Bis-(3-tert-butyl-pyridine-κN)bis-(4-tert-butyl-pyridine-κN)bis(thio-cyanato-κN)cadmium.

The asymmetric unit of the title compound, [Cd(NCS)(2)(C(9)H(13)N)(4)], consists of one Cd(II) cation located on a centre of inversion, one thio-cyanate 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 0.25:0.75 ratio and was refined using a split model. The Cd(II) cation is coordinated by six N atoms of four tert-butyl-pyridine ligands and two N-bonded thio-cyanate anions within a slightly distorted octa-hedral coordination environment.

Related literature

For the synthesis and properties of coordination polymers based on transition metal thio­cyanates and N-donor ligands, see: Boeckmann & Näther (2010 ▶, 2011 ▶). For related structures, see: Nassimbeni et al. (1990 ▶) (4-tert-butyl­pyridine only).

Experimental

Crystal data

[Cd(NCS)2(C9H13N)4]

M = 769.38

Triclinic,

a = 9.5136 (7) Å

b = 10.7582 (7) Å

c = 11.6674 (10) Å

α = 67.142 (8)°

β = 68.242 (9)°

γ = 76.472 (8)°

V = 1016.32 (13) Å3

Z = 1

Mo Kα radiation

μ = 0.67 mm−1

T = 200 K

0.16 × 0.11 × 0.07 mm

Data collection

Stoe IPDS-1 diffractometer

11989 measured reflections

4709 independent reflections

4109 reflections with I > 2σ(I)

R int = 0.077

Refinement

R[F 2 > 2σ(F 2)] = 0.051

wR(F 2) = 0.127

S = 1.02

4709 reflections

226 parameters

3 restraints

H-atom parameters constrained

Δρmax = 1.69 e Å−3

Δρmin = −1.58 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 (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/S1600536812040081/bt6836sup1.cif

Click here for additional data file.

Structure factors: contains datablock(s) I. DOI: 10.1107/S1600536812040081/bt6836Isup2.hkl

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

[Cd(NCS)2(C9H13N)4]	Z = 1
Mr = 769.38	F(000) = 402
Triclinic, P1	Dx = 1.257 Mg m−3
Hall symbol: -P 1	Mo Kα radiation, λ = 0.71073 Å
a = 9.5136 (7) Å	Cell parameters from 8000 reflections
b = 10.7582 (7) Å	θ = 1.9–28.2°
c = 11.6674 (10) Å	µ = 0.67 mm−1
α = 67.142 (8)°	T = 200 K
β = 68.242 (9)°	Needle, colourless
γ = 76.472 (8)°	0.16 × 0.11 × 0.07 mm
V = 1016.32 (13) Å3

Stoe IPDS-1 diffractometer	4109 reflections with I > 2σ(I)
Radiation source: fine-focus sealed tube	Rint = 0.077
Graphite monochromator	θmax = 28.0°, θmin = 2.3°
φ scans	h = −12→12
11989 measured reflections	k = −13→13
4709 independent reflections	l = −15→15

