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The title compound, [PtCl2(C2H8N2)4](HSO4)4 or [Pt(C2H8N2)2][Pt2Cl2(C2H8N2)2](HSO4)4, has a linear chain structure composed of square-planar [Pt(en)2]2+ and elongated octahedral trans-[PtCl2(en)2]2+ cations (en is ethyl­enedi­amine) stacked alternately, bridged by the Cl atoms, along the c axis. The Cl atom bridging the adjacent Pt atoms is disordered over two sites along the ...Cl—PtIV—Cl...PtII... chain, which lies on a twofold axis. The PtIV—Cl and PtII...Cl bond lengths are 2.323 (2) and 3.142 (2) Å, respectively. A structural parameter δ = (PtIV—Cl)/(PtII...Cl), indicating the mixed-valence state of the Pt atom (δ = 0.739), shows a good correlation with the data of the intervalence charge-transfer (IVCT) absorption band.

Supporting information

cif

Crystallographic Information File (CIF) https://doi.org/10.1107/S1600536802022584/ob6201sup1.cif
Contains datablocks global, I

hkl

Structure factor file (CIF format) https://doi.org/10.1107/S1600536802022584/ob6201Isup2.hkl
Contains datablock I

CCDC reference: 202974

Key indicators

  • Single-crystal X-ray study
  • T = 295 K
  • Mean [sigma](C-C) = 0.008 Å
  • Disorder in solvent or counterion
  • R factor = 0.024
  • wR factor = 0.048
  • Data-to-parameter ratio = 14.3

checkCIF results

No syntax errors found

ADDSYM reports no extra symmetry


Yellow Alert Alert Level C:
PLAT_302 Alert C Anion/Solvent Disorder ....................... 38.00 Perc.
0 Alert Level A = Potentially serious problem
0 Alert Level B = Potential problem
1 Alert Level C = Please check

Computing details top

Data collection: AFC Diffractometer Control Software (Rigaku, 1987); cell refinement: AFC Diffractometer Control Software; data reduction: a handmade program; program(s) used to solve structure: UNICS3 (Sakurai & Kobayashi, 1979); program(s) used to refine structure: SHELXL97 (Sheldrick, 1997); molecular graphics: ORTEPII (Johnson, 1976).

