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The title compound, catena-poly[[[bis­(ethyl­ene­di­amine-[kappa]2N,N')platinum(II)]- [mu]-chlorido-[bis­(ethyl­ene­di­amine)­platinum(IV)]-[mu]-chlorido] tetra­kis­{4-[(4-hy­droxy­phenyl)diazenyl]benzene­sulfonate} dihydrate], {[PtIIPtIVCl2(C2H8N2)4](HOC6H4N=NC6H4SO3)4·2H2O}n, has a linear chain structure composed of square-planar [Pt(en)2]2+ (en is ethyl­ene­di­amine) and elongated octa­hedral trans-[PtCl2(en)2]2+ cations stacked alternately, bridged by Cl atoms, along the b axis. The Pt atoms are located on an inversion centre, while the Cl atoms are disordered over two sites and form a zigzag ...Cl-PtIV-Cl...PtII... chain, with a PtIV-Cl bond length of 2.3140 (14) Å, an inter­atomic PtII...Cl distance of 3.5969 (15) Å and a PtIV-Cl...PtII angle of 170.66 (6)°. The structural param­eter indicating the mixed-valence state of the Pt atom, expressed by [delta] = (PtIV-Cl)/(PtII...Cl), is 0.643.

Supporting information

cif

Crystallographic Information File (CIF) https://doi.org/10.1107/S2053229615019877/uk3120sup1.cif
Contains datablocks global, I

hkl

Structure factor file (CIF format) https://doi.org/10.1107/S2053229615019877/uk3120Isup2.hkl
Contains datablock I

CCDC reference: 1432418

Introduction top

The title compound, [Pt(en)2][PtCl2(en)2](HOC6H4N NC6H4SO3)4.2H2O (en is ethyl­enedi­amine), (I), is a member of the family of one-dimensional halogen-bridged mixed-valence metal complexes, formulated as [MII(AA)2][MIVX2(AA)2]Y4 [MII/MIV = PtII/PtIV, PdII/PdIV, NiII/NiIV, PdII/PtIV and NiII/PtIV; X = Cl, Br and I; AA = NH2(CH2)2NH2 etc.; Y = ClO4-, HSO4-, X- etc.], hereinafter abbreviated as MX-chain compounds, which are typical mixed-valence compounds belonging to class II in the classification of Robin & Day (1967). MX-chain compounds have attractedmuch inter­est because of their one-dimensional mixed-valence electron systems, as described in a previous report (Matsushita, 2006).

Compound (I) has been prepared as an MX-chain compound combined with an azo­benzene-derived counter-ion. This counter-ion was chosen because it displays photochromic behaviour on the basis of cis-trans isomerization [Reference?]. However, crystals of (I) do not display photochromic behaviour. Since a certain amount of space is necessary for cistrans isomerization of the azo­benzene counter-ion, the photochromic behaviour may be suppressed by packing in the crystal. Spectroscopic changes in a similar MX-chain compound with an amphiphilic azo­benzene derivative in aqueous solution and in poly(vinyl alcohol) cast films by photo-irradiation have been reported (Einaga et al., 2005). Structural information on MX-chain compounds having such a bulky azo­benzene-derived counter-ion has not been published previously. The present X-ray crystallographic analysis of (I) was performed in order to elucidate the crystal packing and to obtain the metal–halogen distances, which reflect the mixed-valence state, for an MX-chain compound having a bulky azo­benzene-derived counter-ion.

Experimental top

Synthesis and crystallization top

The title compound was prepared by a procedure similar to that of Matsushita & Taira (1999). To an aqueous solution containing [Pt(en)2]2+ (0.26 mmol) and trans-[PtCl2(en)2]2+ (0.26 mmol) was added an aqueous solution of sodium 4-hy­droxy­azo­benzene-4'-sulfonate (1.14 mmol, 0.342 g). After removing a white–orange precipitate by filtration, the deep-yellow filtrate was allowed to stand at room temperature for several days. Yellow platelet crystals of (I) suitable for X-ray analysis were obtained after slow evaporation and were collected by filtration (yield 0.326 g, 68%, based on Pt).

