Bis­(3-tert-butyl­pyridine-κN)bis­(4-tert-butyl­pyridine-κN)bis(thio­cyanato-κN)cadmium

Reinert, T.; Jess, I.; Näther, C.

doi:10.1107/S1600536812040081

metal-organic compounds

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ISSN: 2056-9890

Volume 68| Part 11| November 2012| Page m1372

doi:10.1107/S1600536812040081

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Bis(3-tert-butylpyridine-κN)bis(4-tert-butylpyridine-κN)bis(thiocyanato-κN)cadmium

Thorben Reinert,^a ^* Inke Jess ^a and Christian Näther ^a

^aInstitut für Anorganische Chemie, Christian-Albrechts-Universität Kiel, Max-Eyth Strasse 2, D-24098 Kiel, Germany
^*Correspondence e-mail: treinert@ac.uni-kiel.de

(Received 10 September 2012; accepted 21 September 2012; online 20 October 2012)

The asymmetric unit of the title compound, [Cd(NCS)₂(C₉H₁₃N)₄], consists of one Cd^II cation located on a centre of inversion, one thiocyanate anion, one 3-tert-butylpyridine ligand and one 4-tert-butylpyridine ligand in general positions. The tert-butyl group of the 4-tert-butylpyridine 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-butylpyridine ligands and two N-bonded thiocyanate anions within a slightly distorted octahedral 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_r = 769.38
Triclinic, $[P \overline 1]$
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[F² > 2σ(F²)] = 0.051
wR(F²) = 0.127
S = 1.02
4709 reflections
226 parameters
3 restraints
H-atom parameters constrained
Δρ_max = 1.69 e Å⁻³
Δρ_min = −1.58 e Å⁻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) -x+1, -y+1, -z+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 (Sheldrick, 2008) and DIAMOND (Brandenburg, 2011 ); software used to prepare material for publication: publCIF (Westrip, 2010 ).

Supporting information

Crystal structure: contains datablocks I, global. DOI: 10.1107/S1600536812040081/bt6836sup1.cif

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

checkCIF report

Comment top

The structure determination of the title compound was performed as a part of a project on the synthesis and properties of new coordination polymers based on transition metal thiocyanates and and N-donor ligands (Boeckmann & Näther, 2010, 2011). Within this project we have reacted cadmium(II)thiocyanate with 4-tert-butylpyridine in water, which results in the formation of crystals of the title compound by accident. Apparently, the 4-tert-butylpyridine was contaminated with 3-tert-butylpyridine to a degree that allowed the formation of a few single crystals.

In the crystal structure the Cd atoms are coordinated by six N atoms of four tert-butylpyridine ligands and two N-bonded thiocyanato anions in mutual trans orientation in a slightly distorted octahedral geometry (Fig. 1 and Table 1). The Cd···N distances range from 2.3005 (36) Å to 2.4025 (28) Å. It is also worth mentioning that so far no other compound containing 3-tert-butylpyridine has been reported in the CSD.

Related literature top

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

Experimental top

The title compound was obtained accidently during the reaction of 34.3 mg Cd(NCS)₂ (0.15 mmol) with 88.8 µl 4-tert-butylpyridine (0.60 mmol) in 1.50 ml water at RT in a closed 3 ml snap cap vial. After two weeks colourless needles of the title compound were obtained.

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 (Sheldrick, 2008) and DIAMOND (Brandenburg, 2011); software used to prepare material for publication: publCIF (Westrip, 2010).

Figures top

Fig. 1. Crystal structure of the title compund with labelling and displacement ellipsoids drawn at the 50% probability level. Symmetry codes: i = -x + 1, -y + 1, -z + 2. Disordering is shown as full and open bonds.

Bis(3-tert-butylpyridine-κN)bis(4-tert-butylpyridine- κN)bis(thiocyanato-κN)cadmium top

Crystal data top

[Cd(NCS)₂(C₉H₁₃N)₄]	Z = 1
M_r = 769.38	F(000) = 402
Triclinic, P1	D_x = 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

Data collection top

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

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)] = 0.051	Hydrogen site location: inferred from neighbouring sites
wR(F²) = 0.127	H-atom parameters constrained
S = 1.02	w = 1/[σ²(F_o²) + (0.0811P)²] where P = (F_o² + 2F_c²)/3
4709 reflections	(Δ/σ)_max < 0.001
226 parameters	Δρ_max = 1.69 e Å⁻³
3 restraints	Δρ_min = −1.58 e Å⁻³

