Crystal structure of catena-poly[[(3-tert-butyl-pyridine-κN)(4-tert-butyl-pyridine-κN)cadmium]-di-μ-thio-cyanato-κ(2) N:S;κ(2) S:N].

In the crystal structure of the title compound, [Cd(NCS)2(C9H13N)2] n , the Cd(II) cations are coordinated in a slightly distorted octa-hedral geometry by one 3-tert-butyl-pyridine ligand, one 4-tert-butyl-pyridine ligand and two pairs of translationally-equivalent μ-1,3-bridging thio-cyanate ligands, all of which are in general positions. These μ-1,3-bridging thio-cyante anions bridge the Cd(II) cations, forming chains that propagate parallel to the b axis.

Related literature

For related crystal structures with μ-1,3-bridging thio­cyanate anions, see: Banerjee et al. (2005 ▶); Reinert et al. (2012a ▶,b ▶); Tahli et al. (2011 ▶).

Experimental

Crystal data

[Cd(NCS)2(C9H13N)2]

M = 498.97

Monoclinic,

a = 20.0917 (8) Å

b = 5.9503 (2) Å

c = 21.0198 (9) Å

β = 115.902 (3)°

V = 2260.51 (15) Å3

Z = 4

Mo Kα radiation

μ = 1.16 mm−1

T = 293 K

0.16 × 0.12 × 0.09 mm

Data collection

STOE IPDS-2 diffractometer

Absorption correction: numerical (X-SHAPE and X-RED32; Stoe & Cie, 2008 ▶) T min = 0.760, T max = 0.895

25365 measured reflections

5407 independent reflections

4159 reflections with I > 2σ(I)

R int = 0.044

Refinement

R[F 2 > 2σ(F 2)] = 0.046

wR(F 2) = 0.084

S = 1.14

5407 reflections

244 parameters

H-atom parameters constrained

Δρmax = 0.41 e Å−3

Δρmin = −0.50 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, 2011 ▶); software used to prepare material for publication: publCIF (Westrip, 2010 ▶).

Crystal structure: contains datablock(s) I, global. DOI: 10.1107/S1600536814024647/pk2535sup1.cif

Structure factors: contains datablock(s) I. DOI: 10.1107/S1600536814024647/pk2535Isup2.hkl

Click here for additional data file.

. DOI: 10.1107/S1600536814024647/pk2535fig1.tif

Crystal structure of the title compound. Displacement ellipsoids are drawn at the 50% probability level. Symmetry code: i: (x, y+1, z); ii: (x, y-1, z).

CCDC reference: 1033510

Additional supporting information: crystallographic information; 3D view; checkCIF report

[Cd(NCS)2(C9H13N)2]	F(000) = 1016
Mr = 498.97	Dx = 1.466 Mg m−3
Monoclinic, P21/c	Mo Kα radiation, λ = 0.71073 Å
Hall symbol: -P 2ybc	Cell parameters from 25365 reflections
a = 20.0917 (8) Å	θ = 2.0–28.0°
b = 5.9503 (2) Å	µ = 1.16 mm−1
c = 21.0198 (9) Å	T = 293 K
β = 115.902 (3)°	Block, colourless
V = 2260.51 (15) Å3	0.16 × 0.12 × 0.09 mm
Z = 4

STOE IPDS-2 diffractometer	5407 independent reflections
Radiation source: fine-focus sealed tube	4159 reflections with I > 2σ(I)
Graphite monochromator	Rint = 0.044
ω scans	θmax = 28.0°, θmin = 2.0°
Absorption correction: numerical (X-SHAPE and X-RED32; Stoe & Cie, 2008)	h = −26→26
Tmin = 0.760, Tmax = 0.895	k = −7→7
25365 measured reflections	l = −27→27

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)] = 0.046	Hydrogen site location: inferred from neighbouring sites
wR(F2) = 0.084	H-atom parameters constrained
S = 1.14	w = 1/[σ2(Fo2) + (0.0326P)2 + 0.8678P] where P = (Fo2 + 2Fc2)/3
5407 reflections	(Δ/σ)max = 0.001
244 parameters	Δρmax = 0.41 e Å−3
0 restraints	Δρmin = −0.50 e Å−3

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.

