Tetra­kis(pyridazine-κN)bis­(seleno­cyanato-κN)cobalt(II) pyridazine disolvate

Wöhlert, S.; Wriedt, M.; Jess, I.; Näther, C.

doi:10.1107/S1600536812027742

metal-organic compounds

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ISSN: 2056-9890

Volume 68| Part 7| July 2012| Page m965

https://doi.org/10.1107/S1600536812027742

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Tetrakis(pyridazine-κN)bis(selenocyanato-κN)cobalt(II) pyridazine disolvate

Susanne Wöhlert,^a ^* Mario Wriedt,^b Inke Jess ^a and Christian Näther ^a

^aInstitut für Anorganische Chemie, Christian-Albrechts-Universität Kiel, Max-Eyth-Strasse 2, 24118 Kiel, Germany, and ^bDepartment of Chemistry, Texas A&M University, College Station, Texas 77843, USA
^*Correspondence e-mail: swoehlert@ac.uni-kiel.de

(Received 12 June 2012; accepted 19 June 2012; online 23 June 2012)

Reaction of cobalt(II) nitrate with potassium selenocyanate and pyridazine leads to single crystals of the title compound, [Co(NCSe)₂(C₄H₄N₂)₄]·2C₄H₄N₂, which is isotypic with its nickel(II) thiocyanate analogue. The Co²⁺ cations are coordinated by two N-bonded selenocyanate ligands and four N atoms from four pyridazine ligands into discrete complexes. The complexes are arranged into layers parallel to (001). These layers are separated by additional non-coordinating pyridazine ligands.

Related literature

For background to this work, including related thiocyanato compounds, see: Boeckmann & Näther (2010 , 2011 ); Wöhlert et al. (2011 ). For the isotypic Ni thiocyanate analogue, see: Wöhlert et al. (2012 ). For related pyridazine coordination compounds, see: Boeckmann et al. (2011 ); Lloret et al. (1998 ). For crystallographic analysis, see: Spek (2009 ).

Experimental

Crystal data

[Co(NCSe)₂(C₄H₄N₂)₄]·2C₄H₄N₂
M_r = 749.44
Triclinic, $[P \overline 1]$
a = 11.2138 (9) Å
b = 12.0996 (11) Å
c = 12.7033 (11) Å
α = 62.206 (9)°
β = 88.827 (10)°
γ = 88.682 (10)°
V = 1524.3 (2) Å³
Z = 2
Mo Kα radiation
μ = 2.99 mm⁻¹
T = 170 K
0.15 × 0.11 × 0.08 mm

Data collection

STOE IPDS-1 diffractometer
Absorption correction: numerical (X-SHAPE and X-RED32; Stoe & Cie, 2008 ) T_min = 0.579, T_max = 0.697
16685 measured reflections
7160 independent reflections
4872 reflections with I > 2σ(I)
R_int = 0.047

Refinement

R[F² > 2σ(F²)] = 0.038
wR(F²) = 0.100
S = 0.95
7160 reflections
388 parameters
H-atom parameters constrained
Δρ_max = 0.42 e Å⁻³
Δρ_min = −0.74 e Å⁻³

Table 1
Selected bond lengths (Å)

Co1—N1	2.084 (2)
Co1—N2	2.091 (2)
Co1—N20	2.174 (2)
Co1—N40	2.175 (2)
Co1—N10	2.197 (2)
Co1—N30	2.204 (2)

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: XCIF in SHELXTL.

Supporting information

Crystal structure: contains datablocks I, global. DOI: https://doi.org/10.1107/S1600536812027742/wm2650sup1.cif

Structure factors: contains datablock I. DOI: https://doi.org/10.1107/S1600536812027742/wm2650Isup2.hkl

checkCIF report

Comment top

Recently, we have reported on the synthesis and characterization of coordination polymers based on transition metal(II) thiocyanates and different monodentate and bidentate co-ligands (Boeckmann & Näther, 2010, 2011; Wöhlert et al., 2011). In the course of these investigations we have found that the thiocyanato compounds are frequently isotypic with their selenocyanato analogues and exhibit a similar thermal reactivity and a similar magnetic behaviour (Boeckmann & Näther, 2011). In view of these results, we tried to prepare similar compounds based on pyridazine as co-ligand which results in the formation of single-crystals of the title compound, which are isotypic to [Ni(NCS)₂(N₂C₄H₄)₄]^.2(N₂C₄H₄) reported recently (Wöhlert et al., 2012).

