Crystal structure of bis­(2,2′-bi­pyridine-κ2N,N′)bis­(thio­cyanato-κN)mang­anese(II) 2,2′-bi­pyridine monosolvate

Suckert, S.; Jess, I.; Näther, C.

doi:10.1107/S205698901402516X

metal-organic compounds

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ISSN: 2056-9890

Volume 71| Part 1| January 2015| Pages m3-m4

https://doi.org/10.1107/S205698901402516X

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Crystal structure of bis(2,2′-bipyridine-κ²N,N′)bis(thiocyanato-κN)manganese(II) 2,2′-bipyridine monosolvate

Stefan Suckert,^a ^* Inke Jess ^a and Christian Näther ^a

^aInstitut für Anorganische Chemie, Christian-Albrechts-Universität Kiel, Max-Eyth-Strasse 2, 24118 Kiel, Germany
^*Correspondence e-mail: ssuckert@ac.uni-kiel.de

Edited by M. Weil, Vienna University of Technology, Austria (Received 5 November 2014; accepted 17 November 2014; online 1 January 2015)

In the crystal structure of the mononuclear title compound, [Mn(NCS)₂(C₁₀H₈N₂)₂]·C₁₀H₈N₂, the Mn^II cation is coordinated in an all-cis configuration by two N-bound thiocyanate anions and two 2,2′-bipyridine ligands within a slightly distorted octahedral environment. The asymmetric unit consists of one Mn^II cation, two thiocyanate anions and two 2,2′-bipyridine ligands, as well as two non-coordinating 2,2′-bipyridine ligands that are each located on centres of inversion. In the crystal structure, the discrete [Mn(NCS)₂(C₁₀H₈N₂)₂] complex molecules are arranged in such a way that cavities are formed, in which the solvent 2,2′-bipyridine molecules are located. Apart from van der Waals forces, there are no remarkable intermolecular interactions present in the crystal structure.

Keywords: crystal structure; coordination polymer; octahedral manganese(II) coordination.

CCDC reference: 1034429

1. Related literature

For similar crystal structures with thiocyanate anions in cis-coordination to a manganese(II) cation, see: Małecki et al. (2011 ).

2. Experimental

2.1. Crystal data

[Mn(NCS)₂(C₁₀H₈N₂)₂]·C₁₀H₈N₂
M_r = 639.65
Monoclinic, P 2₁ /c
a = 14.5263 (6) Å
b = 13.5383 (4) Å
c = 16.0726 (7) Å
β = 105.535 (3)°
V = 3045.4 (2) Å³
Z = 4
Mo Kα radiation
μ = 0.61 mm⁻¹
T = 293 K
0.32 × 0.19 × 0.07 mm

2.2. Data collection

Stoe IPDS-2 diffractometer
Absorption correction: numerical (X-SHAPE and X-RED32; Stoe & Cie, 2008 ) T_min = 0.820, T_max = 0.919
41565 measured reflections
6630 independent reflections
5766 reflections with I > 2σ(I)
R_int = 0.037

2.3. Refinement

R[F² > 2σ(F²)] = 0.041
wR(F²) = 0.094
S = 1.08
6630 reflections
389 parameters
H-atom parameters constrained
Δρ_max = 0.27 e Å⁻³
Δρ_min = −0.35 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, 1999 ); software used to prepare material for publication: publCIF (Westrip, 2010 ).

Supporting information

CCDC reference: 1034429

Crystal structure: contains datablocks I, global. DOI: https://doi.org/10.1107/S205698901402516X/wm5090sup1.cif

Structure factors: contains datablock I. DOI: https://doi.org/10.1107/S205698901402516X/wm5090Isup2.hkl

checkCIF report

Synthesis and crystallization top

MnSO₄·H₂O was purchased from Merck and 2,2'-bipyridine and Ba(NCS)₂·3H₂O were purchased from Alfa Aesar. Mn(NCS)₂ was synthesized by stirring 17.97 g (58.44 mmol) Ba(NCS)₂·3H₂O and 9.88 g (58.44 mmol) MnSO₄·H₂O in 300 ml water at room temperature for three hours. The white residue of BaSO₄ was filtered off and the solvent removed with a rotary evaporator. The homogeneity of the product was investigated by X-ray powder diffraction and elemental analysis. The title compound was prepared by the reaction of 25.7 mg (0.15 mmol) Mn(NCS)₂ and 93.7 mg (0.60 mmol) 2,2'-bipyridine in 1.0 ml water at room temperature. After few days, yellow plates of the title compound were obtained.

