catena-Poly[benzyl­triethyl­ammonium [tri-μ-thio­cyanato-κ⁴N:S;κ²S:N-cadmate(II)]]

The title compound, {[(C₆H₅CH₂)N(C₂H₅)₃][Cd(SCN)₃]}_n, contains benzyl­triethyl­ammonium cations lying between one-dimensional chains of stoichiometry {[Cd(SCN)₃]⁻}_n. Each Cd²⁺ ion is 3N,3S-hexa­coordinated by thio­cyanate ligands in an octa­hedral arrangement. The asymmetric unit contains one cation and one anion.

Key indicators

• Single-crystal X-ray study
• T = 173 K
• Mean [sigma](C-C) = 0.004 Å
• R factor = 0.029
• wR factor = 0.052
• Data-to-parameter ratio = 21.1

checkCIF/PLATON results

No syntax errors found



Alert level C
PLAT042_ALERT_1_C Calc. and Rep. MoietyFormula Strings Differ ....          ?
PLAT062_ALERT_4_C Rescale T(min) & T(max) by .....................       0.99
PLAT125_ALERT_4_C No _symmetry_space_group_name_Hall Given .......          ?
PLAT764_ALERT_4_C Overcomplete CIF Bond List Detected (Rep/Expd) .       1.12 Ratio

   0 ALERT level A = In general: serious problem
   0 ALERT level B = Potentially serious problem
   4 ALERT level C = Check and explain
   0 ALERT level G = General alerts; check

   1 ALERT type 1 CIF construction/syntax error, inconsistent or missing data
   0 ALERT type 2 Indicator that the structure model may be wrong or deficient
   0 ALERT type 3 Indicator that the structure quality may be low
   3 ALERT type 4 Improvement, methodology, query or suggestion
   0 ALERT type 5 Informative message, check

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Computing details

Data collection: COLLECT (Hooft, 1998); cell refinement: EVALCCD (Duisenberg et al., 2003); data reduction: EVALCCD; program(s) used to solve structure: SHELXS97 (Sheldrick, 1997); program(s) used to refine structure: SHELXL97 (Sheldrick, 1997); molecular graphics: ORTEPIII (Burnett & Johnson, 1996); software used to prepare material for publication: SHELXTL (Sheldrick, 2001), Mercury (Version 1.4.1; Bruno et al., 2002) and CIFTAB (Sheldrick, 1993).

catena-Poly[benzyltriethylammonium [cadmium(II)-tri-µ-thiocyanato-κ⁴N:S;κ²S:N]]

Crystal data

(C13H22N)[Cd(NCS)3]	F(000) = 968
Mr = 478.96	Dx = 1.551 Mg m^−3
Monoclinic, P21/n	Mo Kα radiation, λ = 0.71073 Å
a = 12.164 (2) Å	Cell parameters from 4011 reflections
b = 10.927 (2) Å	θ = 2.5–27.5°
c = 15.952 (3) Å	µ = 1.38 mm^−1
β = 104.61 (3)°	T = 173 K
V = 2051.8 (7) Å^3	Block, colourless
Z = 4	0.60 × 0.40 × 0.20 mm

Data collection

Nonius KappaCCD diffractometer	4579 independent reflections
Radiation source: fine-focus sealed tube	3895 reflections with I > 2σ(I)
Graphite monochromator	Rint = 0.031
φ and ω scans	θmax = 27.4°, θmin = 5.1°
Absorption correction: multi-scan (SADABS; Sheldrick 2003)	h = −15→15
Tmin = 0.493, Tmax = 0.771	k = −14→14
18486 measured reflections	l = −20→20

Refinement

Refinement on F^2	Primary atom site location: structure-invariant direct methods
Least-squares matrix: full	Secondary atom site location: difference Fourier map
R[F^2 > 2σ(F^2)] = 0.029	Hydrogen site location: inferred from neighbouring sites
wR(F^2) = 0.052	H-atom parameters constrained
S = 1.25	w = 1/[σ^2(Fo^2) + 1.5462P] where P = (Fo^2 + 2Fc^2)/3
4579 reflections	(Δ/σ)max = 0.001
217 parameters	Δρmax = 0.51 e Å^−3
0 restraints	Δρmin = −0.39 e Å^−3

