Tetra-chlorido(1,10-phenanthroline-κN,N')platinum(IV) monohydrate.

In the title complex, [PtCl(4)(C(12)H(8)N(2))]·H(2)O, the Pt(4+) ion is six-coordinated in a distorted octa-hedral environment by two N atoms of a 1,10-phenanthroline ligand and by four Cl atoms. As a result of the different trans effects of the N and Cl atoms, the Pt-Cl bonds trans to the N atom are slightly shorter than those trans to the Cl atom. The compound displays inter-molecular π-π inter-actions between the six-membered rings, with a centroid-centroid distance of 3.834 Å. There are also weak intra-molecular C-H⋯Cl hydrogen bonds. According to the IR spectrum, solvent water was present in the crystal, but owing to the high thermal motion of the uncoordinated O atom, the H atoms could not be detected.

Related literature

For details of some other Pt–phenanthroline complexes, see: Buse et al. (1977 ▶); Fanizzi et al. (1996 ▶). For related Pt–bipyridine complexes, see: Hambley (1986 ▶); Hojjat Kashani et al. (2008 ▶).

Experimental

Crystal data

[PtCl4(C12H8N2)]·H2O

M = 535.11

Orthorhombic,

a = 14.8481 (19) Å

b = 12.4079 (16) Å

c = 17.379 (2) Å

V = 3201.8 (7) Å3

Z = 8

Mo Kα radiation

μ = 9.43 mm−1

T = 293 (2) K

0.25 × 0.08 × 0.06 mm

Data collection

Bruker SMART 1000 CCD diffractometer

Absorption correction: multi-scan (SADABS; Bruker, 2000 ▶) T min = 0.418, T max = 0.568

18465 measured reflections

3521 independent reflections

2414 reflections with I > 2σ(I)

R int = 0.047

Refinement

R[F 2 > 2σ(F 2)] = 0.046

wR(F 2) = 0.141

S = 1.02

3521 reflections

181 parameters

H-atom parameters constrained

Δρmax = 1.41 e Å−3

Δρmin = −0.56 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, 2003 ▶); software used to prepare material for publication: SHELXL97.

Crystal structure: contains datablocks global, I. DOI: 10.1107/S1600536809002694/fj2191sup1.cif

Structure factors: contains datablocks I. DOI: 10.1107/S1600536809002694/fj2191Isup2.hkl

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

[PtCl4(C12H8N2)]·H2O	F(000) = 2000
Mr = 535.11	Dx = 2.220 Mg m−3
Orthorhombic, Pbca	Mo Kα radiation, λ = 0.71073 Å
Hall symbol: -P 2ac 2ab	Cell parameters from 943 reflections
a = 14.8481 (19) Å	θ = 3.2–23.2°
b = 12.4079 (16) Å	µ = 9.43 mm−1
c = 17.379 (2) Å	T = 293 K
V = 3201.8 (7) Å3	Stick, yellow
Z = 8	0.25 × 0.08 × 0.06 mm

Bruker SMART 1000 CCD diffractometer	3521 independent reflections
Radiation source: fine-focus sealed tube	2414 reflections with I > 2σ(I)
graphite	Rint = 0.047
φ and ω scans	θmax = 27.1°, θmin = 2.3°
Absorption correction: multi-scan (SADABS; Bruker, 2000)	h = −18→18
Tmin = 0.418, Tmax = 0.568	k = −11→15
18465 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)] = 0.046	Hydrogen site location: inferred from neighbouring sites
wR(F2) = 0.141	H-atom parameters constrained
S = 1.02	w = 1/[σ2(Fo2) + (0.0738P)2 + 11.9979P] where P = (Fo2 + 2Fc2)/3
3521 reflections	(Δ/σ)max < 0.001
181 parameters	Δρmax = 1.41 e Å−3
0 restraints	Δρmin = −0.56 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.