Refinement top

The hydrogen atoms were positioned with idealized geometry and were refined with C—H = 0.93 Å and U_eq(H) = 1.2 U_eq(C) using a riding model approximation.

Related literature top

For similar crystal structures with thiocyanate anions in cis-coordination to a manganese(II) cation, see: Ma\/ecki et al. (2011).

Structure description top

For similar crystal structures with thiocyanate anions in cis-coordination to a manganese(II) cation, see: Ma\/ecki et al. (2011).

Synthesis and crystallization top

Refinement details top

The hydrogen atoms were positioned with idealized geometry and were refined with C—H = 0.93 Å and U_eq(H) = 1.2 U_eq(C) using a riding model approximation.

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, 1999); software used to prepare material for publication: publCIF (Westrip, 2010).

Figures top

	Fig. 1. The molecular components of the title compound with labelling and displacement ellipsoids drawn at the 50% probability level. [Symmetry codes: (i) -x+1,-y+1,-z+1; (ii) -x+2,-y+1,-z+1.]
	Fig. 2. The packing of the molecules in the crystal structure of the title compound in a view along [010].

Bis(2,2'-bipyridine-κ²N,N')bis(thiocyanato-κN)manganese(II) 2,2'-bipyridine monosolvate top

Crystal data top

[Mn(NCS)₂(C₁₀H₈N₂)₂]·C₁₀H₈N₂	Z = 4
M_r = 639.65	F(000) = 1316
Monoclinic, P2₁/c	D_x = 1.395 Mg m⁻³
Hall symbol: -P 2ybc	Mo Kα radiation, λ = 0.71073 Å
a = 14.5263 (6) Å	θ = 1.5–27.0°
b = 13.5383 (4) Å	µ = 0.61 mm⁻¹
c = 16.0726 (7) Å	T = 293 K
β = 105.535 (3)°	Plate, yellow
V = 3045.4 (2) Å³	0.32 × 0.19 × 0.07 mm

Data collection top

Stoe IPDS-2 diffractometer	6630 independent reflections
Radiation source: fine-focus sealed tube	5766 reflections with I > 2σ(I)
Graphite monochromator	R_int = 0.037
ω scans	θ_max = 27.0°, θ_min = 1.5°
Absorption correction: numerical (X-SHAPE and X-RED32; Stoe & Cie, 2008)	h = −18→18
T_min = 0.820, T_max = 0.919	k = −17→17
41565 measured reflections	l = −20→20

Refinement top

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)] = 0.041	H-atom parameters constrained
wR(F²) = 0.094	w = 1/[σ²(F_o²) + (0.0384P)² + 0.9654P] where P = (F_o² + 2F_c²)/3
S = 1.08	(Δ/σ)_max = 0.001
6630 reflections	Δρ_max = 0.27 e Å⁻³
389 parameters	Δρ_min = −0.35 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: 0.0025 (9)

Crystal data top

[Mn(NCS)₂(C₁₀H₈N₂)₂]·C₁₀H₈N₂	V = 3045.4 (2) Å³
M_r = 639.65	Z = 4
Monoclinic, P2₁/c	Mo Kα radiation
a = 14.5263 (6) Å	µ = 0.61 mm⁻¹
b = 13.5383 (4) Å	T = 293 K
c = 16.0726 (7) Å	0.32 × 0.19 × 0.07 mm
β = 105.535 (3)°

Data collection top

Stoe IPDS-2 diffractometer	6630 independent reflections
Absorption correction: numerical (X-SHAPE and X-RED32; Stoe & Cie, 2008)	5766 reflections with I > 2σ(I)
T_min = 0.820, T_max = 0.919	R_int = 0.037
41565 measured reflections

Refinement top

R[F² > 2σ(F²)] = 0.041	0 restraints
wR(F²) = 0.094	H-atom parameters constrained
S = 1.08	Δρ_max = 0.27 e Å⁻³
6630 reflections	Δρ_min = −0.35 e Å⁻³
389 parameters

Special details top

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.