catena-Poly[bis(ethylenediamine)platinum(II,IV)-µ-chloro bis(hydrogensulfate)] top
Crystal data top
[Pt2Cl2(C2H8N2)4](HSO4)4Dx = 2.48 Mg m3
Mr = 1089.77Melting point: not measured K
Orthorhombic, IbamMo Kα radiation, λ = 0.71069 Å
a = 9.261 (1) ÅCell parameters from 50 reflections
b = 14.422 (2) Åθ = 10.0–14.6°
c = 10.929 (1) ŵ = 10.12 mm1
V = 1459.7 (3) Å3T = 295 K
Z = 2Needle, intense red
F(000) = 10440.28 × 0.16 × 0.12 mm
Data collection top
Rigaku AFC-5S
diffractometer
975 reflections with F > 3σ(F)
Radiation source: X-ray tubeRint = 0.029
Graphite monochromatorθmax = 32.5°, θmin = 1.5°
θ/2θ scansh = 014
Absorption correction: gaussian
(Coppens et al., 1965)
k = 021
Tmin = 0.187, Tmax = 0.702l = 1616
3059 measured reflections3 standard reflections every 50 reflections
1387 independent reflections intensity decay: none
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)] = 0.024H-atom parameters constrained
wR(F2) = 0.048 w = 1/[σ2(Fo2) + (0.0266P)2]
where P = (Fo2 + 2Fc2)/3
S = 1.14(Δ/σ)max < 0.001
975 reflectionsΔρmax = 1.51 e Å3
68 parametersΔρmin = 1.19 e Å3
0 restraintsExtinction correction: SHELXL97, Fc*=kFc[1+0.001xFc2λ3/sin(2θ)]-1/4
Primary atom site location: heavy-atom methodExtinction coefficient: 0.0054 (2)
Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top
xyzUiso*/UeqOcc. (<1)
Pt0.00000.00000.25000.02543 (10)
Cl0.00000.00000.0375 (2)0.0377 (5).5
S0.38104 (19)0.21958 (12)0.00000.0435 (3)
O10.5028 (13)0.2396 (9)0.0858 (10)0.073 (3).5
O20.3372 (9)0.1267 (4)0.00000.100 (3)
O30.2708 (9)0.2814 (6)0.0389 (13)0.117 (7).5
O40.4300 (15)0.2442 (8)0.1248 (9)0.080 (4).5
N0.1654 (4)0.0935 (2)0.2484 (4)0.0416 (7)
C0.3014 (5)0.0456 (4)0.2821 (6)0.0607 (15)
H1O0.57870.24190.04730.109*.5
H1N0.17400.11860.17330.062*
H2N0.14720.13940.30200.062*
H1C0.30600.03650.37000.091*
H2C0.38410.08220.25710.091*
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
Pt0.02861 (14)0.02775 (13)0.01993 (12)0.0000.0000.000
Cl0.0447 (12)0.0469 (12)0.0215 (8)0.0042 (15)0.0000.000
S0.0386 (8)0.0427 (7)0.0492 (9)0.0082 (7)0.0000.000
O10.057 (5)0.090 (7)0.071 (7)0.010 (7)0.032 (6)0.019 (6)
O20.163 (8)0.052 (3)0.086 (4)0.056 (4)0.0000.000
O30.041 (4)0.130 (6)0.18 (2)0.005 (4)0.007 (6)0.095 (11)
O40.135 (14)0.059 (5)0.048 (5)0.012 (7)0.001 (6)0.005 (4)
N0.0401 (16)0.0415 (15)0.0431 (17)0.0098 (13)0.005 (2)0.003 (2)
C0.034 (2)0.078 (4)0.070 (4)0.013 (2)0.006 (2)0.006 (3)
Geometric parameters (Å, º) top
Pt—Cl2.323 (2)N—C1.483 (7)
Pt—Cli3.142 (2)C—Cii1.491 (12)
Cl—Cli0.819 (5)O1—H1O0.8200
Pt—N2.041 (3)N—H1N0.9000
S—O11.494 (10)N—H2N0.9000
S—O21.400 (5)C—H1C0.9700
S—O31.420 (8)C—H2C0.9700
S—O41.480 (11)
Niii—Pt—N179.0 (2)O3v—S—O1127.4 (7)
N—Pt—Niv97.3 (2)O4v—S—O131.2 (6)
N—Pt—Nii82.7 (2)O2—S—O1v113.8 (6)
N—Pt—Cl89.50 (11)O3v—S—O1v103.5 (6)
N—Pt—Cliv90.50 (11)O3—S—O1v127.4 (7)
Cl—Pt—Cliv180.0O4v—S—O1v107.5 (8)
Cl—Pt—Cli0.0O4—S—O1v31.2 (6)
Cli—Pt—Cliv180.0O1—S—O1v77.7 (10)
Cli—Cl—Pt180.0C—N—Pt109.1 (3)
O1—S—O2113.8 (6)N—C—Cii107.1 (4)
O1—S—O3103.5 (6)S—O1—H1O109.5
O1—S—O4107.5 (8)C—N—H1N109.9
O2—S—O3113.1 (5)Pt—N—H1N109.9
O2—S—O4108.6 (5)C—N—H2N109.9
O3—S—O4110.2 (8)Pt—N—H2N109.9
O2—S—O3v113.1 (5)H1N—N—H2N108.3
O3v—S—O334.8 (12)N—C—H1C110.3
O2—S—O4v108.6 (5)Cii—C—H1C110.3
O3v—S—O4v110.2 (8)N—C—H2C110.3
O3—S—O4v78.1 (7)Cii—C—H2C110.3
O3v—S—O478.1 (7)H1C—C—H2C108.6
O4v—S—O4134.2 (10)
Symmetry codes: (i) x, y, z; (ii) x, y, z+1/2; (iii) x, y, z; (iv) x, y, z+1/2; (v) x, y, z.
Hydrogen-bond geometry (Å, º) top
D—H···AD—HH···AD···AD—H···A
N—H2N···O4vi0.901.992.860 (11)162
N—H2N···O3vii0.902.223.002 (12)146
N—H1N···O20.902.433.182 (5)142
O1—H1O···O3viii0.822.042.848 (14)168
Symmetry codes: (vi) x+1/2, y+1/2, z+1/2; (vii) x+1/2, y+1/2, z+1/2; (viii) x+1/2, y+1/2, z.
 

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