Bis(acetonitrile-κN)(1,10-phenanthroline-κN,N')platinum(II) bis-(perchlorate).

The asymmetric unit of the title compound, [Pt(CH(3)CN)(2)(C(12)H(8)N(2))](ClO(4))(2), contains one half of a cationic Pt(II) complex and pair of half perchlorate anions, one of which is disordered over two sites in a 0.53 (3):0.47 (3) ratio. The complex and anions are disposed about a crystallographic mirror plane parallel to the ac plane passing through the Pt and Cl atoms. In the complex, the Pt(II) ion lies in a distorted square-planar environment defined by four N atoms of the chelating 1,10-phenanthroline ligand and two distinct acetonitrile mol-ecules. The component ions inter-act by means of inter-molecular C-H⋯O hydrogen bonds.

Related literature

For the synthesis of [PtCl2(phen)] (phen = 1,10-phenanthroline), see: Hodges & Rund (1975 ▶). For the crystal structure of [Pd(phen)(CH3CN)2](O3SCF3)2, see: Adrian et al. (2008 ▶).

Experimental

Crystal data

[Pt(C2H3N)2(C12H8N2)](ClO4)2

M = 656.30

Orthorhombic,

a = 9.1407 (5) Å

b = 11.7822 (7) Å

c = 18.3215 (11) Å

V = 1973.2 (2) Å3

Z = 4

Mo Kα radiation

μ = 7.44 mm−1

T = 200 K

0.28 × 0.12 × 0.04 mm

Data collection

Bruker SMART 1000 CCD diffractometer

Absorption correction: multi-scan (SADABS; Bruker, 2000 ▶) T min = 0.763, T max = 1.000

11860 measured reflections

2043 independent reflections

1540 reflections with I > 2σ(I)

R int = 0.087

Refinement

R[F 2 > 2σ(F 2)] = 0.042

wR(F 2) = 0.100

S = 1.02

2043 reflections

176 parameters

18 restraints

H-atom parameters constrained

Δρmax = 2.23 e Å−3

Δρmin = −1.82 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 datablocks global, I. DOI: 10.1107/S1600536810008299/pk2230sup1.cif

Structure factors: contains datablocks I. DOI: 10.1107/S1600536810008299/pk2230Isup2.hkl

Additional supplementary materials: crystallographic information; 3D view; checkCIF report

[Pt(C2H3N)2(C12H8N2)](ClO4)2	F(000) = 1256
Mr = 656.30	Dx = 2.209 Mg m−3
Orthorhombic, Pnma	Mo Kα radiation, λ = 0.71073 Å
Hall symbol: -P 2ac 2n	Cell parameters from 3403 reflections
a = 9.1407 (5) Å	θ = 2.2–25.0°
b = 11.7822 (7) Å	µ = 7.44 mm−1
c = 18.3215 (11) Å	T = 200 K
V = 1973.2 (2) Å3	Rod, colorless
Z = 4	0.28 × 0.12 × 0.04 mm

Bruker SMART 1000 CCD diffractometer	2043 independent reflections
Radiation source: fine-focus sealed tube	1540 reflections with I > 2σ(I)
graphite	Rint = 0.087
φ and ω scans	θmax = 26.0°, θmin = 2.1°
Absorption correction: multi-scan (SADABS; Bruker, 2000)	h = −11→7
Tmin = 0.763, Tmax = 1.000	k = −14→14
11860 measured reflections	l = −22→21

Refinement on F2	Primary atom site location: structure-invariant direct methods
Least-squares matrix: full	Secondary atom site location: difference Fourier map
R[F2 > 2σ(F2)] = 0.042	Hydrogen site location: inferred from neighbouring sites
wR(F2) = 0.100	H-atom parameters constrained
S = 1.02	w = 1/[σ2(Fo2) + (0.0514P)2] where P = (Fo2 + 2Fc2)/3
2043 reflections	(Δ/σ)max < 0.001
176 parameters	Δρmax = 2.23 e Å−3
18 restraints	Δρmin = −1.82 e Å−3