In the crystal structure each cobalt(II) cation is coordinated by two terminal N-bonded selenocyanate anions and four pyridazine ligands into discrete complexes (Fig. 1). The octahedral coordination of the cobalt(II) cations is slightly distorted with distances in the range of 2.084 (2) to 2.204 (2) Å and angles ranging from 87.31 (9) ° to 179.70 (10) °. The discrete complexes are arranged into layers parallel to (001) (Fig. 2). These layers are separated by additional non-coordinating pyridazine ligands. The shortest intermolecular Co···Co distances amount to 8.2074 (11) Å.

It must be noted that similar discrete complexes based on cobalt and cadmium as counter cations are already reported in literature (Boeckmann et al., 2011; Lloret et al., 1998).

Related literature top

For background to this work, including related thiocyanato compounds, see: Boeckmann & Näther (2010, 2011); Wöhlert et al. (2011). For the isotypic Ni thiocyanate analogue, see: Wöhlert et al. (2012). For related pyridazine coordination compounds, see: Boeckmann et al. (2011); Lloret et al. (1998). For crystallographic analysis, see: Spek (2009).

Experimental top

Cobalt(II) nitrate hexahydrate (Co(NO₃)₂^.6H₂O) and potassium selenocyanate (KNCSe) as well as pyridazine were obtained from Alfa Aesar. All chemicals were used without further purification. 0.125 mmol (36.4 mg) Co(NO₃)₂^.6H₂O and 0.25 mmol (36.0 mg) KNCSe were reacted in 2.76 mmol (200 µL) pyridazine. Orange single-crystals of the title compound were obtained after three days.

Structure description top

It must be noted that similar discrete complexes based on cobalt and cadmium as counter cations are already reported in literature (Boeckmann et al., 2011; Lloret et al., 1998).

For background to this work, including related thiocyanato compounds, see: Boeckmann & Näther (2010, 2011); Wöhlert et al. (2011). For the isotypic Ni thiocyanate analogue, see: Wöhlert et al. (2012). For related pyridazine coordination compounds, see: Boeckmann et al. (2011); Lloret et al. (1998). For crystallographic analysis, see: Spek (2009).

Computing details top

Data collection: X-AREA (Stoe & Cie, 2008); cell refinement: X-AREA (Stoe & Cie, 2008); data reduction: X-AREA (Stoe & Cie, 2008); 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: XCIF in SHELXTL (Sheldrick, 2008).

Figures top

	Fig. 1. Crystal structure of the title compound with atom labelling and displacement ellipsoids drawn at the 50% probability level.
	Fig. 2. Crystal structure of the title compound in a view along [010].

Tetrakis(pyridazine-κN)bis(selenocyanato-κN)cobalt(II) pyridazine disolvate top

Crystal data top

[Co(SeCN)₂(C₄H₄N₂)₄]·2C₄H₄N₂	Z = 2
M_r = 749.44	F(000) = 746
Triclinic, P1	D_x = 1.633 Mg m⁻³
Hall symbol: -P 1	Mo Kα radiation, λ = 0.71073 Å
a = 11.2138 (9) Å	Cell parameters from 16685 reflections
b = 12.0996 (11) Å	θ = 2.6–28.0°
c = 12.7033 (11) Å	µ = 2.99 mm⁻¹
α = 62.206 (9)°	T = 170 K
β = 88.827 (10)°	Block, orange
γ = 88.682 (10)°	0.15 × 0.11 × 0.08 mm
V = 1524.3 (2) Å³

Data collection top

STOE IPDS-1 diffractometer	7160 independent reflections
Radiation source: fine-focus sealed tube	4872 reflections with I > 2σ(I)
Graphite monochromator	R_int = 0.047
phi scan	θ_max = 28.0°, θ_min = 2.6°
Absorption correction: numerical (X-SHAPE and X-RED32; Stoe & Cie, 2008)	h = −14→14
T_min = 0.579, T_max = 0.697	k = −15→15
16685 measured reflections	l = −16→16

Refinement top

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)] = 0.038	Hydrogen site location: inferred from neighbouring sites
wR(F²) = 0.100	H-atom parameters constrained
S = 0.95	w = 1/[σ²(F_o²) + (0.0561P)²] where P = (F_o² + 2F_c²)/3
7160 reflections	(Δ/σ)_max = 0.001
388 parameters	Δρ_max = 0.42 e Å⁻³
0 restraints	Δρ_min = −0.74 e Å⁻³