Refinement top

Crystal data, data collection and structure refinement details are summarized in Table 1. H atoms were placed in geometrically calculated positions and refined as riding, with methyl­ene C—H = 0.97 Å, aromatic C—H = 0.93 Å, N—H = 0.90 Å and O—H = 0.82 Å, and with the constraint Uiso(H) = 1.2Ueq(C,N,O).

Results and discussion top

The molecular structure of (I) is shown in Fig. 1. As shown in Fig. 2, the structure of (I) is built up from columns composed of square-planar [Pt(en)2]2+ and elongated o­cta­hedral trans-[PtCl2(en)2]2+ cations stacked alternately, bridged by Cl atoms, along the b axis. The Pt atoms lie on an inversion centre. The Cl atoms are not located at the exact mid-point between adjacent Pt atoms, but are disordered over two general sites, related by an inversion centre, close to the mid-point. The Pt and Cl atoms form an infinite zigzag ···Cl—PtIV—Cl···PtII··· chain, with the shorter Pt—Cl bond length [2.3140 (14) Å] assigned to PtIV—Cl and the longer one [3.5969 (15) Å] to PtII···Cl, and a PtIV—Cl···PtII angle of 170.66 (6)° (Table 2). The PtII···Cl bond length is longer than those of other MX-chain compounds, for example, [Pt(en)2][PtCl2(en)2]Y4 [3.191 (4) Å for Y = PF6 (Matsushita, 2005b), 3.142 (2) Å for Y = HSO4 (Matsushita, 2003), 3.101 (4) Å for Y = ClO4 (Huckett et al., 1993), and 3.052 (3) Å for Y = BF4 (Matsushita, 2005a)]. The Pt···Pt distance of 5.8922 (3) Å is the longest of those of the reported MX-chain compounds, cf. [Pt(en)2][PtCl2(en)2]Y4 [5.518 (2) Å for Y = PF6, 5.465 (1) Å for Y = HSO4, 5.428 (4) Å for Y = ClO4 and 5.372 (2) Å for Y = BF4].

Each Pt site is occupied by a disordered combination of PtII and PtIV atoms. The valence order of the Pt site in (I) belongs to one of three different classes of the order–disorder problem pointed out by Keller (1982); the structure of (I) can be regarded as being of the one-dimensionally ordered structure type, with the other two directions being in a disordered state. The structural order–disorder situation of the Pt site in (I) has been observed in a number of other MX-chain compounds (Beauchamp et al., 1982; Yamashita et al., 1985; Matsushita et al.,1992; Toriumi et al., 1993; Huckett et al., 1993; Matsushita, 2003, 2005a,b).

The structural parameter indicating the mixed-valence state of the Pt atom, expressed by δ = (PtIV—Cl)/(PtII···Cl), is 0.643. This value is much smaller than those of [Pt(en)2][PtCl2(en)2]Y4 [0.729 for Y = PF6 (Matsushita, 2005b), 0.739 for Y = HSO4 (Matsushita, 2003), 0.750 for Y = ClO4 (Huckett et al., 1993) and 0.760 for Y = BF4 (Matsushita, 2005a)]. The very small δ value of (I) is produced by the above-mentioned very long PtII···Cl distance. The δ parameter, which correlates well with the energy position of the inter-valence charge-transfer absorption band (Matsushita, 1993), depends on the size of the counter-anion, as described previously (Matsushita et al., 1995). The obviously long PtII···Cl distance and the obviously small δ value of (I) suggest that the bulky azo­benzene-derived counter-ion tends to prevent and weaken the formation of the mixed-valence ···Cl—PtIV—Cl···PtII··· chain.

Hydrogen bonds in (I) (Table 3) stabilize the columnar structure composed only of cationic complexes, as shown in Fig. 2. A [PtII/IV(en)2] unit is bound to an adjacent Pt complex unit in the column by four hydrogen-bond linkages, namely the N1—H1A···O2···H5A—O5···H1B—N1 and N2—H2A···O1···H4A—O4···H2B—N2 linkages, and their symmetry-related counterparts. In addition, the donor N2—H2B group is also hydrogen-bonded to atom O3, and forms a three-centre bond. The crystal packing is further stabilized by inter­columnar hydrogen-bond linkages, as shown in Fig. 3. The presence of the inter-counter-ion hydrogen bond between hy­droxy atom O4 and sulfonate atom O1 is unique compared with other MX-chain compounds.

