Supporting information
Crystallographic Information File (CIF) https://doi.org/10.1107/S0108768104004513/bm5007sup1.cif | |
Structure factor file (CIF format) https://doi.org/10.1107/S0108768104004513/bm5007sup2.fcf |
Data collection: SMART (Bruker, 2001); cell refinement: SAINT (Bruker, 2001); data reduction: SAINT; program(s) used to solve structure: SHELXS97 (Sheldrick, 1997); program(s) used to refine structure: SHELXL97 (Sheldrick, 1997); molecular graphics: KENX (Sakai, 2002); software used to prepare material for publication: SHELXL97, TEXSAN (Molecular Structure Corporation, 2001), KENX, and ORTEP (Johnson, 1976).
Cl2H14N4O10Pt2 | ? # Insert any comments here. |
Mr = 691.23 | Dx = 3.453 Mg m−3 |
Orthorhombic, P212121 | Mo Kα radiation, λ = 0.71073 Å |
Hall symbol: P 2ac 2ab | Cell parameters from 4531 reflections |
a = 7.3422 (4) Å | θ = 2.9–28.1° |
b = 12.9876 (7) Å | µ = 21.47 mm−1 |
c = 13.9429 (8) Å | T = 296 K |
V = 1329.56 (13) Å3 | Needle, pale yellow |
Z = 4 | 0.2 × 0.10 × 0.06 mm |
F(000) = 1248 |
Bruker SMART APEX CCD area detector diffractometer | 2898 independent reflections |
Radiation source: fine-focus sealed tube | 2726 reflections with I > 2σ(I) |
Graphite monochromator | Rint = 0.040 |
Detector resolution: 8.366 pixels mm-1 | θmax = 27.1°, θmin = 2.9° |
ω scans | h = −9→9 |
Absorption correction: multi-scan (SADABS; Sheldrick, 1996) | k = −16→12 |
Tmin = 0.069, Tmax = 0.264 | l = −15→17 |
7867 measured reflections |
Refinement on F2 | Hydrogen site location: inferred from neighbouring sites |
Least-squares matrix: full | H-atom parameters constrained |
R[F2 > 2σ(F2)] = 0.024 | w = 1/[σ2(Fo2)] where P = (Fo2 + 2Fc2)/3 |
wR(F2) = 0.056 | (Δ/σ)max < 0.001 |
S = 0.98 | Δρmax = 1.21 e Å−3 |
2898 reflections | Δρmin = −1.23 e Å−3 |
168 parameters | Extinction correction: SHELXL, Fc*=kFc[1+0.001xFc2λ3/sin(2θ)]-1/4 |
0 restraints | Extinction coefficient: 0.00081 (8) |
Primary atom site location: structure-invariant direct methods | Absolute structure: Flack (1983), 1361 Friedel pairs |
Secondary atom site location: difference Fourier map | Absolute structure parameter: 0.012 (12) |
Cl2H14N4O10Pt2 | V = 1329.56 (13) Å3 |
Mr = 691.23 | Z = 4 |
Orthorhombic, P212121 | Mo Kα radiation |
a = 7.3422 (4) Å | µ = 21.47 mm−1 |
b = 12.9876 (7) Å | T = 296 K |
c = 13.9429 (8) Å | 0.2 × 0.10 × 0.06 mm |
Bruker SMART APEX CCD area detector diffractometer | 2898 independent reflections |
