Trans-bis-(3-tert-butyl-pyridine-κN)bis-(4-tert-butyl-pyridine-κN)bis-(thio-cyanato-κN)manganese(II).

The asymmetric unit of the title compound [Mn(NCS)(2)(C(9)H(13)N)(4)] consists of one Mn(II) cation located on a center of inversion, one thio-cyanato anion, one 3-tert-butyl-pyridine ligand and one 4-tert-butyl-pyridine ligand in general positions. The tert-butyl group of the 4-tert-butyl-pyridine ligand is disordered over two sets of sites in a 0.60:0.40 ratio. The Mn(II) cation is coordinated by six N atoms of four tert-butyl-pyridine ligands and two N-bonded thio-cyanato anions within a slightly distorted octa-hedral coordination environment.

Related literature

For related structures, see: Nassimbeni et al. (1990 ▶) (4-tert-butyl­pyridine only). For the background to this work, see: Boeckmann & Näther (2010 ▶, 2011 ▶).

Experimental

Crystal data

[Mn(NCS)2(C9H13N)4]

M = 711.92

Triclinic,

a = 9.5921 (7) Å

b = 10.7253 (9) Å

c = 11.6286 (10) Å

α = 66.870 (9)°

β = 68.011 (9)°

γ = 76.359 (9)°

V = 1014.59 (17) Å3

Z = 1

Mo Kα radiation

μ = 0.46 mm−1

T = 200 K

0.13 × 0.09 × 0.05 mm

Data collection

STOE IPDS-1 diffractometer

7271 measured reflections

3845 independent reflections

3017 reflections with I > 2σ(I)

R int = 0.037

Refinement

R[F 2 > 2σ(F 2)] = 0.049

wR(F 2) = 0.128

S = 1.03

3845 reflections

241 parameters

3 restraints

H-atom parameters constrained

Δρmax = 0.92 e Å−3

Δρmin = −0.88 e Å−3

Data collection: X-AREA (Stoe, 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: publCIF (Westrip, 2010 ▶).

Click here for additional data file.

Crystal structure: contains datablock(s) I, global. DOI: 10.1107/S1600536812041128/im2404sup1.cif

Click here for additional data file.

Structure factors: contains datablock(s) I. DOI: 10.1107/S1600536812041128/im2404Isup2.hkl

Additional supplementary materials: crystallographic information; 3D view; checkCIF report

[Mn(NCS)2(C9H13N)4]	Z = 1
Mr = 711.92	F(000) = 379
Triclinic, P1	Dx = 1.165 Mg m−3
Hall symbol: -P 1	Mo Kα radiation, λ = 0.71073 Å
a = 9.5921 (7) Å	Cell parameters from 6934 reflections
b = 10.7253 (9) Å	θ = 1.9–28.2°
c = 11.6286 (10) Å	µ = 0.46 mm−1
α = 66.870 (9)°	T = 200 K
β = 68.011 (9)°	Needle, colourless
γ = 76.359 (9)°	0.13 × 0.09 × 0.05 mm
V = 1014.59 (17) Å3

STOE IPDS-1 diffractometer	3017 reflections with I > 2σ(I)
Radiation source: fine-focus sealed tube	Rint = 0.037
Graphite monochromator	θmax = 26.0°, θmin = 2.5°
Phi scans	h = −11→11
7271 measured reflections	k = −13→12
3845 independent reflections	l = −14→14

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)] = 0.049	Hydrogen site location: inferred from neighbouring sites
wR(F2) = 0.128	H-atom parameters constrained
S = 1.03	w = 1/[σ2(Fo2) + (0.0656P)2 + 0.489P] where P = (Fo2 + 2Fc2)/3
3845 reflections	(Δ/σ)max < 0.001
241 parameters	Δρmax = 0.92 e Å−3
3 restraints	Δρmin = −0.88 e Å−3

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.

