Download citation
Download citation
link to html
In the title complex, (C6H8N)2[Cd(C3S5)2], the CdII ion is coordinated by four dmit (2-thioxo-1,3-dithione-4,5-dithiol­ate) S atoms in a distorted tetra­hedral geometry. The N-methyl­pyridinium cations link with the CdII complex anion via weak C—H...S hydrogen bonding.

Supporting information

cif

Crystallographic Information File (CIF) https://doi.org/10.1107/S1600536806055346/xu2187sup1.cif
Contains datablocks I, global

hkl

Structure factor file (CIF format) https://doi.org/10.1107/S1600536806055346/xu2187Isup2.hkl
Contains datablock I

CCDC reference: 636841

Key indicators

  • Single-crystal X-ray study
  • T = 293 K
  • Mean [sigma](C-C) = 0.010 Å
  • R factor = 0.035
  • wR factor = 0.088
  • Data-to-parameter ratio = 21.4

checkCIF/PLATON results

No syntax errors found



Alert level C PLAT180_ALERT_3_C Check Cell Rounding: # of Values Ending with 0 = 3 PLAT231_ALERT_4_C Hirshfeld Test (Solvent) C16 - C17 .. 5.30 su PLAT232_ALERT_2_C Hirshfeld Test Diff (M-X) Cd1 - S4 .. 6.12 su PLAT243_ALERT_4_C High 'Solvent' Ueq as Compared to Neighbors for C16 PLAT244_ALERT_4_C Low 'Solvent' Ueq as Compared to Neighbors for N1 PLAT244_ALERT_4_C Low 'Solvent' Ueq as Compared to Neighbors for N2 PLAT250_ALERT_2_C Large U3/U1 Ratio for Average U(i,j) Tensor .... 2.40 PLAT250_ALERT_2_C Large U3/U1 Ratio for Average U(i,j) Tensor .... 2.29 PLAT342_ALERT_3_C Low Bond Precision on C-C bonds (x 1000) Ang ... 10 PLAT790_ALERT_4_C Centre of Gravity not Within Unit Cell: Resd. # 2 C6 H8 N PLAT790_ALERT_4_C Centre of Gravity not Within Unit Cell: Resd. # 3 C6 H8 N
Alert level G PLAT199_ALERT_1_G Check the Reported _cell_measurement_temperature 293 K PLAT200_ALERT_1_G Check the Reported _diffrn_ambient_temperature . 293 K
0 ALERT level A = In general: serious problem 0 ALERT level B = Potentially serious problem 11 ALERT level C = Check and explain 2 ALERT level G = General alerts; check 2 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 2 ALERT type 3 Indicator that the structure quality may be low 6 ALERT type 4 Improvement, methodology, query or suggestion 0 ALERT type 5 Informative message, check

Computing details top

Data collection: APEX2 (Bruker, 2005); cell refinement: APEX2; data reduction: APEX2; program(s) used to solve structure: SIR97 (Altomare et al., 1999); program(s) used to refine structure: SHELXL97 (Sheldrick, 1997); molecular graphics: SHELXTL (Bruker, 1997); software used to prepare material for publication: WinGX (Farrugia, 1999).

