Literature DB >> 22064814

Dichlorido(2,3-di-2-pyridyl-pyrazine-κN,N)platinum(II).

Kwang Ha1.   

Abstract

The Pt(II) ion in the title complex, [PtCl(2)(C(14)H(10)N(4))], is four-coordinated in a distorted square-planar environment by two N atoms of a chelating 2,3-di-2-pyridyl-pyrazine ligand and two chloride anions. The pyridyl ring coordinated to the Pt(II) atom is inclined slightly to its carrier pyrazine ring [dihedral angle = 13.5 (1)°], whereas the uncoordinated pyridyl ring is inclined considerably to the pyrazine ring [dihedral angle = 54.3 (2)°]. The dihedral angle between the two pyridyl rings is 59.2 (2)°. In the crystal, the complexes are assembled through inter-molecular C-H⋯N and C-H⋯Cl hydrogen bonds, forming a three-dimensional network. Intra-molecular C-H⋯N and C-H⋯Cl hydrogen bonds are also present.

Entities:  

Year:  2011        PMID： 22064814      PMCID： PMC3201246          DOI： 10.1107/S1600536811038906

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


Related literature

For the synthesis and crystal structure of [PtBr2(C14H10N4)], see: Ha (2011 ▶).

Experimental

Crystal data

[PtCl2(C14H10N4)] M = 500.25 Monoclinic, a = 8.894 (5) Å b = 9.711 (5) Å c = 16.461 (9) Å β = 94.429 (11)° V = 1417.5 (13) Å3 Z = 4 Mo Kα radiation μ = 10.27 mm−1 T = 200 K 0.28 × 0.15 × 0.11 mm

Data collection

Bruker SMART 1000 CCD diffractometer Absorption correction: multi-scan (SADABS; Bruker, 2000 ▶) T min = 0.638, T max = 1.000 9749 measured reflections 3370 independent reflections 2756 reflections with I > 2σ(I) R int = 0.029