	x	y	z	Uiso*/Ueq	Occ. (<1)
Mn1	0.5000	0.5000	1.0000	0.03151 (17)
N1	0.6416 (3)	0.6660 (2)	0.9167 (2)	0.0419 (5)
C1	0.6822 (3)	0.7724 (2)	0.8511 (2)	0.0383 (6)
S1	0.73642 (11)	0.92047 (9)	0.75445 (13)	0.0912 (4)
N11	0.3015 (2)	0.65601 (19)	0.94157 (18)	0.0352 (5)
C11	0.1639 (3)	0.6132 (3)	0.9872 (2)	0.0418 (6)
H11	0.1523	0.5200	1.0387	0.050*
C12	0.0397 (3)	0.6983 (3)	0.9625 (3)	0.0481 (7)
H12	−0.0555	0.6641	0.9950	0.058*
C13	0.0547 (3)	0.8350 (3)	0.8892 (3)	0.0433 (6)
H13	−0.0307	0.8950	0.8713	0.052*
C14	0.1938 (3)	0.8843 (2)	0.8421 (2)	0.0367 (5)
C15	0.3133 (3)	0.7888 (2)	0.8708 (2)	0.0370 (5)
H15	0.4103	0.8199	0.8380	0.044*
C16	0.2198 (3)	1.0344 (3)	0.7629 (3)	0.0493 (7)
C17	0.3273 (5)	1.0455 (4)	0.6249 (3)	0.0840 (13)
H17A	0.3451	1.1411	0.5740	0.126*
H17B	0.2825	1.0116	0.5811	0.126*
H17C	0.4235	0.9910	0.6310	0.126*
C18	0.0701 (4)	1.1229 (3)	0.7584 (4)	0.0711 (10)
H18A	0.0896	1.2182	0.7083	0.107*
H18B	0.0043	1.1149	0.8483	0.107*
H18C	0.0206	1.0922	0.7156	0.107*
C19	0.2930 (4)	1.0855 (3)	0.8312 (4)	0.0690 (10)
H19A	0.3097	1.1815	0.7815	0.103*
H19B	0.3899	1.0312	0.8346	0.103*
H19C	0.2258	1.0765	0.9210	0.103*
N21	0.5965 (2)	0.4594 (2)	0.80246 (18)	0.0363 (5)
C21	0.5945 (4)	0.3378 (3)	0.7974 (3)	0.0516 (7)
H21	0.5477	0.2697	0.8769	0.062*
C22	0.6561 (4)	0.3048 (3)	0.6840 (3)	0.0527 (8)
H22	0.6509	0.2160	0.6872	0.063*
C23	0.7253 (3)	0.3997 (2)	0.5657 (2)	0.0349 (5)
C24	0.7275 (4)	0.5254 (3)	0.5714 (2)	0.0540 (8)
H24	0.7735	0.5954	0.4934	0.065*
C25	0.6638 (4)	0.5507 (3)	0.6890 (2)	0.0512 (7)
H25	0.6684	0.6383	0.6888	0.061*
C26	0.7927 (3)	0.3670 (3)	0.4375 (2)	0.0448 (6)
C27	0.6680 (9)	0.3097 (12)	0.4244 (8)	0.100 (3)	0.60
H27A	0.6334	0.2307	0.5030	0.150*	0.60
H27B	0.7087	0.2819	0.3462	0.150*	0.60
H27C	0.5828	0.3802	0.4156	0.150*	0.60
C28	0.8526 (15)	0.4830 (7)	0.3205 (6)	0.113 (4)	0.60
H28A	0.8932	0.4547	0.2426	0.170*	0.60
H28B	0.9333	0.5145	0.3314	0.170*	0.60
H28C	0.7714	0.5572	0.3093	0.170*	0.60
C29	0.9189 (9)	0.2494 (8)	0.4536 (6)	0.084 (2)	0.60
H29A	0.8789	0.1724	0.5324	0.125*	0.60
H29B	1.0016	0.2798	0.4628	0.125*	0.60
H29C	0.9567	0.2210	0.3759	0.125*	0.60
C27'	0.7316 (12)	0.4873 (11)	0.3296 (8)	0.064 (3)	0.40
H27D	0.7487	0.5748	0.3277	0.096*	0.40
H27E	0.6231	0.4843	0.3513	0.096*	0.40
H27F	0.7852	0.4773	0.2431	0.096*	0.40
C28'	0.9667 (10)	0.3858 (13)	0.3845 (9)	0.079 (3)	0.40
H28D	0.9795	0.4746	0.3828	0.118*	0.40
H28E	1.0105	0.3812	0.2952	0.118*	0.40
H28F	1.0181	0.3132	0.4426	0.118*	0.40
C29'	0.769 (2)	0.2383 (12)	0.4445 (10)	0.116 (7)	0.40
H29D	0.8157	0.2285	0.3574	0.174*	0.40
H29E	0.6597	0.2319	0.4733	0.174*	0.40
H29F	0.8134	0.1657	0.5076	0.174*	0.40