Crystal data top

[Cd(NCS)₂(C₉H₁₃N)₄]	γ = 76.472 (8)°
M_r = 769.38	V = 1016.32 (13) Å³
Triclinic, P1	Z = 1
a = 9.5136 (7) Å	Mo Kα radiation
b = 10.7582 (7) Å	µ = 0.67 mm⁻¹
c = 11.6674 (10) Å	T = 200 K
α = 67.142 (8)°	0.16 × 0.11 × 0.07 mm
β = 68.242 (9)°

Data collection top

Stoe IPDS-1 diffractometer	4109 reflections with I > 2σ(I)
11989 measured reflections	R_int = 0.077
4709 independent reflections

Refinement top

R[F² > 2σ(F²)] = 0.051	3 restraints
wR(F²) = 0.127	H-atom parameters constrained
S = 1.02	Δρ_max = 1.69 e Å⁻³
4709 reflections	Δρ_min = −1.58 e Å⁻³
226 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	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

Atomic displacement parameters (Å²) top

	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)

Geometric parameters (Å, º) top

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)

Symmetry code: (i) −x+1, −y+1, −z+2.

Experimental details

Crystal data
Chemical formula	[Cd(NCS)₂(C₉H₁₃N)₄]
M_r	769.38
Crystal system, space group	Triclinic, P1
Temperature (K)	200
a, b, c (Å)	9.5136 (7), 10.7582 (7), 11.6674 (10)
α, β, γ (°)	67.142 (8), 68.242 (9), 76.472 (8)
V (Å³)	1016.32 (13)
Z	1
Radiation type	Mo Kα
µ (mm⁻¹)	0.67
Crystal size (mm)	0.16 × 0.11 × 0.07

Data collection
Diffractometer	Stoe IPDS1 diffractometer
Absorption correction	–
No. of measured, independent and observed [I > 2σ(I)] reflections	11989, 4709, 4109
R_int	0.077
(sin θ/λ)_max (Å⁻¹)	0.661

Refinement
R[F² > 2σ(F²)], wR(F²), S	0.051, 0.127, 1.02
No. of reflections	4709
No. of parameters	226
No. of restraints	3
H-atom treatment	H-atom parameters constrained
Δρ_max, Δρ_min (e Å⁻³)	1.69, −1.58

Computer programs: X-AREA (Stoe & Cie, 2008), SHELXS97 (Sheldrick, 2008), SHELXL97 (Sheldrick, 2008), XP (Sheldrick, 2008) and DIAMOND (Brandenburg, 2011), publCIF (Westrip, 2010).

Selected geometric parameters (Å, º) top

Cd1—N1ⁱ	2.301 (3)	N1—C1	1.155 (5)
Cd1—N21ⁱ	2.375 (3)	C1—S1	1.618 (4)
Cd1—N11ⁱ	2.403 (3)

N1ⁱ—Cd1—N1	180.000 (1)	N1—Cd1—N11ⁱ	89.81 (11)
N1ⁱ—Cd1—N21	90.07 (11)	N21—Cd1—N11ⁱ	85.88 (10)
N1ⁱ—Cd1—N21ⁱ	89.93 (11)	N21ⁱ—Cd1—N11ⁱ	94.12 (10)
N21—Cd1—N21ⁱ	180.000 (1)	N11ⁱ—Cd1—N11	180.00 (13)
N1ⁱ—Cd1—N11ⁱ	90.19 (11)	C1—N1—Cd1	150.8 (3)

Symmetry code: (i) −x+1, −y+1, −z+2.

Acknowledgements

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

References

Boeckmann, J. & Näther, C. (2010). Dalton Trans. 39, 11019–11026. Web of Science CSD CrossRef CAS PubMed Google Scholar
Boeckmann, J. & Näther, C. (2011). Chem. Commun. 47, 7104–7106. Web of Science CSD CrossRef CAS Google Scholar
Brandenburg, K. (2011). DIAMOND. Crystal Impact GbR, Bonn, Germany. Google Scholar
Nassimbeni, L. R., Niven, M. L. & Taylor, M. W. (1990). Acta Cryst. B46, 354–361. CSD CrossRef CAS Web of Science IUCr Journals 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. 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 68| Part 11| November 2012| Page m1372

doi:10.1107/S1600536812040081

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metal-organic compounds\(\def\hfill{\hskip 5em}\def\hfil{\hskip 3em}\def\eqno#1{\hfil {#1}}\)

Bis­(3-tert-butyl­pyridine-κN)bis­­(4-tert-butyl­pyridine-κN)bis­(thio­cyanato-κN)cadmium

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Experimental

Crystal data

Data collection

Refinement

Supporting information

Acknowledgements

References

metal-organic compounds

Bis(3-tert-butylpyridine-κN)bis(4-tert-butylpyridine-κN)bis(thiocyanato-κN)cadmium