Literature DB >> 22058891

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

Kwang Ha1.   

Abstract

The Pt(II) ion in the title complex, [PtBr(2)(C(14)H(10)N(4))], has a slightly distorted square-planar environment defined by the two pyridyl N atoms of the chelating 2,3-di-2-pyridyl-pyrazine ligand and two bromide anions. In the crystal, the pyridyl rings are considerably inclined to the least-squares plane of the PtBr(2)N(2) unit [maximum deviation = 0.064 (2) Å] with dihedral angles of 65.2 (2) and 66.0 (2)°. The nearly planar pyrazine ring [maximum deviation = 0.020 (5) Å] is almost perpendicular to the unit plane with a dihedral angle of 89.2 (2)°. Two independent weak inter-molecular C-H⋯Br hydrogen bonds, both involving the same Br atom as a hydrogen-bond acceptor, give rise to chains running along the a and b axes, forming a layer structure extending parallel to (001). The complexes are stacked in columns along the a axis. When viewed down the b axis, the successive complexes stack in the opposite direction.

Entities:  

Year:  2011        PMID： 22058891      PMCID： PMC3200834          DOI： 10.1107/S160053681103412X

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


Related literature

For an isomer of the title complex, see: Ha (2011 ▶). For crystal structures of the related PtII complexes, see: Granifo et al. (2000 ▶); Cai et al. (2009 ▶).

Experimental

Crystal data

[PtBr2(C14H10N4)] M = 589.17 Monoclinic, a = 8.4989 (12) Å b = 15.348 (2) Å c = 12.0277 (16) Å β = 101.403 (3)° V = 1538.0 (4) Å3 Z = 4 Mo Kα radiation μ = 14.32 mm−1 T = 200 K 0.18 × 0.18 × 0.13 mm

Data collection

Bruker SMART 1000 CCD diffractometer Absorption correction: multi-scan (SADABS; Bruker, 2000 ▶) T min = 0.105, T max = 0.156 10118 measured reflections 3323 independent reflections 2484 reflections with I > 2σ(I) R int = 0.046

