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The title compound, [PtCl
2(C
2H
8N
2)
4](HSO
4)
4 or [Pt(C
2H
8N
2)
2][Pt
2Cl
2(C
2H
8N
2)
2](HSO
4)
4, has a linear chain structure composed of square-planar [Pt(en)
2]
2+ and elongated octahedral
trans-[PtCl
2(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—Pt
IV—Cl
Pt
II chain, which lies on a twofold axis. The Pt
IV—Cl and Pt
IICl bond lengths are 2.323 (2) and 3.142 (2) Å, respectively. A structural parameter δ = (Pt
IV—Cl)/(Pt
IICl), 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
CCDC reference: 202974
Key indicators
- Single-crystal X-ray study
- T = 295 K
- Mean (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
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
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)4 | Dx = 2.48 Mg m−3 |
Mr = 1089.77 | Melting point: not measured K |
Orthorhombic, Ibam | Mo Kα radiation, λ = 0.71069 Å |
a = 9.261 (1) Å | Cell parameters from 50 reflections |
b = 14.422 (2) Å | θ = 10.0–14.6° |
c = 10.929 (1) Å | µ = 10.12 mm−1 |
V = 1459.7 (3) Å3 | T = 295 K |
Z = 2 | Needle, intense red |
F(000) = 1044 | 0.28 × 0.16 × 0.12 mm |
Data collection top
Rigaku AFC-5S diffractometer | 975 reflections with F > 3σ(F) |
Radiation source: X-ray tube | Rint = 0.029 |
Graphite monochromator | θmax = 32.5°, θmin = 1.5° |
θ/2θ scans | h = 0→14 |
Absorption correction: gaussian (Coppens et al., 1965) | k = 0→21 |
Tmin = 0.187, Tmax = 0.702 | l = −16→16 |
3059 measured reflections | 3 standard reflections every 50 reflections |
1387 independent reflections | intensity decay: none |
Refinement top
Refinement on F2 | Secondary atom site location: difference Fourier map |
Least-squares matrix: full | Hydrogen site location: inferred from neighbouring sites |
R[F2 > 2σ(F2)] = 0.024 | H-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 reflections | Δρmax = 1.51 e Å−3 |
68 parameters | Δρmin = −1.19 e Å−3 |
0 restraints | Extinction correction: SHELXL97, Fc*=kFc[1+0.001xFc2λ3/sin(2θ)]-1/4 |
Primary atom site location: heavy-atom method | Extinction coefficient: 0.0054 (2) |
Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top | x | y | z | Uiso*/Ueq | Occ. (<1) |
Pt | 0.0000 | 0.0000 | 0.2500 | 0.02543 (10) | |
Cl | 0.0000 | 0.0000 | 0.0375 (2) | 0.0377 (5) | .5 |
S | 0.38104 (19) | 0.21958 (12) | 0.0000 | 0.0435 (3) | |
O1 | 0.5028 (13) | 0.2396 (9) | 0.0858 (10) | 0.073 (3) | .5 |
O2 | 0.3372 (9) | 0.1267 (4) | 0.0000 | 0.100 (3) | |
O3 | 0.2708 (9) | 0.2814 (6) | 0.0389 (13) | 0.117 (7) | .5 |
O4 | 0.4300 (15) | 0.2442 (8) | −0.1248 (9) | 0.080 (4) | .5 |
N | 0.1654 (4) | 0.0935 (2) | 0.2484 (4) | 0.0416 (7) | |
