Literature DB >> 21581825

Bis(phenanthridinium) hexa-chloridoplatinate(IV) dimethyl sulfoxide disolvate.

Selvi Karaca, Mehmet Akkurt, Nasser Safari, Vahid Amani, Orhan Büyükgüngör, Anita Abedi.   

Abstract

The asymmetric unit of the title compound, (C(13)H(10)N)(2)[PtCl(6)]·2C(2)H(6)OS, contains one independent protonated phenanthridinium cation, half of a centrosymmetric [PtCl(6)](2-)anion and one dimethyl sulfoxide solvent mol-ecule. Intra-molecular N-H⋯O and inter-molecular C-H⋯Cl hydrogen-bonding inter-actions seem to be effective in the stabilization of the structure.

Entities:  

Year:  2009        PMID： 21581825      PMCID： PMC2968284          DOI： 10.1107/S1600536809002736

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


Related literature

For related literature, see: Abedi et al. (2008 ▶); Amani et al. (2008 ▶); Hasan et al. (2001 ▶); Hu et al. (2003 ▶); Juan et al. (1998 ▶); Kalateh et al. (2008 ▶); Li & Liu (2003 ▶); Terzis & Mentzafos (1983 ▶); Yousefi, Ahmadi et al. (2007 ▶); Yousefi, Teimouri et al. (2007a ▶,b ▶); Zafar et al. (2000 ▶); Zordan & Brammer (2004 ▶); Zordan et al. (2005 ▶).

Experimental

Crystal data

(C13H10N)2[PtCl6]·2C2H6OS M = 924.50 Orthorhombic, a = 24.3695 (11) Å b = 7.9061 (3) Å c = 17.4322 (6) Å V = 3358.6 (2) Å3 Z = 4 Mo Kα radiation μ = 4.81 mm−1 T = 295 (2) K 0.80 × 0.35 × 0.09 mm

Data collection

Stoe IPDS-II diffractometer Absorption correction: integration (X-RED32; Stoe & Cie, 2002 ▶) T min = 0.114, T max = 0.671 33029 measured reflections 3533 independent reflections 2992 reflections with I > 2σ(I) R int = 0.106