Computing details top

Data collection: RAPID-AUTO (Rigaku, 2006); cell refinement: RAPID-AUTO (Rigaku, 2006); data reduction: RAPID-AUTO (Rigaku, 2006); program(s) used to solve structure: SHELXS97 (Sheldrick, 2008); program(s) used to refine structure: SHELXL97 (Sheldrick, 2008); molecular graphics: DIAMOND (Brandenburg, 2006); software used to prepare material for publication: SHELXL97 (Sheldrick, 2008) and publCIF (Westrip, 2010).

Figures top
[Figure 1] Fig. 1. A view of the molecular structure of (I), showing the atomic numbering scheme. The symmetry-equivalent ethylenediamine ligands have been included to show the complete coordination environment of the Pt atom. Displacement ellipsoids are drawn at the 50% probability level. Dashed lines represent N—H···O and O—H···O hydrogen bonds. [Symmetry code: (i) -x, -y, -z.]
[Figure 2] Fig. 2. A view of the columnar structure of (I). Displacement ellipsoids are drawn at the 50% probability level. Black dashed lines between Pt and Cl atoms indicate the PtII···Cl contacts. The hollow Cl ellipsoids and the hollow lines between the Pt and Cl atoms represent the disordered structure of the Pt—Cl chain. Hydrogen bonds are indicated by blue dashed lines. The azobenzene-derived counter-ions, except for atoms C3 and C12, have been omitted for clarity. [Symmetry codes: (i) -x, -y, -z; (ii) x, y + 1, z; (iii) -x + 1, y, -z + 1/2.]
[Figure 3] Fig. 3. A packing diagram for (I), projected on the ac plane. Dashed lines represent hydrogen bonds.
catena-Poly[[[bis(ethylenediamine-κ2N,N')platinum(II)]-µ-chlorido-[bis(ethylenediamine)platinum(IV)]-µ-chlorido] tetrakis{4-[(4-hydroxyphenyl)diazenyl]benzenesulfonate} dihydrate] top
Crystal data top
[Pt2Cl2(C2H8N2)4](C12H9N2O4S)4·2H2OF(000) = 918
Mr = 1846.62Dx = 1.822 Mg m3
Monoclinic, P2/cMo Kα radiation, λ = 0.7107 Å
Hall symbol: -P 2ycCell parameters from 19956 reflections
a = 18.0782 (7) Åθ = 3.3–32.1°
b = 5.8922 (3) ŵ = 4.44 mm1
c = 15.8365 (3) ÅT = 296 K
β = 93.7245 (7)°Platelet, yellow
V = 1683.35 (11) Å30.18 × 0.09 × 0.02 mm
Z = 1
Data collection top
Rigaku R-AXIS RAPID imaging-plate
diffractometer
5847 independent reflections
Radiation source: X-ray sealed tube4097 reflections with I > 2σ(I)
Graphite monochromatorRint = 0.037
Detector resolution: 10.00 pixels mm-1θmax = 32.0°, θmin = 3.3°
ω scansh = 2626
Absorption correction: multi-scan
(ABSCOR; Higashi, 1995)
k = 88
Tmin = 0.616, Tmax = 0.915l = 2323
36062 measured reflections
Refinement top
Refinement on F2Secondary atom site location: difference Fourier map
Least-squares matrix: fullHydrogen site location: inferred from neighbouring sites
R[F2 > 2σ(F2)] = 0.030H-atom parameters constrained
wR(F2) = 0.062 w = 1/[σ2(Fo2) + (0.0201P)2 + 1.4401P]
where P = (Fo2 + 2Fc2)/3
S = 1.04(Δ/σ)max < 0.001
5847 reflectionsΔρmax = 0.50 e Å3
229 parametersΔρmin = 0.67 e Å3
0 restraintsExtinction correction: SHELXL97 (Sheldrick, 2008), Fc*=kFc[1+0.001xFc2λ3/sin(2θ)]-1/4
Primary atom site location: heavy-atom methodExtinction coefficient: 0.00058 (13)
Crystal data top
[Pt2Cl2(C2H8N2)4](C12H9N2O4S)4·2H2OV = 1683.35 (11) Å3
Mr = 1846.62Z = 1
Monoclinic, P2/cMo Kα radiation
a = 18.0782 (7) ŵ = 4.44 mm1
b = 5.8922 (3) ÅT = 296 K
c = 15.8365 (3) Å0.18 × 0.09 × 0.02 mm
β = 93.7245 (7)°
Data collection top
Rigaku R-AXIS RAPID imaging-plate
diffractometer
5847 independent reflections
Absorption correction: multi-scan
(ABSCOR; Higashi, 1995)
4097 reflections with I > 2σ(I)
Tmin = 0.616, Tmax = 0.915Rint = 0.037
36062 measured reflections
Refinement top
R[F2 > 2σ(F2)] = 0.0300 restraints
wR(F2) = 0.062H-atom parameters constrained
S = 1.04Δρmax = 0.50 e Å3
5847 reflectionsΔρmin = 0.67 e Å3
229 parameters
Special details top