Refinement

R[F 2 > 2σ(F 2)] = 0.024 wR(F 2) = 0.056 S = 1.02 3370 reflections 190 parameters H-atom parameters constrained Δρmax = 1.83 e Å−3 Δρmin = −0.83 e Å−3 Data collection: SMART (Bruker, 2000 ▶); cell refinement: SAINT (Bruker, 2000 ▶); data reduction: SAINT; program(s) used to solve structure: SHELXS97 (Sheldrick, 2008 ▶); program(s) used to refine structure: SHELXL97 (Sheldrick, 2008 ▶); molecular graphics: ORTEP-3 (Farrugia, 1997 ▶) and PLATON (Spek, 2009 ▶); software used to prepare material for publication: SHELXL97. Crystal structure: contains datablock(s) I. DOI: 10.1107/S1600536811038906/tk2794sup1.cif Structure factors: contains datablock(s) I. DOI: 10.1107/S1600536811038906/tk2794Isup2.hkl Additional supplementary materials: crystallographic information; 3D view; checkCIF report
[PtCl2(C14H10N4)]F(000) = 936
Mr = 500.25Dx = 2.344 Mg m−3
Monoclinic, P21/nMo Kα radiation, λ = 0.71073 Å
Hall symbol: -P 2ynCell parameters from 5943 reflections
a = 8.894 (5) Åθ = 2.4–28.3°
b = 9.711 (5) ŵ = 10.27 mm−1
c = 16.461 (9) ÅT = 200 K
β = 94.429 (11)°Block, yellow
V = 1417.5 (13) Å30.28 × 0.15 × 0.11 mm
Z = 4
Bruker SMART 1000 CCD diffractometer3370 independent reflections
Radiation source: fine-focus sealed tube2756 reflections with I > 2σ(I)
graphiteRint = 0.029
φ and ω scansθmax = 28.4°, θmin = 2.4°
Absorption correction: multi-scan (SADABS; Bruker, 2000)h = −11→11
Tmin = 0.638, Tmax = 1.000k = −12→12
9749 measured reflectionsl = −21→17
Refinement on F2Primary atom site location: structure-invariant direct methods
Least-squares matrix: fullSecondary atom site location: difference Fourier map
R[F2 > 2σ(F2)] = 0.024Hydrogen site location: inferred from neighbouring sites
wR(F2) = 0.056H-atom parameters constrained
S = 1.02w = 1/[σ2(Fo2) + (0.0244P)2] where P = (Fo2 + 2Fc2)/3
3370 reflections(Δ/σ)max = 0.001
190 parametersΔρmax = 1.83 e Å−3
0 restraintsΔρmin = −0.83 e Å−3
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.
xyzUiso*/Ueq
Pt10.364118 (17)0.639554 (16)0.379000 (10)0.02301 (6)
Cl10.44494 (14)0.85790 (11)0.41230 (9)0.0410 (3)
Cl20.12714 (12)0.72595 (12)0.34708 (7)0.0362 (3)
N10.5650 (4)0.5518 (3)0.4076 (2)0.0215 (7)
N20.8366 (4)0.4154 (4)0.4387 (2)0.0260 (8)
N30.3108 (4)0.4412 (4)0.3556 (2)0.0229 (8)
N40.6997 (4)0.1724 (4)0.3059 (2)0.0288 (8)
C10.5721 (4)0.4119 (4)0.3971 (2)0.0207 (8)
C20.7128 (4)0.3476 (4)0.4088 (2)0.0209 (9)
C30.8227 (5)0.5502 (4)0.4532 (3)0.0290 (10)
H30.90750.59920.47690.035*
C40.6902 (5)0.6200 (4)0.4350 (3)0.0259 (9)
H40.68700.71710.44180.031*
C50.4224 (5)0.3480 (4)0.3745 (3)0.0228 (9)