Refinement

R[F 2 > 2σ(F 2)] = 0.045 wR(F 2) = 0.096 S = 1.12 3533 reflections 199 parameters H atoms treated by a mixture of independent and constrained refinement Δρmax = 2.20 e Å−3 Δρmin = −1.01 e Å−3 Data collection: X-AREA (Stoe & Cie, 2002 ▶); cell refinement: X-AREA; data reduction: X-RED32 (Stoe & Cie, 2002 ▶); program(s) used to solve structure: SIR97 (Altomare et al., 1999 ▶); program(s) used to refine structure: SHELXL97 (Sheldrick, 2008 ▶); molecular graphics: ORTEP-3 for Windows (Farrugia, 1997 ▶); software used to prepare material for publication: WinGX (Farrugia, 1999 ▶). Crystal structure: contains datablocks global, I. DOI: 10.1107/S1600536809002736/hg2472sup1.cif Structure factors: contains datablocks I. DOI: 10.1107/S1600536809002736/hg2472Isup2.hkl Additional supplementary materials: crystallographic information; 3D view; checkCIF report
(C13H10N)2[PtCl6]·2C2H6OSF(000) = 1816
Mr = 924.50Dx = 1.828 Mg m−3
Orthorhombic, PbcnMo Kα radiation, λ = 0.71073 Å
Hall symbol: -P 2n 2abCell parameters from 46774 reflections
a = 24.3695 (11) Åθ = 1.4–27.3°
b = 7.9061 (3) ŵ = 4.81 mm−1
c = 17.4322 (6) ÅT = 295 K
V = 3358.6 (2) Å3Prism, yellow
Z = 40.80 × 0.35 × 0.09 mm
Stoe IPDS-2 diffractometer3533 independent reflections
Radiation source: sealed X-ray tube, 12 x 0.4 mm long-fine focus2992 reflections with I > 2σ(I)
plane graphiteRint = 0.106
Detector resolution: 6.67 pixels mm-1θmax = 26.8°, θmin = 1.7°
ω scansh = −30→30
Absorption correction: integration (X-RED32; Stoe & Cie, 2002)k = −9→10
Tmin = 0.114, Tmax = 0.671l = −22→20
33029 measured reflections
Refinement on F2Primary atom site location: structure-invariant direct methods
Least-squares matrix: fullSecondary atom site location: difference Fourier map
R[F2 > 2σ(F2)] = 0.045Hydrogen site location: inferred from neighbouring sites
wR(F2) = 0.096H atoms treated by a mixture of independent and constrained refinement
S = 1.12w = 1/[σ2(Fo2) + (0.0192P)2 + 15.6678P] where P = (Fo2 + 2Fc2)/3
3533 reflections(Δ/σ)max = 0.001
199 parametersΔρmax = 2.20 e Å−3
0 restraintsΔρmin = −1.01 e Å−3
Geometry. Bond distances, angles etc. have been calculated using the rounded fractional coordinates. All su's are estimated from the variances of the (full) variance-covariance matrix. The cell e.s.d.'s are taken into account in the estimation of distances, angles and torsion angles