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

	x	y	z	U_iso*/U_eq
Mn1	0.734793 (17)	0.128336 (19)	0.478914 (17)	0.04106 (9)
N1	0.70830 (14)	0.02009 (14)	0.37737 (12)	0.0665 (5)
C1	0.71894 (13)	−0.04547 (14)	0.33491 (12)	0.0502 (4)
S1	0.73507 (5)	−0.13676 (5)	0.27623 (4)	0.0792 (2)
N2	0.75999 (12)	0.02533 (13)	0.58481 (11)	0.0583 (4)
C2	0.77308 (12)	−0.03438 (13)	0.63794 (12)	0.0453 (4)
S2	0.79008 (5)	−0.11880 (5)	0.71196 (4)	0.07089 (17)
N10	0.88949 (10)	0.14680 (12)	0.47586 (10)	0.0513 (4)
C10	0.92943 (15)	0.09366 (18)	0.42424 (15)	0.0652 (6)
H10	0.8898	0.0546	0.3818	0.078*
C11	1.02539 (17)	0.0938 (2)	0.43073 (19)	0.0824 (8)
H11	1.0502	0.0572	0.3928	0.099*
C12	1.08341 (17)	0.1492 (2)	0.4943 (2)	0.0908 (9)
H12	1.1490	0.1497	0.5010	0.109*
C13	1.04482 (15)	0.2043 (2)	0.54863 (18)	0.0792 (7)
H13	1.0840	0.2420	0.5924	0.095*
C14	0.94611 (13)	0.20298 (15)	0.53718 (13)	0.0541 (5)
C15	0.89768 (13)	0.26359 (14)	0.58963 (12)	0.0517 (4)
C16	0.94487 (18)	0.33141 (19)	0.65064 (15)	0.0728 (6)
H16	1.0108	0.3385	0.6629	0.087*
C17	0.8933 (2)	0.3882 (2)	0.69288 (16)	0.0852 (8)
H17	0.9244	0.4343	0.7337	0.102*
C18	0.7964 (2)	0.37728 (17)	0.67522 (16)	0.0771 (7)
H18	0.7605	0.4157	0.7030	0.092*
C19	0.75380 (16)	0.30723 (16)	0.61475 (13)	0.0607 (5)
H19	0.6880	0.2987	0.6025	0.073*
N11	0.80238 (10)	0.25125 (11)	0.57302 (10)	0.0488 (3)
N20	0.67171 (10)	0.24892 (11)	0.38090 (9)	0.0470 (3)
C20	0.72036 (15)	0.29317 (17)	0.33176 (14)	0.0624 (5)
H20	0.7831	0.2736	0.3374	0.075*
C21	0.68249 (19)	0.36615 (18)	0.27327 (15)	0.0726 (6)
H21	0.7188	0.3955	0.2404	0.087*
C22	0.59047 (19)	0.39454 (17)	0.26467 (14)	0.0713 (6)
H22	0.5632	0.4443	0.2260	0.086*
C24	0.58074 (12)	0.27636 (13)	0.37188 (11)	0.0446 (4)
C25	0.53069 (12)	0.22504 (13)	0.42834 (11)	0.0438 (4)
C26	0.43568 (13)	0.24294 (17)	0.42531 (14)	0.0613 (5)
H26	0.4000	0.2878	0.3858	0.074*
C27	0.39498 (14)	0.19383 (19)	0.48122 (15)	0.0689 (6)
H27	0.3314	0.2050	0.4797	0.083*
C28	0.44834 (15)	0.12849 (17)	0.53914 (15)	0.0652 (6)
H28	0.4223	0.0955	0.5782	0.078*
C29	0.54214 (14)	0.11259 (15)	0.53824 (13)	0.0538 (4)
H29	0.5782	0.0671	0.5768	0.065*
N21	0.58328 (10)	0.15956 (11)	0.48459 (9)	0.0427 (3)
N30	0.45727 (13)	0.57292 (15)	0.40356 (13)	0.0690 (5)
C30	0.52000 (14)	0.52678 (15)	0.46832 (13)	0.0557 (5)
C31	0.61789 (15)	0.52953 (17)	0.47611 (15)	0.0654 (5)
H31	0.6605	0.4974	0.5216	0.078*
C23	0.53780 (16)	0.34899 (15)	0.31364 (13)	0.0597 (5)
H23	0.4745	0.3668	0.3076	0.072*
C32	0.65066 (18)	0.5801 (2)	0.41603 (18)	0.0766 (6)
H32	0.7158	0.5826	0.4203	0.092*
C33	0.5866 (2)	0.6271 (2)	0.34934 (19)	0.0813 (7)
H33	0.6069	0.6617	0.3075	0.098*
C34	0.4917 (2)	0.6212 (2)	0.34664 (18)	0.0822 (7)
H34	0.4483	0.6533	0.3017	0.099*
N40	0.89931 (14)	0.56056 (16)	0.52370 (14)	0.0753 (5)
C40	0.99023 (15)	0.53074 (16)	0.53470 (14)	0.0617 (5)
C41	1.06105 (17)	0.55483 (19)	0.60838 (17)	0.0756 (6)
H41	1.1234	0.5332	0.6150	0.091*
C42	1.0391 (2)	0.6106 (2)	0.67145 (19)	0.0877 (8)
H42	1.0863	0.6269	0.7212	0.105*
C43	0.9471 (2)	0.6423 (2)	0.6607 (2)	0.0887 (8)
H43	0.9301	0.6808	0.7022	0.106*
C44	0.8805 (2)	0.6148 (2)	0.5856 (2)	0.0891 (8)
H44	0.8179	0.6360	0.5779	0.107*

