Literature DB >> 21201369

cis-Bis(2-sulfidopyridine N-oxide)platinum(II).

B Ravindran Durai Nayagam, Samuel Robinson Jebas, Dieter Schollmeyer.   

Abstract

In the crystal structure of the title complex, [Pt(C(5)H(4)NOS)(2)], the Pt atom is coordinated by two O atoms and two S atoms in a cis configuration, forming a distorted square-planar coordination geometry. The mol-ecule exhibits pseudo-C(2v) symmetry and is essentially planar, with a maximum deviation from planarity of 0.0124 (2) Å. The dihedral angle between the two pyridine rings is 5.85 (2)°.

Entities:  

Year:  2008        PMID: 21201369      PMCID: PMC2960410          DOI: 10.1107/S1600536808002006

Source DB:  PubMed          Journal:  Acta Crystallogr Sect E Struct Rep Online        ISSN: 1600-5368


Related literature

For related literature, see: Bovin et al. (1992 ▶); Chen et al. (1991 ▶); Dyksterhouse et al. (2000 ▶); Katsuyuki et al. (1991 ▶); Leonard et al. (1955 ▶); Lobana & Bhatia (1989 ▶); Lydon et al. (1982 ▶); Ohms et al. (1982 ▶); Symons & West (1985 ▶); Zhou et al. (2005 ▶); Shi et al. (1997 ▶).

Experimental

Crystal data

[Pt(C5H4NOS)2] M = 447.39 Monoclinic, a = 6.9832 (3) Å b = 22.3897 (11) Å c = 8.1495 (4) Å β = 113.572 (3)° V = 1167.87 (10) Å3 Z = 4 Mo Kα radiation μ = 12.36 mm−1 T = 193 (2) K 0.27 × 0.22 × 0.08 mm

Data collection

Bruker Kappa APEXII diffractometer Absorption correction: multi-scan (SADABS; Blessing, 1995 ▶, 1997 ▶) T min = 0.051, T max = 0.372 25638 measured reflections 2778 independent reflections 2610 reflections with I > 2σ(I) R int = 0.068