Special details

Experimental. IR (KBr, ν, cm^-1): ν 2116 (s), 2079 (s) (SCN), ν 1650 (m) (–CC–), \n 1555 (m) (–CC–), β 1082 (s), 1025 (s), 1003 (s), (–CH). ¹H NMR (d₆-DMSO): δ 7.5 (s, 5H, HAr), 4.4 (s, 2H, –ArCH₂–), 2.0 (q, 6H, –CH₂–), 1.29 (t, 9H, –CH₃); ¹³C NMR: δ 129–132 (Ar), 127 (SCN), 59 (ArC–), 30 (–CH₂–), 7.5 (–CH₃).

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 (Ų)

	x	y	z	Uiso*/Ueq
Cd1	0.719434 (14)	0.110145 (15)	0.760010 (12)	0.02115 (6)
S1	0.56210 (5)	−0.03304 (5)	0.81169 (4)	0.02454 (14)
C1	0.61965 (19)	−0.1662 (2)	0.79485 (15)	0.0195 (5)
N1	0.84164 (18)	0.23996 (19)	0.71578 (15)	0.0283 (5)
S2	0.53107 (5)	0.24202 (6)	0.67128 (5)	0.03118 (16)
C2	0.5913 (2)	0.3796 (2)	0.67330 (16)	0.0242 (5)
N2	0.86776 (18)	−0.0239 (2)	0.82674 (15)	0.0322 (5)
S3	0.73244 (6)	0.23997 (6)	0.90825 (4)	0.03296 (16)
C3	0.76309 (19)	0.3789 (2)	0.87831 (15)	0.0216 (5)
N3	0.71381 (18)	−0.02321 (19)	0.64172 (14)	0.0286 (5)
C4	0.2888 (2)	0.4406 (2)	0.84738 (15)	0.0240 (5)
C5	0.2360 (2)	0.5484 (2)	0.86420 (17)	0.0285 (6)
H5A	0.1592	0.5460	0.8677	0.034*
C6	0.2947 (2)	0.6596 (3)	0.87587 (17)	0.0333 (6)
H6A	0.2583	0.7321	0.8877	0.040*
C7	0.4069 (2)	0.6634 (3)	0.87000 (18)	0.0364 (7)
H7A	0.4471	0.7388	0.8783	0.044*
C8	0.4601 (2)	0.5580 (3)	0.8521 (2)	0.0401 (7)
H8A	0.5365	0.5614	0.8477	0.048*
C9	0.4019 (2)	0.4472 (3)	0.84055 (18)	0.0334 (6)
H9A	0.4387	0.3754	0.8279	0.040*
C10	0.2242 (2)	0.3200 (2)	0.83268 (15)	0.0261 (5)
H10A	0.2557	0.2694	0.7928	0.031*
H10B	0.1439	0.3375	0.8034	0.031*
N10	0.22745 (16)	0.24387 (18)	0.91522 (12)	0.0215 (4)
C11	0.1644 (2)	0.1246 (2)	0.88378 (18)	0.0350 (6)
H11A	0.0859	0.1446	0.8511	0.042*
H11B	0.2024	0.0836	0.8434	0.042*
C12	0.1591 (3)	0.0354 (3)	0.9565 (2)	0.0520 (9)
H12A	0.1177	−0.0384	0.9317	0.078*
H12B	0.1197	0.0743	0.9961	0.078*
H12C	0.2363	0.0132	0.9884	0.078*
C13	0.3500 (2)	0.2202 (2)	0.96562 (16)	0.0266 (6)
H13A	0.3492	0.1832	1.0221	0.032*
H13B	0.3897	0.2998	0.9775	0.032*
C14	0.4185 (3)	0.1368 (3)	0.9206 (2)	0.0437 (8)
H14A	0.4955	0.1270	0.9576	0.066*
H14B	0.4221	0.1734	0.8653	0.066*
H14C	0.3815	0.0566	0.9100	0.066*
C15	0.1721 (2)	0.3137 (3)	0.97717 (16)	0.0288 (6)
H15A	0.1827	0.2656	1.0312	0.035*
H15B	0.2127	0.3923	0.9923	0.035*
C16	0.0455 (2)	0.3407 (3)	0.9424 (2)	0.0455 (8)
H16A	0.0178	0.3853	0.9863	0.068*
H16B	0.0037	0.2635	0.9289	0.068*
H16C	0.0338	0.3905	0.8898	0.068*