	U11	U22	U33	U12	U13	U23
Mn1	0.0411 (3)	0.0235 (3)	0.0266 (3)	−0.0085 (2)	−0.0061 (2)	−0.00652 (18)
N1	0.0488 (13)	0.0310 (11)	0.0420 (11)	−0.0114 (9)	−0.0091 (9)	−0.0093 (9)
C1	0.0349 (14)	0.0326 (13)	0.0469 (14)	−0.0053 (10)	−0.0150 (11)	−0.0099 (11)
S1	0.0620 (6)	0.0369 (4)	0.1414 (10)	−0.0216 (4)	−0.0427 (6)	0.0232 (5)
N11	0.0437 (12)	0.0289 (10)	0.0315 (10)	−0.0072 (9)	−0.0101 (8)	−0.0083 (8)
C11	0.0470 (15)	0.0324 (12)	0.0417 (13)	−0.0122 (11)	−0.0088 (11)	−0.0086 (10)
C12	0.0404 (15)	0.0459 (15)	0.0531 (15)	−0.0123 (12)	−0.0083 (12)	−0.0137 (12)
C13	0.0407 (15)	0.0400 (14)	0.0451 (14)	−0.0019 (11)	−0.0118 (11)	−0.0133 (11)
C14	0.0417 (14)	0.0324 (12)	0.0315 (11)	−0.0043 (10)	−0.0077 (10)	−0.0095 (9)
C15	0.0393 (14)	0.0326 (12)	0.0340 (12)	−0.0086 (10)	−0.0065 (10)	−0.0080 (9)
C16	0.0475 (16)	0.0301 (13)	0.0551 (16)	−0.0028 (11)	−0.0099 (13)	−0.0055 (11)
C17	0.109 (3)	0.0498 (19)	0.0509 (19)	−0.018 (2)	0.0052 (19)	0.0024 (15)
C18	0.066 (2)	0.0398 (16)	0.091 (2)	−0.0001 (15)	−0.0324 (19)	−0.0019 (16)
C19	0.062 (2)	0.0373 (16)	0.107 (3)	−0.0050 (14)	−0.0248 (19)	−0.0252 (17)
N21	0.0482 (13)	0.0308 (10)	0.0283 (9)	−0.0064 (9)	−0.0089 (8)	−0.0101 (8)
C21	0.078 (2)	0.0334 (13)	0.0322 (12)	−0.0183 (13)	0.0019 (12)	−0.0103 (10)
C22	0.079 (2)	0.0310 (13)	0.0393 (14)	−0.0149 (13)	−0.0011 (13)	−0.0138 (11)
C23	0.0412 (14)	0.0330 (12)	0.0311 (11)	−0.0033 (10)	−0.0115 (10)	−0.0116 (9)
C24	0.086 (2)	0.0397 (14)	0.0294 (12)	−0.0248 (14)	−0.0041 (13)	−0.0078 (11)
C25	0.084 (2)	0.0333 (13)	0.0350 (13)	−0.0208 (13)	−0.0081 (13)	−0.0116 (11)
C26	0.0581 (17)	0.0444 (14)	0.0312 (12)	−0.0050 (12)	−0.0094 (11)	−0.0166 (11)
C27	0.078 (5)	0.181 (10)	0.091 (5)	−0.010 (5)	−0.023 (4)	−0.102 (7)
C28	0.221 (12)	0.065 (4)	0.027 (3)	−0.048 (6)	0.011 (5)	−0.017 (3)
C29	0.082 (5)	0.098 (5)	0.063 (4)	0.024 (4)	−0.012 (3)	−0.048 (4)
C27'	0.079 (6)	0.082 (6)	0.036 (4)	−0.001 (5)	−0.020 (4)	−0.027 (4)
C28'	0.056 (5)	0.114 (8)	0.057 (5)	0.015 (5)	−0.006 (4)	−0.044 (6)
C29'	0.205 (17)	0.079 (7)	0.052 (6)	−0.083 (10)	0.040 (8)	−0.047 (6)