Bis(N-methylpyridinium) bis(2-thioxo-1,3-dithione-4,5-dithiolato)cadmium(II) top
Crystal data top
(C6H8N)2[Cd(C3S5)2]F(000) = 1384
Mr = 693.33Dx = 1.750 Mg m3
Monoclinic, P21/cMo Kα radiation, λ = 0.71073 Å
Hall symbol: -P 2ybcCell parameters from 4431 reflections
a = 14.4624 (12) Åθ = 3.3–26.9°
b = 13.5970 (11) ŵ = 1.64 mm1
c = 14.1880 (11) ÅT = 293 K
β = 109.369 (1)°Plate, purple–red
V = 2632.1 (4) Å30.24 × 0.23 × 0.05 mm
Z = 4
Data collection top
Bruker APEX2 CCD area-detector
diffractometer
6032 independent reflections
Radiation source: fine-focus sealed tube4441 reflections with I > 2σ(I)
Graphite monochromatorRint = 0.020
φ and ω scansθmax = 27.5°, θmin = 3.2°
Absorption correction: multi-scan
(APEX2; Bruker, 2005)
h = 1718
Tmin = 0.694, Tmax = 0.917k = 917
13401 measured reflectionsl = 187
Refinement top
Refinement on F2Primary atom site location: structure-invariant direct methods
Least-squares matrix: fullSecondary atom site location: difference Fourier map
R[F2 > 2σ(F2)] = 0.035Hydrogen site location: inferred from neighbouring sites
wR(F2) = 0.088H-atom parameters constrained
S = 1.01 w = 1/[σ2(Fo2) + (0.0389P)2 + 1.0462P]
where P = (Fo2 + 2Fc2)/3
6032 reflections(Δ/σ)max = 0.001
282 parametersΔρmax = 0.53 e Å3
0 restraintsΔρmin = 0.40 e Å3
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
N10.1291 (4)0.3127 (3)0.1262 (2)0.0864 (11)
N21.4267 (3)0.1587 (2)0.3013 (2)0.0785 (10)
C10.2814 (2)0.4280 (2)0.2073 (3)0.0618 (9)
C20.4673 (2)0.4145 (2)0.2215 (2)0.0475 (7)
C30.4680 (2)0.4137 (2)0.3174 (2)0.0474 (7)
C40.9196 (2)0.3394 (2)0.3854 (2)0.0474 (7)
C50.8867 (2)0.2458 (2)0.3826 (2)0.0451 (7)
C61.0733 (2)0.2281 (3)0.4019 (2)0.0559 (8)
C70.1278 (6)0.4180 (5)0.1175 (4)0.167 (3)
H7A0.19230.44350.10720.250*
H7B0.10750.43540.06180.250*
H7C0.08280.44530.17760.250*
C80.2107 (4)0.2670 (5)0.1253 (3)0.0974 (15)
H80.26650.30320.12120.117*
C90.2123 (5)0.1700 (7)0.1301 (4)0.117 (2)
H90.26910.13880.13160.141*
C100.1363 (7)0.1168 (5)0.1329 (4)0.122 (2)
H100.14110.04860.13340.146*
C110.0536 (5)0.1570 (6)0.1350 (4)0.1070 (17)
H110.00020.11800.13810.128*
C120.0473 (4)0.2588 (5)0.1326 (3)0.0977 (16)
H120.01100.28960.13520.117*
C131.4585 (6)0.1552 (4)0.4089 (4)0.156 (3)
H13A1.52600.17460.43550.234*