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)] = 0.051	Hydrogen site location: inferred from neighbouring sites
wR(F2) = 0.127	H-atom parameters constrained
S = 1.02	w = 1/[σ2(Fo2) + (0.0811P)2] where P = (Fo2 + 2Fc2)/3
4709 reflections	(Δ/σ)max < 0.001
226 parameters	Δρmax = 1.69 e Å−3
3 restraints	Δρmin = −1.58 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)
Cd1	0.5000	0.5000	1.0000	0.02671 (12)
N1	0.6536 (4)	0.6715 (3)	0.9156 (3)	0.0392 (7)
C1	0.6855 (4)	0.7786 (4)	0.8456 (4)	0.0362 (7)
S1	0.73133 (15)	0.92652 (13)	0.74250 (19)	0.0869 (6)
N11	0.2957 (3)	0.6619 (3)	0.9404 (3)	0.0302 (6)
C11	0.1577 (4)	0.6192 (4)	0.9843 (4)	0.0371 (7)
H11	0.1461	0.5265	1.0353	0.044*
C12	0.0319 (4)	0.7042 (4)	0.9587 (4)	0.0419 (8)
H12	−0.0639	0.6702	0.9903	0.050*
C13	0.0472 (4)	0.8402 (4)	0.8861 (4)	0.0384 (8)
H13	−0.0383	0.8999	0.8669	0.046*
C14	0.1875 (4)	0.8890 (3)	0.8415 (3)	0.0316 (7)
C15	0.3087 (4)	0.7938 (3)	0.8709 (3)	0.0322 (7)
H15	0.4063	0.8246	0.8396	0.039*
C16	0.2138 (4)	1.0380 (4)	0.7633 (4)	0.0449 (9)
C17	0.3189 (7)	1.0495 (6)	0.6244 (5)	0.0775 (18)
H17A	0.3363	1.1446	0.5740	0.116*
H17B	0.2713	1.0161	0.5819	0.116*
H17C	0.4163	0.9951	0.6284	0.116*
C18	0.0626 (6)	1.1273 (5)	0.7600 (6)	0.0638 (13)
H18A	0.0827	1.2220	0.7100	0.096*
H18B	−0.0022	1.1199	0.8496	0.096*
H18C	0.0110	1.0971	0.7182	0.096*
C19	0.2904 (5)	1.0892 (5)	0.8294 (6)	0.0611 (13)
H19A	0.3070	1.1847	0.7799	0.092*
H19B	0.3884	1.0351	0.8315	0.092*
H19C	0.2247	1.0805	0.9191	0.092*
N21	0.6000 (3)	0.4588 (3)	0.7974 (3)	0.0328 (6)
C21	0.5908 (5)	0.3401 (4)	0.7924 (4)	0.0477 (10)
H21	0.5393	0.2745	0.8708	0.057*
C22	0.6522 (5)	0.3064 (4)	0.6792 (4)	0.0490 (10)
H22	0.6432	0.2190	0.6820	0.059*
C23	0.7265 (4)	0.3989 (4)	0.5619 (3)	0.0322 (7)
C24	0.7375 (6)	0.5215 (4)	0.5688 (4)	0.0505 (11)
H24	0.7888	0.5889	0.4921	0.061*
C25	0.6746 (5)	0.5472 (4)	0.6861 (4)	0.0479 (10)
H25	0.6853	0.6324	0.6871	0.058*
C26	0.7921 (4)	0.3663 (4)	0.4347 (3)	0.0400 (8)
C27	0.6690 (9)	0.3075 (11)	0.4201 (8)	0.090 (3)	0.75
H27A	0.6344	0.2289	0.4980	0.134*	0.75
H27B	0.7117	0.2793	0.3424	0.134*	0.75
H27C	0.5827	0.3769	0.4105	0.134*	0.75
C28	0.8482 (16)	0.4831 (8)	0.3182 (6)	0.116 (5)	0.75
H28A	0.8887	0.4552	0.2404	0.174*	0.75
H28B	0.9289	0.5167	0.3281	0.174*	0.75
H28C	0.7643	0.5552	0.3086	0.174*	0.75
C29	0.9220 (9)	0.2496 (9)	0.4499 (7)	0.079 (2)	0.75
H29A	0.8831	0.1726	0.5280	0.119*	0.75
H29B	1.0048	0.2811	0.4588	0.119*	0.75
H29C	0.9601	0.2213	0.3724	0.119*	0.75
C27'	0.7280 (17)	0.4863 (16)	0.3290 (16)	0.040 (3)*	0.25
H27D	0.7455	0.5733	0.3275	0.060*	0.25
H27E	0.6186	0.4830	0.3518	0.060*	0.25
H27F	0.7803	0.4769	0.2425	0.060*	0.25
C28'	0.9670 (16)	0.3788 (17)	0.3825 (16)	0.043 (3)*	0.25
H28D	0.9843	0.4665	0.3793	0.065*	0.25
H28E	1.0094	0.3722	0.2944	0.065*	0.25
H28F	1.0168	0.3054	0.4411	0.065*	0.25
C29'	0.768 (2)	0.238 (2)	0.438 (2)	0.063 (5)*	0.25
H29D	0.8160	0.2303	0.3511	0.094*	0.25
H29E	0.6590	0.2316	0.4666	0.094*	0.25
H29F	0.8140	0.1651	0.5004	0.094*	0.25