Atomic displacement parameters (Ų)

	U^11	U^22	U^33	U^12	U^13	U^23
Cd1	0.02302 (9)	0.01335 (9)	0.02879 (10)	−0.00104 (7)	0.00969 (7)	−0.00038 (7)
S1	0.0253 (3)	0.0158 (3)	0.0360 (4)	0.0014 (2)	0.0143 (3)	−0.0013 (3)
C1	0.0184 (11)	0.0204 (12)	0.0207 (12)	−0.0041 (10)	0.0069 (9)	0.0011 (10)
N1	0.0296 (11)	0.0185 (11)	0.0421 (14)	−0.0009 (9)	0.0188 (10)	−0.0018 (10)
S2	0.0233 (3)	0.0206 (3)	0.0462 (4)	−0.0034 (3)	0.0023 (3)	0.0019 (3)
C2	0.0214 (12)	0.0252 (14)	0.0246 (13)	0.0046 (11)	0.0028 (10)	0.0010 (11)
N2	0.0283 (12)	0.0236 (12)	0.0407 (14)	0.0019 (10)	0.0015 (10)	−0.0034 (10)
S3	0.0536 (4)	0.0212 (3)	0.0290 (4)	−0.0100 (3)	0.0196 (3)	−0.0021 (3)
C3	0.0230 (12)	0.0246 (14)	0.0175 (12)	0.0040 (10)	0.0060 (9)	−0.0053 (10)
N3	0.0376 (13)	0.0201 (11)	0.0291 (12)	−0.0008 (10)	0.0103 (10)	0.0000 (9)
C4	0.0247 (13)	0.0277 (14)	0.0185 (12)	0.0011 (10)	0.0036 (10)	0.0034 (10)
C5	0.0261 (13)	0.0298 (14)	0.0302 (14)	0.0029 (11)	0.0083 (11)	0.0029 (12)
C6	0.0444 (17)	0.0269 (14)	0.0281 (15)	0.0001 (12)	0.0085 (12)	0.0019 (12)
C7	0.0401 (16)	0.0370 (16)	0.0279 (15)	−0.0137 (13)	0.0005 (12)	0.0084 (12)
C8	0.0276 (15)	0.0491 (19)	0.0444 (18)	−0.0029 (13)	0.0107 (13)	0.0148 (15)
C9	0.0319 (15)	0.0353 (16)	0.0372 (16)	0.0045 (12)	0.0164 (12)	0.0090 (13)
C10	0.0313 (14)	0.0285 (14)	0.0175 (12)	0.0015 (11)	0.0044 (10)	0.0002 (11)
N10	0.0219 (10)	0.0234 (11)	0.0180 (10)	−0.0007 (8)	0.0024 (8)	−0.0012 (8)
C11	0.0413 (16)	0.0290 (15)	0.0291 (15)	−0.0106 (13)	−0.0014 (12)	−0.0006 (12)
C12	0.062 (2)	0.0413 (18)	0.0438 (19)	−0.0231 (16)	−0.0023 (16)	0.0109 (15)
C13	0.0234 (13)	0.0306 (14)	0.0248 (13)	0.0042 (11)	0.0040 (10)	0.0046 (11)
C14	0.0421 (17)	0.0428 (19)	0.0499 (19)	0.0190 (14)	0.0185 (15)	0.0056 (15)
C15	0.0251 (13)	0.0403 (16)	0.0218 (13)	0.0058 (11)	0.0075 (10)	0.0001 (12)
C16	0.0252 (15)	0.069 (2)	0.0444 (18)	0.0105 (14)	0.0122 (13)	0.0108 (16)