Atomic displacement parameters (Å²) top

	U¹¹	U²²	U³³	U¹²	U¹³	U²³
Mn1	0.03601 (14)	0.04340 (15)	0.04746 (15)	0.00108 (10)	0.01753 (10)	0.00063 (11)
N1	0.0761 (12)	0.0621 (10)	0.0701 (11)	−0.0069 (9)	0.0350 (9)	−0.0150 (9)
C1	0.0426 (9)	0.0562 (11)	0.0537 (10)	−0.0084 (8)	0.0160 (8)	−0.0048 (9)
S1	0.0676 (4)	0.0790 (4)	0.0828 (4)	0.0061 (3)	0.0057 (3)	−0.0377 (3)
N2	0.0596 (10)	0.0556 (9)	0.0651 (10)	0.0078 (8)	0.0263 (8)	0.0123 (8)
C2	0.0384 (9)	0.0475 (9)	0.0520 (10)	0.0034 (7)	0.0156 (7)	−0.0024 (8)
S2	0.0751 (4)	0.0693 (4)	0.0641 (3)	0.0054 (3)	0.0114 (3)	0.0214 (3)
N10	0.0365 (7)	0.0616 (9)	0.0595 (9)	0.0044 (7)	0.0193 (7)	0.0112 (7)
C10	0.0494 (11)	0.0803 (14)	0.0749 (14)	0.0122 (10)	0.0322 (10)	0.0105 (11)
C11	0.0504 (13)	0.110 (2)	0.0989 (19)	0.0219 (13)	0.0401 (13)	0.0237 (16)
C12	0.0393 (12)	0.122 (2)	0.118 (2)	0.0176 (13)	0.0336 (14)	0.0357 (19)
C13	0.0369 (10)	0.1010 (19)	0.0934 (17)	−0.0024 (11)	0.0064 (11)	0.0213 (15)
C14	0.0358 (9)	0.0635 (11)	0.0622 (11)	0.0022 (8)	0.0118 (8)	0.0231 (9)
C15	0.0438 (10)	0.0546 (10)	0.0511 (10)	−0.0077 (8)	0.0028 (8)	0.0144 (8)
C16	0.0667 (14)	0.0834 (16)	0.0601 (13)	−0.0265 (12)	0.0026 (11)	0.0038 (12)
C17	0.107 (2)	0.0806 (17)	0.0594 (13)	−0.0404 (15)	0.0067 (13)	−0.0107 (12)
C18	0.105 (2)	0.0623 (13)	0.0658 (14)	−0.0101 (13)	0.0267 (13)	−0.0163 (11)
C19	0.0612 (12)	0.0589 (12)	0.0613 (12)	0.0014 (9)	0.0152 (10)	−0.0102 (9)
N11	0.0435 (8)	0.0482 (8)	0.0525 (8)	−0.0004 (6)	0.0092 (6)	−0.0006 (7)
N20	0.0417 (8)	0.0520 (8)	0.0484 (8)	−0.0029 (6)	0.0138 (6)	0.0047 (6)
C20	0.0565 (12)	0.0711 (13)	0.0632 (12)	−0.0047 (10)	0.0224 (10)	0.0149 (10)
C21	0.0851 (17)	0.0725 (14)	0.0640 (13)	−0.0082 (12)	0.0263 (12)	0.0184 (11)
C22	0.0941 (18)	0.0619 (13)	0.0537 (12)	0.0076 (12)	0.0124 (11)	0.0127 (10)
C24	0.0443 (9)	0.0451 (9)	0.0416 (8)	−0.0004 (7)	0.0067 (7)	−0.0065 (7)
C25	0.0356 (8)	0.0490 (9)	0.0449 (9)	−0.0015 (7)	0.0074 (7)	−0.0106 (7)
C26	0.0382 (10)	0.0787 (14)	0.0643 (12)	0.0056 (9)	0.0092 (9)	−0.0058 (10)
C27	0.0356 (10)	0.0932 (17)	0.0808 (15)	−0.0046 (10)	0.0204 (10)	−0.0164 (13)
C28	0.0515 (11)	0.0793 (14)	0.0750 (14)	−0.0152 (11)	0.0347 (10)	−0.0095 (11)
C29	0.0471 (10)	0.0600 (11)	0.0604 (11)	−0.0049 (8)	0.0252 (9)	0.0006 (9)
N21	0.0356 (7)	0.0481 (8)	0.0470 (7)	−0.0026 (6)	0.0156 (6)	−0.0036 (6)
N30	0.0588 (11)	0.0760 (12)	0.0703 (11)	0.0131 (9)	0.0142 (9)	0.0083 (10)
C30	0.0503 (10)	0.0544 (11)	0.0604 (11)	0.0062 (8)	0.0114 (9)	−0.0080 (9)
C31	0.0506 (11)	0.0706 (13)	0.0729 (13)	0.0050 (10)	0.0130 (10)	−0.0043 (11)
C23	0.0614 (12)	0.0612 (12)	0.0510 (10)	0.0114 (9)	0.0057 (9)	0.0024 (9)
C32	0.0615 (14)	0.0809 (16)	0.0920 (17)	−0.0015 (12)	0.0284 (13)	−0.0054 (14)
C33	0.0883 (18)	0.0790 (16)	0.0859 (17)	0.0012 (14)	0.0393 (15)	0.0057 (13)
C34	0.0789 (17)	0.0874 (18)	0.0802 (16)	0.0168 (14)	0.0213 (13)	0.0194 (14)
N40	0.0546 (11)	0.0821 (13)	0.0871 (14)	0.0114 (9)	0.0154 (10)	0.0058 (11)
C40	0.0504 (11)	0.0597 (12)	0.0739 (13)	−0.0028 (9)	0.0149 (10)	0.0118 (10)
C41	0.0511 (12)	0.0830 (16)	0.0892 (17)	−0.0076 (11)	0.0129 (11)	−0.0039 (13)
C42	0.0705 (16)	0.101 (2)	0.0909 (19)	−0.0179 (14)	0.0202 (14)	−0.0150 (16)
C43	0.0837 (18)	0.0873 (18)	0.102 (2)	−0.0051 (14)	0.0361 (16)	−0.0132 (15)
C44	0.0668 (16)	0.095 (2)	0.106 (2)	0.0150 (14)	0.0247 (15)	−0.0003 (17)