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.

Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top
xyzUiso*/UeqOcc. (<1)
Pt10.00000.00000.00000.04019 (5)
Cl10.00984 (9)0.3908 (2)0.00989 (10)0.0556 (4)0.50
S10.16616 (4)0.50242 (12)0.16451 (5)0.04404 (14)
O10.18520 (13)0.4493 (4)0.07845 (15)0.0612 (6)
O20.10469 (11)0.3626 (4)0.18888 (15)0.0560 (5)
O30.15447 (13)0.7423 (4)0.17749 (16)0.0611 (6)
O40.74058 (13)0.2157 (4)0.49739 (16)0.0676 (6)
H4A0.75090.34410.48200.081*
O50.00000.6731 (6)0.25000.0734 (10)
H5A0.02970.57780.23540.088*
N10.01072 (16)0.0377 (5)0.12646 (16)0.0583 (7)
H1A0.01610.15760.14600.070*
H1B0.00620.08700.15430.070*
N20.11222 (14)0.0477 (5)0.00391 (17)0.0560 (7)
H2A0.12490.16870.03640.067*
H2B0.13570.07510.02640.067*
N30.44572 (14)0.2412 (4)0.36021 (17)0.0519 (6)
N40.46564 (14)0.0389 (4)0.35194 (18)0.0532 (6)
C10.0905 (2)0.0733 (7)0.1410 (2)0.0739 (10)
H1C0.09960.04150.19950.089*
H1D0.10460.22910.12860.089*
C20.1342 (2)0.0853 (8)0.0835 (2)0.0693 (9)
H2C0.18680.05670.08650.083*
H2D0.12420.24120.10030.083*
C30.24454 (15)0.4195 (5)0.22970 (18)0.0425 (6)
C40.28121 (17)0.5698 (5)0.2843 (2)0.0518 (7)
H40.26200.71410.29200.062*
C50.34708 (16)0.5050 (5)0.3280 (2)0.0523 (7)
H50.37190.60620.36490.063*
C60.37564 (15)0.2905 (5)0.31658 (19)0.0451 (6)
C70.33796 (17)0.1380 (5)0.2625 (2)0.0538 (7)
H70.35680.00700.25530.065*
C80.27236 (17)0.2025 (5)0.2195 (2)0.0533 (7)
H80.24680.10010.18370.064*
C90.53538 (15)0.0153 (5)0.3925 (2)0.0471 (6)
C100.56194 (17)0.2302 (5)0.3751 (2)0.0565 (8)
H100.53350.32780.34020.068*
C110.63043 (18)0.3001 (5)0.4094 (2)0.0563 (8)
H110.64820.44370.39720.068*
C120.67241 (17)0.1553 (6)0.4619 (2)0.0529 (7)
C130.64535 (19)0.0571 (6)0.4808 (2)0.0570 (8)
H130.67330.15300.51680.068*
C140.57760 (17)0.1269 (5)0.4466 (2)0.0519 (7)
H140.55980.26990.45970.062*
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
Pt10.04710 (8)0.03326 (7)0.03823 (8)0.00365 (7)0.01231 (5)0.00233 (6)
Cl10.0687 (10)0.0353 (7)0.0609 (9)0.0027 (6)0.0122 (7)0.0001 (6)
S10.0393 (3)0.0380 (3)0.0542 (4)0.0049 (3)0.0014 (3)0.0007 (3)
O10.0568 (13)0.0728 (16)0.0537 (13)0.0120 (11)0.0008 (10)0.0027 (10)