Refinement

R[F 2 > 2σ(F 2)] = 0.054 wR(F 2) = 0.114 S = 1.32 2778 reflections 154 parameters H-atom parameters constrained Δρmax = 1.73 e Å−3 Δρmin = −3.87 e Å−3 Data collection: APEX2 (Bruker, 2006 ▶); cell refinement: APEX2; data reduction: APEX2; program(s) used to solve structure: SHELXS97 (Sheldrick, 2008 ▶); program(s) used to refine structure: SHELXL97 (Sheldrick, 2008 ▶); molecular graphics: ORTEP2 (Farrugia, 1997 ▶); software used to prepare material for publication: SHELXL97. Crystal structure: contains datablocks global, I. DOI: 10.1107/S1600536808002006/wn2232sup1.cif Structure factors: contains datablocks I. DOI: 10.1107/S1600536808002006/wn2232Isup2.hkl Additional supplementary materials: crystallographic information; 3D view; checkCIF report
[Pt(C5H4NOS)2]F000 = 832
Mr = 447.39Dx = 2.545 Mg m3
Monoclinic, P21/nMo Kα radiation λ = 0.71069 Å
Hall symbol: -P 2ynCell parameters from 9973 reflections
a = 6.9832 (3) Åθ = 2.8–28º
b = 22.3897 (11) ŵ = 12.36 mm1
c = 8.1495 (4) ÅT = 193 (2) K
β = 113.572 (3)ºBlock, orange
V = 1167.87 (10) Å30.27 × 0.22 × 0.08 mm
Z = 4
Bruker APEXII Kappa-CCD diffractometerRint = 0.068
CCD scanθmax = 27.9º
Absorption correction: multi-scan(SADABS; Blessing, 1995, 1997)θmin = 1.8º
Tmin = 0.051, Tmax = 0.372h = −9→9
25638 measured reflectionsk = −29→29
2778 independent reflectionsl = −10→10
2610 reflections with I > 2σ(I)
Refinement on F2H-atom parameters constrained
Least-squares matrix: full  w = 1/[σ2(Fo2) + (0.0153P)2 + 17.8973P] where P = (Fo2 + 2Fc2)/3
R[F2 > 2σ(F2)] = 0.054(Δ/σ)max = 0.001
wR(F2) = 0.114Δρmax = 1.73 e Å3
S = 1.32Δρmin = −3.86 e Å3
2778 reflectionsExtinction correction: none
154 parameters
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.
xyzUiso*/Ueq
Pt10.75198 (6)0.117494 (18)0.60862 (6)0.03763 (14)
N10.5870 (13)0.1570 (4)0.2386 (12)0.0373 (18)
C20.5399 (16)0.1976 (5)0.1045 (15)0.042 (2)
H20.57740.23840.13080.05*
C30.4376 (18)0.1791 (6)−0.0694 (17)0.050 (3)
H30.40970.2066−0.1650.059*
C40.3746 (18)0.1195 (6)−0.1053 (16)0.048 (3)
H40.30070.1064−0.22510.058*
C50.4207 (16)0.0803 (5)0.0340 (15)0.042 (2)
H50.37720.03990.01020.05*
C60.5318 (17)0.0990 (5)0.2124 (15)0.039 (2)
O70.6952 (11)0.1788 (3)0.4073 (10)0.0380 (15)
S80.5946 (4)0.05080 (12)0.3916 (4)0.0413 (6)
N90.9639 (13)0.1639 (4)0.9685 (12)0.0378 (19)
C101.0646 (17)0.2052 (5)1.0962 (16)0.042 (2)
H101.08850.24411.06170.051*
C111.1311 (17)0.1915 (5)1.2724 (16)0.044 (2)
H111.19860.22081.36120.053*
C121.0994 (17)0.1342 (5)1.3215 (15)0.043 (2)
H121.1470.12391.44450.051*
C130.9994 (17)0.0921 (5)1.1923 (15)0.042 (2)
H130.97630.0531.22630.051*
C140.9315 (16)0.1069 (5)1.0105 (14)0.038 (2)
O150.8948 (11)0.1822 (3)0.7947 (9)0.0381 (16)
S160.8174 (4)0.05572 (12)0.8401 (4)0.0394 (6)
U11U22U33U12U13U23
Pt10.0364 (2)0.0382 (2)0.0391 (2)0.00055 (17)0.01591 (17)0.00058 (17)
