Literature DB >> 21201599

Bis(2,6-dimethyl-pyridinium) hexa-chlorido-platinate(IV).

Vahid Amani, Rahmatollah Rahimi, Hamid Reza Khavasi.

Abstract

The asymmetric unit of the title compound, (C(7)H(10)N)(2)[PtCl(6)], contains one independent protonated 2,6-dimethyl-pyridinium cation and half of a centrosymmetric [PtCl(6)](2-) anion. The Pt atom has an octa-hedral coordination. In the crystal structure, inter-molecular N-H⋯Cl and C-H⋯Cl hydrogen bonds result in the formation of a supra-molecular structure. There is a π-π contact between the pyridine rings [centroid-centroid distance = 4.235 (1) Å].

Entities: Chemical Disease Gene Species

Year: 2008 PMID： 21201599 PMCID： PMC2960473 DOI： 10.1107/S1600536808025257

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

Related literature

For related literature, see: Abedi et al. (2008 ▶); Bencini et al. (1992 ▶); Bokach et al. (2003 ▶); Bowmaker et al. (1998 ▶); Ciccarese et al. (1998 ▶); Delafontaine et al. (1987 ▶); Effendy et al. (2006 ▶); Hasan et al. (2001 ▶); Hojjat Kashani et al. (2008 ▶); Hu et al. (2003 ▶); Jin et al. (2000 ▶, 2003 ▶, 2006 ▶); Juan et al. (1998 ▶); Kansikas et al. (1994 ▶); Li & Liu (2003 ▶); Rafizadeh et al. (2006 ▶); Terzis & Mentzafos (1983 ▶); Yousefi, Amani & Khavasi (2007 ▶); Yousefi, Ahmadi et al. (2007 ▶); Yousefi et al. (2007a ▶,b ▶); Zordan & Brammer (2004 ▶); Zordan et al. (2005 ▶).

Experimental

Crystal data

(C7H10N)2[PtCl6] M = 624.10 Monoclinic, a = 9.9142 (12) Å b = 9.6031 (10) Å c = 11.3305 (14) Å β = 107.117 (10)° V = 1031.0 (2) Å3 Z = 2 Mo Kα radiation μ = 7.58 mm−1 T = 298 (2) K 0.48 × 0.45 × 0.38 mm

Data collection

Bruker SMART CCD area-detector diffractometer Absorption correction: numerical (X-SHAPE and X-RED; Stoe & Cie, 2005 ▶)T min = 0.41, T max = 0.60 2756 measured reflections 2756 independent reflections 2387 reflections with I > 2σ(I)

Refinement

R[F 2 > 2σ(F 2)] = 0.069 wR(F 2) = 0.189 S = 1.10 2756 reflections 111 parameters H atoms treated by a mixture of independent and constrained refinement Δρmax = 1.82 e Å−3 Δρmin = −1.09 e Å−3 Data collection: SMART (Bruker, 1998 ▶); cell refinement: SAINT (Bruker, 1998 ▶); data reduction: SAINT; program(s) used to solve structure: SHELXTL (Sheldrick, 2008 ▶); program(s) used to refine structure: SHELXTL; molecular graphics: ORTEP-3 for Windows (Farrugia, 1997 ▶); software used to prepare material for publication: WinGX (Farrugia, 1999 ▶). Crystal structure: contains datablocks I, global. DOI: 10.1107/S1600536808025257/hk2508sup1.cif Structure factors: contains datablocks I. DOI: 10.1107/S1600536808025257/hk2508Isup2.hkl Additional supplementary materials: crystallographic information; 3D view; checkCIF report

(C₇H₁₀N)₂[PtCl₆]	F₀₀₀ = 596
M_r = 624.10	D_x = 2.010 Mg m⁻³
Monoclinic, P2₁/n	Mo Kα radiation λ = 0.71073 Å
Hall symbol: -P 2yn	Cell parameters from 1071 reflections
a = 9.9142 (12) Å	θ = 2.4–29.1º
b = 9.6031 (10) Å	µ = 7.58 mm⁻¹
c = 11.3305 (14) Å	T = 298 (2) K
β = 107.117 (10)º	Prism, orange
V = 1031.0 (2) Å³	0.48 × 0.45 × 0.38 mm
Z = 2

Bruker SMART CCD area-detector diffractometer	2756 independent reflections
Radiation source: fine-focus sealed tube	2387 reflections with I > 2σ(I)
Monochromator: graphite	R_int = 0.094
T = 298(2) K	θ_max = 29.1º
φ and ω scans	θ_min = 2.4º
Absorption correction: numerical(X-SHAPE and X-RED; Stoe & Cie, 2005)	h = −13→13
T_min = 0.41, T_max = 0.60	k = −12→13
2756 measured reflections	l = −15→15

