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The title complex, (C8H20N)2[Cd(C3S5)2], has the Cd atom in a distorted tetrahedral geometry, due to the relatively small bite angles, 88.61 (4)-88.78 (4)°, of the 2-thio­xo-1,3-di­thiole-4,5-di­thiol­ate ligands.

Supporting information

cif

Crystallographic Information File (CIF) https://doi.org/10.1107/S1600536804029277/sj6018sup1.cif
Contains datablocks I, global

hkl

Structure factor file (CIF format) https://doi.org/10.1107/S1600536804029277/sj6018Isup2.hkl
Contains datablock I

CCDC reference: 258695

Key indicators

  • Single-crystal X-ray study
  • T = 293 K
  • Mean [sigma](C-C) = 0.007 Å
  • R factor = 0.038
  • wR factor = 0.095
  • Data-to-parameter ratio = 19.0

checkCIF/PLATON results

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Alert level C PLAT042_ALERT_1_C Calc. and Rep. MoietyFormula Strings Differ .... ? PLAT094_ALERT_2_C Ratio of Maximum / Minimum Residual Density .... 2.24 PLAT241_ALERT_2_C Check High U(eq) as Compared to Neighbors for S4 PLAT241_ALERT_2_C Check High U(eq) as Compared to Neighbors for S7 PLAT244_ALERT_4_C Low Solvent U(eq) as Compared to Neighbors for N1 PLAT244_ALERT_4_C Low Solvent U(eq) as Compared to Neighbors for N2
0 ALERT level A = In general: serious problem 0 ALERT level B = Potentially serious problem 6 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 3 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 2 ALERT type 4 Improvement, methodology, query or suggestion

Computing details top

Data collection: XSCANS (Bruker,1996); cell refinement: XSCANS; data reduction: XSCANS; program(s) used to solve structure: SIR92 (Altomare,1993); program(s) used to refine structure: SHELXTL (Bruker, 1997); molecular graphics: SHELXTL; software used to prepare material for publication: WinGX (Farrugia,1999).

