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In the title compound, (C16H36N2)2[Pd(C4N2S2)2], the PdII ion, located on an inversion centre, is coordinated by the four S atoms of the two ligands, giving a coordination geometry very close to ideal square-planar.

Supporting information

cif

Crystallographic Information File (CIF) https://doi.org/10.1107/S1600536807015541/bh2096sup1.cif
Contains datablocks I, global

hkl

Structure factor file (CIF format) https://doi.org/10.1107/S1600536807015541/bh2096Isup2.hkl
Contains datablock I

CCDC reference: 646727

Key indicators

  • Single-crystal X-ray study
  • T = 293 K
  • Mean [sigma](C-C) = 0.010 Å
  • R factor = 0.065
  • wR factor = 0.148
  • Data-to-parameter ratio = 18.0

checkCIF/PLATON results

No syntax errors found



Alert level C PLAT154_ALERT_1_C The su's on the Cell Angles are Equal (x 10000) 200 Deg. PLAT242_ALERT_2_C Check Low Ueq as Compared to Neighbors for C3 PLAT342_ALERT_3_C Low Bond Precision on C-C bonds (x 1000) Ang ... 10 PLAT371_ALERT_2_C Long C(sp2)-C(sp1) Bond C1 - C2 ... 1.43 Ang. PLAT371_ALERT_2_C Long C(sp2)-C(sp1) Bond C3 - C4 ... 1.42 Ang. PLAT790_ALERT_4_C Centre of Gravity not Within Unit Cell: Resd. # 1 C16 H36 N PLAT790_ALERT_4_C Centre of Gravity not Within Unit Cell: Resd. # 2 C8 N4 Pd S4
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 7 ALERT level C = Check and explain 2 ALERT level G = General alerts; check 3 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 1 ALERT type 3 Indicator that the structure quality may be low 2 ALERT type 4 Improvement, methodology, query or suggestion 0 ALERT type 5 Informative message, check

Computing details top

Data collection: SMART (Siemens, 1996); cell refinement: SAINT (Siemens, 1994); data reduction: XPREP (Siemens, 1994); program(s) used to solve structure: SHELXTL (Siemens, 1994); program(s) used to refine structure: SHELXTL; molecular graphics: SHELXTL; software used to prepare material for publication: SHELXTL.

