trans-Chloridobis­(ethane-1,2-di­amine-κ2N,N′)(thio­cyanato-κN)cobalt(III) diammine­tetra­kis­(thio­cyanato-κN)cromate(III)

Rusanova, J.A.; Semenaka, V.V.; Zubatyuk, R.I.

doi:10.1107/S1600536814003869

metal-organic compounds

CRYSTALLOGRAPHIC
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ISSN: 2056-9890

Volume 70| Part 3| March 2014| Pages m110-m111

doi:10.1107/S1600536814003869

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trans-Chloridobis(ethane-1,2-diamine-κ²N,N′)(thiocyanato-κN)cobalt(III) diamminetetrakis(thiocyanato-κN)cromate(III)

Julia A. Rusanova,^a Valentyna V. Semenaka ^a ^* and Roman I. Zubatyuk ^b

^aTaras Shevchenko National University, Department of Inorganic Chemistry, Volodymyrska str. 64/13, 01601 Kyiv, Ukraine, and ^bInstitute for Scintillation Materials, "Institute for Single Crystals", National Academy of Sciences of Ukraine, Lenina ave. 60, Kharkov 61001, Ukraine
^*Correspondence e-mail: valya.semenaka@gmail.com

(Received 21 January 2014; accepted 19 February 2014; online 26 February 2014)

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-diamine) 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 molecules into a three-dimentional supramolecular network. Intensity statistic indicated twinning by non-merohedry with refined weighs of twin components are 0.5662:0.4338.

CCDC reference: 987894

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_r = 591.05
Triclinic, $[P \overline 1]$
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 $[Oxford Diffraction (2010). CrysAlis PRO. Oxford Diffraction Ltd, Abingdon, England.]$ ) T_min = 0.855, T_max = 0.883
8238 measured reflections
8238 independent reflections
6185 reflections with I > 2σ(I)

Refinement

R[F² > 2σ(F²)] = 0.052
wR(F²) = 0.141
S = 1.03
8238 reflections
256 parameters
H-atom parameters constrained
Δρ_max = 1.19 e Å⁻³
Δρ_min = −0.72 e Å⁻³

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⋯S4^iv	0.97	2.54	3.411 (4)	150
N4—H4A⋯Cl1^v	0.97	2.59	3.398 (4)	141
N10—H10B⋯S1^iv	0.89	2.81	3.696 (6)	171
N11—H11C⋯S5^vi	0.89	2.70	3.578 (5)	168
Symmetry codes: (iii) x+1, y, z; (iv) -x+1, -y, -z+1; (v) -x+1, -y+1, -z+2; (vi) -x, -y, -z+2.

Data collection: CrysAlis PRO (Oxford Diffraction, 2010 $[Oxford Diffraction (2010). CrysAlis PRO. Oxford Diffraction Ltd, Abingdon, England.]$ ); 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 ).

Supporting information

CCDC reference: 987894

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

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

checkCIF report

Experimental top

Synthesis and crystallization top

Cobalt powder (0.074 g, 1.25 mmol), NH₄[Cr(NCS)₄(NH₃)₂]·H₂O (0.443 g, 1.25 mmol), en·2HCl (0.166 g, 1.25 mmol) and methanol (20 ml) were heated in air to 323–333 K and stirred magnetically during 7 h. The resulting blue solution was slowly evaporated at room temperature until light-brown crystals suitable for crystallographic study were formed. The crystals were filtered off, washed with dry PriOH and finally dried in vacuo at room temperature. Yield: 0.12 g, 17.1%.

Refinement top

Crystal data, data collection and structure refinement details are summarized in Table 1. All of the hydrogen atoms were positioned geometricaly and refined using a riding model approximation with U_iso = 1.2 or 1.5 U_eq of the carrier atom. A rotating model was used for NH₃ and CH₃ groups. Intensity statistic indicated a nonmerohedral twinning with refined weights of twin components are 0.5662:0.4338.

Results and discussion top

In order to continue our research on direct synthesis of coordination compounds (Kovbasyuk et al., 1997; Pryma et al., 2003; Buvaylo et al., 2005; Vassilyeva et al., 1997; Makhankova et al., 2002; Nesterova (Pryma) et al., 2004; Nesterova et al., 2005, 2008; Nikitina et al., 2008, 2009) in this paper we present a novel Co/Cr heterometallic ionic complex which has been synthesized using zerovalent cobalt, Reinecke's salt and non-aqueous solution of ethylenediamine as a starting materials.