Refinement

R[F 2 > 2σ(F 2)] = 0.032 wR(F 2) = 0.067 S = 0.99 3323 reflections 190 parameters H-atom parameters constrained Δρmax = 1.66 e Å−3 Δρmin = −0.84 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) global, I. DOI: 10.1107/S160053681103412X/xu5295sup1.cif Structure factors: contains datablock(s) I. DOI: 10.1107/S160053681103412X/xu5295Isup2.hkl Additional supplementary materials: crystallographic information; 3D view; checkCIF report
[PtBr2(C14H10N4)]F(000) = 1080
Mr = 589.17Dx = 2.544 Mg m−3
Monoclinic, P21/nMo Kα radiation, λ = 0.71073 Å
Hall symbol: -P 2ynCell parameters from 4242 reflections
a = 8.4989 (12) Åθ = 2.7–27.0°
b = 15.348 (2) ŵ = 14.32 mm−1
c = 12.0277 (16) ÅT = 200 K
β = 101.403 (3)°Block, yellow
V = 1538.0 (4) Å30.18 × 0.18 × 0.13 mm
Z = 4
Bruker SMART 1000 CCD diffractometer3323 independent reflections
Radiation source: fine-focus sealed tube2484 reflections with I > 2σ(I)
graphiteRint = 0.046
φ and ω scansθmax = 27.0°, θmin = 2.2°
Absorption correction: multi-scan (SADABS; Bruker, 2000)h = −9→10
Tmin = 0.105, Tmax = 0.156k = −11→19
10118 measured reflectionsl = −13→15
Refinement on F2Primary atom site location: structure-invariant direct methods
Least-squares matrix: fullSecondary atom site location: difference Fourier map
R[F2 > 2σ(F2)] = 0.032Hydrogen site location: inferred from neighbouring sites
wR(F2) = 0.067H-atom parameters constrained
S = 0.99w = 1/[σ2(Fo2) + (0.0237P)2] where P = (Fo2 + 2Fc2)/3
3323 reflections(Δ/σ)max < 0.001
190 parametersΔρmax = 1.66 e Å−3
0 restraintsΔρmin = −0.84 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
Pt10.52128 (3)0.060963 (16)0.31708 (2)0.02517 (9)
Br10.38241 (9)−0.07734 (4)0.30704 (6)0.03471 (18)
Br20.27287 (9)0.14353 (5)0.26735 (6)0.0413 (2)
N10.8219 (7)0.0077 (3)0.0833 (5)0.0314 (14)
N20.7631 (7)0.1861 (4)0.0810 (5)0.0368 (15)
N30.7311 (6)−0.0055 (3)0.3550 (4)0.0238 (12)
N40.6520 (7)0.1724 (3)0.3406 (4)0.0284 (13)
C10.8029 (8)0.0499 (4)0.1780 (5)0.0265 (15)
C20.7701 (8)0.1400 (4)0.1755 (6)0.0304 (16)
C30.7799 (10)0.1437 (5)−0.0117 (6)0.042 (2)
H30.77380.1755−0.08020.051*
C40.8060 (9)0.0552 (5)−0.0126 (6)0.0394 (19)
H40.81280.0272−0.08190.047*
C50.8339 (8)−0.0057 (4)0.2819 (5)0.0231 (14)
C60.9675 (8)−0.0587 (4)0.3011 (6)0.0305 (16)
H61.0386−0.05900.24920.037*
C70.9973 (9)−0.1111 (5)0.3954 (6)0.0392 (18)
H71.0881−0.14850.40870.047*
C80.8944 (8)−0.1088 (4)0.4708 (6)0.0333 (17)
H80.9149−0.14360.53750.040*
C90.7622 (8)−0.0557 (4)0.4483 (5)0.0266 (15)
H90.6909−0.05440.49990.032*
C100.7583 (9)0.1933 (4)0.2760 (5)0.0307 (16)
C110.8525 (9)0.2669 (4)0.3000 (6)0.0397 (19)
H110.92740.28150.25400.048*
C120.8379 (10)0.3187 (5)0.3903 (6)0.043 (2)
H120.90260.36930.40730.052*
C130.7293 (10)0.2969 (5)0.4557 (6)0.044 (2)
H130.71860.33220.51870.053*
C140.6361 (9)0.2243 (4)0.4303 (5)0.0352 (18)
H140.55980.20960.47530.042*
U11U22U33U12U13U23
Pt10.02370 (16)0.02954 (16)0.02362 (14)0.00465 (12)0.00797 (11)0.00200 (11)
Br10.0235 (4)0.0404 (4)0.0414 (4)−0.0026 (3)0.0092 (3)−0.0002 (3)
Br20.0357 (5)0.0529 (5)0.0367 (4)0.0204 (4)0.0108 (3)0.0100 (3)
N10.035 (4)0.029 (3)0.033 (3)0.004 (3)0.014 (3)−0.002 (3)
N20.043 (4)0.035 (4)0.033 (3)0.001 (3)0.009 (3)0.012 (3)
N30.026 (3)0.024 (3)0.021 (3)−0.004 (2)0.003 (2)0.000 (2)
N40.032 (4)0.025 (3)0.028 (3)0.004 (3)0.005 (3)0.003 (2)
C10.019 (4)0.036 (4)0.025 (4)−0.003 (3)0.005 (3)0.001 (3)