Crystal data top

[Co(SeCN)₂(C₄H₄N₂)₄]·2C₄H₄N₂	γ = 88.682 (10)°
M_r = 749.44	V = 1524.3 (2) Å³
Triclinic, P1	Z = 2
a = 11.2138 (9) Å	Mo Kα radiation
b = 12.0996 (11) Å	µ = 2.99 mm⁻¹
c = 12.7033 (11) Å	T = 170 K
α = 62.206 (9)°	0.15 × 0.11 × 0.08 mm
β = 88.827 (10)°

Data collection top

STOE IPDS-1 diffractometer	7160 independent reflections
Absorption correction: numerical (X-SHAPE and X-RED32; Stoe & Cie, 2008)	4872 reflections with I > 2σ(I)
T_min = 0.579, T_max = 0.697	R_int = 0.047
16685 measured reflections

Refinement top

R[F² > 2σ(F²)] = 0.038	0 restraints
wR(F²) = 0.100	H-atom parameters constrained
S = 0.95	Δρ_max = 0.42 e Å⁻³
7160 reflections	Δρ_min = −0.74 e Å⁻³
388 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.

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.

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

	x	y	z	U_iso*/U_eq
Co1	0.74918 (3)	0.74770 (4)	0.50943 (3)	0.01251 (9)
N1	0.8568 (2)	0.6511 (2)	0.6576 (2)	0.0193 (5)
C1	0.9395 (3)	0.6035 (3)	0.7155 (3)	0.0170 (6)
Se1	1.06840 (3)	0.53113 (3)	0.80450 (3)	0.02804 (10)
N2	0.6414 (2)	0.8434 (2)	0.3603 (2)	0.0194 (5)
C2	0.5651 (3)	0.8969 (3)	0.2944 (3)	0.0166 (6)
Se2	0.44604 (3)	0.97836 (3)	0.19407 (3)	0.02555 (10)
N10	0.8043 (2)	0.9230 (2)	0.5048 (2)	0.0166 (5)
N11	0.8491 (2)	1.0109 (2)	0.4008 (2)	0.0224 (5)
C11	0.8829 (3)	1.1191 (3)	0.3937 (3)	0.0253 (7)
H11	0.9165	1.1796	0.3208	0.030*
C12	0.8715 (3)	1.1488 (3)	0.4871 (3)	0.0282 (7)
H12	0.8946	1.2277	0.4782	0.034*
C13	0.8255 (3)	1.0588 (3)	0.5925 (3)	0.0307 (8)
H13	0.8157	1.0728	0.6598	0.037*
C14	0.7938 (3)	0.9459 (3)	0.5969 (3)	0.0236 (7)
H14	0.7630	0.8821	0.6697	0.028*
N20	0.8926 (2)	0.7545 (2)	0.3889 (2)	0.0140 (5)
N21	0.9612 (2)	0.6494 (2)	0.4300 (2)	0.0169 (5)
C21	1.0463 (3)	0.6422 (3)	0.3595 (3)	0.0219 (6)
H21	1.0933	0.5677	0.3882	0.026*
C22	1.0709 (3)	0.7375 (3)	0.2457 (3)	0.0273 (7)