H13B1.45140.08950.43020.234*
H13C1.41920.19930.43270.234*
C141.3304 (4)0.1654 (3)0.2461 (4)0.0867 (13)
H141.28360.16990.27780.104*
C151.3026 (4)0.1657 (4)0.1476 (5)0.1018 (16)
H151.23640.17120.11070.122*
C161.3665 (7)0.1584 (4)0.1013 (4)0.122 (2)
H161.34540.15750.03180.146*
C171.4615 (6)0.1522 (4)0.1526 (6)0.107 (2)
H171.50660.14760.11880.129*
C181.4933 (4)0.1524 (3)0.2536 (5)0.0932 (15)
H181.55980.14820.28970.112*
Cd10.692162 (16)0.371879 (19)0.344166 (18)0.05574 (9)
S10.16088 (7)0.43368 (9)0.16789 (11)0.0923 (4)
S20.35143 (6)0.42627 (7)0.13049 (7)0.0619 (2)
S30.35278 (6)0.42363 (7)0.33143 (7)0.0642 (2)
S40.56473 (6)0.40392 (7)0.17572 (6)0.0569 (2)
S50.56732 (6)0.40260 (8)0.42737 (6)0.0611 (2)
S60.85600 (6)0.44964 (7)0.37631 (8)0.0647 (2)
S70.76922 (6)0.20357 (6)0.36866 (7)0.0552 (2)
S81.04368 (6)0.35074 (7)0.39865 (7)0.0628 (2)
S90.97581 (5)0.15422 (6)0.39551 (6)0.0534 (2)
S101.18316 (7)0.18619 (9)0.41022 (9)0.0834 (3)
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
N10.133 (4)0.075 (3)0.0525 (19)0.010 (2)0.033 (2)0.0091 (17)
N20.120 (3)0.0491 (19)0.065 (2)0.0102 (19)0.029 (2)0.0036 (15)
C10.0463 (17)0.0415 (19)0.092 (3)0.0025 (14)0.0157 (17)0.0034 (17)
C20.0428 (15)0.0393 (17)0.0575 (18)0.0021 (13)0.0129 (13)0.0001 (14)
C30.0403 (15)0.0437 (17)0.0573 (18)0.0036 (13)0.0152 (13)0.0020 (14)
C40.0409 (15)0.0554 (19)0.0439 (16)0.0020 (14)0.0112 (12)0.0015 (14)
C50.0384 (14)0.0535 (19)0.0413 (15)0.0006 (13)0.0104 (12)0.0027 (13)
C60.0427 (16)0.075 (2)0.0477 (17)0.0003 (15)0.0119 (13)0.0050 (16)
C70.313 (11)0.083 (4)0.103 (4)0.002 (5)0.068 (6)0.011 (3)
C80.085 (3)0.142 (5)0.064 (3)0.008 (3)0.022 (2)0.002 (3)
C90.130 (5)0.148 (6)0.066 (3)0.053 (5)0.022 (3)0.015 (4)
C100.194 (8)0.101 (5)0.071 (3)0.012 (5)0.045 (5)0.002 (3)
C110.124 (5)0.132 (6)0.066 (3)0.019 (4)0.033 (3)0.008 (3)
C120.094 (3)0.144 (5)0.059 (3)0.023 (3)0.030 (2)0.000 (3)
C130.272 (9)0.092 (4)0.073 (3)0.026 (5)0.016 (4)0.010 (3)
C140.092 (3)0.074 (3)0.112 (4)0.001 (2)0.057 (3)0.002 (3)
C150.117 (4)0.072 (3)0.103 (4)0.008 (3)0.019 (3)0.006 (3)
C160.221 (8)0.070 (3)0.086 (4)0.023 (4)0.068 (5)0.003 (3)
C170.154 (5)0.060 (3)0.151 (6)0.022 (3)0.109 (5)0.021 (3)
C180.080 (3)0.047 (2)0.154 (5)0.000 (2)0.041 (3)0.010 (3)