	x	y	z	Uiso*/Ueq
Pt1	−0.12471 (3)	0.29079 (3)	0.18568 (2)	0.04495 (16)
Cl1	−0.27151 (18)	0.3484 (2)	0.20445 (16)	0.0580 (7)
Cl2	−0.15722 (18)	0.12006 (19)	0.23250 (16)	0.0549 (6)
Cl3	−0.16047 (19)	0.23631 (19)	0.06024 (15)	0.0537 (6)
Cl4	−0.0833 (2)	0.3517 (2)	0.30779 (14)	0.0568 (6)
N1	0.0092 (5)	0.2536 (6)	0.1619 (4)	0.0364 (16)
N2	−0.0815 (5)	0.4383 (5)	0.1425 (4)	0.0368 (16)
C1	0.0512 (7)	0.1599 (7)	0.1735 (5)	0.045 (2)
H1	0.0193	0.1016	0.1932	0.054*
C2	0.1400 (7)	0.1490 (8)	0.1567 (7)	0.051 (2)
H2	0.1690	0.0845	0.1679	0.062*
C3	0.1871 (7)	0.2308 (8)	0.1239 (6)	0.052 (3)
H3	0.2471	0.2204	0.1105	0.062*
C4	0.1462 (6)	0.3308 (7)	0.1100 (6)	0.041 (2)
C5	0.1870 (6)	0.4213 (8)	0.0779 (6)	0.048 (2)
H5	0.2472	0.4177	0.0633	0.058*
C6	0.1405 (6)	0.5157 (8)	0.0675 (5)	0.048 (2)
H6	0.1697	0.5738	0.0448	0.058*
C7	0.0491 (6)	0.5276 (7)	0.0901 (5)	0.039 (2)
C8	−0.0011 (6)	0.6212 (7)	0.0837 (6)	0.047 (2)
H8	0.0249	0.6832	0.0634	0.057*
C9	−0.0879 (8)	0.6221 (7)	0.1068 (6)	0.056 (3)
H9	−0.1213	0.6853	0.1028	0.067*
C10	−0.1284 (6)	0.5293 (7)	0.1368 (6)	0.047 (2)
H10	−0.1882	0.5311	0.1526	0.057*
C11	0.0064 (6)	0.4363 (6)	0.1212 (5)	0.0369 (19)
C12	0.0537 (6)	0.3380 (7)	0.1308 (5)	0.0361 (19)
O1	0.0973 (14)	0.4296 (19)	0.4629 (12)	0.258 (11)

	U11	U22	U33	U12	U13	U23
Pt1	0.0506 (3)	0.0368 (2)	0.0475 (3)	0.00031 (15)	−0.00128 (17)	0.00387 (15)
Cl1	0.0537 (14)	0.0544 (15)	0.0658 (17)	0.0055 (11)	0.0089 (12)	0.0134 (12)
Cl2	0.0589 (14)	0.0404 (12)	0.0653 (17)	−0.0065 (11)	0.0036 (12)	0.0105 (11)
Cl3	0.0648 (15)	0.0489 (13)	0.0475 (15)	−0.0084 (11)	−0.0064 (12)	0.0002 (11)
Cl4	0.0744 (17)	0.0486 (14)	0.0473 (15)	0.0025 (12)	−0.0074 (12)	−0.0021 (11)
N1	0.036 (4)	0.036 (4)	0.037 (4)	−0.001 (3)	0.002 (3)	−0.006 (3)
N2	0.043 (4)	0.024 (3)	0.044 (4)	−0.001 (3)	0.000 (3)	0.004 (3)
C1	0.053 (6)	0.030 (5)	0.053 (6)	0.002 (4)	0.003 (5)	−0.002 (4)
C2	0.056 (6)	0.037 (5)	0.062 (7)	0.008 (4)	−0.008 (5)	−0.001 (5)
C3	0.041 (5)	0.058 (6)	0.056 (6)	0.012 (4)	−0.006 (5)	−0.017 (5)
C4	0.041 (5)	0.042 (5)	0.040 (5)	−0.007 (4)	0.002 (4)	−0.011 (4)
C5	0.040 (5)	0.056 (6)	0.048 (6)	−0.010 (4)	0.003 (4)	−0.008 (5)
C6	0.058 (6)	0.050 (6)	0.037 (5)	−0.017 (4)	0.001 (4)	0.001 (4)
C7	0.054 (5)	0.036 (5)	0.027 (4)	−0.010 (4)	−0.006 (4)	−0.004 (3)
C8	0.062 (6)	0.032 (5)	0.048 (6)	−0.013 (4)	−0.002 (5)	−0.003 (4)
C9	0.084 (7)	0.025 (4)	0.059 (7)	0.003 (5)	−0.010 (6)	0.000 (4)
C10	0.053 (5)	0.039 (5)	0.050 (6)	0.002 (4)	−0.002 (5)	0.002 (4)
C11	0.048 (5)	0.032 (4)	0.030 (5)	−0.002 (4)	−0.007 (4)	−0.006 (4)
C12	0.044 (5)	0.032 (4)	0.032 (5)	−0.006 (4)	−0.006 (4)	−0.005 (3)
O1	0.33 (3)	0.29 (3)	0.151 (17)	0.06 (2)	0.028 (17)	0.043 (17)