Mn1—N1	2.180 (2)	C21—C22	1.378 (4)
Mn1—N1i	2.180 (2)	C21—H21	0.9500
Mn1—N21	2.3081 (18)	C22—C23	1.380 (3)
Mn1—N21i	2.3081 (18)	C22—H22	0.9500
Mn1—N11i	2.337 (2)	C23—C24	1.381 (4)
Mn1—N11	2.337 (2)	C23—C26	1.531 (3)
N1—C1	1.157 (3)	C24—C25	1.380 (4)
C1—S1	1.614 (3)	C24—H24	0.9500
N11—C11	1.343 (3)	C25—H25	0.9500
N11—C15	1.344 (3)	C26—C29'	1.419 (9)
C11—C12	1.368 (4)	C26—C28	1.467 (7)
C11—H11	0.9500	C26—C29	1.534 (7)
C12—C13	1.387 (4)	C26—C27	1.546 (8)
C12—H12	0.9500	C26—C28'	1.580 (10)
C13—C14	1.385 (4)	C26—C27'	1.583 (9)
C13—H13	0.9500	C27—H27A	0.9800
C14—C15	1.393 (4)	C27—H27B	0.9800
C14—C16	1.535 (3)	C27—H27C	0.9800
C15—H15	0.9500	C28—H28A	0.9800
C16—C17	1.524 (4)	C28—H28B	0.9800
C16—C18	1.530 (4)	C28—H28C	0.9800
C16—C19	1.537 (5)	C29—H29A	0.9800
C17—H17A	0.9800	C29—H29B	0.9800
C17—H17B	0.9800	C29—H29C	0.9800
C17—H17C	0.9800	C27'—H27D	0.9800
C18—H18A	0.9800	C27'—H27E	0.9800
C18—H18B	0.9800	C27'—H27F	0.9800
C18—H18C	0.9800	C28'—H28D	0.9800
C19—H19A	0.9800	C28'—H28E	0.9800
C19—H19B	0.9800	C28'—H28F	0.9800
C19—H19C	0.9800	C29'—H29D	0.9800
N21—C25	1.327 (3)	C29'—H29E	0.9800
N21—C21	1.333 (3)	C29'—H29F	0.9800
N1—Mn1—N1i	180.000 (1)	C23—C22—H22	119.8
N1—Mn1—N21	89.88 (8)	C22—C23—C24	115.3 (2)
N1i—Mn1—N21	90.12 (8)	C22—C23—C26	121.8 (2)
N1—Mn1—N21i	90.12 (8)	C24—C23—C26	122.9 (2)
N1i—Mn1—N21i	89.88 (8)	C25—C24—C23	120.9 (2)
N21—Mn1—N21i	180.000 (1)	C25—C24—H24	119.6
N1—Mn1—N11i	90.23 (8)	C23—C24—H24	119.6
N1i—Mn1—N11i	89.77 (8)	N21—C25—C24	123.6 (2)
N21—Mn1—N11i	86.16 (7)	N21—C25—H25	118.2
N21i—Mn1—N11i	93.84 (7)	C24—C25—H25	118.2
N1—Mn1—N11	89.77 (8)	C29'—C26—C28	128.7 (5)
N1i—Mn1—N11	90.23 (8)	C29'—C26—C23	116.5 (4)
N21—Mn1—N11	93.84 (7)	C28—C26—C23	114.0 (3)
N21i—Mn1—N11	86.16 (7)	C29'—C26—C29	61.8 (8)
N11i—Mn1—N11	180.00 (10)	C28—C26—C29	109.6 (6)
C1—N1—Mn1	157.6 (2)	C23—C26—C29	108.3 (3)
N1—C1—S1	177.4 (2)	C29'—C26—C27	44.1 (8)
C11—N11—C15	117.1 (2)	C28—C26—C27	111.9 (6)
C11—N11—Mn1	118.51 (16)	C23—C26—C27	106.9 (3)