O20.0430 (11)0.0545 (13)0.0701 (14)0.0077 (10)0.0005 (10)0.0059 (11)
O30.0563 (13)0.0442 (12)0.0813 (16)0.0002 (10)0.0071 (11)0.0016 (11)
O40.0557 (13)0.0708 (16)0.0749 (16)0.0146 (12)0.0055 (12)0.0087 (13)
O50.059 (2)0.072 (2)0.091 (3)0.0000.0227 (19)0.000
N10.0737 (18)0.0621 (18)0.0377 (12)0.0179 (13)0.0075 (12)0.0073 (11)
N20.0487 (14)0.0630 (18)0.0543 (15)0.0060 (11)0.0130 (12)0.0023 (12)
N30.0430 (13)0.0467 (14)0.0656 (16)0.0001 (11)0.0003 (12)0.0036 (12)
N40.0410 (12)0.0519 (17)0.0667 (16)0.0010 (10)0.0041 (11)0.0029 (12)
C10.087 (3)0.076 (2)0.059 (2)0.003 (2)0.011 (2)0.0150 (18)
C20.056 (2)0.085 (2)0.067 (2)0.0059 (19)0.0018 (17)0.0009 (19)
C30.0375 (13)0.0381 (12)0.0519 (16)0.0035 (11)0.0020 (12)0.0032 (11)
C40.0480 (16)0.0420 (14)0.0646 (19)0.0046 (12)0.0018 (14)0.0149 (13)
C50.0489 (14)0.0445 (14)0.0621 (17)0.0013 (14)0.0065 (13)0.0146 (15)
C60.0378 (14)0.0444 (15)0.0531 (16)0.0029 (11)0.0037 (12)0.0036 (12)
C70.0476 (16)0.0376 (14)0.076 (2)0.0020 (12)0.0009 (15)0.0110 (14)
C80.0471 (16)0.0424 (15)0.069 (2)0.0045 (12)0.0031 (14)0.0137 (14)
C90.0398 (13)0.0435 (14)0.0589 (16)0.0006 (13)0.0095 (12)0.0021 (14)
C100.0475 (17)0.0444 (16)0.078 (2)0.0043 (13)0.0034 (15)0.0059 (15)
C110.0493 (17)0.0428 (16)0.077 (2)0.0040 (13)0.0095 (16)0.0010 (15)
C120.0454 (16)0.0578 (19)0.0564 (18)0.0029 (14)0.0092 (14)0.0043 (14)
C130.0519 (17)0.059 (2)0.0601 (19)0.0048 (14)0.0010 (15)0.0089 (14)
C140.0510 (17)0.0438 (16)0.0612 (19)0.0044 (13)0.0059 (14)0.0030 (14)
Geometric parameters (Å, º) top
Pt1—N12.037 (2)C4—C51.391 (4)
Pt1—N22.045 (3)C4—H40.9300
Pt1—Cl12.3140 (14)C5—C61.381 (4)
Pt1—Cl1i2.3140 (14)C5—H50.9300
Pt1—Cl1ii3.5969 (15)C6—C71.389 (4)
Cl1—Cl1ii1.366 (3)C6—N31.433 (4)
Cl1—Pt1iii3.5969 (15)C7—C81.382 (4)
N1—C11.489 (5)C7—H70.9300
N1—H1A0.9000C8—H80.9300
N1—H1B0.9000N3—N41.255 (3)
N2—C21.481 (5)N4—C91.414 (4)
N2—H2A0.9000C9—C101.388 (4)
N2—H2B0.9000C9—C141.391 (4)
C1—C21.495 (5)C10—C111.382 (4)
C1—H1C0.9700C10—H100.9300
C1—H1D0.9700C11—C121.383 (5)
C2—H2C0.9700C11—H110.9300
C2—H2D0.9700C12—O41.368 (4)
S1—O11.461 (2)C12—C131.383 (5)
S1—O21.455 (2)C13—C141.370 (4)
S1—O31.446 (2)C13—H130.9300