Absorption correction: multi-scan (SADABS; Sheldrick, 1996) | 2726 reflections with I > 2σ(I) |
Tmin = 0.069, Tmax = 0.264 | Rint = 0.040 |
7867 measured reflections |
R[F2 > 2σ(F2)] = 0.024 | H-atom parameters constrained |
wR(F2) = 0.056 | Δρmax = 1.21 e Å−3 |
S = 0.98 | Δρmin = −1.23 e Å−3 |
2898 reflections | Absolute structure: Flack (1983), 1361 Friedel pairs |
168 parameters | Absolute structure parameter: 0.012 (12) |
0 restraints |
Experimental. The first 50 frames were rescanned at the end of data collection to evaluate any possible decay phenomenon. Since it was judged to be negligible, no decay correction was applied to the data. |
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. Mean-plane data from final SHELXL refinement run:- Least-squares planes (x,y,z in crystal coordinates) and deviations from them (* indicates atom used to define plane) 7.1270 (0.0037) x + 3.0328 (0.0260) y − 0.7941 (0.0284) z = 6.2499 (0.0039) * −0.0161 (0.0029) O1 * 0.0161 (0.0029) O2 * 0.0146 (0.0026) N3 * −0.0146 (0.0026) N4 0.0310 (0.0030) Pt2 0.7507 (0.0063) Pt1 Rms deviation of fitted atoms = 0.0153 7.1121 (0.0038) x − 3.1013 (0.0265) y + 0.9546 (0.0269) z = 5.4248 (0.0096) Angle to previous plane (with approximate e.s.d.) = 28.29 (0.10) * −0.0404 (0.0031) O1 * 0.0404 (0.0031) O2 * 0.0368 (0.0028) N1 * −0.0368 (0.0029) N2 0.0059 (0.0031) Pt1 0.7714 (0.0062) Pt2 Rms deviation of fitted atoms = 0.0386 |
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 | 0.87442 (5) | 0.249357 (19) | −0.015596 (18) | 0.01961 (8) | |
Pt2 | 0.87601 (4) | 0.020626 (19) | 0.031398 (19) | 0.01794 (8) | |
Cl1 | 1.0718 (3) | 0.11488 (15) | −0.31269 (16) | 0.0296 (5) | |
Cl2 | 1.0543 (3) | 0.14878 (14) | 0.33508 (16) | 0.0292 (4) | |
O1 | 0.8174 (7) | 0.1129 (4) | −0.0827 (4) | 0.0280 (13) | |
O2 | 0.8235 (7) | 0.1571 (4) | 0.1003 (4) | 0.0243 (13) | |
O3 | 1.1636 (9) | 0.0593 (5) | −0.3873 (5) | 0.052 (2) | |
O4 | 0.9658 (9) | 0.0408 (5) | −0.2563 (6) | 0.0475 (17) | |
O5 | 1.2023 (9) | 0.1631 (6) | −0.2529 (6) | 0.071 (2) | |
O6 | 0.9489 (8) | 0.1907 (5) | −0.3511 (6) | 0.061 (2) | |
O7 | 1.0152 (13) | 0.2144 (5) | 0.4129 (5) | 0.078 (3) | |
O8 | 1.0798 (7) | 0.2088 (5) | 0.2501 (5) | 0.0407 (15) | |
O9 | 0.9051 (8) | 0.0804 (5) | 0.3221 (5) | 0.0488 (17) | |
O10 | 1.2105 (10) | 0.0890 (6) | 0.3486 (8) | 0.088 (3) | |
N1 | 0.9294 (8) | 0.3279 (5) | −0.1379 (5) | 0.0281 (16) | |