Pt1—N2	2.080 (7)	C3—H3	0.9300
Pt1—N1	2.083 (7)	C4—C5	1.393 (13)
Pt1—Cl1	2.317 (3)	C4—C12	1.424 (12)
Pt1—Cl2	2.320 (2)	C5—C6	1.372 (13)
Pt1—Cl4	2.335 (3)	C5—H5	0.9300
Pt1—Cl3	2.343 (3)	C6—C7	1.421 (13)
N1—C1	1.335 (11)	C6—H6	0.9300
N1—C12	1.351 (11)	C7—C8	1.384 (13)
N2—C10	1.330 (11)	C7—C11	1.405 (11)
N2—C11	1.357 (11)	C8—C9	1.351 (14)
C1—C2	1.357 (13)	C8—H8	0.9300
C1—H1	0.9300	C9—C10	1.400 (14)
C2—C3	1.358 (14)	C9—H9	0.9300
C2—H2	0.9300	C10—H10	0.9300
C3—C4	1.402 (13)	C11—C12	1.417 (12)
N2—Pt1—N1	80.1 (3)	C4—C3—H3	119.7
N2—Pt1—Cl1	94.0 (2)	C5—C4—C3	126.5 (8)
N1—Pt1—Cl1	174.0 (2)	C5—C4—C12	118.0 (8)
N2—Pt1—Cl2	173.9 (2)	C3—C4—C12	115.5 (8)
N1—Pt1—Cl2	93.8 (2)	C6—C5—C4	121.5 (9)
Cl1—Pt1—Cl2	92.10 (9)	C6—C5—H5	119.2
N2—Pt1—Cl4	87.8 (2)	C4—C5—H5	119.2
N1—Pt1—Cl4	90.0 (2)	C5—C6—C7	122.2 (8)
Cl1—Pt1—Cl4	91.14 (10)	C5—C6—H6	118.9
Cl2—Pt1—Cl4	91.81 (10)	C7—C6—H6	118.9
N2—Pt1—Cl3	89.3 (2)	C8—C7—C11	117.7 (8)
N1—Pt1—Cl3	88.2 (2)	C8—C7—C6	125.4 (8)
Cl1—Pt1—Cl3	90.39 (10)	C11—C7—C6	117.0 (8)
Cl2—Pt1—Cl3	90.90 (9)	C9—C8—C7	119.8 (9)
Cl4—Pt1—Cl3	176.84 (10)	C9—C8—H8	120.1
C1—N1—C12	120.5 (8)	C7—C8—H8	120.1
C1—N1—Pt1	127.5 (6)	C8—C9—C10	120.9 (9)
C12—N1—Pt1	112.0 (6)	C8—C9—H9	119.5
C10—N2—C11	120.0 (7)	C10—C9—H9	119.5
C10—N2—Pt1	127.7 (6)	N2—C10—C9	120.0 (9)
C11—N2—Pt1	112.3 (5)	N2—C10—H10	120.0
N1—C1—C2	120.5 (9)	C9—C10—H10	120.0
N1—C1—H1	119.7	N2—C11—C7	121.6 (8)
C2—C1—H1	119.7	N2—C11—C12	117.4 (7)
C1—C2—C3	121.1 (9)	C7—C11—C12	121.0 (8)
C1—C2—H2	119.5	N1—C12—C11	118.2 (8)
C3—C2—H2	119.5	N1—C12—C4	121.6 (8)