Geometric parameters (Å, º)

Cd1—S1	2.7543 (8)	C9—H9A	0.9500
Cd1—N1	2.291 (2)	C10—H10A	0.9900
Cd1—S2	2.7738 (10)	C10—H10B	0.9900
Cd1—N2	2.359 (2)	C10—N10	1.550 (3)
Cd1—S3	2.7278 (8)	N10—C11	1.531 (3)
Cd1—N3	2.371 (2)	N10—C13	1.526 (3)
S1—C1	1.666 (2)	N10—C15	1.532 (3)
C1—N1^i	1.159 (3)	C11—H11A	0.9900
N1—C1^ii	1.159 (3)	C11—H11B	0.9900
S2—C2	1.669 (3)	C11—C12	1.529 (4)
C2—N2^ii	1.166 (3)	C12—H12A	0.9800
N2—C2^i	1.166 (3)	C12—H12B	0.9800
S3—C3	1.661 (3)	C12—H12C	0.9800
C3—N3^ii	1.171 (3)	C13—H13A	0.9900
N3—C3^i	1.171 (3)	C13—H13B	0.9900
C4—C5	1.399 (3)	C13—C14	1.531 (4)
C4—C9	1.410 (3)	C14—H14A	0.9800
C4—C10	1.521 (3)	C14—H14B	0.9800
C5—H5A	0.9500	C14—H14C	0.9800
C5—C6	1.398 (4)	C15—H15A	0.9900
C6—H6A	0.9500	C15—H15B	0.9900
C6—C7	1.391 (4)	C15—C16	1.528 (4)
C7—H7A	0.9500	C16—H16A	0.9800
C7—C8	1.386 (4)	C16—H16B	0.9800
C8—H8A	0.9500	C16—H16C	0.9800
C8—C9	1.391 (4)
S1—Cd1—N1	176.11 (5)	H10A—C10—H10B	107.4
S1—Cd1—S2	84.32 (2)	H10A—C10—N10	108.4
S1—Cd1—N2	91.28 (6)	H10B—C10—N10	108.4
S1—Cd1—S3	85.91 (3)	C10—N10—C11	105.99 (18)
S1—Cd1—N3	90.36 (6)	C10—N10—C13	110.52 (18)
N1—Cd1—S2	92.17 (6)	C10—N10—C15	111.08 (18)
N1—Cd1—N2	92.39 (8)	C11—N10—C13	111.72 (19)
N1—Cd1—S3	92.56 (6)	C11—N10—C15	111.70 (19)
N1—Cd1—N3	91.50 (8)	C13—N10—C15	105.91 (18)
S2—Cd1—N2	172.82 (5)	N10—C11—H11A	108.7
S2—Cd1—S3	91.83 (3)	N10—C11—H11B	108.7
S2—Cd1—N3	93.37 (6)	N10—C11—C12	114.0 (2)
N2—Cd1—S3	93.51 (6)	H11A—C11—H11B	107.6
N2—Cd1—N3	80.96 (8)	H11A—C11—C12	108.7
S3—Cd1—N3	173.27 (5)	H11B—C11—C12	108.7
Cd1—S1—C1	95.50 (8)	C11—C12—H12A	109.5
S1—C1—N1^i	178.5 (2)	C11—C12—H12B	109.5
Cd1—N1—C1^ii	155.83 (18)	C11—C12—H12C	109.5
Cd1—S2—C2	98.98 (8)	H12A—C12—H12B	109.5
S2—C2—N2^ii	178.8 (2)	H12A—C12—H12C	109.5
Cd1—N2—C2^i	147.07 (19)	H12B—C12—H12C	109.5
Cd1—S3—C3	101.19 (8)	N10—C13—H13A	108.4
S3—C3—N3^ii	178.9 (2)	N10—C13—H13B	108.4
Cd1—N3—C3^i	144.87 (19)	N10—C13—C14	115.4 (2)
C5—C4—C9	118.4 (2)	H13A—C13—H13B	107.5