Refinement. Refinement on F2 for ALL reflections except those flagged by the user for potential systematic errors. Weighted R-factors wR and all goodnesses of fit S are based on F2, conventional R-factors R are based on F, with F set to zero for negative F2. The observed criterion of F2 > σ(F2) is used only for calculating -R-factor-obs 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.
xyzUiso*/Ueq
N10.3026 (2)0.7872 (7)0.9147 (3)0.0450 (17)
C10.2284 (2)0.9236 (7)0.8111 (3)0.0380 (17)
C20.1935 (3)0.9962 (8)0.7558 (4)0.051 (2)
C30.2148 (3)1.0700 (9)0.6916 (4)0.057 (3)
C40.2715 (3)1.0779 (9)0.6797 (4)0.059 (3)
C50.3067 (3)1.0107 (9)0.7327 (4)0.052 (2)
C60.2855 (2)0.9333 (8)0.7987 (3)0.0417 (17)
C70.3209 (3)0.8621 (8)0.8539 (4)0.048 (2)
C80.2463 (3)0.7702 (8)0.9301 (3)0.0403 (17)
C90.2309 (3)0.6859 (9)0.9972 (4)0.049 (2)
C100.1764 (3)0.6683 (9)1.0126 (4)0.056 (2)
C110.1378 (3)0.7337 (9)0.9637 (5)0.060 (3)
C120.1527 (3)0.8186 (8)0.8981 (4)0.051 (2)
C130.2085 (2)0.8394 (7)0.8797 (3)0.0383 (17)
S10.42059 (10)0.6422 (3)1.04509 (15)0.0776 (8)
O10.3643 (2)0.7031 (10)1.0318 (4)0.099 (3)
C140.4292 (4)0.6686 (12)1.1452 (5)0.080 (3)
C150.4641 (5)0.7984 (15)1.0151 (6)0.111 (5)
Pt11.000000.67772 (4)0.250000.0358 (1)
Cl10.95124 (7)0.8825 (2)0.18305 (10)0.0533 (5)
Cl21.04739 (6)0.4687 (2)0.31590 (9)0.0509 (5)
Cl31.06735 (7)0.6805 (2)0.15568 (9)0.0525 (5)
HN10.325 (4)0.753 (11)0.948 (5)0.09 (3)*
H20.155700.993800.763000.0610*
H30.191201.115800.655200.0690*
H40.285201.128900.635600.0710*
H50.344401.016400.724900.0620*
H70.358600.869200.846400.0580*
H90.257200.642901.030500.0590*
H100.165300.611501.056600.0670*
H110.100700.720300.975100.0710*
H120.125900.862500.865800.0610*
H14A0.406700.588101.172000.1200*
H14B0.418400.781101.159500.1200*
H14C0.467000.651001.158500.1200*
H15A0.464700.801500.960100.1660*
H15B0.500400.776001.034000.1660*
H15C0.451700.905401.034500.1660*
U11U22U33U12U13U23
N10.030 (3)0.053 (3)0.052 (3)−0.001 (2)−0.008 (2)−0.008 (3)
C10.036 (3)0.037 (3)0.041 (3)0.002 (2)−0.004 (2)−0.009 (2)
C20.043 (3)0.056 (4)0.054 (4)0.007 (3)−0.005 (3)−0.007 (3)
C30.062 (5)0.059 (4)0.051 (4)0.011 (4)−0.007 (4)−0.001 (3)
C40.074 (5)0.057 (4)0.046 (4)0.004 (4)0.013 (4)0.000 (3)
C50.051 (4)0.061 (4)0.044 (4)−0.005 (3)0.008 (3)−0.009 (3)
C60.034 (3)0.047 (3)0.044 (3)0.005 (3)0.001 (3)−0.013 (3)
C70.026 (3)0.057 (4)0.061 (4)0.002 (3)−0.002 (3)−0.012 (3)
C80.036 (3)0.043 (3)0.042 (3)0.002 (3)−0.001 (3)−0.013 (3)
C90.053 (4)0.053 (4)0.042 (3)−0.002 (3)−0.006 (3)−0.004 (3)
C100.059 (4)0.055 (4)0.053 (4)−0.005 (4)0.006 (4)0.000 (3)
C110.040 (4)0.061 (4)0.078 (5)0.000 (3)0.018 (4)0.003 (4)
C120.035 (3)0.054 (4)0.064 (4)0.005 (3)0.002 (3)0.000 (3)
C130.032 (3)0.041 (3)0.042 (3)0.004 (2)−0.001 (2)−0.013 (3)