	x	y	z	Uiso*/Ueq
Cd1	0.732991 (14)	0.24172 (4)	0.269228 (13)	0.04067 (8)
N1	0.67220 (19)	0.5638 (5)	0.20986 (17)	0.0535 (7)
C1	0.65872 (17)	0.7440 (6)	0.18809 (16)	0.0415 (6)
S1	0.63714 (5)	0.99805 (14)	0.15449 (5)	0.0484 (2)
N2	0.79392 (17)	−0.0756 (5)	0.32949 (17)	0.0514 (7)
C2	0.80555 (17)	−0.2557 (6)	0.35212 (16)	0.0421 (6)
S2	0.82427 (6)	−0.51157 (15)	0.38460 (5)	0.0554 (2)
N11	0.81232 (17)	0.2863 (5)	0.21360 (15)	0.0482 (7)
C11	0.8505 (3)	0.4716 (7)	0.2206 (2)	0.0724 (13)
H11	0.8473	0.5835	0.2501	0.087*
C12	0.8948 (3)	0.5105 (7)	0.1870 (2)	0.0713 (13)
H12	0.9209	0.6449	0.1950	0.086*
C13	0.9014 (2)	0.3547 (6)	0.14183 (19)	0.0443 (7)
C14	0.8606 (2)	0.1617 (7)	0.1342 (3)	0.0638 (11)
H14	0.8622	0.0474	0.1047	0.077*
C15	0.8174 (2)	0.1363 (7)	0.1698 (2)	0.0638 (11)
H15	0.7901	0.0047	0.1623	0.077*
C16	0.9479 (2)	0.3988 (7)	0.1019 (2)	0.0509 (8)
C17	0.9747 (3)	0.1778 (9)	0.0830 (3)	0.0847 (15)
H17A	1.0038	0.2105	0.0580	0.127*
H17B	0.9328	0.0882	0.0536	0.127*
H17C	1.0043	0.0967	0.1255	0.127*
C18	0.8990 (3)	0.5207 (10)	0.0334 (3)	0.0867 (16)
H18A	0.9269	0.5508	0.0072	0.130*
H18B	0.8821	0.6598	0.0444	0.130*
H18C	0.8571	0.4282	0.0056	0.130*
C19	1.0150 (3)	0.5424 (10)	0.1453 (3)	0.0862 (16)
H19A	1.0432	0.5674	0.1191	0.129*
H19B	1.0452	0.4664	0.1888	0.129*
H19C	0.9990	0.6840	0.1557	0.129*
N21	0.64660 (16)	0.2045 (5)	0.31532 (16)	0.0470 (7)
C21	0.5826 (2)	0.3142 (7)	0.2852 (2)	0.0546 (9)
H21	0.5733	0.4039	0.2459	0.066*
C22	0.5296 (2)	0.2999 (7)	0.3098 (2)	0.0629 (11)
H22	0.4855	0.3795	0.2879	0.076*
C23	0.5429 (2)	0.1660 (7)	0.3673 (2)	0.0573 (10)
H23	0.5075	0.1554	0.3846	0.069*
C24	0.60838 (19)	0.0467 (6)	0.39999 (18)	0.0454 (8)
C25	0.6582 (2)	0.0755 (6)	0.37141 (19)	0.0473 (8)
H25	0.7030	−0.0005	0.3928	0.057*
C26	0.6255 (2)	−0.0980 (7)	0.4648 (2)	0.0587 (10)
C27	0.6837 (4)	−0.2738 (12)	0.4745 (4)	0.133 (3)
H27A	0.6662	−0.3706	0.4339	0.200*
H27B	0.6933	−0.3611	0.5160	0.200*
H27C	0.7285	−0.2011	0.4797	0.200*
C28	0.6512 (6)	0.0518 (13)	0.5280 (3)	0.171 (4)
H28A	0.6627	−0.0373	0.5696	0.257*
H28B	0.6127	0.1569	0.5223	0.257*
H28C	0.6945	0.1319	0.5327	0.257*
C29	0.5577 (3)	−0.2282 (11)	0.4579 (4)	0.1055 (19)
H29A	0.5416	−0.3255	0.4175	0.158*
H29B	0.5188	−0.1249	0.4521	0.158*
H29C	0.5699	−0.3165	0.4997	0.158*