H22	1.1337	0.7294	0.1983	0.033*
C23	1.0007 (3)	0.8436 (3)	0.2047 (3)	0.0223 (6)
H23	1.0133	0.9119	0.1279	0.027*
C24	0.9105 (3)	0.8474 (3)	0.2800 (3)	0.0189 (6)
H24	0.8597	0.9192	0.2525	0.023*
N30	0.6947 (2)	0.5719 (2)	0.5135 (2)	0.0170 (5)
N31	0.6603 (2)	0.4772 (2)	0.6183 (2)	0.0223 (5)
C31	0.6270 (3)	0.3707 (3)	0.6204 (3)	0.0290 (7)
H31	0.6007	0.3049	0.6941	0.035*
C32	0.6284 (3)	0.3506 (3)	0.5212 (3)	0.0321 (8)
H32	0.6048	0.2732	0.5266	0.038*
C33	0.6653 (3)	0.4469 (4)	0.4155 (3)	0.0325 (8)
H33	0.6692	0.4388	0.3446	0.039*
C34	0.6971 (3)	0.5576 (3)	0.4160 (3)	0.0240 (7)
H34	0.7216	0.6260	0.3432	0.029*
N40	0.6010 (2)	0.7439 (2)	0.6242 (2)	0.0151 (5)
N41	0.5359 (2)	0.8514 (2)	0.5780 (2)	0.0180 (5)
C41	0.4414 (3)	0.8588 (3)	0.6389 (3)	0.0220 (6)
H41	0.3961	0.9345	0.6065	0.026*
C42	0.4049 (3)	0.7623 (3)	0.7473 (3)	0.0249 (7)
H42	0.3354	0.7707	0.7872	0.030*
C43	0.4725 (3)	0.6542 (3)	0.7949 (3)	0.0228 (7)
H43	0.4525	0.5856	0.8694	0.027*
C44	0.5718 (3)	0.6497 (3)	0.7289 (3)	0.0199 (6)
H44	0.6205	0.5763	0.7602	0.024*
N50	0.6844 (3)	0.6254 (3)	1.0041 (3)	0.0348 (7)
N51	0.6207 (3)	0.6544 (3)	1.0784 (3)	0.0413 (8)
C51	0.6508 (4)	0.7539 (4)	1.0884 (4)	0.0467 (11)
H51	0.6039	0.7751	1.1396	0.056*
C52	0.7464 (4)	0.8295 (4)	1.0291 (4)	0.0470 (12)
H52	0.7661	0.8992	1.0404	0.056*
C53	0.8102 (3)	0.7995 (4)	0.9544 (4)	0.0456 (11)
H53	0.8763	0.8477	0.9100	0.055*
C54	0.7752 (3)	0.6955 (4)	0.9454 (4)	0.0373 (9)
H54	0.8195	0.6732	0.8935	0.045*
N60	0.2024 (3)	0.8989 (3)	0.9578 (3)	0.0301 (6)
N61	0.1110 (3)	0.8398 (3)	0.9384 (3)	0.0300 (6)
C61	0.1245 (3)	0.7193 (3)	0.9688 (3)	0.0320 (8)
H61	0.0601	0.6787	0.9546	0.038*
C62	0.2272 (3)	0.6484 (3)	1.0205 (3)	0.0325 (8)
H62	0.2328	0.5622	1.0412	0.039*
C63	0.3189 (3)	0.7088 (3)	1.0397 (3)	0.0308 (8)
H63	0.3913	0.6663	1.0745	0.037*
C64	0.3023 (3)	0.8353 (3)	1.0065 (3)	0.0281 (7)
H64	0.3656	0.8784	1.0191	0.034*