Bis(Tetra-n-butylammonium) bis(1,2-dicyanoethylene-1,2-dithiolato-κ2S,S')palladium(II) top
Crystal data top
(C16H36N2)2[Pd(C4N2S2)2]Z = 1
Mr = 871.74F(000) = 464
Triclinic, P1Dx = 1.215 Mg m3
Hall symbol: -P 1Mo Kα radiation, λ = 0.71073 Å
a = 9.7986 (11) ÅCell parameters from 2635 reflections
b = 10.8084 (12) Åθ = 1.7–25.1°
c = 12.4030 (13) ŵ = 0.60 mm1
α = 85.631 (2)°T = 293 K
β = 87.964 (2)°Prism, green
γ = 65.476 (2)°0.56 × 0.26 × 0.22 mm
V = 1191.6 (2) Å3
Data collection top
Siemens SMART CCD
diffractometer
4181 independent reflections
Radiation source: fine-focus sealed tube3178 reflections with I > 2σ(I)
Graphite monochromatorRint = 0.031
φ and ω scansθmax = 25.1°, θmin = 1.7°
Absorption correction: multi-scan
(SADABS; Sheldrick, 1996)
h = 711
Tmin = 0.713, Tmax = 0.877k = 1212
6213 measured reflectionsl = 1414
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)] = 0.065Hydrogen site location: inferred from neighbouring sites
wR(F2) = 0.148H-atom parameters constrained
S = 1.15 w = 1/[σ2(Fo2) + (0.0377P)2 + 2.3236P]
where P = (Fo2 + 2Fc2)/3
4181 reflections(Δ/σ)max < 0.001
232 parametersΔρmax = 0.47 e Å3
0 restraintsΔρmin = 0.64 e Å3
Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top
xyzUiso*/Ueq
Pd11.50001.00001.50000.0542 (2)
S11.38629 (18)0.77325 (16)1.53277 (14)0.0704 (5)
S21.34516 (17)0.95959 (15)1.35469 (13)0.0628 (4)
N11.3909 (8)0.5371 (7)1.7292 (7)0.132 (3)
N21.2810 (7)1.1325 (7)1.1311 (5)0.0892 (18)
N111.2083 (5)1.0866 (4)0.7782 (3)0.0533 (11)
C11.3412 (7)1.1296 (6)1.2076 (5)0.0664 (16)
C21.4106 (6)1.1202 (6)1.3043 (5)0.0564 (14)
C31.4780 (6)0.7688 (6)1.6478 (5)0.0584 (14)
C41.4313 (7)0.6401 (8)1.6925 (6)0.083 (2)
C111.2052 (7)1.0010 (6)0.8701 (4)0.0610 (15)
H11A1.22801.05890.93670.073*
H11B1.10410.93130.87680.073*
C121.3124 (8)0.9320 (7)0.8594 (6)0.0809 (19)
H12A1.30120.88450.78850.097*
H12B1.41471.00060.86580.097*
C131.2821 (9)0.8301 (7)0.9468 (6)0.091 (2)
H13A1.27610.87421.01670.109*
H13B1.36580.80440.94870.109*
C141.1425 (11)0.7059 (9)0.9283 (8)0.127 (3)
H14A1.12840.64670.98550.191*
H14B1.05900.73040.92690.191*
H14C1.14910.65970.86040.191*
C211.1580 (6)0.9990 (6)0.6738 (4)0.0590 (14)
H21A1.16221.05750.61700.071*
H21B1.22940.95980.65500.071*
C221.0018 (7)0.8838 (7)0.6745 (6)0.084 (2)
H22A0.92830.92240.68230.101*
H22B0.99220.83140.73670.101*
C230.9692 (8)0.7932 (8)0.5774 (6)0.101 (3)
H23A0.98150.84680.51560.122*
H23B1.04290.75470.57050.122*
C240.8150 (8)0.6777 (8)0.5724 (6)0.101 (3)
H24A0.80460.62300.50590.151*
H24B0.80170.62240.63230.151*
H24C0.74060.71400.57580.151*
C311.3672 (6)1.1915 (6)0.7584 (5)0.0572 (14)
H31A1.36541.24090.69680.069*
H31B1.42961.14310.73870.069*
C321.4407 (6)1.2937 (6)0.8512 (5)0.0609 (15)
H32A1.38891.35280.86480.073*
H32B1.43381.24640.91600.073*