C | 0.3014 (5) | 0.0456 (4) | 0.2821 (6) | 0.0607 (15) | |
H1O | 0.5787 | 0.2419 | 0.0473 | 0.109* | .5 |
H1N | 0.1740 | 0.1186 | 0.1733 | 0.062* | |
H2N | 0.1472 | 0.1394 | 0.3020 | 0.062* | |
H1C | 0.3060 | 0.0365 | 0.3700 | 0.091* | |
H2C | 0.3841 | 0.0822 | 0.2571 | 0.091* | |
Atomic displacement parameters (Å2) top | U11 | U22 | U33 | U12 | U13 | U23 |
Pt | 0.02861 (14) | 0.02775 (13) | 0.01993 (12) | 0.000 | 0.000 | 0.000 |
Cl | 0.0447 (12) | 0.0469 (12) | 0.0215 (8) | 0.0042 (15) | 0.000 | 0.000 |
S | 0.0386 (8) | 0.0427 (7) | 0.0492 (9) | −0.0082 (7) | 0.000 | 0.000 |
O1 | 0.057 (5) | 0.090 (7) | 0.071 (7) | −0.010 (7) | −0.032 (6) | −0.019 (6) |
O2 | 0.163 (8) | 0.052 (3) | 0.086 (4) | −0.056 (4) | 0.000 | 0.000 |
O3 | 0.041 (4) | 0.130 (6) | 0.18 (2) | 0.005 (4) | −0.007 (6) | −0.095 (11) |
O4 | 0.135 (14) | 0.059 (5) | 0.048 (5) | 0.012 (7) | −0.001 (6) | 0.005 (4) |
N | 0.0401 (16) | 0.0415 (15) | 0.0431 (17) | −0.0098 (13) | 0.005 (2) | −0.003 (2) |
C | 0.034 (2) | 0.078 (4) | 0.070 (4) | −0.013 (2) | −0.006 (2) | 0.006 (3) |
Geometric parameters (Å, º) top
Pt—Cl | 2.323 (2) | N—C | 1.483 (7) |
Pt—Cli | 3.142 (2) | C—Cii | 1.491 (12) |
Cl—Cli | 0.819 (5) | O1—H1O | 0.8200 |
Pt—N | 2.041 (3) | N—H1N | 0.9000 |
S—O1 | 1.494 (10) | N—H2N | 0.9000 |
S—O2 | 1.400 (5) | C—H1C | 0.9700 |
S—O3 | 1.420 (8) | C—H2C | 0.9700 |
S—O4 | 1.480 (11) | | |
| | | |
Niii—Pt—N | 179.0 (2) | O3v—S—O1 | 127.4 (7) |
N—Pt—Niv | 97.3 (2) | O4v—S—O1 | 31.2 (6) |
N—Pt—Nii | 82.7 (2) | O2—S—O1v | 113.8 (6) |
N—Pt—Cl | 89.50 (11) | O3v—S—O1v | 103.5 (6) |
N—Pt—Cliv | 90.50 (11) | O3—S—O1v | 127.4 (7) |
Cl—Pt—Cliv | 180.0 | O4v—S—O1v | 107.5 (8) |
Cl—Pt—Cli | 0.0 | O4—S—O1v | 31.2 (6) |
Cli—Pt—Cliv | 180.0 | O1—S—O1v | 77.7 (10) |
Cli—Cl—Pt | 180.0 | C—N—Pt | 109.1 (3) |
O1—S—O2 | 113.8 (6) | N—C—Cii | 107.1 (4) |
O1—S—O3 | 103.5 (6) | S—O1—H1O | 109.5 |
O1—S—O4 | 107.5 (8) | C—N—H1N | 109.9 |
O2—S—O3 | 113.1 (5) | Pt—N—H1N | 109.9 |
O2—S—O4 | 108.6 (5) | C—N—H2N | 109.9 |
O3—S—O4 | 110.2 (8) | Pt—N—H2N | 109.9 |
O2—S—O3v | 113.1 (5) | H1N—N—H2N | 108.3 |
O3v—S—O3 | 34.8 (12) | N—C—H1C | 110.3 |
O2—S—O4v | 108.6 (5) | Cii—C—H1C | 110.3 |
O3v—S—O4v | 110.2 (8) | N—C—H2C | 110.3 |
O3—S—O4v | 78.1 (7) | Cii—C—H2C | 110.3 |
O3v—S—O4 | 78.1 (7) | H1C—C—H2C | 108.6 |
O4v—S—O4 | 134.2 (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···A | D—H | H···A | D···A | D—H···A |
N—H2N···O4vi | 0.90 | 1.99 | 2.860 (11) | 162 |
N—H2N···O3vii | 0.90 | 2.22 | 3.002 (12) | 146 |
N—H1N···O2 | 0.90 | 2.43 | 3.182 (5) | 142 |
O1—H1O···O3viii | 0.82 | 2.04 | 2.848 (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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