H1A | 1.0490 | 0.3381 | −0.1426 | 0.042* | |
H1B | 0.8726 | 0.3884 | −0.1365 | 0.042* | |
H1C | 0.8909 | 0.2917 | −0.1881 | 0.042* | |
N2 | 0.9146 (10) | 0.3792 (4) | 0.0625 (6) | 0.036 (2) | |
H2A | 1.0332 | 0.3878 | 0.0727 | 0.053* | |
H2B | 0.8571 | 0.3735 | 0.1185 | 0.053* | |
H2C | 0.8709 | 0.4331 | 0.0305 | 0.053* | |
N3 | 0.9196 (9) | −0.1083 (4) | −0.0491 (5) | 0.0322 (17) | |
H3A | 0.8147 | −0.1414 | −0.0575 | 0.048* | |
H3B | 0.9982 | −0.1492 | −0.0190 | 0.048* | |
H3C | 0.9649 | −0.0903 | −0.1059 | 0.048* | |
N4 | 0.9178 (9) | −0.0607 (5) | 0.1527 (5) | 0.0295 (17) | |
H4A | 0.8307 | −0.1080 | 0.1589 | 0.044* | |
H4B | 0.9152 | −0.0185 | 0.2030 | 0.044* | |
H4C | 1.0258 | −0.0917 | 0.1498 | 0.044* |
U11 | U22 | U33 | U12 | U13 | U23 | |
Pt1 | 0.02276 (14) | 0.01375 (14) | 0.02233 (15) | 0.00010 (10) | −0.00278 (16) | −0.00024 (11) |
Pt2 | 0.01989 (12) | 0.01450 (13) | 0.01942 (14) | 0.00092 (11) | 0.00017 (15) | 0.00038 (10) |
Cl1 | 0.0301 (10) | 0.0272 (10) | 0.0314 (11) | 0.0014 (7) | 0.0021 (8) | −0.0056 (9) |
Cl2 | 0.0413 (11) | 0.0203 (10) | 0.0261 (11) | −0.0039 (8) | −0.0013 (8) | −0.0022 (8) |
O1 | 0.039 (3) | 0.020 (3) | 0.025 (3) | −0.006 (2) | −0.005 (2) | 0.001 (2) |
O2 | 0.031 (3) | 0.022 (3) | 0.020 (3) | 0.003 (2) | 0.001 (2) | −0.004 (2) |
O3 | 0.051 (5) | 0.050 (4) | 0.055 (5) | 0.001 (3) | 0.024 (4) | −0.013 (4) |
O4 | 0.061 (4) | 0.039 (4) | 0.042 (4) | −0.003 (3) | 0.018 (3) | 0.005 (3) |
O5 | 0.054 (4) | 0.072 (5) | 0.085 (6) | −0.014 (4) | −0.024 (4) | −0.031 (5) |
O6 | 0.054 (4) | 0.034 (4) | 0.094 (6) | 0.016 (3) | 0.005 (4) | 0.021 (4) |
O7 | 0.160 (8) | 0.033 (4) | 0.041 (4) | −0.028 (5) | 0.016 (5) | −0.017 (4) |
O8 | 0.039 (4) | 0.050 (4) | 0.033 (3) | −0.001 (3) | 0.004 (3) | 0.010 (3) |
O9 | 0.044 (4) | 0.051 (4) | 0.051 (4) | −0.018 (3) | 0.013 (3) | −0.013 (3) |
O10 | 0.062 (5) | 0.055 (5) | 0.146 (9) | 0.004 (4) | −0.005 (5) | 0.041 (6) |
N1 | 0.035 (4) | 0.018 (3) | 0.032 (4) | 0.000 (3) | −0.004 (3) | 0.003 (3) |
N2 | 0.044 (5) | 0.017 (3) | 0.047 (5) | 0.005 (3) | −0.007 (4) | −0.003 (3) |
N3 | 0.037 (4) | 0.024 (3) | 0.036 (4) | 0.007 (3) | −0.004 (3) | −0.008 (3) |
N4 | 0.036 (4) | 0.024 (3) | 0.028 (4) | 0.003 (3) | 0.005 (3) | 0.007 (3) |
Pt1—N1 | 2.027 (7) | Cl2—O7 | 1.409 (7) |
Pt1—N2 | 2.029 (6) | Cl2—O9 | 1.422 (6) |
Pt1—O2 | 2.046 (6) | Cl2—O8 | 1.431 (6) |
Pt1—O1 | 2.047 (5) | N1—H1A | 0.8900 |
Pt2—N4 | 2.018 (6) | N1—H1B | 0.8900 |