C2—C3—C4	120.7 (9)	C11—C12—C4	120.2 (8)
C2—C3—H3	119.7
N2—Pt1—N1—C1	179.4 (8)	C11—C7—C8—C9	−0.1 (13)
Cl2—Pt1—N1—C1	−0.2 (8)	C6—C7—C8—C9	179.5 (9)
Cl4—Pt1—N1—C1	91.6 (7)	C7—C8—C9—C10	−0.6 (15)
Cl3—Pt1—N1—C1	−91.0 (7)	C11—N2—C10—C9	1.7 (14)
N2—Pt1—N1—C12	−1.2 (6)	Pt1—N2—C10—C9	179.3 (7)
Cl2—Pt1—N1—C12	179.2 (5)	C8—C9—C10—N2	−0.2 (15)
Cl4—Pt1—N1—C12	−89.0 (5)	C10—N2—C11—C7	−2.5 (13)
Cl3—Pt1—N1—C12	88.4 (5)	Pt1—N2—C11—C7	179.6 (6)
N1—Pt1—N2—C10	−177.2 (8)	C10—N2—C11—C12	178.2 (8)
Cl1—Pt1—N2—C10	4.2 (8)	Pt1—N2—C11—C12	0.3 (9)
Cl4—Pt1—N2—C10	−86.8 (8)	C8—C7—C11—N2	1.7 (12)
Cl3—Pt1—N2—C10	94.6 (8)	C6—C7—C11—N2	−178.0 (8)
N1—Pt1—N2—C11	0.5 (6)	C8—C7—C11—C12	−179.0 (8)
Cl1—Pt1—N2—C11	−178.1 (6)	C6—C7—C11—C12	1.3 (12)
Cl4—Pt1—N2—C11	90.9 (6)	C1—N1—C12—C11	−178.7 (8)
Cl3—Pt1—N2—C11	−87.7 (6)	Pt1—N1—C12—C11	1.8 (9)
C12—N1—C1—C2	2.3 (13)	C1—N1—C12—C4	−0.6 (12)
Pt1—N1—C1—C2	−178.3 (7)	Pt1—N1—C12—C4	180.0 (6)
N1—C1—C2—C3	−3.7 (16)	N2—C11—C12—N1	−1.4 (12)
C1—C2—C3—C4	3.2 (16)	C7—C11—C12—N1	179.2 (7)
C2—C3—C4—C5	179.0 (10)	N2—C11—C12—C4	−179.6 (8)
C2—C3—C4—C12	−1.4 (14)	C7—C11—C12—C4	1.0 (12)
C3—C4—C5—C6	−179.5 (9)	C5—C4—C12—N1	179.7 (8)
C12—C4—C5—C6	1.0 (14)	C3—C4—C12—N1	0.1 (12)
C4—C5—C6—C7	1.4 (15)	C5—C4—C12—C11	−2.2 (13)
C5—C6—C7—C8	177.8 (9)	C3—C4—C12—C11	178.2 (8)
C5—C6—C7—C11	−2.6 (13)

D—H···A	D—H	H···A	D···A	D—H···A
C1—H1···Cl2	0.93	2.72	3.298 (10)	121
C10—H10···Cl1	0.93	2.74	3.306 (10)	121

Table 1

Hydrogen-bond geometry (Å, °)

D—H⋯A	D—H	H⋯A	D⋯A	D—H⋯A
C1—H1⋯Cl2	0.93	2.72	3.298 (10)	121
C10—H10⋯Cl1	0.93	2.74	3.306 (10)	121