Geometry. All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds 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.

	x	y	z	Uiso*/Ueq	Occ. (<1)
Pt1	0.96551 (5)	0.2500	0.10603 (2)	0.02158 (17)
N1	0.8473 (6)	0.1387 (5)	0.0483 (3)	0.0219 (14)
N2	1.0774 (7)	0.1326 (5)	0.1611 (4)	0.0278 (16)
C1	0.8490 (8)	0.0253 (6)	0.0516 (4)	0.0264 (18)
H1	0.9141	−0.0111	0.0845	0.032*
C2	0.7580 (9)	−0.0405 (7)	0.0081 (5)	0.034 (2)
H2	0.7628	−0.1209	0.0110	0.041*
C3	0.6622 (9)	0.0097 (7)	−0.0387 (5)	0.031 (2)
H3	0.5999	−0.0355	−0.0682	0.038*
C4	0.6557 (8)	0.1302 (7)	−0.0431 (5)	0.0304 (19)
C5	0.7512 (7)	0.1902 (6)	0.0018 (4)	0.0229 (17)
C6	0.5587 (9)	0.1932 (8)	−0.0901 (4)	0.034 (2)
H6	0.4937	0.1535	−0.1215	0.041*
C7	1.2397 (10)	0.0000 (8)	0.2375 (5)	0.040 (2)
H7A	1.2170	−0.0791	0.2254	0.061*
H7B	1.2217	0.0129	0.2896	0.061*
H7C	1.3427	0.0154	0.2264	0.061*
C8	1.1474 (8)	0.0750 (6)	0.1947 (4)	0.0255 (18)
Cl1	0.4808 (3)	0.2500	0.14861 (16)	0.0273 (6)
O1	0.3890 (9)	0.2500	0.2122 (5)	0.040 (2)
O2	0.3939 (10)	0.2500	0.0837 (4)	0.040 (2)
O3	0.5699 (7)	0.1506 (6)	0.1490 (4)	0.0515 (19)
Cl2	0.430 (2)	0.7500	0.341 (4)	0.033 (2)	0.53 (3)
O4	0.272 (2)	0.7500	0.340 (2)	0.080 (10)	0.53 (3)
O5	0.468 (3)	0.7500	0.4176 (11)	0.088 (10)	0.53 (3)
O6	0.4825 (19)	0.6495 (12)	0.3106 (12)	0.077 (8)	0.53 (3)
Cl2'	0.461 (3)	0.7500	0.340 (4)	0.033 (2)	0.47 (3)
O4'	0.312 (3)	0.7500	0.365 (2)	0.068 (10)	0.47 (3)
O5'	0.453 (3)	0.7500	0.2625 (11)	0.111 (15)	0.47 (3)
O6'	0.5367 (19)	0.6564 (15)	0.3651 (15)	0.073 (8)	0.47 (3)

