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In the title compound, [Pt(C5H5NS)4]Cl2, the PtII ion is located at a crystallographic inversion centre, with each S-donor ligand in its thione tautomeric form [Pt—S = 2.3439 (7) and 2.3444 (7) Å]. The Cl ion positioned at each axial site of the PtII ion [Pt...Cl = 3.5171 (8) Å] is hydrogen-bonded to the N—H units of the ligands [Cl...N = 3.103 (3) and 3.125 (3) Å].

Supporting information

cif

Crystallographic Information File (CIF) https://doi.org/10.1107/S1600536805020209/ob6541sup1.cif
Contains datablocks global, I

hkl

Structure factor file (CIF format) https://doi.org/10.1107/S1600536805020209/ob6541Isup2.hkl
Contains datablock I

CCDC reference: 282555

Key indicators

  • Single-crystal X-ray study
  • T = 296 K
  • Mean [sigma](C-C) = 0.006 Å
  • R factor = 0.019
  • wR factor = 0.041
  • Data-to-parameter ratio = 18.5

checkCIF/PLATON results

No syntax errors found



Alert level C PLAT042_ALERT_1_C Calc. and Rep. MoietyFormula Strings Differ .... ? PLAT220_ALERT_2_C Large Non-Solvent C Ueq(max)/Ueq(min) ... 2.75 Ratio PLAT241_ALERT_2_C Check High Ueq as Compared to Neighbors for C9
0 ALERT level A = In general: serious problem 0 ALERT level B = Potentially serious problem 3 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 2 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 0 ALERT type 4 Improvement, methodology, query or suggestion

Computing details top

Data collection: SMART (Bruker, 2001); cell refinement: SAINT (Bruker, 2001); data reduction: SAINT; program(s) used to solve structure: SHELXS97 (Sheldrick, 1997); program(s) used to refine structure: SHELXL97 (Sheldrick, 1997); molecular graphics: KENX (Sakai, 2004); software used to prepare material for publication: SHELXL97, TEXSAN (Molecular Structure Corporation, 2001), KENX and ORTEP (Johnson, 1976).

Tetrakis(2-thiopyridone)platinum(II) dichloride top
Crystal data top
[Pt(C5H5NS)4]Cl2Z = 1
Mr = 710.63F(000) = 344
Triclinic, P1? # Insert any comments here.
Hall symbol: -P 1Dx = 1.837 Mg m3
a = 8.3372 (8) ÅMo Kα radiation, λ = 0.71073 Å
b = 9.0754 (8) ÅCell parameters from 5806 reflections
c = 10.1261 (9) Åθ = 2.4–28.2°
α = 99.709 (1)°µ = 6.01 mm1
β = 114.142 (1)°T = 296 K
γ = 104.871 (1)°Plate, yellow
V = 642.4 (1) Å30.44 × 0.23 × 0.11 mm
Data collection top
Bruker SMART APEX CCD area-detector
diffractometer
2632 independent reflections
Radiation source: fine-focus sealed tube2629 reflections with I > 2σ(I)
Graphite monochromatorRint = 0.058
Detector resolution: 8.366 pixels mm-1θmax = 26.4°, θmin = 2.3°
ω scansh = 1010
Absorption correction: gaussian
(XPREP in SAINT; Bruker, 2001)
k = 1111
Tmin = 0.162, Tmax = 0.535l = 1212
7352 measured reflections
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)] = 0.019Hydrogen site location: inferred from neighbouring sites
wR(F2) = 0.041H-atom parameters constrained
S = 1.02 w = 1/[σ2(Fo2) + (0.0093P)2]
where P = (Fo2 + 2Fc2)/3
2632 reflections(Δ/σ)max = 0.001
142 parametersΔρmax = 0.98 e Å3
0 restraintsΔρmin = 0.70 e Å3
Special details top

Experimental. The first 50 frames were rescanned at the end of data collection to evaluate any possible decay phenomenon. Since it was judged to be negligible, no decay correction was applied to the data.

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.

Mean-plane data from final SHELXL refinement run:-

Least-squares planes (x,y,z in crystal coordinates) and deviations from them (* indicates atom used to define plane)

3.4625 (0.0089) x - 6.8353 (0.0069) y + 5.6127 (0.0101) z = 0.0772 (0.0049)

* 0.0021 (0.0018) N1 * -0.0020 (0.0019) C1 * 0.0002 (0.0022) C2 * 0.0014 (0.0025) C3 * -0.0014 (0.0025) C4 * -0.0004 (0.0021) C5 0.0223 (0.0036) S1

Rms deviation of fitted atoms = 0.0014

7.7545 (0.0060) x + 0.5896 (0.0174) y - 3.0822 (0.0194) z = 0.3065 (0.0082)

Angle to previous plane (with approximate e.s.d.) = 72.94 (0.13)

* 0.0028 (0.0028) N2 * -0.0078 (0.0025) C6 * 0.0051 (0.0030) C7 * 0.0025 (0.0040) C8 * -0.0077 (0.0045) C9 * 0.0050 (0.0039) C10 - 0.0495 (0.0056) S2