N10.032 (4)0.039 (5)0.042 (5)−0.002 (3)0.017 (4)−0.001 (4)
C20.033 (5)0.049 (6)0.039 (6)0.006 (4)0.009 (4)0.011 (5)
C30.043 (6)0.063 (7)0.046 (7)0.003 (5)0.021 (5)0.013 (6)
C40.040 (6)0.062 (7)0.041 (6)0.001 (5)0.014 (5)0.000 (5)
C50.031 (5)0.056 (7)0.041 (6)−0.003 (5)0.016 (4)−0.003 (5)
C60.037 (5)0.041 (5)0.045 (6)0.001 (4)0.023 (5)0.000 (4)
O70.035 (4)0.043 (4)0.036 (4)−0.003 (3)0.016 (3)−0.002 (3)
S80.0440 (14)0.0404 (13)0.0391 (14)−0.0015 (11)0.0164 (12)0.0009 (11)
N90.032 (4)0.041 (5)0.044 (5)0.002 (3)0.020 (4)0.000 (4)
C100.039 (6)0.039 (5)0.050 (7)−0.001 (4)0.019 (5)−0.003 (5)
C110.037 (6)0.050 (6)0.044 (6)0.000 (5)0.016 (5)−0.009 (5)
C120.039 (6)0.052 (6)0.038 (6)0.003 (5)0.016 (5)−0.001 (5)
C130.042 (6)0.047 (6)0.043 (6)0.004 (5)0.024 (5)0.007 (5)
C140.032 (5)0.044 (6)0.040 (6)0.001 (4)0.017 (4)−0.001 (4)
O150.038 (4)0.042 (4)0.034 (4)0.000 (3)0.014 (3)0.005 (3)
S160.0399 (14)0.0399 (13)0.0381 (14)−0.0016 (10)0.0154 (11)−0.0001 (10)
Pt1—O152.045 (7)N9—C141.364 (13)
Pt1—O72.052 (7)C10—C111.356 (16)
Pt1—S162.234 (3)C11—C121.389 (16)
Pt1—S82.239 (3)C12—C131.376 (16)
N1—C61.348 (13)C13—C141.403 (15)
N1—C21.357 (13)C14—S161.730 (11)
N1—O71.367 (11)C2—H20.9500
C2—C31.372 (16)C3—H30.9500
C3—C41.399 (17)C4—H40.9500
C4—C51.367 (16)C5—H50.9500
C5—C61.410 (15)C10—H100.9500
C6—S81.725 (11)C11—H110.9500
N9—C101.359 (14)C12—H120.9500
N9—O151.363 (11)C13—H130.9500
O15—Pt1—O790.0 (3)C10—N9—C14122.1 (10)
O15—Pt1—S1686.4 (2)O15—N9—C14121.0 (9)
O7—Pt1—S16176.3 (2)C11—C10—N9120.6 (10)
O15—Pt1—S8176.4 (2)C10—C11—C12119.2 (11)
O7—Pt1—S886.4 (2)C13—C12—C11120.2 (11)
S16—Pt1—S897.13 (10)C12—C13—C14120.0 (10)
C6—N1—C2123.8 (10)N9—C14—C13117.8 (10)
C6—N1—O7120.7 (9)N9—C14—S16119.2 (8)
C2—N1—O7115.4 (9)C13—C14—S16122.9 (9)
N1—C2—C3119.2 (11)N9—O15—Pt1115.1 (6)
C2—C3—C4119.6 (11)C14—S16—Pt198.1 (4)
C5—C4—C3119.3 (11)N1—C2—H2120.0
C4—C5—C6121.0 (11)C3—C2—H2120.0
N1—C6—C5117.0 (10)C2—C3—H3120.0
N1—C6—S8120.6 (8)C4—C3—H3120.0
C5—C6—S8122.4 (9)C3—C4—H4120.0
N1—O7—Pt1114.7 (6)C5—C4—H4120.0
C6—S8—Pt197.5 (4)C4—C5—H5119.0
C10—N9—O15116.8 (9)C6—C5—H5120.0
Pt1—O152.045 (7)
Pt1—O72.052 (7)
Pt1—S162.234 (3)
Pt1—S82.239 (3)
O15—Pt1—O790.0 (3)
O15—Pt1—S1686.4 (2)
O7—Pt1—S16176.3 (2)
O15—Pt1—S8176.4 (2)
O7—Pt1—S886.4 (2)
S16—Pt1—S897.13 (10)
  3 in total

1.  A short history of SHELX.

Authors:  George M Sheldrick
Journal:  Acta Crystallogr A       Date:  2007-12-21       Impact factor: 2.290

2.  An empirical correction for absorption anisotropy.

Authors:  R H Blessing
Journal:  Acta Crystallogr A       Date:  1995-01-01       Impact factor: 2.290

3.  cis- and trans-dichloro(3,6-dihydro-1,2-oxazine-N)(dimethyl sulfoxide-S)- platinum(II).

Authors:  R M Dyksterhouse; B A Howell; P J Squattrito
Journal:  Acta Crystallogr C       Date:  2000-01       Impact factor: 1.172

  3 in total

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