As it shown on Fig.1 Co atom in complex cation is in distorted square bypiramidal coordination enviroment with one NCS group and chlorine atom at the axial positions and four N atoms from two ethylenediamine molecules in equatorial plane. The Cr centers are in the similar to Co coordination enviroment and coordinated to six N atoms - four NCS-groups in equatorial position and two NH₃ molecules in axial position. The bond distances and angles in the title molecule agree well with the corresponding bond distances and angles reported in closely related compounds (Schubert et al.,1981, Tang et al., 1993, Foust et al., 1980, Anbalagan et al., 2009, Nikitina et al., 2008, 2009). There are short interanionic S···S contacts between NCS-groups of the complex anions with the distances 3.538 (1) (S5···S5) and 3.489 (1) Å (S2···S2) whereas sum of standard Van-der-Vaals radius of the sulfur atom is 3.68 Å. Two NCS-groups of the ligand which involve S2 and S3 atoms show relatively large thermal displacements (U_eq is 0.1063 (9) Å² and 0.0984 (8) Å², resp.). Also these NCS-groups show notably non-linear Cr–N–C bond angles (166.2 (5)° and 163.2 (5)°).This might be caused by intermolecular contacts involving S2 and S3. S···S contacts as well as a network of hydrogen bonds link the molecule into threedimentional supramolecular network. The crystal packing of the title compound is presented on Fig 2.

Related literature top

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).

Computing details top

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

Figures top

	Fig. 1. Crystal structure of the complex, showing the atom numbering, with 30% probability displacement ellipsoids
	Fig. 2. The crystal packing of the title compound. Hydrogen bonds are shown as dashed lines.

trans-Chloridobis(ethane-1,2-diamine-κ²N,N')(thiocyanato-κN)cobalt(III) diamminetetrakis(thiocyanato-κN)cromate(III) top

Crystal data top

[CoCl(NCS)(C₂H₈N₂)₂][Cr(NCS)₄(NH₃)₂]	Z = 2
M_r = 591.05	F(000) = 602
Triclinic, P1	D_x = 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

Data collection top

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	θ_max = 28.6°, θ_min = 2.9°
ω scans	h = −11→11
Absorption correction: multi-scan (CrysAlis PRO; Oxford Diffraction, 2010)	k = −13→13
T_min = 0.855, T_max = 0.883	l = −17→17

Refinement top

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(F_o²) + (0.080P)² + 0.5674P] where P = (F_o² + 2F_c²)/3
S = 1.03	(Δ/σ)_max = 0.001
8238 reflections	Δρ_max = 1.19 e Å⁻³
256 parameters	Δρ_min = −0.72 e Å⁻³
0 restraints

Crystal data top

[CoCl(NCS)(C₂H₈N₂)₂][Cr(NCS)₄(NH₃)₂]	γ = 90.646 (17)°
M_r = 591.05	V = 1202.1 (5) Å³
Triclinic, P1	Z = 2
a = 8.8290 (15) Å	Mo Kα radiation
b = 10.745 (3) Å	µ = 1.71 mm⁻¹
c = 13.275 (3) Å	T = 293 K
α = 106.98 (2)°	0.27 × 0.24 × 0.08 mm
β = 93.131 (17)°

Data collection top

Oxford Diffraction Xcalibur Sapphire3 diffractometer	8238 measured reflections
Absorption correction: multi-scan (CrysAlis PRO; Oxford Diffraction, 2010)	8238 independent reflections
T_min = 0.855, T_max = 0.883	6185 reflections with I > 2σ(I)

Refinement top

R[F² > 2σ(F²)] = 0.052	0 restraints
wR(F²) = 0.141	H-atom parameters constrained
S = 1.03	Δρ_max = 1.19 e Å⁻³
8238 reflections	Δρ_min = −0.72 e Å⁻³
256 parameters

Special details top

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.

Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å²) top

	x	y	z	U_iso*/U_eq
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)

Atomic displacement parameters (Å²) top

	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)

Geometric parameters (Å, º) top

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)

Symmetry codes: (i) −x, −y−1, −z+2; (ii) −x−1, −y, −z+2.

Hydrogen-bond geometry (Å, º) top

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···S4^iv	0.97	2.54	3.411 (4)	150
N4—H4A···Cl1^v	0.97	2.59	3.398 (4)	141
N10—H10B···S1^iv	0.89	2.81	3.696 (6)	171
N11—H11C···S5^vi	0.89	2.70	3.578 (5)	168

Symmetry codes: (iii) x+1, y, z; (iv) −x+1, −y, −z+1; (v) −x+1, −y+1, −z+2; (vi) −x, −y, −z+2.

Experimental details

Crystal data
Chemical formula	[CoCl(NCS)(C₂H₈N₂)₂][Cr(NCS)₄(NH₃)₂]
M_r	591.05
Crystal system, space group	Triclinic, P1
Temperature (K)	293
a, b, c (Å)	8.8290 (15), 10.745 (3), 13.275 (3)
α, β, γ (°)	106.98 (2), 93.131 (17), 90.646 (17)
V (Å³)	1202.1 (5)
Z	2
Radiation type	Mo Kα
µ (mm⁻¹)	1.71
Crystal size (mm)	0.27 × 0.24 × 0.08

Data collection
Diffractometer	Oxford Diffraction Xcalibur Sapphire3 diffractometer
Absorption correction	Multi-scan (CrysAlis PRO; Oxford Diffraction, 2010)
T_min, T_max	0.855, 0.883
No. of measured, independent and observed [I > 2σ(I)] reflections	8238, 8238, 6185
R_int	?
(sin θ/λ)_max (Å⁻¹)	0.674

Refinement
R[F² > 2σ(F²)], wR(F²), S	0.052, 0.141, 1.03
No. of reflections	8238
No. of parameters	256
H-atom treatment	H-atom parameters constrained
Δρ_max, Δρ_min (e Å⁻³)	1.19, −0.72

Computer programs: CrysAlis PRO (Oxford Diffraction, 2010), SHELXTL (Sheldrick, 2008), publCIF (Westrip, 2010).