Bis(tetraethylammonium) bis(2-thioxo-1,3-dithiole-4,5-dithiolato)cadmium(II) top
Crystal data top
(C8H20N)[Cd(C3S5)2]F(000) = 1576
Mr = 765.56Dx = 1.488 Mg m3
Monoclinic, P21/cMo Kα radiation, λ = 0.71073 Å
Hall symbol: -P 2ybcCell parameters from 35 reflections
a = 9.9739 (14) Åθ = 5.3–12.5°
b = 20.116 (2) ŵ = 1.27 mm1
c = 17.033 (4) ÅT = 293 K
β = 90.860 (16)°Prism, dark red
V = 3417 (1) Å30.42 × 0.40 × 0.38 mm
Z = 4
Data collection top
Bruker P4
diffractometer
4621 reflections with I > 2σ(I)
Radiation source: fine-focus sealed tubeRint = 0.020
Graphite monochromatorθmax = 25.0°, θmin = 2.0°
ω scansh = 111
Absorption correction: empirical (using intensity measurements)
(XSCANS; Bruker, 1996)
k = 231
Tmin = 0.573, Tmax = 0.620l = 2020
7577 measured reflections3 standard reflections every 97 reflections
6020 independent reflections intensity decay: 0.1%
Refinement top
Refinement on F2Secondary atom site location: difference Fourier map
Least-squares matrix: fullHydrogen site location: inferred from neighbouring sites
R[F2 > 2σ(F2)] = 0.038H-atom parameters constrained
wR(F2) = 0.095 w = 1/[σ2(Fo2) + (0.0398P)2 + 3.2613P]
where P = (Fo2 + 2Fc2)/3
S = 1.02(Δ/σ)max = 0.002
6017 reflectionsΔρmax = 0.83 e Å3
317 parametersΔρmin = 0.37 e Å3
6 restraintsExtinction correction: SHELXL97, Fc*=kFc[1+0.001xFc2λ3/sin(2θ)]-1/4
Primary atom site location: structure-invariant direct methodsExtinction coefficient: 0.0063 (3)
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
xyzUiso*/Ueq
C10.8452 (4)0.5165 (2)0.6067 (2)0.0543 (10)
C20.7130 (4)0.62379 (18)0.6503 (2)0.0483 (9)
C30.6748 (4)0.61348 (19)0.5750 (2)0.0471 (9)
C40.3269 (4)0.87814 (18)0.5993 (2)0.0436 (9)
C50.2568 (4)0.84172 (19)0.6517 (2)0.0492 (9)
C60.1046 (4)0.9454 (2)0.6225 (2)0.0544 (10)
C70.4650 (7)0.5224 (3)0.7824 (3)0.111 (2)
H7A0.53520.49390.80350.134*
H7B0.50850.55730.75290.134*
C80.3968 (8)0.5534 (4)0.8485 (4)0.153 (3)
H8A0.46080.57740.88020.230*
H8B0.35530.51960.87970.230*
H8C0.32940.58350.82900.230*
C90.2632 (5)0.5191 (3)0.6954 (3)0.0856 (15)
H9A0.21380.48950.66060.103*
H9B0.20580.52880.73940.103*
C100.2859 (6)0.5818 (3)0.6528 (4)0.103 (2)
H10A0.20120.60020.63630.155*
H10B0.33960.57330.60760.155*
H10C0.33150.61270.68680.155*
C110.3300 (6)0.4212 (3)0.7702 (3)0.0955 (17)
H11A0.40540.40010.79680.115*
H11B0.26940.43660.81030.115*