C15—N11—Mn1	124.28 (17)	C29—C26—C27	105.7 (5)
N11—C11—C12	122.7 (2)	C29'—C26—C28'	111.6 (8)
N11—C11—H11	118.7	C28—C26—C28'	59.6 (6)
C12—C11—H11	118.7	C23—C26—C28'	107.0 (4)
C11—C12—C13	119.2 (3)	C29—C26—C28'	55.6 (5)
C11—C12—H12	120.4	C27—C26—C28'	145.3 (5)
C13—C12—H12	120.4	C29'—C26—C27'	111.2 (8)
C14—C13—C12	120.2 (3)	C28—C26—C27'	42.7 (5)
C14—C13—H13	119.9	C23—C26—C27'	107.4 (4)
C12—C13—H13	119.9	C29—C26—C27'	142.3 (4)
C13—C14—C15	116.1 (2)	C27—C26—C27'	74.8 (6)
C13—C14—C16	123.6 (2)	C28'—C26—C27'	102.1 (6)
C15—C14—C16	120.3 (2)	C26—C27—H27A	109.5
N11—C15—C14	124.7 (2)	C26—C27—H27B	109.5
N11—C15—H15	117.6	H27A—C27—H27B	109.5
C14—C15—H15	117.6	C26—C27—H27C	109.5
C17—C16—C18	111.4 (3)	H27A—C27—H27C	109.5
C17—C16—C14	109.0 (2)	H27B—C27—H27C	109.5
C18—C16—C14	111.0 (2)	C26—C28—H28A	109.5
C17—C16—C19	108.8 (3)	C26—C28—H28B	109.5
C18—C16—C19	107.7 (3)	H28A—C28—H28B	109.5
C14—C16—C19	108.8 (2)	C26—C28—H28C	109.5
C16—C17—H17A	109.5	H28A—C28—H28C	109.5
C16—C17—H17B	109.5	H28B—C28—H28C	109.5
H17A—C17—H17B	109.5	C26—C29—H29A	109.5
C16—C17—H17C	109.5	C26—C29—H29B	109.5
H17A—C17—H17C	109.5	H29A—C29—H29B	109.5
H17B—C17—H17C	109.5	C26—C29—H29C	109.5
C16—C18—H18A	109.5	H29A—C29—H29C	109.5
C16—C18—H18B	109.5	H29B—C29—H29C	109.5
H18A—C18—H18B	109.5	C26—C27'—H27D	109.5
C16—C18—H18C	109.5	C26—C27'—H27E	109.5
H18A—C18—H18C	109.5	H27D—C27'—H27E	109.5
H18B—C18—H18C	109.5	C26—C27'—H27F	109.5
C16—C19—H19A	109.5	H27D—C27'—H27F	109.5
C16—C19—H19B	109.5	H27E—C27'—H27F	109.5
H19A—C19—H19B	109.5	C26—C28'—H28D	109.5
C16—C19—H19C	109.5	C26—C28'—H28E	109.5
H19A—C19—H19C	109.5	H28D—C28'—H28E	109.5
H19B—C19—H19C	109.5	C26—C28'—H28F	109.5
C25—N21—C21	115.7 (2)	H28D—C28'—H28F	109.5
C25—N21—Mn1	123.21 (16)	H28E—C28'—H28F	109.5
C21—N21—Mn1	121.01 (15)	C26—C29'—H29D	109.5
N21—C21—C22	124.0 (2)	C26—C29'—H29E	109.5
N21—C21—H21	118.0	H29D—C29'—H29E	109.5
C22—C21—H21	118.0	C26—C29'—H29F	109.5
C21—C22—C23	120.5 (2)	H29D—C29'—H29F	109.5
C21—C22—H22	119.8	H29E—C29'—H29F	109.5