	U11	U22	U33	U12	U13	U23
Cd1	0.03329 (19)	0.02083 (18)	0.02336 (16)	−0.00619 (11)	−0.00577 (12)	−0.00565 (12)
N1	0.0426 (16)	0.0288 (16)	0.0430 (16)	−0.0125 (12)	−0.0074 (13)	−0.0095 (13)
C1	0.0312 (16)	0.0308 (19)	0.0447 (19)	−0.0041 (13)	−0.0115 (14)	−0.0107 (15)
S1	0.0540 (7)	0.0380 (7)	0.1310 (14)	−0.0182 (5)	−0.0373 (8)	0.0262 (7)
N11	0.0350 (14)	0.0263 (14)	0.0261 (12)	−0.0048 (11)	−0.0076 (10)	−0.0063 (11)
C11	0.0397 (18)	0.0288 (18)	0.0397 (18)	−0.0084 (13)	−0.0076 (14)	−0.0101 (14)
C12	0.0362 (18)	0.037 (2)	0.050 (2)	−0.0093 (14)	−0.0095 (15)	−0.0123 (17)
C13	0.0319 (17)	0.038 (2)	0.0422 (18)	−0.0007 (14)	−0.0098 (14)	−0.0136 (15)
C14	0.0352 (17)	0.0252 (17)	0.0291 (15)	−0.0020 (12)	−0.0071 (12)	−0.0072 (12)
C15	0.0339 (16)	0.0314 (18)	0.0279 (15)	−0.0043 (13)	−0.0069 (12)	−0.0086 (13)
C16	0.042 (2)	0.029 (2)	0.047 (2)	−0.0015 (14)	−0.0076 (16)	−0.0028 (15)
C17	0.099 (4)	0.049 (3)	0.044 (2)	−0.014 (3)	0.007 (3)	0.001 (2)
C18	0.062 (3)	0.033 (2)	0.082 (3)	0.0014 (19)	−0.032 (3)	0.001 (2)
C19	0.049 (2)	0.034 (2)	0.099 (4)	−0.0025 (17)	−0.020 (2)	−0.024 (2)
N21	0.0418 (16)	0.0299 (15)	0.0253 (12)	−0.0062 (11)	−0.0089 (11)	−0.0079 (11)
C21	0.069 (3)	0.033 (2)	0.0310 (17)	−0.0172 (17)	0.0013 (17)	−0.0092 (15)
C22	0.075 (3)	0.030 (2)	0.0347 (18)	−0.0162 (18)	0.0013 (18)	−0.0146 (15)
C23	0.0373 (17)	0.0295 (17)	0.0272 (14)	−0.0020 (13)	−0.0093 (13)	−0.0086 (13)
C24	0.080 (3)	0.039 (2)	0.0277 (17)	−0.028 (2)	−0.0004 (17)	−0.0092 (15)
C25	0.076 (3)	0.034 (2)	0.0332 (17)	−0.0239 (18)	−0.0063 (18)	−0.0113 (15)
C26	0.050 (2)	0.039 (2)	0.0310 (16)	−0.0035 (15)	−0.0087 (15)	−0.0165 (15)
C27	0.078 (5)	0.153 (9)	0.075 (5)	−0.032 (5)	−0.017 (4)	−0.073 (6)
C28	0.243 (14)	0.057 (5)	0.027 (3)	−0.056 (6)	0.006 (5)	−0.015 (3)
C29	0.073 (5)	0.098 (6)	0.062 (4)	0.023 (4)	−0.013 (4)	−0.048 (4)