Pt2—O1 | 2.038 (6) | N1—H1C | 0.8900 |
Pt2—N3 | 2.040 (6) | N2—H2A | 0.8900 |
Pt2—O2 | 2.053 (5) | N2—H2B | 0.8900 |
Pt1—Pt2 | 3.0421 (4) | N2—H2C | 0.8900 |
Pt1—Pt1i | 3.6968 (6) | N3—H3A | 0.8900 |
Cl1—O5 | 1.416 (7) | N3—H3B | 0.8900 |
Cl1—O3 | 1.435 (7) | N3—H3C | 0.8900 |
Cl1—O6 | 1.439 (6) | N4—H4A | 0.8900 |
Cl1—O4 | 1.466 (7) | N4—H4B | 0.8900 |
Cl2—O10 | 1.398 (8) | N4—H4C | 0.8900 |
O1···O4 | 2.814 (9) | O2···O8 | 2.891 (8) |
N1—Pt1—N2 | 90.2 (3) | O6—Cl1—O4 | 108.4 (4) |
N1—Pt1—O2 | 174.4 (2) | O10—Cl2—O7 | 113.5 (6) |
N2—Pt1—O2 | 95.1 (3) | O10—Cl2—O9 | 107.6 (4) |
N1—Pt1—O1 | 95.3 (2) | O7—Cl2—O9 | 108.6 (5) |
N2—Pt1—O1 | 174.0 (3) | O10—Cl2—O8 | 107.9 (5) |
O2—Pt1—O1 | 79.5 (2) | O7—Cl2—O8 | 109.6 (4) |
N4—Pt2—O1 | 174.0 (3) | O9—Cl2—O8 | 109.6 (4) |
N4—Pt2—N3 | 90.4 (3) | Pt1—N1—H1A | 109.5 |
O1—Pt2—N3 | 94.9 (3) | Pt1—N1—H1B | 109.5 |
N4—Pt2—O2 | 95.1 (2) | H1A—N1—H1B | 109.5 |
O1—Pt2—O2 | 79.5 (2) | Pt1—N1—H1C | 109.5 |
N3—Pt2—O2 | 174.4 (3) | H1A—N1—H1C | 109.5 |
Pt2—O1—Pt1 | 96.3 (2) | H1B—N1—H1C | 109.5 |
Pt1—O2—Pt2 | 95.8 (2) | Pt1—N2—H2A | 109.5 |
N1—Pt1—Pt2 | 132.21 (19) | Pt1—N2—H2B | 109.5 |
N2—Pt1—Pt2 | 134.1 (2) | H2A—N2—H2B | 109.5 |
O2—Pt1—Pt2 | 42.17 (15) | Pt1—N2—H2C | 109.5 |
O1—Pt1—Pt2 | 41.75 (16) | H2A—N2—H2C | 109.5 |
N1—Pt1—Pt1i | 84.19 (18) | H2B—N2—H2C | 109.5 |
N2—Pt1—Pt1i | 77.8 (2) | Pt2—N3—H3A | 109.5 |
O2—Pt1—Pt1i | 95.23 (14) | Pt2—N3—H3B | 109.5 |
O1—Pt1—Pt1i | 105.11 (15) | H3A—N3—H3B | 109.5 |
Pt2—Pt1—Pt1i | 88.583 (12) | Pt2—N3—H3C | 109.5 |
N4—Pt2—Pt1 | 133.8 (2) | H3A—N3—H3C | 109.5 |
O1—Pt2—Pt1 | 41.99 (15) | H3B—N3—H3C | 109.5 |
N3—Pt2—Pt1 | 133.1 (2) | Pt2—N4—H4A | 109.5 |
O2—Pt2—Pt1 | 42.00 (16) | Pt2—N4—H4B | 109.5 |
O5—Cl1—O3 | 109.3 (5) | H4A—N4—H4B | 109.5 |
O5—Cl1—O6 | 109.9 (4) | Pt2—N4—H4C | 109.5 |
O3—Cl1—O6 | 111.6 (5) | H4A—N4—H4C | 109.5 |
O5—Cl1—O4 | 109.5 (5) | H4B—N4—H4C | 109.5 |
O3—Cl1—O4 | 107.9 (4) |
Symmetry code: (i) x+1/2, −y+1/2, −z. |
D—H···A | D—H | H···A | D···A | D—H···A |
N1—H1A···O2i | 0.89 | 2.10 | 2.947 (8) | 158 |
N2—H2A···O1i | 0.89 | 2.09 | 2.973 (9) | 171 |
N2—H2B···O5ii | 0.89 | 2.24 | 3.127 (11) | 172 |
N4—H4A···O4iii | 0.89 | 2.63 | 3.100 (10) | 114 |
N4—H4A···O6iii | 0.89 | 2.32 | 3.178 (9) | 161 |
N1—H1C···O8ii | 0.89 | 2.44 | 3.044 (8) | 125 |
N4—H4B···O9 | 0.89 | 2.10 | 2.990 (9) | 179 |
N3—H3A···O9iv | 0.89 | 2.46 | 3.007 (9) | 120 |