Atomic displacement parameters (Å²) top

	U¹¹	U²²	U³³	U¹²	U¹³	U²³
Co1	0.01260 (17)	0.00907 (17)	0.01339 (18)	0.00259 (13)	−0.00004 (13)	−0.00327 (14)
N1	0.0210 (12)	0.0180 (13)	0.0168 (12)	0.0044 (10)	−0.0027 (10)	−0.0064 (11)
C1	0.0224 (14)	0.0111 (14)	0.0165 (14)	−0.0024 (12)	0.0025 (11)	−0.0056 (11)
Se1	0.02541 (17)	0.02162 (19)	0.02991 (18)	0.00417 (14)	−0.01359 (14)	−0.00566 (15)
N2	0.0195 (12)	0.0165 (13)	0.0185 (12)	0.0046 (10)	−0.0032 (10)	−0.0051 (11)
C2	0.0190 (14)	0.0130 (14)	0.0174 (14)	−0.0002 (11)	0.0033 (11)	−0.0069 (12)
Se2	0.02245 (16)	0.02343 (19)	0.02468 (17)	0.00506 (13)	−0.01067 (13)	−0.00593 (14)
N10	0.0152 (11)	0.0115 (12)	0.0198 (12)	−0.0001 (9)	−0.0010 (9)	−0.0046 (10)
N11	0.0274 (13)	0.0140 (13)	0.0243 (13)	−0.0024 (11)	0.0058 (11)	−0.0078 (11)
C11	0.0258 (15)	0.0143 (15)	0.0315 (17)	−0.0040 (13)	0.0030 (13)	−0.0071 (14)
C12	0.0231 (15)	0.0214 (17)	0.045 (2)	−0.0046 (13)	−0.0019 (14)	−0.0196 (16)
C13	0.0326 (18)	0.037 (2)	0.0356 (19)	−0.0078 (16)	0.0009 (15)	−0.0273 (18)
C14	0.0239 (15)	0.0245 (17)	0.0237 (16)	−0.0069 (13)	0.0017 (12)	−0.0121 (14)
N20	0.0146 (11)	0.0123 (12)	0.0145 (11)	0.0027 (9)	0.0014 (9)	−0.0060 (10)
N21	0.0187 (11)	0.0129 (12)	0.0168 (12)	0.0063 (10)	−0.0003 (9)	−0.0052 (10)
C21	0.0210 (14)	0.0201 (16)	0.0254 (16)	0.0068 (13)	0.0021 (12)	−0.0117 (14)
C22	0.0249 (16)	0.033 (2)	0.0251 (16)	0.0050 (14)	0.0051 (13)	−0.0145 (15)
C23	0.0274 (16)	0.0206 (16)	0.0140 (14)	−0.0009 (13)	0.0042 (12)	−0.0041 (12)
C24	0.0234 (14)	0.0144 (15)	0.0166 (14)	0.0031 (12)	0.0011 (11)	−0.0054 (12)
N30	0.0156 (11)	0.0142 (12)	0.0210 (12)	0.0002 (10)	−0.0011 (9)	−0.0081 (10)
N31	0.0235 (13)	0.0161 (13)	0.0256 (13)	−0.0021 (11)	0.0038 (11)	−0.0083 (11)
C31	0.0313 (17)	0.0179 (16)	0.0352 (18)	−0.0046 (14)	0.0055 (14)	−0.0102 (15)
C32	0.0259 (17)	0.0266 (19)	0.050 (2)	−0.0100 (15)	0.0035 (16)	−0.0226 (18)
C33	0.0369 (19)	0.037 (2)	0.0339 (19)	−0.0111 (17)	−0.0009 (15)	−0.0251 (18)
C34	0.0244 (15)	0.0237 (17)	0.0238 (16)	−0.0037 (13)	−0.0027 (13)	−0.0108 (14)
N40	0.0142 (11)	0.0125 (12)	0.0165 (11)	0.0028 (9)	−0.0004 (9)	−0.0051 (10)
N41	0.0169 (11)	0.0154 (13)	0.0183 (12)	0.0049 (10)	0.0013 (9)	−0.0053 (10)
C41	0.0198 (14)	0.0210 (16)	0.0257 (16)	0.0067 (12)	0.0006 (12)	−0.0117 (14)
C42	0.0226 (15)	0.0308 (18)	0.0232 (16)	−0.0004 (13)	0.0091 (12)	−0.0145 (14)
C43	0.0274 (16)	0.0217 (17)	0.0166 (14)	−0.0065 (13)	0.0079 (12)	−0.0066 (13)
C44	0.0254 (15)	0.0126 (14)	0.0183 (14)	0.0031 (12)	−0.0018 (12)	−0.0042 (12)
N50	0.0330 (16)	0.0267 (16)	0.0481 (19)	0.0020 (13)	−0.0082 (14)	−0.0201 (15)
N51	0.0368 (17)	0.0308 (18)	0.049 (2)	0.0033 (14)	0.0010 (15)	−0.0126 (16)
C51	0.063 (3)	0.042 (2)	0.038 (2)	0.026 (2)	−0.013 (2)	−0.022 (2)
C52	0.059 (3)	0.0233 (19)	0.068 (3)	0.0145 (19)	−0.045 (2)	−0.028 (2)
C53	0.0251 (18)	0.026 (2)	0.064 (3)	−0.0011 (16)	−0.0099 (18)	−0.003 (2)
C54	0.039 (2)	0.033 (2)	0.037 (2)	0.0072 (17)	−0.0001 (16)	−0.0142 (18)
N60	0.0389 (16)	0.0172 (14)	0.0306 (15)	−0.0035 (12)	−0.0028 (13)	−0.0078 (12)
N61	0.0323 (15)	0.0254 (16)	0.0284 (15)	−0.0049 (13)	−0.0009 (12)	−0.0090 (13)
C61	0.0370 (19)	0.0288 (19)	0.0330 (19)	−0.0126 (16)	0.0046 (15)	−0.0164 (16)
C62	0.044 (2)	0.0183 (17)	0.0356 (19)	−0.0008 (15)	0.0095 (16)	−0.0133 (15)
C63	0.0279 (17)	0.033 (2)	0.0293 (18)	0.0060 (15)	0.0038 (14)	−0.0127 (16)
C64	0.0307 (17)	0.0275 (18)	0.0270 (17)	−0.0102 (14)	0.0052 (13)	−0.0132 (15)