Geometric parameters (Å, º) top

Mn1—N1	2.1501 (18)	C22—C23	1.381 (3)
Mn1—N2	2.1546 (17)	C22—H22	0.9300
Mn1—N21	2.2669 (13)	C24—C23	1.386 (3)
Mn1—N10	2.2746 (14)	C24—C25	1.479 (2)
Mn1—N20	2.2833 (15)	C25—N21	1.348 (2)
Mn1—N11	2.2859 (15)	C25—C26	1.389 (2)
N1—C1	1.155 (2)	C26—C27	1.372 (3)
C1—S1	1.609 (2)	C26—H26	0.9300
N2—C2	1.154 (2)	C27—C28	1.365 (3)
C2—S2	1.6203 (19)	C27—H27	0.9300
N10—C14	1.339 (3)	C28—C29	1.383 (3)
N10—C10	1.342 (3)	C28—H28	0.9300
C10—C11	1.370 (3)	C29—N21	1.335 (2)
C10—H10	0.9300	C29—H29	0.9300
C11—C12	1.362 (4)	N30—C34	1.326 (3)
C11—H11	0.9300	N30—C30	1.340 (3)
C12—C13	1.377 (4)	C30—C31	1.394 (3)
C12—H12	0.9300	C30—C30ⁱ	1.489 (4)
C13—C14	1.396 (3)	C31—C32	1.369 (3)
C13—H13	0.9300	C31—H31	0.9300
C14—C15	1.482 (3)	C23—H23	0.9300
C15—N11	1.348 (2)	C32—C33	1.373 (4)
C15—C16	1.384 (3)	C32—H32	0.9300
C16—C17	1.373 (4)	C33—C34	1.370 (4)
C16—H16	0.9300	C33—H33	0.9300
C17—C18	1.367 (4)	C34—H34	0.9300
C17—H17	0.9300	N40—C44	1.322 (3)
C18—C19	1.380 (3)	N40—C40	1.347 (3)
C18—H18	0.9300	C40—C41	1.384 (3)
C19—N11	1.333 (2)	C40—C40ⁱⁱ	1.479 (5)
C19—H19	0.9300	C41—C42	1.368 (4)
N20—C20	1.335 (2)	C41—H41	0.9300
N20—C24	1.343 (2)	C42—C43	1.371 (4)
C20—C21	1.373 (3)	C42—H42	0.9300
C20—H20	0.9300	C43—C44	1.380 (4)
C21—C22	1.362 (4)	C43—H43	0.9300
C21—H21	0.9300	C44—H44	0.9300

N1—Mn1—N2	96.69 (7)	C22—C21—H21	120.8
N1—Mn1—N21	100.33 (6)	C20—C21—H21	120.8
N2—Mn1—N21	92.88 (6)	C21—C22—C23	119.6 (2)
N1—Mn1—N10	92.04 (7)	C21—C22—H22	120.2
N2—Mn1—N10	97.38 (6)	C23—C22—H22	120.2
N21—Mn1—N10	162.91 (6)	N20—C24—C23	121.42 (18)
N1—Mn1—N20	90.37 (7)	N20—C24—C25	115.79 (15)
N2—Mn1—N20	163.68 (6)	C23—C24—C25	122.79 (17)
N21—Mn1—N20	71.33 (5)	N21—C25—C26	121.16 (18)
N10—Mn1—N20	97.05 (5)	N21—C25—C24	115.91 (14)
N1—Mn1—N11	163.00 (6)	C26—C25—C24	122.92 (17)
N2—Mn1—N11	89.80 (6)	C27—C26—C25	119.4 (2)
N21—Mn1—N11	95.00 (5)	C27—C26—H26	120.3
N10—Mn1—N11	71.49 (6)	C25—C26—H26	120.3
N20—Mn1—N11	87.59 (5)	C28—C27—C26	119.67 (19)