Symmetry codes: (i) x+1/2, −y+1/2, −z; (ii) x−1/2, −y+1/2, −z; (iii) −x+3/2, −y, z+1/2; (iv) −x+3/2, −y, z−1/2. |
Experimental details
Crystal data | |
Chemical formula | Cl2H14N4O10Pt2 |
Mr | 691.23 |
Crystal system, space group | Orthorhombic, P212121 |
Temperature (K) | 296 |
a, b, c (Å) | 7.3422 (4), 12.9876 (7), 13.9429 (8) |
V (Å3) | 1329.56 (13) |
Z | 4 |
Radiation type | Mo Kα |
µ (mm−1) | 21.47 |
Crystal size (mm) | 0.2 × 0.10 × 0.06 |
Data collection | |
Diffractometer | Bruker SMART APEX CCD area detector diffractometer |
Absorption correction | Multi-scan (SADABS; Sheldrick, 1996) |
Tmin, Tmax | 0.069, 0.264 |
No. of measured, independent and observed [I > 2σ(I)] reflections | 7867, 2898, 2726 |
Rint | 0.040 |
(sin θ/λ)max (Å−1) | 0.641 |
Refinement | |
R[F2 > 2σ(F2)], wR(F2), S | 0.024, 0.056, 0.98 |
No. of reflections | 2898 |
No. of parameters | 168 |
H-atom treatment | H-atom parameters constrained |
Δρmax, Δρmin (e Å−3) | 1.21, −1.23 |
Absolute structure | Flack (1983), 1361 Friedel pairs |
Absolute structure parameter | 0.012 (12) |
Computer programs: SMART (Bruker, 2001), SAINT (Bruker, 2001), SAINT, SHELXS97 (Sheldrick, 1997), SHELXL97 (Sheldrick, 1997), KENX (Sakai, 2002), SHELXL97, TEXSAN (Molecular Structure Corporation, 2001), KENX, and ORTEP (Johnson, 1976).
Pt1—N1 | 2.027 (7) | Pt2—O1 | 2.038 (6) |
Pt1—N2 | 2.029 (6) | Pt2—N3 | 2.040 (6) |
Pt1—O2 | 2.046 (6) | Pt2—O2 | 2.053 (5) |
Pt1—O1 | 2.047 (5) | Pt1—Pt2 | 3.0421 (4) |
Pt2—N4 | 2.018 (6) | Pt1—Pt1i | 3.6968 (6) |
O1···O4 | 2.814 (9) | O2···O8 | 2.891 (8) |
N1—Pt1—N2 | 90.2 (3) | N4—Pt2—N3 | 90.4 (3) |
N1—Pt1—O2 | 174.4 (2) | O1—Pt2—N3 | 94.9 (3) |
N2—Pt1—O2 | 95.1 (3) | N4—Pt2—O2 | 95.1 (2) |
N1—Pt1—O1 | 95.3 (2) | O1—Pt2—O2 | 79.5 (2) |
N2—Pt1—O1 | 174.0 (3) | N3—Pt2—O2 | 174.4 (3) |
O2—Pt1—O1 | 79.5 (2) | Pt2—O1—Pt1 | 96.3 (2) |
N4—Pt2—O1 | 174.0 (3) | Pt1—O2—Pt2 | 95.8 (2) |
Symmetry code: (i) x+1/2, −y+1/2, −z. |
D—H···A | D—H | H···A | D···A | D—H···A |
N1—H1A···O2i | 0.89 | 2.10 | 2.947 (8) | 158 |
N2—H2A···O1i | 0.89 | 2.09 | 2.973 (9) | 171 |
N2—H2B···O5ii | 0.89 | 2.24 | 3.127 (11) | 172 |
N4—H4A···O6iii | 0.89 | 2.32 | 3.178 (9) | 161 |
N1—H1C···O8ii | 0.89 | 2.44 | 3.044 (8) | 125 |
N4—H4B···O9 | 0.89 | 2.10 | 2.990 (9) | 179 |
N3—H3A···O9iv | 0.89 | 2.46 | 3.007 (9) | 120 |
Symmetry codes: (i) x+1/2, −y+1/2, −z; (ii) x−1/2, −y+1/2, −z; (iii) −x+3/2, −y, z+1/2; (iv) −x+3/2, −y, z−1/2. |
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