	U11	U22	U33	U12	U13	U23
Cd1	0.04773 (12)	0.03305 (11)	0.04745 (12)	0.00141 (12)	0.02654 (10)	0.00495 (11)
N1	0.064 (2)	0.0352 (15)	0.0566 (18)	0.0003 (14)	0.0216 (16)	0.0037 (14)
C1	0.0434 (15)	0.0405 (15)	0.0407 (15)	−0.0062 (17)	0.0185 (13)	−0.0032 (17)
S1	0.0550 (5)	0.0374 (4)	0.0470 (5)	0.0007 (4)	0.0167 (4)	0.0063 (4)
N2	0.0536 (18)	0.0355 (14)	0.0603 (19)	0.0036 (13)	0.0204 (15)	0.0053 (14)
C2	0.0422 (15)	0.0421 (16)	0.0425 (15)	−0.0014 (17)	0.0190 (13)	−0.0044 (17)
S2	0.0675 (6)	0.0385 (4)	0.0481 (5)	−0.0007 (4)	0.0141 (5)	0.0058 (4)
N11	0.0579 (17)	0.0447 (16)	0.0456 (15)	−0.0034 (14)	0.0260 (14)	−0.0023 (13)
C11	0.108 (4)	0.055 (2)	0.084 (3)	−0.028 (2)	0.070 (3)	−0.024 (2)
C12	0.097 (3)	0.057 (2)	0.086 (3)	−0.032 (2)	0.065 (3)	−0.021 (2)
C13	0.0418 (18)	0.0475 (18)	0.0463 (19)	0.0013 (15)	0.0218 (16)	0.0042 (15)
C14	0.069 (3)	0.055 (2)	0.090 (3)	−0.017 (2)	0.055 (3)	−0.023 (2)
C15	0.063 (2)	0.052 (2)	0.088 (3)	−0.017 (2)	0.044 (2)	−0.011 (2)
C16	0.048 (2)	0.059 (2)	0.053 (2)	0.0025 (17)	0.0279 (17)	0.0068 (17)
C17	0.087 (3)	0.081 (3)	0.115 (4)	0.013 (3)	0.071 (3)	0.004 (3)
C18	0.082 (3)	0.117 (4)	0.074 (3)	0.019 (3)	0.047 (3)	0.038 (3)
C19	0.064 (3)	0.111 (4)	0.097 (4)	−0.026 (3)	0.047 (3)	−0.013 (3)
N21	0.0460 (15)	0.0488 (17)	0.0530 (16)	0.0030 (13)	0.0278 (14)	0.0065 (13)
C21	0.052 (2)	0.060 (2)	0.054 (2)	0.0076 (17)	0.0246 (18)	0.0103 (17)
C22	0.046 (2)	0.074 (3)	0.071 (3)	0.0149 (19)	0.0288 (19)	0.013 (2)
C23	0.048 (2)	0.075 (2)	0.058 (2)	−0.0019 (19)	0.0309 (19)	−0.0028 (19)
C24	0.0450 (18)	0.055 (2)	0.0395 (17)	−0.0068 (16)	0.0220 (15)	−0.0049 (15)
C25	0.0436 (18)	0.054 (2)	0.0477 (19)	0.0038 (16)	0.0230 (16)	0.0046 (16)
C26	0.063 (2)	0.071 (3)	0.049 (2)	−0.007 (2)	0.0303 (19)	0.0052 (19)
C27	0.118 (5)	0.159 (7)	0.151 (6)	0.059 (5)	0.084 (5)	0.103 (5)
C28	0.323 (12)	0.124 (6)	0.047 (3)	−0.086 (7)	0.063 (5)	−0.013 (3)
C29	0.094 (4)	0.110 (5)	0.124 (5)	−0.012 (4)	0.058 (4)	0.038 (4)