	U11	U22	U33	U12	U13	U23
Pt1	0.0226 (3)	0.0172 (2)	0.0250 (3)	0.000	−0.00007 (19)	0.000
N1	0.027 (4)	0.014 (3)	0.025 (4)	−0.002 (2)	0.003 (3)	−0.003 (3)
N2	0.032 (4)	0.020 (3)	0.031 (4)	−0.005 (3)	−0.005 (3)	−0.003 (3)
C1	0.026 (4)	0.022 (4)	0.031 (5)	0.004 (3)	0.001 (3)	−0.005 (3)
C2	0.038 (5)	0.020 (4)	0.044 (6)	−0.006 (4)	0.006 (4)	−0.006 (4)
C3	0.031 (5)	0.030 (5)	0.034 (5)	−0.012 (4)	0.003 (4)	−0.010 (4)
C4	0.028 (5)	0.033 (5)	0.030 (5)	0.001 (3)	−0.004 (4)	−0.006 (4)
C5	0.019 (4)	0.027 (4)	0.022 (4)	0.000 (3)	0.003 (3)	0.002 (3)
C6	0.037 (5)	0.057 (6)	0.008 (4)	−0.011 (4)	0.000 (3)	−0.005 (3)
C7	0.047 (6)	0.038 (5)	0.036 (6)	0.012 (4)	−0.012 (4)	0.002 (4)
C8	0.025 (4)	0.020 (4)	0.032 (5)	−0.001 (3)	−0.002 (4)	0.000 (4)
Cl1	0.0272 (14)	0.0256 (14)	0.0292 (17)	0.000	−0.0033 (12)	0.000
O1	0.038 (5)	0.039 (5)	0.042 (6)	0.000	0.004 (4)	0.000
O2	0.055 (6)	0.031 (5)	0.035 (5)	0.000	−0.014 (4)	0.000
O3	0.058 (4)	0.055 (4)	0.041 (4)	0.033 (3)	−0.003 (3)	−0.003 (3)
Cl2	0.030 (7)	0.0226 (15)	0.047 (3)	0.000	−0.003 (11)	0.000
O4	0.031 (9)	0.077 (18)	0.13 (3)	0.000	−0.017 (11)	0.000
O5	0.11 (2)	0.09 (2)	0.063 (10)	0.000	−0.040 (13)	0.000
O6	0.072 (11)	0.034 (8)	0.124 (19)	0.002 (8)	0.025 (12)	−0.031 (10)
Cl2'	0.030 (7)	0.0226 (15)	0.047 (3)	0.000	−0.003 (11)	0.000
O4'	0.023 (11)	0.09 (2)	0.09 (2)	0.000	0.005 (13)	0.000
O5'	0.09 (2)	0.21 (4)	0.034 (9)	0.000	−0.016 (11)	0.000
O6'	0.057 (11)	0.037 (10)	0.12 (2)	0.013 (8)	0.007 (11)	0.028 (12)