C120.2586 (6)0.3695 (3)0.7221 (4)0.112 (2)
H12A0.23080.33380.75550.168*
H12B0.31790.35250.68290.168*
H12C0.18130.38890.69690.168*
C130.4683 (5)0.4611 (3)0.6582 (3)0.0819 (15)
H13A0.41030.44090.61870.098*
H13B0.50670.50070.63510.098*
C140.5792 (5)0.4140 (3)0.6761 (3)0.0871 (16)
H14A0.62670.40430.62890.131*
H14B0.54290.37360.69700.131*
H14C0.63950.43350.71400.131*
C150.1583 (4)0.7836 (2)0.4547 (2)0.0612 (11)
H15A0.18560.82460.42960.073*
H15B0.17190.78920.51080.073*
C160.2482 (5)0.7288 (3)0.4274 (3)0.0947 (18)
H16A0.33970.73970.44010.142*
H16B0.23810.72360.37160.142*
H16C0.22440.68810.45300.142*
C170.0382 (5)0.7111 (2)0.4789 (3)0.0758 (14)
H17A0.13300.70570.46690.091*
H17B0.00820.67330.45660.091*
C180.0192 (6)0.7089 (3)0.5670 (3)0.104 (2)
H18A0.05300.66760.58680.156*
H18B0.06710.74510.59030.156*
H18C0.07450.71270.58000.156*
C190.0166 (5)0.7661 (2)0.3517 (3)0.0688 (13)
H19A0.02620.72550.33410.083*
H19B0.11240.76070.34340.083*
C200.0295 (6)0.8214 (3)0.3020 (3)0.0878 (17)
H20A0.00790.81190.24800.132*
H20B0.12470.82640.30820.132*
H20C0.01430.86170.31740.132*
C210.0609 (5)0.8345 (2)0.4703 (3)0.0703 (13)
H21A0.04400.83700.52640.084*
H21B0.02160.87370.44680.084*
C220.2094 (6)0.8365 (3)0.4560 (4)0.113 (2)
H22A0.24530.87660.47780.169*
H22B0.25030.79880.48050.169*
H22C0.22780.83540.40050.169*
N10.3826 (3)0.48223 (17)0.72616 (18)0.0526 (8)
N20.0103 (3)0.77346 (15)0.43861 (19)0.0502 (8)
S10.94392 (13)0.45092 (6)0.60200 (9)0.0791 (4)
S20.82566 (11)0.56490 (5)0.68888 (6)0.0581 (3)
S30.74790 (12)0.54445 (6)0.52998 (6)0.0615 (3)
S40.66730 (13)0.68796 (6)0.71259 (7)0.0680 (3)
S50.56884 (12)0.66058 (6)0.51522 (6)0.0642 (3)
S60.47966 (11)0.85972 (5)0.55655 (6)0.0562 (3)
S70.29622 (13)0.76468 (6)0.69181 (8)0.0714 (4)
S80.24853 (11)0.95207 (5)0.56918 (6)0.0557 (3)
S90.10391 (11)0.87560 (6)0.67969 (7)0.0607 (3)
S100.02195 (13)0.99874 (7)0.61780 (9)0.0816 (4)
Cd10.50881 (3)0.745628 (15)0.617380 (18)0.05502 (13)
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
C10.046 (2)0.047 (2)0.069 (3)0.0019 (19)0.003 (2)0.002 (2)
C20.046 (2)0.042 (2)0.056 (2)0.0029 (18)0.0074 (18)0.0020 (18)
C30.045 (2)0.049 (2)0.047 (2)0.0080 (18)0.0033 (17)0.0040 (18)
C40.044 (2)0.040 (2)0.047 (2)0.0059 (17)0.0032 (17)0.0041 (17)
C50.056 (2)0.045 (2)0.047 (2)0.0051 (19)0.0049 (18)0.0035 (17)