Rms deviation of fitted atoms = 0.0055

1.3052 (0.0026) x + 2.5585 (0.0028) y + 6.5637 (0.0026) z = 0.0000 (0.0000)

Angle to previous plane (with approximate e.s.d.) = 64.71 (0.14)

* 0.0000 (0.0000) Pt1 * 0.0000 (0.0000) S1 * 0.0000 (0.0000) S2 3.2811 (0.0009) Cl1

Rms deviation of fitted atoms = 0.0000

3.4625 (0.0089) x - 6.8353 (0.0069) y + 5.6127 (0.0101) z = 0.0772 (0.0049)

Angle to previous plane (with approximate e.s.d.) = 65.47 (0.07)

* 0.0021 (0.0018) N1 * -0.0020 (0.0019) C1 * 0.0002 (0.0022) C2 * 0.0014 (0.0025) C3 * -0.0014 (0.0025) C4 * -0.0004 (0.0021) C5 0.0223 (0.0036) S1

Rms deviation of fitted atoms = 0.0014

3.4625 (0.0089) x - 6.8353 (0.0069) y + 5.6127 (0.0101) z = 0.0772 (0.0049)

Angle to previous plane (with approximate e.s.d.) = 0.00 (1/5)

* 0.0021 (0.0018) N1 * -0.0020 (0.0019) C1 * 0.0002 (0.0022) C2 * 0.0014 (0.0025) C3 * -0.0014 (0.0025) C4 * -0.0004 (0.0021) C5 - 3.5292 (0.0038) N1_$12 - 3.5251 (0.0036) C1_$12 - 3.5273 (0.0036) C2_$12 - 3.5284 (0.0042) C3_$12 - 3.5257 (0.0039) C4_$12 - 3.5267 (0.0036) C5_$12

Rms deviation of fitted atoms = 0.0014

1.3052 (0.0026) x + 2.5585 (0.0028) y + 6.5637 (0.0026) z = 0.0000 (0.0000)

Angle to previous plane (with approximate e.s.d.) = 65.47 (0.07)

* 0.0000 (0.0000) Pt1 * 0.0000 (0.0000) S1 * 0.0000 (0.0000) S2 3.2811 (0.0009) Cl1