Cd1—N1i	2.301 (3)	C21—C22	1.385 (5)
Cd1—N1	2.301 (3)	C21—H21	0.9500
Cd1—N21	2.375 (3)	C22—C23	1.385 (5)
Cd1—N21i	2.375 (3)	C22—H22	0.9500
Cd1—N11i	2.403 (3)	C23—C24	1.382 (5)
Cd1—N11	2.403 (3)	C23—C26	1.527 (4)
N1—C1	1.155 (5)	C24—C25	1.385 (5)
C1—S1	1.618 (4)	C24—H24	0.9500
N11—C11	1.341 (5)	C25—H25	0.9500
N11—C15	1.342 (4)	C26—C29'	1.43 (2)
C11—C12	1.378 (6)	C26—C28	1.469 (8)
C11—H11	0.9500	C26—C27	1.542 (8)
C12—C13	1.388 (6)	C26—C29	1.548 (8)
C12—H12	0.9500	C26—C28'	1.564 (15)
C13—C14	1.389 (5)	C26—C27'	1.585 (16)
C13—H13	0.9500	C27—H27A	0.9800
C14—C15	1.402 (5)	C27—H27B	0.9800
C14—C16	1.532 (5)	C27—H27C	0.9800
C15—H15	0.9500	C28—H28A	0.9800
C16—C17	1.529 (6)	C28—H28B	0.9800
C16—C18	1.536 (6)	C28—H28C	0.9800
C16—C19	1.539 (7)	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—C21	1.325 (5)	C29'—H29E	0.9800
N21—C25	1.330 (5)	C29'—H29F	0.9800
N1i—Cd1—N1	180.000 (1)	N21—C21—H21	118.2
N1i—Cd1—N21	90.07 (11)	C22—C21—H21	118.2
N1—Cd1—N21	89.93 (11)	C23—C22—C21	120.5 (4)
N1i—Cd1—N21i	89.93 (11)	C23—C22—H22	119.7
N1—Cd1—N21i	90.07 (11)	C21—C22—H22	119.7
N21—Cd1—N21i	180.000 (1)	C24—C23—C22	115.3 (3)
N1i—Cd1—N11i	90.19 (11)	C24—C23—C26	122.8 (3)
N1—Cd1—N11i	89.81 (11)	C22—C23—C26	121.9 (3)
N21—Cd1—N11i	85.88 (10)	C23—C24—C25	120.8 (3)
N21i—Cd1—N11i	94.12 (10)	C23—C24—H24	119.6
N1i—Cd1—N11	89.81 (11)	C25—C24—H24	119.6
N1—Cd1—N11	90.19 (11)	N21—C25—C24	123.3 (3)
N21—Cd1—N11	94.12 (10)	N21—C25—H25	118.3
N21i—Cd1—N11	85.88 (10)	C24—C25—H25	118.3
N11i—Cd1—N11	180.00 (13)	C29'—C26—C23	117.8 (9)
C1—N1—Cd1	150.8 (3)	C28—C26—C23	113.7 (4)
N1—C1—S1	177.6 (4)	C28—C26—C27	110.8 (7)
C11—N11—C15	117.6 (3)	C23—C26—C27	108.3 (4)
C11—N11—Cd1	117.9 (2)	C28—C26—C29	110.3 (7)
C15—N11—Cd1	124.3 (2)	C23—C26—C29	107.9 (4)
N11—C11—C12	122.7 (3)	C27—C26—C29	105.5 (6)
N11—C11—H11	118.6	C29'—C26—C28'	108.9 (10)
C12—C11—H11	118.6	C23—C26—C28'	107.7 (6)
C11—C12—C13	119.0 (3)	C29'—C26—C27'	110.5 (11)
C11—C12—H12	120.5	C23—C26—C27'	107.0 (6)
C13—C12—H12	120.5	C28'—C26—C27'	104.0 (8)
C12—C13—C14	119.9 (3)	C26—C27—H27A	109.5
C12—C13—H13	120.0	C26—C27—H27B	109.5
C14—C13—H13	120.0	H27A—C27—H27B	109.5
C13—C14—C15	116.5 (3)	C26—C27—H27C	109.5
C13—C14—C16	123.4 (3)	H27A—C27—H27C	109.5
C15—C14—C16	120.0 (3)	H27B—C27—H27C	109.5
N11—C15—C14	124.1 (3)	C26—C28—H28A	109.5
N11—C15—H15	118.0	C26—C28—H28B	109.5
C14—C15—H15	118.0	H28A—C28—H28B	109.5
C17—C16—C14	109.1 (3)	C26—C28—H28C	109.5
C17—C16—C18	110.7 (4)	H28A—C28—H28C	109.5
C14—C16—C18	111.2 (3)	H28B—C28—H28C	109.5
C17—C16—C19	109.0 (4)	C26—C29—H29A	109.5
C14—C16—C19	109.3 (4)	C26—C29—H29B	109.5
C18—C16—C19	107.5 (4)	H29A—C29—H29B	109.5
C16—C17—H17A	109.5	C26—C29—H29C	109.5
C16—C17—H17B	109.5	H29A—C29—H29C	109.5
H17A—C17—H17B	109.5	H29B—C29—H29C	109.5
C16—C17—H17C	109.5	C26—C27'—H27D	109.5
H17A—C17—H17C	109.5	C26—C27'—H27E	109.5
H17B—C17—H17C	109.5	H27D—C27'—H27E	109.5
C16—C18—H18A	109.5	C26—C27'—H27F	109.5
C16—C18—H18B	109.5	H27D—C27'—H27F	109.5
H18A—C18—H18B	109.5	H27E—C27'—H27F	109.5
C16—C18—H18C	109.5	C26—C28'—H28D	109.5
H18A—C18—H18C	109.5	C26—C28'—H28E	109.5
H18B—C18—H18C	109.5	H28D—C28'—H28E	109.5
C16—C19—H19A	109.5	C26—C28'—H28F	109.5
C16—C19—H19B	109.5	H28D—C28'—H28F	109.5
H19A—C19—H19B	109.5	H28E—C28'—H28F	109.5
C16—C19—H19C	109.5	C26—C29'—H29D	109.5
H19A—C19—H19C	109.5	C26—C29'—H29E	109.5
H19B—C19—H19C	109.5	H29D—C29'—H29E	109.5
C21—N21—C25	116.4 (3)	C26—C29'—H29F	109.5
C21—N21—Cd1	120.2 (2)	H29D—C29'—H29F	109.5
C25—N21—Cd1	123.3 (2)	H29E—C29'—H29F	109.5
N21—C21—C22	123.6 (3)

Table 1

Selected bond lengths (Å)

Cd1—N1i	2.301 (3)
Cd1—N21i	2.375 (3)
Cd1—N11i	2.403 (3)

Symmetry code: (i) .