C60.060 (3)0.045 (2)0.058 (2)0.006 (2)0.006 (2)0.0059 (19)
C70.122 (5)0.116 (5)0.095 (4)0.013 (4)0.027 (4)0.029 (4)
C80.149 (7)0.199 (9)0.112 (5)0.015 (6)0.004 (5)0.083 (6)
C90.081 (3)0.076 (3)0.099 (4)0.015 (3)0.007 (3)0.001 (3)
C100.118 (5)0.058 (3)0.133 (5)0.016 (3)0.013 (4)0.024 (3)
C110.102 (4)0.096 (4)0.089 (4)0.000 (3)0.004 (3)0.024 (3)
C120.084 (4)0.064 (3)0.187 (7)0.016 (3)0.004 (4)0.026 (4)
C130.086 (4)0.081 (4)0.079 (3)0.002 (3)0.009 (3)0.005 (3)
C140.068 (3)0.081 (4)0.113 (4)0.017 (3)0.000 (3)0.005 (3)
C150.060 (3)0.072 (3)0.052 (2)0.011 (2)0.009 (2)0.001 (2)
C160.062 (3)0.129 (5)0.093 (4)0.027 (3)0.014 (3)0.003 (4)
C170.072 (3)0.050 (3)0.105 (4)0.013 (2)0.004 (3)0.008 (3)
C180.117 (5)0.094 (4)0.101 (4)0.021 (4)0.004 (4)0.040 (4)
C190.067 (3)0.074 (3)0.065 (3)0.020 (2)0.018 (2)0.022 (2)
C200.104 (4)0.110 (4)0.050 (3)0.032 (4)0.002 (3)0.001 (3)
C210.090 (4)0.048 (3)0.073 (3)0.011 (2)0.022 (3)0.005 (2)
C220.081 (4)0.110 (5)0.149 (6)0.036 (4)0.040 (4)0.005 (4)
N10.0493 (19)0.058 (2)0.0499 (18)0.0028 (16)0.0030 (15)0.0024 (16)
N20.0514 (19)0.0406 (17)0.059 (2)0.0005 (15)0.0012 (16)0.0080 (15)
S10.0653 (8)0.0580 (7)0.1136 (10)0.0216 (6)0.0107 (7)0.0095 (7)
S20.0609 (7)0.0502 (6)0.0628 (6)0.0076 (5)0.0164 (5)0.0018 (5)
S30.0655 (7)0.0606 (7)0.0582 (6)0.0195 (6)0.0053 (5)0.0135 (5)
S40.0821 (8)0.0637 (7)0.0578 (6)0.0230 (6)0.0191 (6)0.0171 (5)
S50.0729 (8)0.0689 (7)0.0505 (6)0.0265 (6)0.0133 (5)0.0090 (5)
S60.0506 (6)0.0568 (6)0.0615 (6)0.0076 (5)0.0106 (5)0.0086 (5)
S70.0814 (8)0.0552 (7)0.0784 (8)0.0181 (6)0.0281 (7)0.0207 (6)
S80.0560 (6)0.0464 (6)0.0649 (6)0.0070 (5)0.0059 (5)0.0074 (5)
S90.0618 (7)0.0564 (6)0.0644 (7)0.0109 (5)0.0204 (5)0.0028 (5)
S100.0716 (8)0.0654 (8)0.1084 (10)0.0272 (6)0.0183 (8)0.0080 (7)
Cd10.0562 (2)0.04846 (19)0.0604 (2)0.01214 (15)0.00117 (14)0.00392 (14)
Geometric parameters (Å, º) top
C1—S11.649 (4)C13—N11.511 (6)
C1—S31.711 (4)C13—H13A0.9700
C1—S21.718 (4)C13—H13B0.9700
C2—C31.349 (5)C14—H14A0.9600
C2—S41.736 (4)C14—H14B0.9600
C2—S21.753 (4)C14—H14C0.9600
C3—S51.737 (4)C15—C161.499 (7)
C3—S31.750 (4)C15—N21.511 (5)
C4—C51.356 (5)C15—H15A0.9700
C4—S61.739 (4)C15—H15B0.9700
C4—S81.753 (4)C16—H16A0.9600
C5—S71.737 (4)C16—H16B0.9600
C5—S91.743 (4)C16—H16C0.9600
C6—S101.658 (4)C17—C181.510 (7)
C6—S91.708 (4)C17—N21.513 (5)
C6—S81.715 (4)C17—H17A0.9700