Cd10.04440 (13)0.06217 (18)0.05960 (16)0.00753 (11)0.01586 (10)0.00337 (12)
S10.0423 (5)0.0857 (8)0.1394 (10)0.0015 (5)0.0173 (6)0.0053 (7)
S20.0463 (4)0.0627 (6)0.0658 (5)0.0030 (4)0.0040 (4)0.0022 (4)
S30.0505 (4)0.0670 (6)0.0805 (6)0.0077 (4)0.0290 (4)0.0028 (5)
S40.0509 (4)0.0695 (6)0.0501 (4)0.0068 (4)0.0163 (4)0.0020 (4)
S50.0527 (5)0.0818 (6)0.0500 (4)0.0108 (4)0.0184 (4)0.0058 (4)
S60.0553 (5)0.0511 (5)0.0871 (6)0.0009 (4)0.0228 (4)0.0015 (5)
S70.0412 (4)0.0536 (5)0.0704 (5)0.0006 (3)0.0181 (4)0.0013 (4)
S80.0441 (4)0.0668 (6)0.0755 (6)0.0082 (4)0.0172 (4)0.0029 (5)
S90.0431 (4)0.0573 (5)0.0571 (5)0.0041 (3)0.0131 (3)0.0045 (4)
S100.0448 (5)0.1068 (9)0.1002 (8)0.0087 (5)0.0261 (5)0.0069 (7)
Geometric parameters (Å, º) top
N1—C81.330 (6)C8—C91.322 (8)
N1—C121.370 (6)C8—H80.9300
N1—C71.437 (7)C9—C101.306 (9)
N2—C181.351 (6)C9—H90.9300
N2—C141.356 (6)C10—C111.306 (9)
N2—C131.442 (6)C10—H100.9300
C1—S11.647 (3)C11—C121.389 (8)
C1—S21.716 (4)C11—H110.9300
C1—S31.722 (4)C12—H120.9300
C2—C31.358 (4)C13—H13A0.9600
C2—S41.742 (3)C13—H13B0.9600
C2—S21.751 (3)C13—H13C0.9600
C3—S51.742 (3)C14—C151.319 (7)
C3—S31.748 (3)C14—H140.9300
C4—C51.355 (4)C15—C161.304 (8)
C4—S61.741 (3)C15—H150.9300
C4—S81.747 (3)C16—C171.327 (9)
C5—S71.742 (3)C16—H160.9300
C5—S91.757 (3)C17—C181.353 (8)
C6—S101.655 (3)C17—H170.9300
C6—S91.709 (3)C18—H180.9300
C6—S81.718 (4)Cd1—S62.4947 (9)
C7—H7A0.9600Cd1—S52.4983 (9)
C7—H7B0.9600Cd1—S72.5185 (9)
C7—H7C0.9600Cd1—S42.5252 (9)
C8—N1—C12119.7 (5)C10—C11—H11120.5
C8—N1—C7120.1 (6)C12—C11—H11120.5
C12—N1—C7120.2 (6)N1—C12—C11118.2 (5)
C18—N2—C14118.7 (4)N1—C12—H12120.9
C18—N2—C13119.9 (6)C11—C12—H12120.9
C14—N2—C13121.4 (5)N2—C13—H13A109.5
S1—C1—S2124.5 (2)N2—C13—H13B109.5
S1—C1—S3123.8 (2)H13A—C13—H13B109.5
S2—C1—S3111.67 (18)N2—C13—H13C109.5
C3—C2—S4129.4 (2)H13A—C13—H13C109.5
C3—C2—S2115.3 (2)H13B—C13—H13C109.5
S4—C2—S2115.32 (18)C15—C14—N2120.4 (4)
C2—C3—S5128.9 (2)C15—C14—H14119.8
C2—C3—S3115.1 (2)N2—C14—H14119.8
S5—C3—S3116.02 (18)C16—C15—C14121.1 (6)
C5—C4—S6129.4 (2)C16—C15—H15119.5
C5—C4—S8115.1 (2)C14—C15—H15119.5
S6—C4—S8115.51 (18)C15—C16—C17120.5 (6)
C4—C5—S7129.2 (2)C15—C16—H16119.8
C4—C5—S9115.1 (2)C17—C16—H16119.8