Geometric parameters (Å, º) top

Co1—N1	2.084 (2)	C32—C33	1.369 (5)
Co1—N2	2.091 (2)	C32—H32	0.9500
Co1—N20	2.174 (2)	C33—C34	1.398 (5)
Co1—N40	2.175 (2)	C33—H33	0.9500
Co1—N10	2.197 (2)	C34—H34	0.9500
Co1—N30	2.204 (2)	N40—C44	1.327 (4)
N1—C1	1.157 (4)	N40—N41	1.353 (3)
C1—Se1	1.795 (3)	N41—C41	1.325 (4)
N2—C2	1.163 (4)	C41—C42	1.388 (5)
C2—Se2	1.793 (3)	C41—H41	0.9500
N10—C14	1.325 (4)	C42—C43	1.373 (5)
N10—N11	1.348 (4)	C42—H42	0.9500
N11—C11	1.334 (4)	C43—C44	1.395 (4)
C11—C12	1.393 (5)	C43—H43	0.9500
C11—H11	0.9500	C44—H44	0.9500
C12—C13	1.372 (5)	N50—C54	1.316 (5)
C12—H12	0.9500	N50—N51	1.340 (5)
C13—C14	1.395 (5)	N51—C51	1.320 (5)
C13—H13	0.9500	C51—C52	1.387 (7)
C14—H14	0.9500	C51—H51	0.9500
N20—C24	1.329 (4)	C52—C53	1.352 (7)
N20—N21	1.354 (3)	C52—H52	0.9500
N21—C21	1.325 (4)	C53—C54	1.381 (6)
C21—C22	1.392 (5)	C53—H53	0.9500
C21—H21	0.9500	C54—H54	0.9500
C22—C23	1.373 (5)	N60—C64	1.332 (4)
C22—H22	0.9500	N60—N61	1.353 (4)
C23—C24	1.393 (4)	N61—C61	1.328 (5)
C23—H23	0.9500	C61—C62	1.397 (5)
C24—H24	0.9500	C61—H61	0.9500
N30—C34	1.327 (4)	C62—C63	1.365 (5)
N30—N31	1.345 (4)	C62—H62	0.9500
N31—C31	1.337 (4)	C63—C64	1.393 (5)
C31—C32	1.390 (5)	C63—H63	0.9500
C31—H31	0.9500	C64—H64	0.9500