S10.0602 (13)0.0891 (16)0.0836 (15)−0.0018 (11)−0.0189 (11)−0.0056 (12)
O10.049 (3)0.170 (7)0.077 (4)0.013 (4)−0.021 (3)0.027 (4)
C140.072 (6)0.106 (7)0.062 (5)−0.016 (5)−0.017 (4)0.030 (5)
C150.095 (8)0.166 (11)0.071 (6)−0.051 (8)0.009 (6)−0.023 (7)
Pt10.0247 (2)0.0484 (2)0.0342 (2)0.00000.0005 (1)0.0000
Cl10.0434 (9)0.0616 (9)0.0548 (9)0.0150 (8)−0.0025 (7)0.0076 (8)
Cl20.0390 (8)0.0611 (9)0.0527 (9)0.0007 (7)−0.0073 (7)0.0160 (8)
Cl30.0396 (8)0.0715 (10)0.0463 (8)0.0082 (8)0.0145 (7)0.0067 (8)
Pt1—Cl1i2.3228 (17)C8—C131.386 (8)
Pt1—Cl2i2.3204 (16)C9—C101.362 (10)
Pt1—Cl3i2.3233 (16)C10—C111.371 (11)
Pt1—Cl32.3233 (16)C11—C121.375 (11)
Pt1—Cl12.3228 (17)C12—C131.407 (9)
Pt1—Cl22.3204 (16)C2—H20.9300
S1—C141.770 (9)C3—H30.9300
S1—C151.710 (12)C4—H40.9300
S1—O11.472 (6)C5—H50.9300
N1—C71.293 (9)C7—H70.9300
N1—C81.405 (9)C9—H90.9300
N1—HN10.84 (9)C10—H100.9300
C1—C61.410 (7)C11—H110.9300
C1—C21.408 (9)C12—H120.9300
C1—C131.452 (7)C14—H14B0.9600
C2—C31.365 (10)C14—H14A0.9600
C3—C41.399 (10)C14—H14C0.9600
C4—C51.368 (10)C15—H15C0.9600
C5—C61.402 (9)C15—H15A0.9600
C6—C71.410 (9)C15—H15B0.9600
C8—C91.398 (9)
Cl1···Cl1i3.331 (2)C8···O13.420 (9)
Cl1···Cl2i3.272 (2)C8···C6ix3.598 (8)
Cl1···Cl3i3.265 (2)C8···C9viii3.533 (9)
Cl1···Cl33.284 (2)C8···C1ix3.492 (8)
Cl2···Cl1i3.272 (2)C9···O13.309 (9)
Cl2···Cl3i3.297 (2)C9···C8ix3.533 (9)
Cl2···Cl33.293 (2)C10···Cl3xi3.646 (7)
Cl2···C7ii3.540 (7)C13···C6ix3.511 (8)
Cl2···Cl2i3.258 (2)C2···H122.7400
Cl3···Cl23.293 (2)C2···H14Axii2.9200
Cl3···Cl13.284 (2)C4···H10xii3.0400
Cl3···Cl1i3.265 (2)C10···H3xiii3.0400
Cl3···C10iii3.646 (7)C12···H22.7300
Cl3···Cl2i3.297 (2)HN1···H92.3600
Cl1···H15Aiv2.9100HN1···S13.01 (9)
Cl1···H14Cv2.9400HN1···O11.79 (9)
Cl1···H2vi2.9400H2···H122.1900
Cl1···H7iv3.0500H2···H14Axii2.2900
Cl1···H12vi2.8900H2···C122.7300
Cl2···H7ii2.6800H2···Cl1vi2.9400
Cl2···H15Aii3.1200H3···C10xiv3.0400
Cl2···H5ii3.0800H5···H72.4400
Cl3···H15Cvii3.0700H5···Cl2x3.0800
Cl3···H10iii3.0000H5···Cl3x2.9200
Cl3···H5ii2.9200H7···Cl1xv3.0500
S1···HN13.01 (9)H7···H52.4400
O1···N12.621 (8)H7···Cl2x2.6800
O1···C93.309 (9)H9···O12.6500
O1···C83.420 (9)H9···HN12.3600
O1···HN11.79 (9)H10···C4xvi3.0400
O1···H92.6500H10···Cl3xi3.0000
N1···O12.621 (8)H11···H15Bxvii2.4500
C1···C8viii3.492 (8)H12···C22.7400
C1···C4ix3.566 (9)H12···H22.1900
C2···C7viii3.379 (9)H12···Cl1vi2.8900
C2···C6viii3.573 (9)H14A···C2xvi2.9200
C3···C6viii3.426 (9)H14A···H2xvi2.2900
C3···C5viii3.596 (10)H14B···H15C2.5200
C4···C1viii3.566 (9)H14C···H15B2.5200