C60.3948 (5)0.2085 (5)0.3771 (3)0.0297 (10)
H60.47290.14540.39360.036*
C70.2471 (5)0.1621 (4)0.3545 (3)0.0300 (10)
H70.22360.06680.35650.036*
C80.1382 (5)0.2558 (5)0.3297 (3)0.0324 (11)
H80.04000.22570.31080.039*
C90.1721 (5)0.3938 (5)0.3324 (3)0.0314 (10)
H90.09450.45820.31730.038*
C100.7422 (4)0.2020 (4)0.3837 (2)0.0216 (9)
C110.8186 (5)0.1104 (4)0.4368 (3)0.0280 (10)
H110.84500.13520.49190.034*
C120.8553 (5)−0.0175 (5)0.4078 (3)0.0349 (11)
H120.9090−0.08190.44240.042*
C130.8132 (5)−0.0508 (5)0.3275 (3)0.0346 (11)
H130.8371−0.13800.30590.041*
C140.7356 (5)0.0462 (5)0.2800 (3)0.0320 (11)
H140.70530.02230.22510.038*
U11U22U33U12U13U23
Pt10.02249 (10)0.02038 (10)0.02625 (10)0.00622 (7)0.00249 (7)0.00141 (7)
Cl10.0379 (7)0.0187 (6)0.0665 (9)0.0050 (5)0.0044 (6)−0.0015 (5)
Cl20.0281 (6)0.0377 (6)0.0421 (7)0.0163 (5)−0.0008 (5)0.0003 (5)
N10.0188 (17)0.0216 (18)0.0243 (18)0.0027 (14)0.0033 (14)0.0017 (14)
N20.0217 (18)0.0280 (19)0.028 (2)0.0017 (16)−0.0002 (15)−0.0016 (16)
N30.0141 (16)0.026 (2)0.0280 (19)0.0044 (15)−0.0008 (14)0.0001 (15)
N40.028 (2)0.031 (2)0.028 (2)0.0018 (16)0.0037 (16)−0.0023 (16)
C10.024 (2)0.018 (2)0.021 (2)0.0021 (17)0.0024 (17)0.0021 (16)
C20.019 (2)0.023 (2)0.021 (2)0.0014 (16)−0.0006 (16)0.0040 (16)
C30.027 (2)0.030 (2)0.030 (2)−0.0040 (19)−0.0012 (19)−0.0042 (19)
C40.024 (2)0.022 (2)0.032 (2)−0.0016 (17)0.0037 (19)−0.0034 (17)
C50.023 (2)0.021 (2)0.025 (2)0.0007 (17)0.0037 (17)0.0001 (17)
C60.024 (2)0.031 (2)0.035 (3)0.001 (2)0.004 (2)0.000 (2)
C70.024 (2)0.028 (3)0.039 (3)−0.0041 (19)0.006 (2)−0.0041 (19)
C80.021 (2)0.034 (3)0.042 (3)−0.0058 (19)0.002 (2)−0.009 (2)
C90.023 (2)0.033 (3)0.038 (3)0.0064 (19)0.000 (2)−0.001 (2)
C100.0161 (19)0.023 (2)0.026 (2)0.0019 (17)0.0046 (17)−0.0011 (17)
C110.024 (2)0.031 (3)0.028 (2)0.0054 (18)−0.0043 (19)−0.0010 (18)
C120.031 (3)0.028 (2)0.045 (3)0.008 (2)−0.006 (2)0.001 (2)
C130.032 (3)0.025 (2)0.048 (3)0.005 (2)0.006 (2)−0.008 (2)
C140.032 (2)0.035 (3)0.029 (3)−0.002 (2)0.002 (2)−0.008 (2)
Pt1—N12.003 (3)C4—H40.9500
Pt1—N32.014 (4)C5—C61.378 (6)
Pt1—Cl22.2916 (15)C6—C71.411 (6)
Pt1—Cl12.2918 (15)C6—H60.9500
N1—C41.344 (5)C7—C81.368 (6)
N1—C11.372 (5)C7—H70.9500
N2—C31.337 (5)C8—C91.374 (6)
N2—C21.343 (5)C8—H80.9500
N3—C91.344 (5)C9—H90.9500
N3—C51.361 (5)C10—C111.388 (6)
N4—C101.339 (5)C11—C121.379 (6)
N4—C141.344 (5)C11—H110.9500
C1—C21.399 (5)C12—C131.383 (7)
C1—C51.489 (6)C12—H120.9500
C2—C101.501 (5)C13—C141.375 (6)
C3—C41.373 (6)C13—H130.9500
C3—H30.9500C14—H140.9500
N1—Pt1—N380.25 (13)C6—C5—C1124.0 (4)
N1—Pt1—Cl2176.21 (10)C5—C6—C7118.0 (4)
N3—Pt1—Cl296.16 (10)C5—C6—H6121.0