Cd1—N2	2.305 (3)	C18—H18A	0.9600
Cd1—N1	2.322 (3)	C18—H18B	0.9600
Cd1—N21	2.339 (3)	C18—H18C	0.9600
Cd1—N11	2.368 (3)	C19—H19A	0.9600
Cd1—S2i	2.7412 (10)	C19—H19B	0.9600
Cd1—S1ii	2.7513 (10)	C19—H19C	0.9600
N1—C1	1.151 (4)	N21—C21	1.330 (5)
C1—S1	1.644 (4)	N21—C25	1.339 (4)
S1—Cd1i	2.7513 (10)	C21—C22	1.375 (5)
N2—C2	1.154 (4)	C21—H21	0.9300
C2—S2	1.644 (4)	C22—C23	1.374 (6)
S2—Cd1ii	2.7412 (10)	C22—H22	0.9300
N11—C11	1.314 (5)	C23—C24	1.385 (5)
N11—C15	1.319 (5)	C23—H23	0.9300
C11—C12	1.378 (5)	C24—C25	1.384 (4)
C11—H11	0.9300	C24—C26	1.518 (5)
C12—C13	1.373 (5)	C25—H25	0.9300
C12—H12	0.9300	C26—C28	1.492 (7)
C13—C14	1.379 (5)	C26—C27	1.514 (7)
C13—C16	1.527 (5)	C26—C29	1.518 (6)
C14—C15	1.379 (5)	C27—H27A	0.9600
C14—H14	0.9300	C27—H27B	0.9600
C15—H15	0.9300	C27—H27C	0.9600
C16—C19	1.519 (6)	C28—H28A	0.9600
C16—C18	1.525 (6)	C28—H28B	0.9600
C16—C17	1.537 (6)	C28—H28C	0.9600
C17—H17A	0.9600	C29—H29A	0.9600
C17—H17B	0.9600	C29—H29B	0.9600
C17—H17C	0.9600	C29—H29C	0.9600
N2—Cd1—N1	179.28 (11)	H18A—C18—H18B	109.5
N2—Cd1—N21	90.40 (11)	C16—C18—H18C	109.5
N1—Cd1—N21	89.39 (11)	H18A—C18—H18C	109.5
N2—Cd1—N11	93.03 (11)	H18B—C18—H18C	109.5
N1—Cd1—N11	87.23 (11)	C16—C19—H19A	109.5
N21—Cd1—N11	175.34 (11)	C16—C19—H19B	109.5
N2—Cd1—S2i	87.88 (8)	H19A—C19—H19B	109.5
N1—Cd1—S2i	91.43 (8)	C16—C19—H19C	109.5
N21—Cd1—S2i	90.86 (8)	H19A—C19—H19C	109.5
N11—Cd1—S2i	92.42 (8)	H19B—C19—H19C	109.5
N2—Cd1—S1ii	92.89 (8)	C21—N21—C25	117.4 (3)
N1—Cd1—S1ii	87.79 (8)	C21—N21—Cd1	119.6 (2)
N21—Cd1—S1ii	87.21 (8)	C25—N21—Cd1	123.0 (2)
N11—Cd1—S1ii	89.46 (8)	N21—C21—C22	122.5 (4)
S2i—Cd1—S1ii	177.92 (3)	N21—C21—H21	118.8
C1—N1—Cd1	163.7 (3)	C22—C21—H21	118.8
N1—C1—S1	178.0 (3)	C23—C22—C21	118.8 (4)
C1—S1—Cd1i	98.96 (11)	C23—C22—H22	120.6
C2—N2—Cd1	161.9 (3)	C21—C22—H22	120.6
N2—C2—S2	178.6 (3)	C22—C23—C24	120.7 (3)
C2—S2—Cd1ii	100.68 (11)	C22—C23—H23	119.6
C11—N11—C15	115.2 (3)	C24—C23—H23	119.6
C11—N11—Cd1	121.6 (2)	C25—C24—C23	115.6 (3)
C15—N11—Cd1	122.9 (2)	C25—C24—C26	122.4 (3)
N11—C11—C12	124.1 (4)	C23—C24—C26	122.0 (3)
N11—C11—H11	118.0	N21—C25—C24	124.9 (3)
C12—C11—H11	118.0	N21—C25—H25	117.5
C13—C12—C11	121.3 (4)	C24—C25—H25	117.5
C13—C12—H12	119.3	C28—C26—C27	110.3 (6)
C11—C12—H12	119.3	C28—C26—C24	108.3 (4)
C12—C13—C14	114.3 (3)	C27—C26—C24	111.8 (3)
C12—C13—C16	122.0 (3)	C28—C26—C29	109.6 (5)
C14—C13—C16	123.6 (3)	C27—C26—C29	105.6 (5)
C13—C14—C15	120.7 (4)	C24—C26—C29	111.2 (4)
C13—C14—H14	119.6	C26—C27—H27A	109.5
C15—C14—H14	119.6	C26—C27—H27B	109.5
N11—C15—C14	124.3 (4)	H27A—C27—H27B	109.5
N11—C15—H15	117.8	C26—C27—H27C	109.5
C14—C15—H15	117.8	H27A—C27—H27C	109.5
C19—C16—C18	109.7 (4)	H27B—C27—H27C	109.5
C19—C16—C13	111.2 (3)	C26—C28—H28A	109.5
C18—C16—C13	107.7 (3)	C26—C28—H28B	109.5
C19—C16—C17	108.5 (4)	H28A—C28—H28B	109.5
C18—C16—C17	108.5 (4)	C26—C28—H28C	109.5
C13—C16—C17	111.3 (3)	H28A—C28—H28C	109.5
C16—C17—H17A	109.5	H28B—C28—H28C	109.5
C16—C17—H17B	109.5	C26—C29—H29A	109.5
H17A—C17—H17B	109.5	C26—C29—H29B	109.5
C16—C17—H17C	109.5	H29A—C29—H29B	109.5
H17A—C17—H17C	109.5	C26—C29—H29C	109.5
H17B—C17—H17C	109.5	H29A—C29—H29C	109.5
C16—C18—H18A	109.5	H29B—C29—H29C	109.5
C16—C18—H18B	109.5