C5···C3ix3.596 (10)H14C···Cl1xviii2.9400
C6···C3ix3.426 (9)H15A···Cl2x3.1200
C6···C13viii3.511 (8)H15A···Cl1xv2.9100
C6···C2ix3.573 (9)H15B···H14C2.5200
C6···C8viii3.598 (8)H15B···H11xix2.4500
C7···C2ix3.379 (9)H15C···H14B2.5200
C7···Cl2x3.540 (7)H15C···Cl3xx3.0700
Cl1i—Pt1—Cl289.60 (6)C9—C10—C11120.5 (7)
Cl2—Pt1—Cl2i89.18 (6)C10—C11—C12121.4 (7)
Cl2—Pt1—Cl3i90.46 (5)C11—C12—C13120.1 (6)
Cl1i—Pt1—Cl389.29 (6)C1—C13—C8118.8 (5)
Cl2i—Pt1—Cl390.46 (5)C1—C13—C12124.4 (5)
Cl3—Pt1—Cl3i178.92 (6)C8—C13—C12116.9 (5)
Cl1i—Pt1—Cl2i178.75 (6)C1—C2—H2120.00
Cl1i—Pt1—Cl3i89.96 (6)C3—C2—H2120.00
Cl2i—Pt1—Cl3i90.32 (5)C2—C3—H3119.00
Cl2—Pt1—Cl390.32 (5)C4—C3—H3120.00
Cl1—Pt1—Cl1i91.62 (6)C3—C4—H4120.00
Cl1—Pt1—Cl2178.75 (6)C5—C4—H4120.00
Cl1—Pt1—Cl389.96 (6)C6—C5—H5120.00
Cl1—Pt1—Cl2i89.60 (6)C4—C5—H5120.00
Cl1—Pt1—Cl3i89.29 (6)N1—C7—H7119.00
O1—S1—C14103.1 (4)C6—C7—H7119.00
O1—S1—C15107.1 (5)C8—C9—H9121.00
C14—S1—C1598.2 (5)C10—C9—H9121.00
C7—N1—C8122.5 (5)C11—C10—H10120.00
C8—N1—HN1118 (6)C9—C10—H10120.00
C7—N1—HN1119 (6)C12—C11—H11119.00
C2—C1—C13123.3 (5)C10—C11—H11119.00
C2—C1—C6118.0 (5)C13—C12—H12120.00
C6—C1—C13118.7 (5)C11—C12—H12120.00
C1—C2—C3120.4 (6)S1—C14—H14A109.00
C2—C3—C4121.1 (7)S1—C14—H14B109.00
C3—C4—C5120.1 (7)S1—C14—H14C110.00
C4—C5—C6119.5 (6)H14A—C14—H14B109.00
C1—C6—C5120.9 (5)H14A—C14—H14C110.00
C5—C6—C7120.6 (5)H14B—C14—H14C110.00
C1—C6—C7118.5 (5)S1—C15—H15A109.00
N1—C7—C6122.1 (6)S1—C15—H15B109.00
C9—C8—C13122.7 (6)S1—C15—H15C109.00
N1—C8—C9117.9 (6)H15A—C15—H15B109.00
N1—C8—C13119.4 (5)H15A—C15—H15C110.00
C8—C9—C10118.4 (7)H15B—C15—H15C109.00
C7—N1—C8—C9179.5 (6)C4—C5—C6—C10.1 (10)
C7—N1—C8—C13−1.7 (9)C4—C5—C6—C7179.6 (6)
C8—N1—C7—C60.4 (10)C1—C6—C7—N10.7 (9)
C6—C1—C2—C31.4 (9)C5—C6—C7—N1−178.8 (6)
C13—C1—C2—C3−178.4 (6)N1—C8—C9—C10−179.8 (6)
C13—C1—C6—C7−0.6 (8)C13—C8—C9—C101.4 (10)
C2—C1—C13—C8179.2 (6)N1—C8—C13—C11.7 (8)
C2—C1—C13—C121.0 (9)N1—C8—C13—C12−179.9 (5)
C6—C1—C13—C8−0.6 (8)C9—C8—C13—C1−179.5 (6)
C6—C1—C13—C12−178.8 (6)C9—C8—C13—C12−1.2 (9)
C2—C1—C6—C5−0.9 (9)C8—C9—C10—C11−0.8 (11)
C2—C1—C6—C7179.6 (6)C9—C10—C11—C12−0.1 (11)
C13—C1—C6—C5178.9 (6)C10—C11—C12—C130.3 (11)
C1—C2—C3—C4−1.1 (10)C11—C12—C13—C1178.6 (6)
C2—C3—C4—C50.2 (11)C11—C12—C13—C80.4 (9)
C3—C4—C5—C60.3 (10)
D—H···AD—HH···AD···AD—H···A
N1—HN1···O10.84 (9)1.79 (9)2.621 (8)169 (8)
C7—H7···Cl2x0.932.683.540 (7)154
Table 1

Hydrogen-bond geometry (Å, °)

D—H⋯AD—HH⋯AD⋯AD—H⋯A
N1—HN1⋯O10.84 (9)1.79 (9)2.621 (8)169 (8)
C7—H7⋯Cl2i0.932.683.540 (7)154

Symmetry code: (i) .

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