N1—Pt1—Cl194.59 (10)C7—C6—H6121.0
N3—Pt1—Cl1174.63 (10)C8—C7—C6119.3 (4)
Cl2—Pt1—Cl188.97 (5)C8—C7—H7120.3
C4—N1—C1119.1 (3)C6—C7—H7120.3
C4—N1—Pt1124.8 (3)C7—C8—C9119.3 (4)
C1—N1—Pt1116.2 (3)C7—C8—H8120.3
C3—N2—C2117.5 (4)C9—C8—H8120.3
C9—N3—C5118.3 (4)N3—C9—C8122.5 (4)
C9—N3—Pt1125.4 (3)N3—C9—H9118.7
C5—N3—Pt1115.8 (3)C8—C9—H9118.7
C10—N4—C14116.3 (4)N4—C10—C11123.6 (4)
N1—C1—C2118.3 (4)N4—C10—C2115.0 (4)
N1—C1—C5113.3 (3)C11—C10—C2121.1 (4)
C2—C1—C5128.4 (4)C12—C11—C10118.4 (4)
N2—C2—C1122.1 (4)C12—C11—H11120.8
N2—C2—C10114.1 (3)C10—C11—H11120.8
C1—C2—C10123.7 (4)C11—C12—C13119.2 (4)
N2—C3—C4122.3 (4)C11—C12—H12120.4
N2—C3—H3118.9C13—C12—H12120.4
C4—C3—H3118.9C14—C13—C12118.1 (4)
N1—C4—C3120.3 (4)C14—C13—H13121.0
N1—C4—H4119.8C12—C13—H13121.0
C3—C4—H4119.8N4—C14—C13124.3 (4)
N3—C5—C6122.1 (4)N4—C14—H14117.8
N3—C5—C1113.7 (3)C13—C14—H14117.8
N3—Pt1—N1—C4−179.3 (3)Pt1—N3—C5—C1−9.1 (4)
Cl1—Pt1—N1—C4−0.8 (3)N1—C1—C5—N310.1 (5)
N3—Pt1—N1—C11.3 (3)C2—C1—C5—N3−170.4 (4)
Cl1—Pt1—N1—C1179.8 (3)N1—C1—C5—C6−166.0 (4)
N1—Pt1—N3—C9176.5 (4)C2—C1—C5—C613.5 (7)
Cl2—Pt1—N3—C9−2.3 (3)N3—C5—C6—C73.8 (6)
N1—Pt1—N3—C54.6 (3)C1—C5—C6—C7179.6 (4)
Cl2—Pt1—N3—C5−174.2 (3)C5—C6—C7—C81.2 (6)
C4—N1—C1—C2−5.3 (5)C6—C7—C8—C9−4.3 (7)
Pt1—N1—C1—C2174.0 (3)C5—N3—C9—C82.2 (6)
C4—N1—C1—C5174.2 (3)Pt1—N3—C9—C8−169.5 (3)
Pt1—N1—C1—C5−6.4 (4)C7—C8—C9—N32.7 (7)
C3—N2—C2—C1−3.5 (6)C14—N4—C10—C11−0.2 (6)
C3—N2—C2—C10172.2 (3)C14—N4—C10—C2174.8 (3)
N1—C1—C2—N27.7 (6)N2—C2—C10—N4−122.6 (4)
C5—C1—C2—N2−171.8 (4)C1—C2—C10—N452.9 (5)
N1—C1—C2—C10−167.5 (4)N2—C2—C10—C1152.5 (5)
C5—C1—C2—C1013.0 (6)C1—C2—C10—C11−131.9 (4)
C2—N2—C3—C4−3.1 (6)N4—C10—C11—C121.1 (6)
C1—N1—C4—C3−0.9 (6)C2—C10—C11—C12−173.6 (4)
Pt1—N1—C4—C3179.8 (3)C10—C11—C12—C13−0.9 (7)
N2—C3—C4—N15.4 (6)C11—C12—C13—C14−0.1 (7)
C9—N3—C5—C6−5.5 (6)C10—N4—C14—C13−0.9 (6)
Pt1—N3—C5—C6167.0 (3)C12—C13—C14—N41.1 (7)
C9—N3—C5—C1178.3 (3)
D—H···AD—HH···AD···AD—H···A
C3—H3···N2i0.952.583.410 (6)147
C4—H4···Cl10.952.573.180 (4)123
C6—H6···Cl1ii0.952.823.477 (5)127
C6—H6···N40.952.583.056 (6)111
C9—H9···Cl20.952.663.261 (5)122
C13—H13···N4iii0.952.613.468 (6)151
Pt1—N12.003 (3)
Pt1—N32.014 (4)
Pt1—Cl22.2916 (15)
Pt1—Cl12.2918 (15)
N1—Pt1—N380.25 (13)
Cl2—Pt1—Cl188.97 (5)
Table 2

Hydrogen-bond geometry (Å, °)

D—H⋯AD—HH⋯AD⋯AD—H⋯A
C3—H3⋯N2i0.952.583.410 (6)147
C4—H4⋯Cl10.952.573.180 (4)123
C6—H6⋯Cl1ii0.952.823.477 (5)127
C6—H6⋯N40.952.583.056 (6)111
C9—H9⋯Cl20.952.663.261 (5)122
C13—H13⋯N4iii0.952.613.468 (6)151

Symmetry codes: (i) ; (ii) ; (iii) .

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