Rms deviation of fitted atoms = 0.0000

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
Pt10.00000.00000.00000.03305 (6)
Cl10.17941 (12)0.29805 (9)0.34802 (8)0.05307 (18)
S10.24113 (10)0.05168 (9)0.06809 (9)0.04593 (17)
S20.07700 (11)0.21624 (9)0.06898 (8)0.04473 (17)
N10.4062 (3)0.3311 (3)0.1668 (3)0.0405 (5)
N20.1851 (4)0.0406 (3)0.3576 (3)0.0514 (6)
C10.4119 (4)0.2379 (3)0.0490 (3)0.0370 (6)
C20.5701 (4)0.2994 (4)0.0268 (3)0.0474 (7)
C30.7081 (5)0.4465 (5)0.1209 (4)0.0612 (9)
C40.6949 (5)0.5379 (4)0.2399 (4)0.0594 (8)
C50.5418 (4)0.4770 (4)0.2603 (3)0.0488 (7)
C60.1565 (4)0.1816 (4)0.2622 (3)0.0425 (6)
C70.1934 (5)0.3030 (4)0.3276 (4)0.0562 (8)
C80.2521 (8)0.2753 (6)0.4813 (5)0.0891 (15)
C90.2762 (9)0.1311 (7)0.5728 (5)0.1019 (19)
C100.2438 (7)0.0146 (6)0.5094 (4)0.0817 (14)
H1A0.31190.29590.18280.049*
H2A0.16520.03530.32020.062*
H20.58070.24030.05170.057*
H30.81140.48570.10540.073*
H40.78780.63730.30320.071*
H50.53010.53530.33840.059*
H70.17830.40040.26770.067*
H80.27590.35530.52420.107*
H90.31390.11450.67590.122*
H100.26160.08370.56980.098*
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
Pt10.03738 (9)0.02724 (8)0.03740 (9)0.01067 (6)0.02166 (7)0.00813 (6)
Cl10.0765 (5)0.0351 (4)0.0506 (4)0.0155 (4)0.0387 (4)0.0055 (3)
S10.0480 (4)0.0348 (4)0.0587 (4)0.0094 (3)0.0356 (4)0.0045 (3)
S20.0606 (4)0.0380 (4)0.0487 (4)0.0256 (4)0.0324 (4)0.0158 (3)
N10.0403 (12)0.0414 (15)0.0420 (12)0.0137 (11)0.0221 (10)0.0128 (10)
N20.0656 (16)0.0391 (15)0.0465 (14)0.0222 (13)0.0226 (13)0.0117 (11)
C10.0383 (14)0.0358 (16)0.0414 (14)0.0154 (12)0.0209 (12)0.0139 (12)
C20.0459 (16)0.0466 (19)0.0544 (17)0.0145 (14)0.0305 (14)0.0127 (14)
C30.0457 (17)0.058 (2)0.073 (2)0.0047 (16)0.0334 (17)0.0136 (18)
C40.0495 (18)0.044 (2)0.064 (2)0.0026 (15)0.0214 (16)0.0051 (15)
C50.0530 (17)0.0437 (19)0.0410 (15)0.0152 (15)0.0177 (14)0.0078 (13)
C60.0410 (14)0.0375 (17)0.0508 (16)0.0151 (13)0.0225 (13)0.0149 (13)
C70.064 (2)0.045 (2)0.0583 (19)0.0278 (17)0.0221 (17)0.0190 (15)
C80.127 (4)0.078 (3)0.065 (2)0.056 (3)0.031 (3)0.038 (2)
C90.159 (5)0.098 (4)0.051 (2)0.070 (4)0.036 (3)0.030 (2)
C100.120 (4)0.068 (3)0.052 (2)0.046 (3)0.032 (2)0.0115 (19)
Geometric parameters (Å, º) top
Pt1—S22.3439 (7)C6—C71.414 (4)
Pt1—S2i2.3439 (7)C7—C81.381 (5)
Pt1—S12.3444 (7)C8—C91.384 (6)
Pt1—S1i2.3444 (7)C9—C101.356 (6)
S1—C11.731 (3)N1—H1A0.8600
S2—C61.729 (3)N2—H2A0.8600
N1—C51.364 (4)C2—H20.9300
N1—C11.367 (4)C3—H30.9300
N2—C101.365 (4)C4—H40.9300
N2—C61.366 (4)C5—H50.9300
C1—C21.417 (4)C7—H70.9300
C2—C31.379 (5)C8—H80.9300
C3—C41.404 (5)C9—H90.9300
C4—C51.367 (5)C10—H100.9300
C2···C4ii3.534 (4)C4···C2ii3.534 (4)
S2—Pt1—S2i180.00 (4)C4—C3—H3119.6
S2—Pt1—S188.47 (3)C5—C4—C3118.2 (3)
S2i—Pt1—S191.53 (3)C5—C4—H4120.9
S2—Pt1—S1i91.53 (3)C3—C4—H4120.9
S2i—Pt1—S1i88.47 (3)N1—C5—C4120.5 (3)
S1—Pt1—S1i180.00 (5)N1—C5—H5119.8
C1—S1—Pt1109.05 (9)C4—C5—H5119.8
C6—S2—Pt1109.67 (10)N2—C6—C7117.1 (3)
C5—N1—C1123.6 (3)N2—C6—S2123.0 (2)
C5—N1—H1A118.2C7—C6—S2119.9 (2)
C1—N1—H1A118.2C8—C7—C6119.3 (3)
C10—N2—C6123.0 (3)C8—C7—H7120.4
C10—N2—H2A118.5C6—C7—H7120.4
C6—N2—H2A118.5C7—C8—C9121.4 (3)
N1—C1—C2116.6 (3)C7—C8—H8119.3
N1—C1—S1123.5 (2)C9—C8—H8119.3
C2—C1—S1119.9 (2)C10—C9—C8118.8 (4)
C3—C2—C1120.3 (3)C10—C9—H9120.6
C3—C2—H2119.9C8—C9—H9120.6
C1—C2—H2119.9C9—C10—N2120.4 (4)
C2—C3—C4120.9 (3)C9—C10—H10119.8
C2—C3—H3119.6N2—C10—H10119.8
S2—Pt1—S1—C1116.25 (10)C1—N1—C5—C40.3 (4)
S2i—Pt1—S1—C163.75 (10)C3—C4—C5—N10.1 (5)
S1—Pt1—S2—C6116.23 (11)C10—N2—C6—C71.0 (5)
S1i—Pt1—S2—C663.77 (11)C10—N2—C6—S2178.5 (3)
C5—N1—C1—C20.4 (4)Pt1—S2—C6—N25.8 (3)
C5—N1—C1—S1179.2 (2)Pt1—S2—C6—C7173.6 (2)
Pt1—S1—C1—N13.6 (2)N2—C6—C7—C81.2 (5)
Pt1—S1—C1—C2177.71 (19)S2—C6—C7—C8178.3 (3)
N1—C1—C2—C30.2 (4)C6—C7—C8—C90.2 (8)
S1—C1—C2—C3179.0 (2)C7—C8—C9—C101.0 (10)
C1—C2—C3—C40.1 (5)C8—C9—C10—N21.2 (9)
C2—C3—C4—C50.2 (5)C6—N2—C10—C90.2 (7)
Symmetry codes: (i) x, y, z; (ii) x+1, y+1, z.
Hydrogen-bond geometry (Å, º) top
D—H···AD—HH···AD···AD—H···A
N1—H1A···Cl10.862.353.125 (3)150
N2—H2A···Cl10.862.323.103 (3)152
 

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