C1—N1—Mn1	161.31 (18)	C28—C27—H27	120.2
N1—C1—S1	179.3 (2)	C26—C27—H27	120.2
C2—N2—Mn1	175.86 (16)	C27—C28—C29	118.3 (2)
N2—C2—S2	179.25 (19)	C27—C28—H28	120.8
C14—N10—C10	118.54 (17)	C29—C28—H28	120.8
C14—N10—Mn1	117.53 (12)	N21—C29—C28	123.0 (2)
C10—N10—Mn1	123.21 (14)	N21—C29—H29	118.5
N10—C10—C11	123.5 (2)	C28—C29—H29	118.5
N10—C10—H10	118.3	C29—N21—C25	118.38 (15)
C11—C10—H10	118.3	C29—N21—Mn1	123.00 (12)
C12—C11—C10	118.1 (3)	C25—N21—Mn1	118.53 (11)
C12—C11—H11	121.0	C34—N30—C30	117.5 (2)
C10—C11—H11	121.0	N30—C30—C31	121.5 (2)
C11—C12—C13	119.9 (2)	N30—C30—C30ⁱ	116.7 (2)
C11—C12—H12	120.0	C31—C30—C30ⁱ	121.8 (2)
C13—C12—H12	120.0	C32—C31—C30	119.3 (2)
C12—C13—C14	119.2 (3)	C32—C31—H31	120.4
C12—C13—H13	120.4	C30—C31—H31	120.4
C14—C13—H13	120.4	C22—C23—C24	119.0 (2)
N10—C14—C13	120.7 (2)	C22—C23—H23	120.5
N10—C14—C15	116.21 (15)	C24—C23—H23	120.5
C13—C14—C15	123.0 (2)	C31—C32—C33	119.4 (2)
N11—C15—C16	120.7 (2)	C31—C32—H32	120.3
N11—C15—C14	115.93 (16)	C33—C32—H32	120.3
C16—C15—C14	123.36 (19)	C34—C33—C32	117.6 (2)
C17—C16—C15	119.3 (2)	C34—C33—H33	121.2
C17—C16—H16	120.3	C32—C33—H33	121.2
C15—C16—H16	120.3	N30—C34—C33	124.7 (2)
C18—C17—C16	120.3 (2)	N30—C34—H34	117.7
C18—C17—H17	119.9	C33—C34—H34	117.7
C16—C17—H17	119.9	C44—N40—C40	117.4 (2)
C17—C18—C19	117.6 (2)	N40—C40—C41	121.3 (2)
C17—C18—H18	121.2	N40—C40—C40ⁱⁱ	116.7 (2)
C19—C18—H18	121.2	C41—C40—C40ⁱⁱ	122.0 (3)
N11—C19—C18	123.2 (2)	C42—C41—C40	119.8 (2)
N11—C19—H19	118.4	C42—C41—H41	120.1
C18—C19—H19	118.4	C40—C41—H41	120.1
C19—N11—C15	118.94 (17)	C41—C42—C43	119.5 (3)
C19—N11—Mn1	123.75 (13)	C41—C42—H42	120.3
C15—N11—Mn1	117.23 (13)	C43—C42—H42	120.3
C20—N20—C24	118.28 (17)	C42—C43—C44	117.2 (3)
C20—N20—Mn1	123.43 (13)	C42—C43—H43	121.4
C24—N20—Mn1	118.28 (11)	C44—C43—H43	121.4
N20—C20—C21	123.3 (2)	N40—C44—C43	124.8 (3)
N20—C20—H20	118.3	N40—C44—H44	117.6
C21—C20—H20	118.3	C43—C44—H44	117.6
C22—C21—C20	118.4 (2)