N1—Co1—N2	179.50 (11)	N31—C31—H31	118.0
N1—Co1—N20	91.87 (9)	C32—C31—H31	118.0
N2—Co1—N20	87.88 (9)	C33—C32—C31	117.2 (3)
N1—Co1—N40	90.35 (10)	C33—C32—H32	121.4
N2—Co1—N40	89.90 (9)	C31—C32—H32	121.4
N20—Co1—N40	177.76 (8)	C32—C33—C34	117.3 (3)
N1—Co1—N10	88.58 (9)	C32—C33—H33	121.4
N2—Co1—N10	91.87 (9)	C34—C33—H33	121.4
N20—Co1—N10	92.39 (9)	N30—C34—C33	123.1 (3)
N40—Co1—N10	87.93 (9)	N30—C34—H34	118.4
N1—Co1—N30	91.41 (9)	C33—C34—H34	118.4
N2—Co1—N30	88.14 (9)	C44—N40—N41	120.5 (2)
N20—Co1—N30	87.31 (9)	C44—N40—Co1	126.6 (2)
N40—Co1—N30	92.36 (9)	N41—N40—Co1	112.88 (17)
N10—Co1—N30	179.70 (10)	C41—N41—N40	118.2 (3)
C1—N1—Co1	161.1 (2)	N41—C41—C42	123.8 (3)
N1—C1—Se1	179.5 (3)	N41—C41—H41	118.1
C2—N2—Co1	166.1 (3)	C42—C41—H41	118.1
N2—C2—Se2	179.3 (3)	C43—C42—C41	117.8 (3)
C14—N10—N11	119.7 (3)	C43—C42—H42	121.1
C14—N10—Co1	123.5 (2)	C41—C42—H42	121.1
N11—N10—Co1	116.70 (18)	C42—C43—C44	117.0 (3)
C11—N11—N10	118.7 (3)	C42—C43—H43	121.5
N11—C11—C12	123.8 (3)	C44—C43—H43	121.5
N11—C11—H11	118.1	N40—C44—C43	122.6 (3)
C12—C11—H11	118.1	N40—C44—H44	118.7
C13—C12—C11	117.0 (3)	C43—C44—H44	118.7
C13—C12—H12	121.5	C54—N50—N51	119.1 (3)
C11—C12—H12	121.5	C51—N51—N50	118.3 (4)
C12—C13—C14	117.4 (3)	N51—C51—C52	124.4 (4)
C12—C13—H13	121.3	N51—C51—H51	117.8
C14—C13—H13	121.3	C52—C51—H51	117.8
N10—C14—C13	123.3 (3)	C53—C52—C51	116.8 (3)
N10—C14—H14	118.3	C53—C52—H52	121.6
C13—C14—H14	118.3	C51—C52—H52	121.6
C24—N20—N21	120.4 (2)	C52—C53—C54	117.0 (4)
C24—N20—Co1	125.23 (19)	C52—C53—H53	121.5
N21—N20—Co1	114.20 (17)	C54—C53—H53	121.5
C21—N21—N20	118.4 (2)	N50—C54—C53	124.3 (4)
N21—C21—C22	123.8 (3)	N50—C54—H54	117.8
N21—C21—H21	118.1	C53—C54—H54	117.8
C22—C21—H21	118.1	C64—N60—N61	119.5 (3)
C23—C22—C21	117.3 (3)	C61—N61—N60	118.4 (3)
C23—C22—H22	121.3	N61—C61—C62	124.4 (3)
C21—C22—H22	121.3	N61—C61—H61	117.8
C22—C23—C24	117.5 (3)	C62—C61—H61	117.8
C22—C23—H23	121.2	C63—C62—C61	116.8 (3)
C24—C23—H23	121.2	C63—C62—H62	121.6
N20—C24—C23	122.5 (3)	C61—C62—H62	121.6
N20—C24—H24	118.7	C62—C63—C64	117.5 (3)
C23—C24—H24	118.7	C62—C63—H63	121.3
C34—N30—N31	120.1 (3)	C64—C63—H63	121.3
C34—N30—Co1	121.5 (2)	N60—C64—C63	123.5 (3)
N31—N30—Co1	118.45 (19)	N60—C64—H64	118.3
C31—N31—N30	118.3 (3)	C63—C64—H64	118.3
N31—C31—C32	124.0 (3)

Experimental details

Crystal data
Chemical formula	[Co(SeCN)₂(C₄H₄N₂)₄]·2C₄H₄N₂
M_r	749.44
Crystal system, space group	Triclinic, P1
Temperature (K)	170
a, b, c (Å)	11.2138 (9), 12.0996 (11), 12.7033 (11)
α, β, γ (°)	62.206 (9), 88.827 (10), 88.682 (10)
V (Å³)	1524.3 (2)
Z	2
Radiation type	Mo Kα
µ (mm⁻¹)	2.99
Crystal size (mm)	0.15 × 0.11 × 0.08

Data collection
Diffractometer	STOE IPDS1
Absorption correction	Numerical (X-SHAPE and X-RED32; Stoe & Cie, 2008)
T_min, T_max	0.579, 0.697
No. of measured, independent and observed [I > 2σ(I)] reflections	16685, 7160, 4872
R_int	0.047
(sin θ/λ)_max (Å⁻¹)	0.660

Refinement
R[F² > 2σ(F²)], wR(F²), S	0.038, 0.100, 0.95
No. of reflections	7160
No. of parameters	388
H-atom treatment	H-atom parameters constrained
Δρ_max, Δρ_min (e Å⁻³)	0.42, −0.74

Computer programs: X-AREA (Stoe & Cie, 2008), SHELXS97 (Sheldrick, 2008), SHELXL97 (Sheldrick, 2008), XP in SHELXTL (Sheldrick, 2008) and DIAMOND (Brandenburg, 2011), XCIF in SHELXTL (Sheldrick, 2008).

Selected bond lengths (Å) top

Co1—N1	2.084 (2)	Co1—N40	2.175 (2)
Co1—N2	2.091 (2)	Co1—N10	2.197 (2)
Co1—N20	2.174 (2)	Co1—N30	2.204 (2)

Acknowledgements

We gratefully acknowledge financial support by the DFG (project No. NA 720/3–1) and the State of Schleswig-Holstein. We also thank Professor Dr Wolfgang Bensch for access to his experimental facilities.

References

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