C5—C4—C10	121.0 (2)	H13A—C13—C14	108.4
C9—C4—C10	120.5 (2)	H13B—C13—C14	108.4
C4—C5—H5A	119.6	C13—C14—H14A	109.5
C4—C5—C6	120.9 (2)	C13—C14—H14B	109.5
H5A—C5—C6	119.6	C13—C14—H14C	109.5
C5—C6—H6A	120.2	H14A—C14—H14B	109.5
C5—C6—C7	119.6 (3)	H14A—C14—H14C	109.5
H6A—C6—C7	120.2	H14B—C14—H14C	109.5
C6—C7—H7A	119.8	N10—C15—H15A	108.4
C6—C7—C8	120.4 (3)	N10—C15—H15B	108.4
H7A—C7—C8	119.8	N10—C15—C16	115.4 (2)
C7—C8—H8A	120.0	H15A—C15—H15B	107.5
C7—C8—C9	120.1 (3)	H15A—C15—C16	108.4
H8A—C8—C9	120.0	H15B—C15—C16	108.4
C4—C9—C8	120.6 (3)	C15—C16—H16A	109.5
C4—C9—H9A	119.7	C15—C16—H16B	109.5
C8—C9—H9A	119.7	C15—C16—H16C	109.5
C4—C10—H10A	108.4	H16A—C16—H16B	109.5
C4—C10—H10B	108.4	H16A—C16—H16C	109.5
C4—C10—N10	115.64 (19)	H16B—C16—H16C	109.5
S2—Cd1—S1—C1	135.60 (9)	N2—Cd1—N3—C3^i	22.6 (3)
N2—Cd1—S1—C1	−38.71 (10)	C9—C4—C5—C6	−1.4 (4)
S3—Cd1—S1—C1	−132.14 (9)	C10—C4—C5—C6	−178.6 (2)
N3—Cd1—S1—C1	42.25 (10)	C4—C5—C6—C7	0.5 (4)
S2—Cd1—N1—C1^ii	51.4 (5)	C5—C6—C7—C8	0.4 (4)
N2—Cd1—N1—C1^ii	−134.1 (5)	C6—C7—C8—C9	−0.5 (4)
S3—Cd1—N1—C1^ii	−40.5 (5)	C7—C8—C9—C4	−0.4 (4)
N3—Cd1—N1—C1^ii	144.9 (5)	C5—C4—C9—C8	1.3 (4)
S1—Cd1—S2—C2	150.57 (9)	C10—C4—C9—C8	178.6 (2)
N1—Cd1—S2—C2	−27.77 (10)	C5—C4—C10—N10	−88.6 (3)
S3—Cd1—S2—C2	64.86 (9)	C9—C4—C10—N10	94.2 (3)
N3—Cd1—S2—C2	−119.40 (10)	C4—C10—N10—C11	−176.3 (2)
S1—Cd1—N2—C2^i	68.1 (4)	C4—C10—N10—C13	−55.1 (3)
N1—Cd1—N2—C2^i	−113.2 (4)	C4—C10—N10—C15	62.2 (3)
S3—Cd1—N2—C2^i	154.1 (4)	C10—N10—C11—C12	179.5 (2)
N3—Cd1—N2—C2^i	−22.1 (4)	C13—N10—C11—C12	59.1 (3)
S1—Cd1—S3—C3	−149.38 (9)	C15—N10—C11—C12	−59.4 (3)
N1—Cd1—S3—C3	27.04 (10)	C10—N10—C13—C14	−67.1 (3)
S2—Cd1—S3—C3	−65.21 (9)	C11—N10—C13—C14	50.7 (3)
N2—Cd1—S3—C3	119.59 (10)	C15—N10—C13—C14	172.5 (2)
S1—Cd1—N3—C3^i	−68.6 (3)	C10—N10—C15—C16	63.7 (3)
N1—Cd1—N3—C3^i	114.8 (3)	C11—N10—C15—C16	−54.4 (3)
S2—Cd1—N3—C3^i	−152.9 (3)	C13—N10—C15—C16	−176.2 (2)

Symmetry codes: (i) −x+3/2, y−1/2, −z+3/2; (ii) −x+3/2, y+1/2, −z+3/2.