S1—C31.767 (3)C14—H140.9300
C3—C41.377 (4)O4—H4A0.8200
C3—C81.387 (4)O5—H5A0.8200
N1—Pt1—N1i180.0 (2)O3—S1—O1112.80 (15)
N1—Pt1—N2i96.47 (11)O2—S1—O1110.87 (14)
N1i—Pt1—N2i83.53 (11)O3—S1—C3107.84 (13)
N1—Pt1—N283.53 (11)O2—S1—C3106.60 (13)
N1i—Pt1—N296.47 (11)O1—S1—C3104.90 (14)
N2i—Pt1—N2180.00 (2)C4—C3—C8120.1 (3)
N1—Pt1—Cl1i86.91 (9)C4—C3—S1121.6 (2)
N1i—Pt1—Cl1i93.09 (9)C8—C3—S1118.0 (2)
N2i—Pt1—Cl1i86.39 (9)C3—C4—C5119.8 (3)
N2—Pt1—Cl1i93.61 (9)C3—C4—H4120.1
N1—Pt1—Cl193.09 (9)C5—C4—H4120.1
N1i—Pt1—Cl186.91 (9)C6—C5—C4120.1 (3)
N2i—Pt1—Cl193.61 (9)C6—C5—H5120.0
N2—Pt1—Cl186.39 (9)C4—C5—H5120.0
Cl1i—Pt1—Cl1180.00 (10)C5—C6—C7120.0 (3)
N1—Pt1—Cl1ii98.29 (8)C5—C6—N3116.7 (3)
N1i—Pt1—Cl1ii81.71 (8)C7—C6—N3123.3 (3)
N2i—Pt1—Cl1ii100.64 (8)C8—C7—C6119.8 (3)
N2—Pt1—Cl1ii79.36 (8)C8—C7—H7120.1
Pt1—Cl1—Pt1iii170.66 (6)C6—C7—H7120.1
C1—N1—Pt1108.8 (2)C7—C8—C3120.1 (3)
C1—N1—H1A109.9C7—C8—H8119.9
Pt1—N1—H1A109.9C3—C8—H8119.9
C1—N1—H1B109.9N4—N3—C6113.1 (2)
Pt1—N1—H1B109.9N3—N4—C9114.9 (3)
H1A—N1—H1B108.3C10—C9—C14119.3 (3)
C2—N2—Pt1108.5 (2)C10—C9—N4115.2 (3)
C2—N2—H2A110.0C14—C9—N4125.5 (3)
Pt1—N2—H2A110.0C11—C10—C9120.4 (3)
C2—N2—H2B110.0C11—C10—H10119.8
Pt1—N2—H2B110.0C9—C10—H10119.8
H2A—N2—H2B108.4C10—C11—C12119.7 (3)
N1—C1—C2107.3 (3)C10—C11—H11120.2
N1—C1—H1C110.3C12—C11—H11120.2
C2—C1—H1C110.3O4—C12—C11122.1 (3)
N1—C1—H1D110.3O4—C12—C13117.9 (3)
C2—C1—H1D110.3C11—C12—C13120.0 (3)
H1C—C1—H1D108.5C14—C13—C12120.4 (3)
N2—C2—C1108.2 (3)C14—C13—H13119.8
N2—C2—H2C110.0C12—C13—H13119.8
C1—C2—H2C110.0C13—C14—C9120.2 (3)
N2—C2—H2D110.0C13—C14—H14119.9
C1—C2—H2D110.0C9—C14—H14119.9
H2C—C2—H2D108.4C12—O4—H4A109.5
O3—S1—O2113.23 (14)N1ii—O5—H5A109.5
Symmetry codes: (i) x, y, z; (ii) x, y+1, z; (iii) x, y+1, z.
Hydrogen-bond geometry (Å, º) top
D—H···AD—HH···AD···AD—H···A
N1—H1A···O2i0.902.082.954 (3)162
N1—H1B···O5ii0.902.082.904 (4)151
N2—H2A···O10.902.072.920 (3)158
N2—H2B···O4iv0.902.443.082 (4)129
N2—H2B···O3v0.902.633.332 (4)136
O4—H4A···O1vi0.821.972.711 (3)150
O5—H5A···O20.822.032.847 (3)174
Symmetry codes: (i) x, y, z; (ii) x, y+1, z; (iv) x+1, y, z+1/2; (v) x, y1, z; (vi) x+1, y1, z+1/2.