C20.023 (4)0.028 (4)0.042 (4)−0.001 (3)0.009 (3)0.004 (3)
C30.058 (6)0.041 (5)0.033 (4)−0.002 (4)0.021 (4)0.013 (3)
C40.042 (5)0.051 (5)0.029 (4)0.006 (4)0.014 (3)0.014 (3)
C50.023 (4)0.027 (4)0.018 (3)−0.002 (3)0.001 (3)0.000 (3)
C60.017 (4)0.035 (4)0.042 (4)0.003 (3)0.012 (3)0.006 (3)
C70.024 (4)0.044 (5)0.050 (5)0.008 (3)0.010 (4)0.013 (4)
C80.030 (4)0.031 (4)0.038 (4)0.004 (3)0.005 (3)0.006 (3)
C90.025 (4)0.031 (4)0.024 (3)−0.006 (3)0.004 (3)0.004 (3)
C100.035 (4)0.022 (4)0.032 (4)−0.001 (3)0.001 (3)0.008 (3)
C110.042 (5)0.032 (4)0.046 (5)0.001 (4)0.012 (4)0.003 (4)
C120.045 (5)0.029 (4)0.048 (5)0.000 (4)−0.009 (4)−0.004 (4)
C130.067 (6)0.030 (5)0.031 (4)0.009 (4)0.002 (4)−0.005 (3)
C140.055 (5)0.030 (4)0.019 (4)0.009 (4)0.007 (3)0.002 (3)
Pt1—N32.026 (5)C4—H40.9500
Pt1—N42.029 (5)C5—C61.380 (8)
Pt1—Br12.4202 (8)C6—C71.373 (9)
Pt1—Br22.4335 (8)C6—H60.9500
N1—C11.347 (8)C7—C81.379 (9)
N1—C41.349 (8)C7—H70.9500
N2—C31.323 (8)C8—C91.371 (9)
N2—C21.329 (8)C8—H80.9500
N3—C91.344 (7)C9—H90.9500
N3—C51.357 (7)C10—C111.381 (9)
N4—C101.341 (8)C11—C121.372 (9)
N4—C141.368 (8)C11—H110.9500
C1—C21.410 (9)C12—C131.367 (10)
C1—C51.493 (8)C12—H120.9500
C2—C101.479 (9)C13—C141.366 (10)
C3—C41.376 (9)C13—H130.9500
C3—H30.9500C14—H140.9500
N3—Pt1—N487.7 (2)C6—C5—C1118.7 (6)
N3—Pt1—Br188.20 (14)C7—C6—C5119.7 (6)
N4—Pt1—Br1174.08 (15)C7—C6—H6120.2
N3—Pt1—Br2178.19 (14)C5—C6—H6120.2
N4—Pt1—Br291.13 (15)C6—C7—C8119.5 (7)
Br1—Pt1—Br293.08 (3)C6—C7—H7120.3
C1—N1—C4117.0 (6)C8—C7—H7120.3
C3—N2—C2117.7 (6)C9—C8—C7119.1 (6)
C9—N3—C5119.6 (5)C9—C8—H8120.5
C9—N3—Pt1119.7 (4)C7—C8—H8120.5
C5—N3—Pt1120.4 (4)N3—C9—C8121.7 (6)
C10—N4—C14120.0 (6)N3—C9—H9119.2
C10—N4—Pt1122.2 (4)C8—C9—H9119.2
C14—N4—Pt1117.6 (5)N4—C10—C11120.2 (6)
N1—C1—C2120.7 (6)N4—C10—C2120.3 (6)
N1—C1—C5113.7 (6)C11—C10—C2119.5 (6)
C2—C1—C5125.4 (6)C12—C11—C10120.0 (7)
N2—C2—C1121.0 (6)C12—C11—H11120.0
N2—C2—C10113.9 (6)C10—C11—H11120.0
C1—C2—C10124.7 (6)C13—C12—C11119.3 (7)
N2—C3—C4122.4 (6)C13—C12—H12120.3
N2—C3—H3118.8C11—C12—H12120.3
C4—C3—H3118.8C14—C13—C12119.9 (7)
N1—C4—C3121.1 (7)C14—C13—H13120.0
N1—C4—H4119.4C12—C13—H13120.0
C3—C4—H4119.4C13—C14—N4120.5 (7)
N3—C5—C6120.5 (6)C13—C14—H14119.8
N3—C5—C1120.8 (6)N4—C14—H14119.8
N4—Pt1—N3—C9115.6 (5)N1—C1—C5—C645.0 (8)
Br1—Pt1—N3—C9−60.1 (4)C2—C1—C5—C6−129.7 (7)
N4—Pt1—N3—C5−70.2 (5)N3—C5—C6—C7−0.6 (10)
Br1—Pt1—N3—C5114.1 (4)C1—C5—C6—C7−179.3 (6)
N3—Pt1—N4—C1062.4 (5)C5—C6—C7—C8−1.1 (11)
Br2—Pt1—N4—C10−116.2 (5)C6—C7—C8—C91.6 (11)
N3—Pt1—N4—C14−113.5 (5)C5—N3—C9—C8−1.2 (9)
Br2—Pt1—N4—C1467.8 (5)Pt1—N3—C9—C8173.0 (5)
C4—N1—C1—C2−0.9 (9)C7—C8—C9—N3−0.4 (10)
C4—N1—C1—C5−175.9 (6)C14—N4—C10—C110.3 (10)
C3—N2—C2—C13.3 (10)Pt1—N4—C10—C11−175.6 (5)
C3—N2—C2—C10177.1 (6)C14—N4—C10—C2−176.9 (6)
N1—C1—C2—N2−2.5 (10)Pt1—N4—C10—C27.3 (9)
C5—C1—C2—N2171.9 (6)N2—C2—C10—N4128.9 (7)
N1—C1—C2—C10−175.6 (6)C1—C2—C10—N4−57.6 (10)
C5—C1—C2—C10−1.2 (11)N2—C2—C10—C11−48.3 (9)
C2—N2—C3—C4−0.8 (11)C1—C2—C10—C11125.3 (7)
C1—N1—C4—C33.3 (10)N4—C10—C11—C120.2 (11)
N2—C3—C4—N1−2.6 (12)C2—C10—C11—C12177.4 (6)
C9—N3—C5—C61.7 (9)C10—C11—C12—C13−0.1 (11)
Pt1—N3—C5—C6−172.5 (5)C11—C12—C13—C14−0.3 (11)
C9—N3—C5—C1−179.6 (6)C12—C13—C14—N40.8 (11)
Pt1—N3—C5—C16.2 (8)C10—N4—C14—C13−0.8 (10)
N1—C1—C5—N3−133.7 (6)Pt1—N4—C14—C13175.3 (5)
C2—C1—C5—N351.5 (9)
D—H···AD—HH···AD···AD—H···A
C6—H6···Br1i0.952.883.524 (6)126.
C11—H11···Br1ii0.952.883.688 (7)143.
Table 1