C331.6041 (7)1.3785 (7)0.8252 (7)0.090 (2)
H33A1.65801.32070.82160.108*
H33B1.61091.41380.75460.108*
C341.6782 (8)1.4969 (8)0.9084 (7)0.110 (3)
H34A1.78091.54790.88810.165*
H34B1.62601.55520.91170.165*
H34C1.67461.46250.97810.165*
C411.1043 (6)1.1553 (6)0.8100 (5)0.0583 (14)
H41A1.14331.21390.87510.070*
H41B1.00711.08540.82810.070*
C421.0813 (6)1.2396 (6)0.7266 (5)0.0635 (15)
H42A1.17771.29790.69700.076*
H42B1.02101.17960.66780.076*
C431.0041 (7)1.3267 (7)0.7752 (6)0.0759 (18)
H43A1.06521.38700.83350.091*
H43B0.90861.26810.80590.091*
C440.9774 (8)1.4111 (7)0.6932 (6)0.089 (2)
H44A0.92901.46470.72800.133*
H44B1.07171.47040.66340.133*
H44C0.91471.35180.63630.133*
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
Pd10.0468 (4)0.0486 (4)0.0631 (4)0.0165 (3)0.0000 (3)0.0016 (3)
S10.0651 (10)0.0511 (9)0.0857 (12)0.0138 (8)0.0196 (9)0.0021 (8)
S20.0562 (9)0.0532 (9)0.0703 (10)0.0140 (7)0.0094 (8)0.0013 (8)
N10.098 (5)0.087 (5)0.192 (8)0.007 (4)0.044 (5)0.058 (5)
N20.096 (4)0.105 (5)0.061 (4)0.035 (4)0.010 (3)0.003 (3)
N110.048 (2)0.057 (3)0.052 (3)0.020 (2)0.004 (2)0.002 (2)
C10.059 (4)0.067 (4)0.066 (4)0.019 (3)0.003 (3)0.003 (3)
C20.049 (3)0.063 (4)0.058 (4)0.023 (3)0.000 (3)0.005 (3)
C30.050 (3)0.055 (3)0.071 (4)0.021 (3)0.001 (3)0.007 (3)
C40.064 (4)0.075 (5)0.105 (6)0.018 (4)0.022 (4)0.023 (4)
C110.065 (4)0.060 (3)0.051 (3)0.019 (3)0.002 (3)0.001 (3)
C120.078 (4)0.087 (5)0.085 (5)0.040 (4)0.008 (4)0.018 (4)
C130.111 (6)0.075 (5)0.084 (5)0.034 (4)0.009 (4)0.014 (4)
C140.141 (8)0.084 (6)0.138 (8)0.025 (6)0.009 (7)0.019 (6)
C210.065 (4)0.063 (4)0.049 (3)0.029 (3)0.005 (3)0.011 (3)
C220.063 (4)0.091 (5)0.078 (5)0.017 (4)0.005 (3)0.022 (4)
C230.084 (5)0.099 (6)0.093 (6)0.016 (5)0.005 (4)0.025 (5)
C240.081 (5)0.092 (5)0.103 (6)0.016 (4)0.013 (4)0.034 (5)
C310.048 (3)0.062 (3)0.060 (3)0.021 (3)0.006 (3)0.011 (3)
C320.054 (3)0.056 (3)0.068 (4)0.018 (3)0.005 (3)0.001 (3)
C330.056 (4)0.079 (5)0.125 (6)0.019 (4)0.005 (4)0.001 (4)
C340.066 (5)0.085 (5)0.155 (8)0.011 (4)0.021 (5)0.023 (5)
C410.046 (3)0.064 (4)0.061 (3)0.021 (3)0.003 (3)0.009 (3)
C420.057 (3)0.066 (4)0.070 (4)0.029 (3)0.004 (3)0.008 (3)
C430.062 (4)0.071 (4)0.096 (5)0.032 (3)0.006 (4)0.011 (4)
C440.080 (5)0.080 (5)0.115 (6)0.043 (4)0.013 (4)0.002 (4)
Geometric parameters (Å, º) top
Pd1—S12.2947 (16)C22—H22A0.9700
Pd1—S1i2.2947 (16)C22—H22B0.9700
Pd1—S2i2.2945 (15)C23—C241.508 (9)
Pd1—S22.2945 (16)C23—H23A0.9700
S1—C31.727 (6)C23—H23B0.9700
S2—C21.740 (6)C24—H24A0.9600
N1—C41.141 (8)C24—H24B0.9600
N2—C11.144 (8)C24—H24C0.9600
N11—C211.512 (6)C31—C321.506 (8)
N11—C111.514 (7)C31—H31A0.9700
N11—C411.518 (7)C31—H31B0.9700
N11—C311.524 (6)C32—C331.516 (8)
C1—C21.431 (9)C32—H32A0.9700
C2—C3i1.355 (8)C32—H32B0.9700
C3—C2i1.355 (8)C33—C341.521 (10)