Refinement on F²	Hydrogen site location: inferred from neighbouring sites
Least-squares matrix: full	H atoms treated by a mixture of independent and constrained refinement
R[F² > 2σ(F²)] = 0.069	w = 1/[σ²(F_o²) + (0.1499P)² + 0.5352P] where P = (F_o² + 2F_c²)/3
wR(F²) = 0.189	(Δ/σ)_max = 0.019
S = 1.10	Δρ_max = 1.82 e Å⁻³
2756 reflections	Δρ_min = −1.09 e Å⁻³
111 parameters	Extinction correction: SHELXTL (Sheldrick, 2008), Fc^*=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4
Primary atom site location: structure-invariant direct methods	Extinction coefficient: 0.029 (3)
Secondary atom site location: difference Fourier map

Experimental. shape of crystal determined optically (X-SHAPE and X-RED; Stoe & Cie, 2005)

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 > 2sigma(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.

	x	y	z	U_iso*/U_eq
Pt1	0.0000	0.5000	0.0000	0.0265 (2)
Cl1	0.14887 (17)	0.56949 (18)	−0.11435 (15)	0.0411 (4)
Cl2	0.0667 (2)	0.6927 (2)	0.12679 (17)	0.0504 (5)
Cl3	−0.18455 (17)	0.6275 (2)	−0.12863 (15)	0.0486 (5)
N1	0.3768 (6)	0.8089 (7)	0.1075 (5)	0.0409 (12)
H1D	0.348 (8)	0.822 (8)	0.170 (7)	0.029 (17)*
C1	0.5069 (11)	0.6118 (11)	0.2190 (9)	0.069 (2)
H1A	0.4229	0.5663	0.2249	0.082*
H1B	0.5475	0.6653	0.2924	0.082*
H1C	0.5735	0.5431	0.2100	0.082*
C2	0.4710 (8)	0.7054 (9)	0.1103 (8)	0.0503 (18)
C3	0.5217 (11)	0.6928 (17)	0.0112 (9)	0.062 (3)
H3	0.5875	0.6241	0.0104	0.074*
C4	0.4756 (12)	0.7819 (14)	−0.0875 (10)	0.076 (3)
H4	0.5090	0.7727	−0.1557	0.091*
C5	0.3790 (11)	0.8854 (11)	−0.0849 (7)	0.064 (3)
H5	0.3482	0.9462	−0.1513	0.077*
C6	0.3278 (8)	0.8987 (8)	0.0163 (7)	0.0472 (16)
C7	0.224 (2)	1.0036 (8)	0.033 (2)	0.071 (5)
H7A	0.1375	0.9938	−0.0325	0.085*
H7B	0.2617	1.0955	0.0302	0.085*
H7C	0.2072	0.9892	0.1109	0.085*

	U¹¹	U²²	U³³	U¹²	U¹³	U²³
C1	0.057 (5)	0.061 (5)	0.073 (6)	0.009 (4)	−0.003 (4)	−0.008 (4)
C2	0.034 (3)	0.053 (4)	0.060 (4)	−0.009 (3)	0.009 (3)	−0.022 (3)
C3	0.046 (4)	0.071 (7)	0.076 (7)	−0.015 (5)	0.028 (4)	−0.031 (5)
C4	0.069 (6)	0.111 (9)	0.061 (5)	−0.038 (6)	0.041 (5)	−0.029 (6)
C5	0.067 (5)	0.086 (6)	0.036 (3)	−0.035 (5)	0.011 (4)	0.001 (4)
C6	0.040 (3)	0.051 (4)	0.044 (3)	−0.013 (3)	0.003 (3)	0.001 (3)
C7	0.060 (10)	0.054 (8)	0.092 (15)	−0.002 (3)	0.011 (10)	0.016 (4)
N1	0.039 (3)	0.053 (3)	0.034 (2)	−0.005 (2)	0.016 (2)	−0.007 (2)
Pt1	0.0244 (3)	0.0322 (3)	0.0223 (3)	−0.00137 (8)	0.00597 (18)	0.00008 (7)
Cl1	0.0382 (8)	0.0514 (9)	0.0389 (8)	−0.0048 (6)	0.0196 (6)	0.0033 (6)
Cl2	0.0563 (10)	0.0491 (9)	0.0502 (9)	−0.0189 (7)	0.0224 (8)	−0.0207 (7)
Cl3	0.0365 (8)	0.0688 (11)	0.0390 (8)	0.0165 (7)	0.0087 (6)	0.0169 (7)