Pt1—N2i	1.994 (7)	C6—H6	0.9500
Pt1—N2	1.994 (7)	C7—C8	1.452 (11)
Pt1—N1	2.001 (6)	C7—H7A	0.9800
Pt1—N1i	2.001 (6)	C7—H7B	0.9800
N1—C1	1.337 (9)	C7—H7C	0.9800
N1—C5	1.366 (9)	Cl1—O3i	1.427 (6)
N2—C8	1.118 (9)	Cl1—O3	1.427 (6)
C1—C2	1.388 (11)	Cl1—O2	1.430 (9)
C1—H1	0.9500	Cl1—O1	1.436 (9)
C2—C3	1.360 (12)	Cl2—O6ii	1.40 (3)
C2—H2	0.9500	Cl2—O6	1.40 (3)
C3—C4	1.424 (11)	Cl2—O5	1.44 (7)
C3—H3	0.9500	Cl2—O4	1.44 (2)
C4—C5	1.392 (10)	Cl2'—O6'ii	1.38 (3)
C4—C6	1.442 (11)	Cl2'—O6'	1.38 (3)
C5—C5i	1.410 (14)	Cl2'—O5'	1.42 (8)
C6—C6i	1.338 (19)	Cl2'—O4'	1.44 (2)
N2i—Pt1—N2	87.9 (3)	C4—C6—H6	119.5
N2i—Pt1—N1	177.0 (2)	C8—C7—H7A	109.5
N2—Pt1—N1	95.1 (2)	C8—C7—H7B	109.5
N2i—Pt1—N1i	95.1 (2)	H7A—C7—H7B	109.5
N2—Pt1—N1i	177.0 (2)	C8—C7—H7C	109.5
N1—Pt1—N1i	81.9 (3)	H7A—C7—H7C	109.5
C1—N1—C5	118.6 (6)	H7B—C7—H7C	109.5
C1—N1—Pt1	128.7 (5)	N2—C8—C7	179.2 (9)
C5—N1—Pt1	112.7 (5)	O3i—Cl1—O3	110.4 (6)
C8—N2—Pt1	173.4 (6)	O3i—Cl1—O2	108.7 (3)
N1—C1—C2	121.7 (7)	O3—Cl1—O2	108.7 (3)
N1—C1—H1	119.1	O3i—Cl1—O1	109.3 (3)
C2—C1—H1	119.1	O3—Cl1—O1	109.3 (3)
C3—C2—C1	120.3 (8)	O2—Cl1—O1	110.5 (6)
C3—C2—H2	119.9	O6ii—Cl2—O6	116 (4)
C1—C2—H2	119.9	O6ii—Cl2—O5	108 (3)
C2—C3—C4	119.7 (7)	O6—Cl2—O5	108 (3)
C2—C3—H3	120.1	O6ii—Cl2—O4	110 (2)
C4—C3—H3	120.1	O6—Cl2—O4	110 (2)
C5—C4—C3	116.5 (7)	O5—Cl2—O4	105 (3)
C5—C4—C6	118.5 (7)	O6'ii—Cl2'—O6'	106 (4)
C3—C4—C6	125.0 (8)	O6'ii—Cl2'—O5'	111 (3)
N1—C5—C4	123.1 (7)	O6'—Cl2'—O5'	111 (3)
N1—C5—C5i	116.3 (4)	O6'ii—Cl2'—O4'	111 (3)
C4—C5—C5i	120.5 (5)	O6'—Cl2'—O4'	111 (3)
C6i—C6—C4	121.0 (5)	O5'—Cl2'—O4'	106 (4)
C6i—C6—H6	119.5
N2—Pt1—N1—C1	1.5 (7)	C1—N1—C5—C4	−0.7 (11)
N1i—Pt1—N1—C1	−178.3 (5)	Pt1—N1—C5—C4	−179.0 (6)
N2—Pt1—N1—C5	179.6 (5)	C1—N1—C5—C5i	178.5 (5)
N1i—Pt1—N1—C5	−0.2 (6)	Pt1—N1—C5—C5i	0.2 (5)
C5—N1—C1—C2	1.2 (11)	C3—C4—C5—N1	−0.1 (11)
Pt1—N1—C1—C2	179.2 (6)	C6—C4—C5—N1	179.9 (7)
N1—C1—C2—C3	−1.0 (12)	C3—C4—C5—C5i	−179.2 (5)
C1—C2—C3—C4	0.2 (12)	C6—C4—C5—C5i	0.8 (9)
C2—C3—C4—C5	0.3 (12)	C5—C4—C6—C6i	−0.8 (9)
C2—C3—C4—C6	−179.7 (8)	C3—C4—C6—C6i	179.2 (6)

D—H···A	D—H	H···A	D···A	D—H···A
C1—H1···O6iii	0.95	2.60	3.48 (2)	155
C3—H3···O2iv	0.95	2.54	3.210 (8)	127
C3—H3···O3v	0.95	2.54	3.486 (11)	178
C7—H7A···O6iii	0.98	2.39	3.066 (18)	126
C7—H7B···O3vi	0.98	2.41	3.143 (11)	131

Table 1

Selected bond angles (°)

N2i—Pt1—N2	87.9 (3)
N1—Pt1—N1i	81.9 (3)

Symmetry code: (i) .

Table 2

Hydrogen-bond geometry (Å, °)

D—H⋯A	D—H	H⋯A	D⋯A	D—H⋯A
C1—H1⋯O6ii	0.95	2.60	3.48 (2)	155
C3—H3⋯O2iii	0.95	2.54	3.210 (8)	127
C3—H3⋯O3iv	0.95	2.54	3.486 (11)	178
C7—H7A⋯O6ii	0.98	2.39	3.066 (18)	126
C7—H7B⋯O3v	0.98	2.41	3.143 (11)	131

Symmetry codes: (ii) ; (iii) ; (iv) ; (v) .