C3—C41.422 (9)C33—H33A0.9700
C11—C121.517 (8)C33—H33B0.9700
C11—H11A0.9700C34—H34A0.9600
C11—H11B0.9700C34—H34B0.9600
C12—C131.538 (9)C34—H34C0.9600
C12—H12A0.9700C41—C421.511 (8)
C12—H12B0.9700C41—H41A0.9700
C13—C141.476 (10)C41—H41B0.9700
C13—H13A0.9700C42—C431.515 (8)
C13—H13B0.9700C42—H42A0.9700
C14—H14A0.9600C42—H42B0.9700
C14—H14B0.9600C43—C441.515 (9)
C14—H14C0.9600C43—H43A0.9700
C21—C221.521 (8)C43—H43B0.9700
C21—H21A0.9700C44—H44A0.9600
C21—H21B0.9700C44—H44B0.9600
C22—C231.449 (9)C44—H44C0.9600
S2i—Pd1—S2180.000 (1)C22—C23—H23A108.4
S2i—Pd1—S190.10 (6)C24—C23—H23A108.4
S2—Pd1—S189.90 (6)C22—C23—H23B108.4
S2i—Pd1—S1i89.90 (6)C24—C23—H23B108.4
S2—Pd1—S1i90.10 (6)H23A—C23—H23B107.4
S1—Pd1—S1i180.000 (1)C23—C24—H24A109.5
C3—S1—Pd1101.8 (2)C23—C24—H24B109.5
C2—S2—Pd1101.8 (2)H24A—C24—H24B109.5
C21—N11—C11110.9 (4)C23—C24—H24C109.5
C21—N11—C41110.9 (4)H24A—C24—H24C109.5
C11—N11—C41106.9 (4)H24B—C24—H24C109.5
C21—N11—C31106.4 (4)C32—C31—N11116.3 (4)
C11—N11—C31110.7 (4)C32—C31—H31A108.2
C41—N11—C31111.1 (4)N11—C31—H31A108.2
N2—C1—C2177.3 (7)C32—C31—H31B108.2
C3i—C2—C1121.0 (5)N11—C31—H31B108.2
C3i—C2—S2122.7 (4)H31A—C31—H31B107.4
C1—C2—S2116.3 (4)C31—C32—C33110.2 (5)
C2i—C3—C4119.8 (6)C31—C32—H32A109.6
C2i—C3—S1123.5 (5)C33—C32—H32A109.6
C4—C3—S1116.7 (5)C31—C32—H32B109.6
N1—C4—C3178.4 (9)C33—C32—H32B109.6
N11—C11—C12115.8 (5)H32A—C32—H32B108.1
N11—C11—H11A108.3C32—C33—C34112.6 (6)
C12—C11—H11A108.3C32—C33—H33A109.1
N11—C11—H11B108.3C34—C33—H33A109.1
C12—C11—H11B108.3C32—C33—H33B109.1
H11A—C11—H11B107.4C34—C33—H33B109.1
C11—C12—C13111.3 (6)H33A—C33—H33B107.8
C11—C12—H12A109.4C33—C34—H34A109.5
C13—C12—H12A109.4C33—C34—H34B109.5
C11—C12—H12B109.4H34A—C34—H34B109.5
C13—C12—H12B109.4C33—C34—H34C109.5
H12A—C12—H12B108.0H34A—C34—H34C109.5
C14—C13—C12113.0 (7)H34B—C34—H34C109.5
C14—C13—H13A109.0C42—C41—N11116.3 (4)
C12—C13—H13A109.0C42—C41—H41A108.2
C14—C13—H13B109.0N11—C41—H41A108.2
C12—C13—H13B109.0C42—C41—H41B108.2
H13A—C13—H13B107.8N11—C41—H41B108.2
C13—C14—H14A109.5H41A—C41—H41B107.4
C13—C14—H14B109.5C41—C42—C43111.3 (5)
H14A—C14—H14B109.5C41—C42—H42A109.4
C13—C14—H14C109.5C43—C42—H42A109.4
H14A—C14—H14C109.5C41—C42—H42B109.4
H14B—C14—H14C109.5C43—C42—H42B109.4
N11—C21—C22116.1 (5)H42A—C42—H42B108.0
N11—C21—H21A108.3C44—C43—C42112.7 (6)
C22—C21—H21A108.3C44—C43—H43A109.1
N11—C21—H21B108.3C42—C43—H43A109.1
C22—C21—H21B108.3C44—C43—H43B109.1
H21A—C21—H21B107.4C42—C43—H43B109.1
C23—C22—C21113.0 (5)H43A—C43—H43B107.8
C23—C22—H22A109.0C43—C44—H44A109.5
C21—C22—H22A109.0C43—C44—H44B109.5
C23—C22—H22B109.0H44A—C44—H44B109.5
C21—C22—H22B109.0C43—C44—H44C109.5
H22A—C22—H22B107.8H44A—C44—H44C109.5
C22—C23—C24115.7 (6)H44B—C44—H44C109.5
Symmetry code: (i) x+3, y2, z+3.
 

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