Experimental details

Crystal data
Chemical formula[Pt2Cl2(C2H8N2)4](C12H9N2O4S)4·2H2O
Mr1846.62
Crystal system, space groupMonoclinic, P2/c
Temperature (K)296
a, b, c (Å)18.0782 (7), 5.8922 (3), 15.8365 (3)
β (°) 93.7245 (7)
V3)1683.35 (11)
Z1
Radiation typeMo Kα
µ (mm1)4.44
Crystal size (mm)0.18 × 0.09 × 0.02
Data collection
DiffractometerRigaku R-AXIS RAPID imaging-plate
diffractometer
Absorption correctionMulti-scan
(ABSCOR; Higashi, 1995)
Tmin, Tmax0.616, 0.915
No. of measured, independent and
observed [I > 2σ(I)] reflections
36062, 5847, 4097
Rint0.037
(sin θ/λ)max1)0.746
Refinement
R[F2 > 2σ(F2)], wR(F2), S 0.030, 0.062, 1.04
No. of reflections5847
No. of parameters229
H-atom treatmentH-atom parameters constrained
Δρmax, Δρmin (e Å3)0.50, 0.67

Computer programs: RAPID-AUTO (Rigaku, 2006), SHELXS97 (Sheldrick, 2008), DIAMOND (Brandenburg, 2006), SHELXL97 (Sheldrick, 2008) and publCIF (Westrip, 2010).

Selected geometric parameters (Å, º) top
Pt1—N12.037 (2)C1—C21.495 (5)
Pt1—N22.045 (3)S1—O11.461 (2)
Pt1—Cl12.3140 (14)S1—O21.455 (2)
Pt1—Cl1i3.5969 (15)S1—O31.446 (2)
N1—C11.489 (5)S1—C31.767 (3)
N2—C21.481 (5)
N1—Pt1—N283.53 (11)O3—S1—O2113.23 (14)
N1—Pt1—Cl193.09 (9)O3—S1—O1112.80 (15)
N2—Pt1—Cl186.39 (9)O2—S1—O1110.87 (14)
Pt1—Cl1—Pt1ii170.66 (6)O3—S1—C3107.84 (13)
C1—N1—Pt1108.8 (2)O2—S1—C3106.60 (13)
C2—N2—Pt1108.5 (2)O1—S1—C3104.90 (14)
Symmetry codes: (i) x, y+1, z; (ii) x, y+1, z.
Hydrogen-bond geometry (Å, º) top
D—H···AD—HH···AD···AD—H···A
N1—H1A···O2iii0.902.082.954 (3)162
N1—H1B···O5i0.902.082.904 (4)151
N2—H2A···O10.902.072.920 (3)158
N2—H2B···O4iv0.902.443.082 (4)129
N2—H2B···O3v0.902.633.332 (4)136
O4—H4A···O1vi0.821.972.711 (3)150
O5—H5A···O20.822.032.847 (3)174
Symmetry codes: (i) x, y+1, z; (iii) x, y, z; (iv) x+1, y, z+1/2; (v) x, y1, z; (vi) x+1, y1, z+1/2.
 

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