N11—H11B	109.5
N6—Cr1—N11	90.3 (2)	H11A—N11—H11C	109.5
N7—Cr1—N10	91.1 (2)	H11B—N11—H11C	109.5
N7—Cr1—N11	87.9 (2)	N1—C1—H1C	110.1
N8—Cr1—N7	90.8 (2)	N1—C1—H1D	110.1
N8—Cr1—N9	179.7 (2)	H1C—C1—H1D	108.4
N8—Cr1—N10	89.1 (2)	C2—C1—N1	108.0 (4)
N8—Cr1—N11	90.47 (19)	C2—C1—H1C	110.1
N9—Cr1—N7	88.9 (2)	C2—C1—H1D	110.1
N9—Cr1—N10	90.9 (2)	N2—C2—H2C	110.2
N9—Cr1—N11	89.51 (19)	N2—C2—H2D	110.2
N10—Cr1—N11	179.0 (2)	C1—C2—N2	107.6 (4)
Co1—N1—H1A	110.1	C1—C2—H2C	110.2
Co1—N1—H1B	110.1	C1—C2—H2D	110.2
H1A—N1—H1B	108.4	H2C—C2—H2D	108.5
C1—N1—Co1	108.2 (3)	N3—C3—H3C	110.3
C1—N1—H1A	110.1	N3—C3—H3D	110.3
C1—N1—H1B	110.1	N3—C3—C4	107.1 (4)
Co1—N2—H2A	109.9	H3C—C3—H3D	108.5
Co1—N2—H2B	109.9	C4—C3—H3C	110.3
H2A—N2—H2B	108.3	C4—C3—H3D	110.3
C2—N2—Co1	108.7 (3)	N4—C4—C3	107.1 (4)
C2—N2—H2A	109.9	N4—C4—H4C	110.3
C2—N2—H2B	109.9	N4—C4—H4D	110.3
Co1—N3—H3A	109.8	C3—C4—H4C	110.3
Co1—N3—H3B	109.8	C3—C4—H4D	110.3
H3A—N3—H3B	108.2	H4C—C4—H4D	108.5
C3—N3—Co1	109.4 (3)	N5—C5—S1	176.7 (5)
C3—N3—H3A	109.8	N6—C6—S2	176.6 (6)
C3—N3—H3B	109.8	N7—C7—S3	179.0 (7)
Co1—N4—H4A	110.2	N8—C8—S4	177.7 (5)
Co1—N4—H4B	110.2	N9—C9—S5	178.3 (5)
Co1—N1—C1—C2	−38.5 (5)	Co1—N4—C4—C3	42.6 (5)
Co1—N2—C2—C1	−38.6 (5)	N1—C1—C2—N2	50.6 (5)
Co1—N3—C3—C4	35.7 (5)	N3—C3—C4—N4	−51.3 (5)

D—H···A	D—H	H···A	D···A	D—H···A
N1—H1A···S3iii	0.97	2.60	3.485 (5)	152
N1—H1B···S5iii	0.97	2.70	3.598 (5)	154
N2—H2A···S3	0.97	2.54	3.473 (4)	163
N2—H2B···S4iv	0.97	2.54	3.411 (4)	150
N4—H4A···Cl1v	0.97	2.59	3.398 (4)	141
N10—H10B···S1iv	0.89	2.81	3.696 (6)	171
N11—H11C···S5vi	0.89	2.70	3.578 (5)	168

Table 1

Hydrogen-bond geometry (Å, °)

D—H⋯A	D—H	H⋯A	D⋯A	D—H⋯A
N1—H1A⋯S3iii	0.97	2.60	3.485 (5)	152
N1—H1B⋯S5iii	0.97	2.70	3.598 (5)	154
N2—H2A⋯S3	0.97	2.54	3.473 (4)	163
N2—H2B⋯S4iv	0.97	2.54	3.411 (4)	150
N4—H4A⋯Cl1v	0.97	2.59	3.398 (4)	141
N10—H10B⋯S1iv	0.89	2.81	3.696 (6)	171
N11—H11C⋯S5vi	0.89	2.70	3.578 (5)	168

Symmetry codes: (iii) ; (iv) ; (v) ; (vi) .