C7—C81.464 (8)C17—H17B0.9700
C7—N11.490 (6)C18—H18A0.9600
C7—H7A0.9700C18—H18B0.9600
C7—H7B0.9700C18—H18C0.9600
C8—H8A0.9600C19—C201.475 (7)
C8—H8B0.9600C19—N21.508 (5)
C8—H8C0.9600C19—H19A0.9700
C9—C101.473 (7)C19—H19B0.9700
C9—N11.492 (6)C20—H20A0.9600
C9—H9A0.9700C20—H20B0.9600
C9—H9B0.9700C20—H20C0.9600
C10—H10A0.9600C21—C221.498 (7)
C10—H10B0.9600C21—N21.522 (5)
C10—H10C0.9600C21—H21A0.9700
C11—C121.498 (9)C21—H21B0.9700
C11—N11.535 (6)C22—H22A0.9600
C11—H11A0.9700C22—H22B0.9600
C11—H11B0.9700C22—H22C0.9600
C12—H12A0.9600S4—Cd12.5293 (12)
C12—H12B0.9600S5—Cd12.5189 (12)
C12—H12C0.9600S6—Cd12.5330 (11)
C13—C141.484 (7)S7—Cd12.5162 (13)
S1—C1—S3123.9 (3)N2—C15—H15B108.4
S1—C1—S2124.6 (3)H15A—C15—H15B107.4
S3—C1—S2111.5 (2)C15—C16—H16A109.5
C3—C2—S4128.5 (3)C15—C16—H16B109.5
C3—C2—S2115.0 (3)H16A—C16—H16B109.5
S4—C2—S2116.5 (2)C15—C16—H16C109.5
C2—C3—S5129.4 (3)H16A—C16—H16C109.5
C2—C3—S3115.1 (3)H16B—C16—H16C109.5
S5—C3—S3115.5 (2)C18—C17—N2116.0 (4)
C5—C4—S6128.6 (3)C18—C17—H17A108.3
C5—C4—S8114.8 (3)N2—C17—H17A108.3
S6—C4—S8116.6 (2)C18—C17—H17B108.3
C4—C5—S7128.7 (3)N2—C17—H17B108.3
C4—C5—S9115.5 (3)H17A—C17—H17B107.4
S7—C5—S9115.8 (2)C17—C18—H18A109.5
S10—C6—S9123.4 (3)C17—C18—H18B109.5
S10—C6—S8124.5 (3)H18A—C18—H18B109.5
S9—C6—S8112.2 (2)C17—C18—H18C109.5
C8—C7—N1117.8 (6)H18A—C18—H18C109.5
C8—C7—H7A107.9H18B—C18—H18C109.5
N1—C7—H7A107.9C20—C19—N2115.9 (4)
C8—C7—H7B107.9C20—C19—H19A108.3
N1—C7—H7B107.9N2—C19—H19A108.3
H7A—C7—H7B107.2C20—C19—H19B108.3
C7—C8—H8A109.5N2—C19—H19B108.3
C7—C8—H8B109.5H19A—C19—H19B107.4
H8A—C8—H8B109.5C19—C20—H20A109.5
C7—C8—H8C109.5C19—C20—H20B109.5
H8A—C8—H8C109.5H20A—C20—H20B109.5
H8B—C8—H8C109.5C19—C20—H20C109.5
C10—C9—N1118.1 (5)H20A—C20—H20C109.5
C10—C9—H9A107.8H20B—C20—H20C109.5
N1—C9—H9A107.8C22—C21—N2115.4 (4)
C10—C9—H9B107.8C22—C21—H21A108.4
N1—C9—H9B107.8N2—C21—H21A108.4
H9A—C9—H9B107.1C22—C21—H21B108.4
C9—C10—H10A109.5N2—C21—H21B108.4
C9—C10—H10B109.5H21A—C21—H21B107.5
H10A—C10—H10B109.5C21—C22—H22A109.5
C9—C10—H10C109.5C21—C22—H22B109.5
H10A—C10—H10C109.5H22A—C22—H22B109.5
H10B—C10—H10C109.5C21—C22—H22C109.5
C12—C11—N1116.8 (4)H22A—C22—H22C109.5
C12—C11—H11A108.1H22B—C22—H22C109.5
N1—C11—H11A108.1C7—N1—C9112.7 (4)
C12—C11—H11B108.1C7—N1—C13109.4 (4)
N1—C11—H11B108.1C9—N1—C13109.2 (4)
H11A—C11—H11B107.3C7—N1—C11108.0 (4)