Hydrogen-bond geometry (Å, º) top

D—H···A	D—H	H···A	D···A	D—H···A
N1—H1A···S3ⁱⁱⁱ	0.9700	2.6000	3.485 (5)	152.00
N1—H1B···S5ⁱⁱⁱ	0.9700	2.7000	3.598 (5)	154.00
N2—H2A···S3	0.9700	2.5400	3.473 (4)	163.00
N2—H2B···S4^iv	0.9700	2.5400	3.411 (4)	150.00
N4—H4A···Cl1^v	0.9700	2.5900	3.398 (4)	141.00
N10—H10B···S1^iv	0.8900	2.8100	3.696 (6)	171.00
N11—H11C···S5^vi	0.8900	2.7000	3.578 (5)	168.00

Symmetry codes: (iii) x+1, y, z; (iv) −x+1, −y, −z+1; (v) −x+1, −y+1, −z+2; (vi) −x, −y, −z+2.

Acknowledgements

This work was partly supported by the State Fund for Fundamental Research of Ukraine (project 54.3/005).

References

Anbalagan, K., Tamilselvan, M., Nirmala, S. & Sudha, L. (2009). Acta Cryst. E65, m836–m837. Web of Science CSD CrossRef CAS IUCr Journals Google Scholar
Buvaylo, E. A., Kokozay, V. N., Vassilyeva, O. Yu., Skelton, B. W., Jezierska, J., Brunel, L. C. & Ozarowski, A. (2005). Chem. Commun. pp. 4976–4978. Web of Science CSD CrossRef Google Scholar
Foust, A. S. & Janickis, V. (1980). Inorg. Chem. 19, 1048–1050. CSD CrossRef CAS Web of Science Google Scholar
Kovbasyuk, L. A., Babich, O. A. & Kokozay, V. N. (1997). Polyhedron, 16, 161–163. CSD CrossRef CAS Web of Science Google Scholar
Makhankova, V. G., Vassilyeva, O. Yu., Kokozay, V. N., Skelton, B. W., Sorace, L. & Gatteschi, D. (2002). J. Chem. Soc. Dalton Trans. pp. 4253–4259. Web of Science CSD CrossRef Google Scholar
Nesterova, O. V., Lipetskaya, A. V., Petrusenko, S. R., Kokozay, V. N., Skelton, B. W. & Jezierska, J. (2005). Polyhedron, 24, 1425–1434. Web of Science CSD CrossRef CAS Google Scholar
Nesterova, O. V., Petrusenko, S. R., Kokozay, V. N., Skelton, B. W., Jezierska, J., Linert, W. & Ozarowski, A. (2008). Dalton Trans. pp. 1431–1436. Web of Science CSD CrossRef PubMed Google Scholar
Nesterova (Pryma), O. V., Petrusenko, S. R., Kokozay, V. N., Skelton, B. W. & Linert, W. (2004). Inorg. Chem. Commun. 7, 450–454. Google Scholar
Nikitina, V. M., Nesterova, O. V., Kokozay, V. N., Dyakonenko, V. V., Shishkin, O. V. & Jezierska, J. (2009). Polyhedron, 28, 1265–1272. Web of Science CSD CrossRef CAS Google Scholar
Nikitina, V. M., Nesterova, O. V., Kokozay, V. N., Goreshnik, E. A. & Jezierska, J. (2008). Polyhedron, 27, 2426–2430. Web of Science CSD CrossRef CAS Google Scholar
Oxford Diffraction (2010). CrysAlis PRO. Oxford Diffraction Ltd, Abingdon, England. Google Scholar
Pryma, O. V., Petrusenko, S. R., Kokozay, V. N., Skelton, B. W., Shishkin, O. V. & Teplytska, T. S. (2003). Eur. J. Inorg. Chem. pp. 1426–1432. CSD CrossRef Google Scholar
Schubert, U., Zimmer-Gasser, B., Dash, K. C. & Chaudhury, G. R. (1981). Cryst. Struct. Commun. 10, 251–254. CAS Google Scholar
Sheldrick, G. M. (2008). Acta Cryst. A64, 112–122. Web of Science CrossRef CAS IUCr Journals Google Scholar
Tang, K., Kastner, M. E., Cooper, J. N., Kanaskie, M. & Monoski, A. (1993). Acta Cryst. C49, 1265–1267. CSD CrossRef CAS Web of Science IUCr Journals Google Scholar
Vassilyeva, O. Yu., Kokozay, V. N., Zhukova, N. I. & Kovbasyuk, L. A. (1997). Polyhedron, 16, 263–266. CSD CrossRef CAS Web of Science Google Scholar
Westrip, S. P. (2010). J. Appl. Cryst. 43, 920–925. Web of Science CrossRef CAS IUCr Journals Google Scholar

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Volume 70| Part 3| March 2014| Pages m110-m111

doi:10.1107/S1600536814003869

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