Selected bond lengths (Å)

Pt1—N32.026 (5)
Pt1—N42.029 (5)
Pt1—Br12.4202 (8)
Pt1—Br22.4335 (8)
Table 2

Hydrogen-bond geometry (Å, °)

D—H⋯AD—HH⋯AD⋯AD—H⋯A
C6—H6⋯Br1i0.952.883.524 (6)126
C11—H11⋯Br1ii0.952.883.688 (7)143

Symmetry codes: (i) ; (ii) .

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

2.  Structural, UV-visible, and electrochemical studies on 2,3-dicyano-5,6-di-2-pyridylpyrazine, [(CN)2Py2Pyz], related species and its complexes [(CN)2Py2PyzMCl2] (M = Pt(II), Pd(II)).

Authors:  Xiaohui Cai; Maria Pia Donzello; Elisa Viola; Corrado Rizzoli; Claudio Ercolani; Karl M Kadish
Journal:  Inorg Chem       Date:  2009-08-03       Impact factor: 5.165

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

Authors:  Kwang Ha
Journal:  Acta Crystallogr Sect E Struct Rep Online       Date:  2011-08-11

4.  Structure validation in chemical crystallography.

Authors:  Anthony L Spek
Journal:  Acta Crystallogr D Biol Crystallogr       Date:  2009-01-20
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  3 in total

1.  (2,3-Di-2-pyridyl-pyrazine-κN,N)diiodidopalladium(II).

Authors:  Kwang Ha
Journal:  Acta Crystallogr Sect E Struct Rep Online       Date:  2011-10-29

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

Authors:  Kwang Ha
Journal:  Acta Crystallogr Sect E Struct Rep Online       Date:  2011-10-29

3.  (2,3-Di-2-pyridyl-pyrazine-κ(2)N(2),N(3))diiodidoplatinum(II).

Authors:  Kwang Ha
Journal:  Acta Crystallogr Sect E Struct Rep Online       Date:  2012-05-31
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