C11—C12—H12A109.5C9—N1—C11107.0 (4)
C11—C12—H12B109.5C13—N1—C11110.5 (4)
H12A—C12—H12B109.5C19—N2—C15110.5 (3)
C11—C12—H12C109.5C19—N2—C17108.1 (3)
H12A—C12—H12C109.5C15—N2—C17110.3 (3)
H12B—C12—H12C109.5C19—N2—C21110.5 (3)
C14—C13—N1116.8 (4)C15—N2—C21106.7 (3)
C14—C13—H13A108.1C17—N2—C21110.8 (3)
N1—C13—H13A108.1C1—S2—C299.07 (19)
C14—C13—H13B108.1C1—S3—C399.28 (19)
N1—C13—H13B108.1C2—S4—Cd196.70 (13)
H13A—C13—H13B107.3C3—S5—Cd196.57 (13)
C13—C14—H14A109.5C4—S6—Cd196.74 (13)
C13—C14—H14B109.5C5—S7—Cd197.19 (14)
H14A—C14—H14B109.5C6—S8—C498.68 (19)
C13—C14—H14C109.5C6—S9—C598.9 (2)
H14A—C14—H14C109.5S7—Cd1—S5131.48 (5)
H14B—C14—H14C109.5S7—Cd1—S4105.67 (4)
C16—C15—N2115.6 (4)S5—Cd1—S488.78 (4)
C16—C15—H15A108.4S7—Cd1—S688.61 (4)
N2—C15—H15A108.4S5—Cd1—S6111.09 (4)
C16—C15—H15B108.4S4—Cd1—S6138.13 (4)
S4—C2—C3—S50.4 (6)C3—C2—S2—C11.9 (4)
S2—C2—C3—S5178.5 (2)S4—C2—S2—C1177.1 (2)
S4—C2—C3—S3177.6 (2)S1—C1—S3—C3179.3 (3)
S2—C2—C3—S31.3 (4)S2—C1—S3—C31.2 (3)
S6—C4—C5—S70.8 (6)C2—C3—S3—C10.1 (4)
S8—C4—C5—S7176.9 (2)S5—C3—S3—C1177.7 (2)
S6—C4—C5—S9178.4 (2)C3—C2—S4—Cd12.1 (4)
S8—C4—C5—S90.7 (4)S2—C2—S4—Cd1179.0 (2)
C8—C7—N1—C952.3 (8)C2—C3—S5—Cd12.6 (4)
C8—C7—N1—C13173.9 (6)S3—C3—S5—Cd1179.8 (2)
C8—C7—N1—C1165.7 (8)C5—C4—S6—Cd13.3 (4)
C10—C9—N1—C759.2 (6)S8—C4—S6—Cd1174.26 (18)
C10—C9—N1—C1362.6 (6)C4—C5—S7—Cd12.4 (4)
C10—C9—N1—C11177.7 (5)S9—C5—S7—Cd1175.18 (19)
C14—C13—N1—C766.4 (6)S10—C6—S8—C4176.6 (3)
C14—C13—N1—C9169.8 (4)S9—C6—S8—C41.7 (3)
C14—C13—N1—C1152.4 (6)C5—C4—S8—C60.6 (3)
C12—C11—N1—C7172.6 (5)S6—C4—S8—C6177.3 (2)
C12—C11—N1—C965.8 (6)S10—C6—S9—C5176.3 (3)
C12—C11—N1—C1353.0 (6)S8—C6—S9—C52.0 (3)
C20—C19—N2—C1556.8 (5)C4—C5—S9—C61.7 (3)
C20—C19—N2—C17177.6 (4)S7—C5—S9—C6176.2 (2)
C20—C19—N2—C2161.1 (5)C5—S7—Cd1—S5114.31 (14)
C16—C15—N2—C1959.4 (5)C5—S7—Cd1—S4143.07 (14)
C16—C15—N2—C1760.0 (5)C5—S7—Cd1—S63.00 (14)
C16—C15—N2—C21179.6 (4)C3—S5—Cd1—S7107.34 (14)
C18—C17—N2—C19179.7 (4)C3—S5—Cd1—S42.64 (14)
C18—C17—N2—C1558.9 (6)C3—S5—Cd1—S6144.83 (14)
C18—C17—N2—C2159.0 (6)C2—S4—Cd1—S7130.47 (14)
C22—C21—N2—C1956.4 (5)C2—S4—Cd1—S52.54 (14)
C22—C21—N2—C15176.5 (4)C2—S4—Cd1—S6123.56 (14)
C22—C21—N2—C1763.4 (5)C4—S6—Cd1—S73.24 (13)
S1—C1—S2—C2178.7 (3)C4—S6—Cd1—S5131.25 (13)
S3—C1—S2—C21.7 (3)C4—S6—Cd1—S4115.43 (13)
 

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