Pt1—Cl2	2.3161 (16)	C2—C3	1.365 (11)
Pt1—Cl2ⁱ	2.3161 (16)	C3—C4	1.374 (19)
Pt1—Cl3ⁱ	2.3239 (16)	C3—H3	0.9300
Pt1—Cl3	2.3239 (16)	C4—C5	1.387 (18)
Pt1—Cl1ⁱ	2.3298 (14)	C4—H4	0.9300
Pt1—Cl1	2.3298 (14)	C5—C6	1.390 (12)
N1—H1D	0.85 (7)	C5—H5	0.9300
C1—C2	1.480 (14)	C6—N1	1.323 (10)
C1—H1A	0.9600	C6—C7	1.49 (2)
C1—H1B	0.9600	C7—H7A	0.9600
C1—H1C	0.9600	C7—H7B	0.9600
C2—N1	1.357 (10)	C7—H7C	0.9600

Cl1ⁱ—Pt1—Cl1	180.00 (8)	H1B—C1—H1C	109.5
Cl2—Pt1—Cl1ⁱ	89.75 (6)	N1—C2—C3	117.6 (10)
Cl2ⁱ—Pt1—Cl1ⁱ	90.25 (6)	N1—C2—C1	117.4 (8)
Cl2—Pt1—Cl1	90.25 (6)	C3—C2—C1	125.0 (10)
Cl2ⁱ—Pt1—Cl1	89.75 (6)	C2—C3—C4	120.0 (12)
Cl2—Pt1—Cl2ⁱ	180.00 (6)	C2—C3—H3	120.0
Cl2—Pt1—Cl3ⁱ	90.20 (8)	C4—C3—H3	120.0
Cl2ⁱ—Pt1—Cl3ⁱ	89.80 (8)	C3—C4—C5	119.7 (9)
Cl2—Pt1—Cl3	89.80 (8)	C3—C4—H4	120.2
Cl2ⁱ—Pt1—Cl3	90.20 (8)	C5—C4—H4	120.2
Cl3ⁱ—Pt1—Cl1ⁱ	90.63 (6)	C4—C5—C6	120.4 (9)
Cl3—Pt1—Cl1ⁱ	89.37 (6)	C4—C5—H5	119.8
Cl3ⁱ—Pt1—Cl3	180.0	C6—C5—H5	119.8
Cl3ⁱ—Pt1—Cl1	89.37 (6)	N1—C6—C5	116.4 (8)
Cl3—Pt1—Cl1	90.63 (6)	N1—C6—C7	116.9 (11)
C6—N1—C2	126.0 (7)	C5—C6—C7	126.7 (12)
C6—N1—H1D	115 (5)	C6—C7—H7A	109.5
C2—N1—H1D	119 (5)	C6—C7—H7B	109.5
C2—C1—H1A	109.5	H7A—C7—H7B	109.5
C2—C1—H1B	109.5	C6—C7—H7C	109.5
H1A—C1—H1B	109.5	H7A—C7—H7C	109.5
C2—C1—H1C	109.5	H7B—C7—H7C	109.5
H1A—C1—H1C	109.5

N1—C2—C3—C4	−1.0 (14)	C4—C5—C6—C7	−179.9 (12)
C1—C2—C3—C4	176.8 (10)	C5—C6—N1—C2	−0.5 (11)
C2—C3—C4—C5	0.9 (15)	C7—C6—N1—C2	179.7 (10)
C3—C4—C5—C6	−0.5 (14)	C3—C2—N1—C6	0.8 (11)
C4—C5—C6—N1	0.3 (11)	C1—C2—N1—C6	−177.1 (7)

D—H···A	D—H	H···A	D···A	D—H···A
N1—H1D···Cl3ⁱⁱ	0.85 (8)	2.45 (8)	3.279 (6)	168 (7)
C1—H1B···Cl1ⁱⁱ	0.96	2.83	3.654 (11)	145
C4—H4···Cl2ⁱⁱⁱ	0.93	2.71	3.616 (11)	165

Pt1—Cl2	2.3161 (16)
Pt1—Cl3	2.3239 (16)
Pt1—Cl1	2.3298 (14)

Cl2—Pt1—Cl1	90.25 (6)
Cl2ⁱ—Pt1—Cl1	89.75 (6)
Cl2—Pt1—Cl3ⁱ	90.20 (8)
Cl2—Pt1—Cl3	89.80 (8)
Cl3—Pt1—Cl1ⁱ	89.37 (6)
Cl3—Pt1—Cl1	90.63 (6)

Symmetry code: (i) .

Table 2

Hydrogen-bond geometry (Å, °)

D—H⋯A	D—H	H⋯A	D⋯A	D—H⋯A
N1—H1D⋯Cl3ⁱⁱ	0.85 (8)	2.45 (8)	3.279 (6)	168 (7)
C1—H1B⋯Cl1ⁱⁱ	0.96	2.83	3.654 (11)	145
C4—H4⋯Cl2ⁱⁱⁱ	0.93	2.71	3.616 (11)	165

Symmetry codes: (ii) ; (iii) .

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