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

Experimental details

Crystal data
Chemical formula	[Mn(NCS)₂(C₁₀H₈N₂)₂]·C₁₀H₈N₂
M_r	639.65
Crystal system, space group	Monoclinic, P2₁/c
Temperature (K)	293
a, b, c (Å)	14.5263 (6), 13.5383 (4), 16.0726 (7)
β (°)	105.535 (3)
V (Å³)	3045.4 (2)
Z	4
Radiation type	Mo Kα
µ (mm⁻¹)	0.61
Crystal size (mm)	0.32 × 0.19 × 0.07

Data collection
Diffractometer	Stoe IPDS2
Absorption correction	Numerical (X-SHAPE and X-RED32; Stoe & Cie, 2008)
T_min, T_max	0.820, 0.919
No. of measured, independent and observed [I > 2σ(I)] reflections	41565, 6630, 5766
R_int	0.037

Refinement
R[F² > 2σ(F²)], wR(F²), S	0.041, 0.094, 1.08
No. of reflections	6630
No. of parameters	389
H-atom treatment	H-atom parameters constrained
Δρ_max, Δρ_min (e Å⁻³)	0.27, −0.35

Computer programs: X-AREA (Stoe & Cie, 2008), SHELXS97 (Sheldrick, 2008), SHELXL97 (Sheldrick, 2008), XP in SHELXTL (Sheldrick, 2008) and DIAMOND (Brandenburg, 1999), publCIF (Westrip, 2010).

Acknowledgements

We gratefully acknowledge financial support by the DFG (project No. NA 720/5–1) and the State of Schleswig–Holstein. We thank Professor Dr Wolfgang Bensch for access to his experimental facilities.

References

Brandenburg, K. (1999). DIAMOND. Crystal Impact GbR, Bonn, Germany. Google Scholar
Małecki, J. G., Machura, B., Świtlicka, A., Groń, T. & Bałanda, M. (2011). Polyhedron, 30, 746–753. Google Scholar
Sheldrick, G. M. (2008). Acta Cryst. A64, 112–122. Web of Science CrossRef CAS IUCr Journals Google Scholar
Stoe & Cie (2008). X-AREA, X-RED32 and X-SHAPE. Stoe & Cie, Darmstadt, Germany. 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 71| Part 1| January 2015| Pages m3-m4

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