S7—C5—S9115.64 (18)C16—C17—C18120.4 (5)
S10—C6—S9123.8 (2)C16—C17—H17119.8
S10—C6—S8124.1 (2)C18—C17—H17119.8
S9—C6—S8112.03 (17)N2—C18—C17118.9 (5)
N1—C7—H7A109.5N2—C18—H18120.6
N1—C7—H7B109.5C17—C18—H18120.6
H7A—C7—H7B109.5S6—Cd1—S5129.36 (3)
N1—C7—H7C109.5S6—Cd1—S790.57 (3)
H7A—C7—H7C109.5S5—Cd1—S7116.28 (3)
H7B—C7—H7C109.5S6—Cd1—S4116.79 (3)
C9—C8—N1119.8 (6)S5—Cd1—S490.19 (3)
C9—C8—H8120.1S7—Cd1—S4115.98 (3)
N1—C8—H8120.1C1—S2—C298.93 (16)
C10—C9—C8121.6 (7)C1—S3—C399.01 (16)
C10—C9—H9119.2C2—S4—Cd195.06 (11)
C8—C9—H9119.2C3—S5—Cd195.84 (10)
C11—C10—C9121.7 (7)C4—S6—Cd195.47 (10)
C11—C10—H10119.2C5—S7—Cd194.98 (11)
C9—C10—H10119.2C6—S8—C498.94 (15)
C10—C11—C12118.9 (6)C6—S9—C598.76 (16)
S4—C2—C3—S50.5 (5)C2—C3—S3—C11.3 (3)
S2—C2—C3—S5179.59 (19)S5—C3—S3—C1177.93 (19)
S4—C2—C3—S3178.64 (19)C3—C2—S4—Cd15.1 (3)
S2—C2—C3—S30.5 (3)S2—C2—S4—Cd1174.02 (15)
S6—C4—C5—S70.1 (5)S6—Cd1—S4—C2141.30 (11)
S8—C4—C5—S7179.08 (17)S5—Cd1—S4—C25.89 (11)
S6—C4—C5—S9179.51 (18)S7—Cd1—S4—C2113.72 (11)
S8—C4—C5—S91.4 (3)C2—C3—S5—Cd15.8 (3)
C12—N1—C8—C90.2 (6)S3—C3—S5—Cd1173.33 (16)
C7—N1—C8—C9177.9 (5)S6—Cd1—S5—C3131.90 (11)
N1—C8—C9—C102.1 (8)S7—Cd1—S5—C3113.30 (11)
C8—C9—C10—C112.8 (9)S4—Cd1—S5—C36.05 (11)
C9—C10—C11—C121.1 (9)C5—C4—S6—Cd14.2 (3)
C8—N1—C12—C111.8 (6)S8—C4—S6—Cd1174.93 (15)
C7—N1—C12—C11176.3 (4)S5—Cd1—S6—C4130.07 (10)
C10—C11—C12—N11.1 (7)S7—Cd1—S6—C44.57 (10)
C18—N2—C14—C150.1 (7)S4—Cd1—S6—C4115.15 (10)
C13—N2—C14—C15178.1 (5)C4—C5—S7—Cd14.1 (3)
N2—C14—C15—C160.8 (8)S9—C5—S7—Cd1176.35 (14)
C14—C15—C16—C171.1 (9)S6—Cd1—S7—C54.55 (10)
C15—C16—C17—C180.6 (9)S5—Cd1—S7—C5139.96 (10)
C14—N2—C18—C170.6 (6)S4—Cd1—S7—C5115.87 (10)
C13—N2—C18—C17177.6 (4)S10—C6—S8—C4178.0 (2)
C16—C17—C18—N20.2 (8)S9—C6—S8—C42.0 (2)
S1—C1—S2—C2177.5 (2)C5—C4—S8—C60.4 (3)
S3—C1—S2—C22.8 (2)S6—C4—S8—C6178.87 (17)
C3—C2—S2—C12.0 (3)S10—C6—S9—C5177.4 (2)
S4—C2—S2—C1177.22 (18)S8—C6—S9—C52.6 (2)
S1—C1—S3—C3177.7 (2)C4—C5—S9—C62.4 (3)
S2—C1—S3—C32.6 (2)S7—C5—S9—C6177.94 (17)
Hydrogen-bond geometry (Å, º) top
D—H···AD—HH···AD···AD—H···A
C12—H12···S10.932.843.737 (6)161
C14—H14···S100.932.743.650 (5)167
 

Follow Acta Cryst. E
Sign up for e-alerts
Follow Acta Cryst. on Twitter
Follow us on facebook
Sign up for RSS feeds