Supporting information
Crystallographic Information File (CIF) https://doi.org/10.1107/S1600536803014521/ob6266sup1.cif | |
Structure factor file (CIF format) https://doi.org/10.1107/S1600536803014521/ob6266Isup2.hkl |
CCDC reference: 221615
Key indicators
- Single-crystal X-ray study
- T = 296 K
- Mean (C-C) = 0.013 Å
- Disorder in solvent or counterion
- R factor = 0.035
- wR factor = 0.062
- Data-to-parameter ratio = 10.5
checkCIF results
No syntax errors found ADDSYM reports no extra symmetry
Alert Level B:
THETM_01 Alert B The value of sine(theta_max)/wavelength is less than 0.575 Calculated sin(theta_max)/wavelength = 0.5554
Alert Level C:
RINTA_01 Alert C The value of Rint is greater than 0.10 Rint given 0.116 PLAT_302 Alert C Anion/Solvent Disorder ......................... 17.00 Perc.
0 Alert Level A = Potentially serious problem
1 Alert Level B = Potential problem
2 Alert Level C = Please check
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 ORTEPII (Johnson, 1976).
[Pt2(C7H8N2O)2(NH3)4](ClO4)4 | F(000) = 2144 |
Mr = 1128.42 | Dx = 2.416 Mg m−3 |
Orthorhombic, Pnma | Mo Kα radiation, λ = 0.71073 Å |
Hall symbol: -P 2ac 2n | Cell parameters from 2336 reflections |
a = 17.9590 (7) Å | θ = 2.3–22.0° |
b = 17.0728 (7) Å | µ = 9.44 mm−1 |
c = 10.1189 (4) Å | T = 296 K |
V = 3102.6 (2) Å3 | Prism, pale green |
Z = 4 | 0.06 × 0.05 × 0.03 mm |
Bruker SMART APEX CCD-detector diffractometer | 2317 independent reflections |
Radiation source: fine-focus sealed tube | 1576 reflections with I > 2σ(I) |
Graphite monochromator | Rint = 0.117 |
Detector resolution: 8.366 pixels mm-1 | θmax = 23.3°, θmin = 2.3° |
ω scans | h = −19→19 |
Absorption correction: multi-scan (SADABS; Sheldrick, 1996) | k = −18→18 |
Tmin = 0.540, Tmax = 0.753 | l = −11→8 |
16797 measured reflections |
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)] = 0.035 | Hydrogen site location: inferred from neighbouring sites |
wR(F2) = 0.062 | H-atom parameters constrained |
S = 0.88 | w = 1/[σ2(Fo2) + (0.0194P)2] where P = (Fo2 + 2Fc2)/3 |
2317 reflections | (Δ/σ)max = 0.001 |
221 parameters | Δρmax = 1.43 e Å−3 |
0 restraints | Δρmin = −0.66 e Å−3 |
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) 2.2104 (0.0689) x - 0.0000 (0.0000) y + 10.0420 (0.0048) z = 7.5908 (0.0136) * 0.0000 (0.0000) N1 * 0.0000 (0.0000) N3 * 0.0000 (0.0000) N1_$2 * 0.0000 (0.0000) N3_$2 0.0666 (0.0053) Pt1 2.8762 (0.0071) Pt2 Rms deviation of fitted atoms = 0.0000 - 9.1575 (0.0541) x + 0.0000 (0.0002) y + 8.7046 (0.0181) z = 7.0753 (0.0279) Angle to previous plane (with approximate e.s.d.) = 37.73 (0.23) * 0.0000 (0.0000) O1 * 0.0000 (0.0000) N2 * 0.0000 (0.0000) O1_$2 * 0.0000 (0.0000) N2_$2 - 3.0082 (0.0052) Pt1 - 0.0489 (0.0048) Pt2 Rms deviation of fitted atoms = 0.0000 12.1367 (0.2207) x - 11.9206 (0.2258) y + 2.3898 (0.0576) z = 1.6468 (0.1032) Angle to previous plane (with approximate e.s.d.) = 81.87 (0.48) * 0.0000 (0.0000) O1 * 0.0000 (0.0000) C1 * 0.0000 (0.0000) N3 Rms deviation of fitted atoms = 0.0000 8.9020 (0.0587) x - 8.0276 (0.0551) y + 7.3889 (0.0285) z = 5.7518 (0.0220) Angle to previous plane (with approximate e.s.d.) = 33.31 (0.91) * 0.0150 (0.0066) C2 * -0.0100 (0.0071) C3 * 0.0001 (0.0072) C4 * 0.0005 (0.0066) C5 * -0.0104 (0.0067) C6 * 0.0049 (0.0065) N4 Rms deviation of fitted atoms = 0.0087 2.2031 (0.0689) x - 0.7756 (0.0613) y + 10.0319 (0.0051) z = 7.4546 (0.0208) Angle to previous plane (with approximate e.s.d.) = 36.28 (1/3) * 0.0000 (0.0000) N1 * 0.0000 (0.0000) Pt1 * 0.0000 (0.0000) N3 Rms deviation of fitted atoms = 0.0000 - 9.1594 (0.0541) x + 0.5871 (0.0572) y + 8.6969 (0.0183) z = 7.1652 (0.0295) Angle to previous plane (with approximate e.s.d.) = 38.00 (0.23) * 0.0000 (0.0000) N2 * 0.0000 (0.0000) Pt2 * 0.0000 (0.0000) O1 Rms deviation of fitted atoms = 0.0000 12.1367 (0.2207) x - 11.9206 (0.2258) y + 2.3898 (0.0576) z = 1.6468 (0.1032) Angle to previous plane (with approximate e.s.d.) = 80.46 (1/2) * 0.0000 (0.0000) O1 * 0.0000 (0.0000) C1 * 0.0000 (0.0000) N3 Rms deviation of fitted atoms = 0.0000 8.9020 (0.0587) x - 8.0276 (0.0551) y + 7.3889 (0.0285) z = 5.7518 (0.0220) Angle to previous plane (with approximate e.s.d.) = 33.31 (0.91) * 0.0150 (0.0066) C2 * -0.0100 (0.0071) C3 * 0.0001 (0.0072) C4 * 0.0005 (0.0066) C5 * -0.0104 (0.0067) C6 * 0.0049 (0.0065) N4 Rms deviation of fitted atoms = 0.0087 12.1367 (0.2207) x - 11.9206 (0.2258) y + 2.3898 (0.0576) z = 1.6468 (0.1032) Angle to previous plane (with approximate e.s.d.) = 33.31 (0.91) * 0.0000 (0.0000) O1 * 0.0000 (0.0000) C1 * 0.0000 (0.0000) N3 Rms deviation of fitted atoms = 0.0000 2.2031 (0.0689) x - 0.7756 (0.0613) y + 10.0319 (0.0051) z = 7.4546 (0.0208) Angle to previous plane (with approximate e.s.d.) = 69.59 (0.42) * 0.0000 (0.0000) N1 * 0.0000 (0.0000) Pt1 * 0.0000 (0.0000) N3 Rms deviation of fitted atoms = 0.0000 8.9020 (0.0587) x - 8.0276 (0.0551) y + 7.3889 (0.0285) z = 5.7518 (0.0220) Angle to previous plane (with approximate e.s.d.) = 36.28 (1/3) * 0.0150 (0.0066) C2 * -0.0100 (0.0071) C3 * 0.0001 (0.0072) C4 * 0.0005 (0.0066) C5 * -0.0104 (0.0067) C6 * 0.0049 (0.0065) N4 3.2593 (0.0165) C2_$4 3.2843 (0.0170) C3_$4 3.2743 (0.0165) C4_$4 3.2739 (0.0166) C5_$4 3.2848 (0.0165) C6_$4 3.2694 (0.0167) N4_$4 Rms deviation of fitted atoms = 0.0087 |
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 | Occ. (<1) | |
Pt1 | 0.23213 (3) | 0.2500 | 0.71144 (6) | 0.03159 (17) | |
Pt2 | 0.18482 (3) | 0.2500 | 1.00164 (6) | 0.03133 (16) | |
Cl1 | 0.23659 (17) | 0.02242 (15) | 0.4016 (3) | 0.0449 (7) | |
Cl2 | 0.3939 (3) | 0.2500 | 0.3650 (5) | 0.0643 (13) | |
Cl3 | 0.4567 (2) | 0.2500 | 0.9050 (4) | 0.0437 (10) | |
O1 | 0.1145 (3) | 0.1655 (4) | 0.9333 (7) | 0.0468 (19) | |
O2 | 0.2474 (4) | 0.0326 (5) | 0.2665 (7) | 0.086 (3) | |
O3 | 0.1775 (4) | −0.0338 (4) | 0.4210 (8) | 0.076 (2) | |
O4 | 0.2140 (4) | 0.0932 (4) | 0.4580 (8) | 0.086 (3) | |
O5 | 0.3029 (4) | −0.0059 (4) | 0.4624 (7) | 0.072 (3) | |
O6 | 0.4070 (9) | 0.2500 | 0.2335 (14) | 0.129 (5) | |
O7 | 0.3148 (12) | 0.2500 | 0.365 (2) | 0.193 (9) | |
O8 | 0.4091 (7) | 0.1827 (7) | 0.4249 (11) | 0.189 (6) | |
O9 | 0.4660 (5) | 0.2500 | 0.7644 (9) | 0.054 (3) | |
O10A | 0.4133 (6) | 0.1802 (6) | 0.9417 (10) | 0.072 (3)* | 0.740 (9) |
O10B | 0.4988 (16) | 0.1797 (18) | 0.952 (3) | 0.072 (3)* | 0.260 (9) |
O11A | 0.5245 (8) | 0.2500 | 0.9767 (15) | 0.072 (3)* | 0.740 (9) |
O11B | 0.376 (2) | 0.2500 | 0.942 (4) | 0.072 (3)* | 0.260 (17) |
N1 | 0.3103 (4) | 0.1637 (4) | 0.6876 (8) | 0.047 (2) | |
H4 | 0.3204 | 0.1580 | 0.6021 | 0.071* | |
H2 | 0.2927 | 0.1188 | 0.7197 | 0.071* | |
H3 | 0.3516 | 0.1768 | 0.7307 | 0.071* | |
N2 | 0.2534 (4) | 0.1679 (4) | 1.0794 (8) | 0.041 (2) | |
H6 | 0.2533 | 0.1718 | 1.1671 | 0.062* | |
H7 | 0.2994 | 0.1753 | 1.0493 | 0.062* | |
H5 | 0.2377 | 0.1204 | 1.0560 | 0.062* | |
N3 | 0.1554 (4) | 0.1647 (4) | 0.7217 (7) | 0.032 (2) | |
H1 | 0.1497 | 0.1395 | 0.6489 | 0.039* | |
N4 | −0.0258 (4) | −0.0557 (4) | 0.7497 (9) | 0.037 (2) | |
C1 | 0.1138 (5) | 0.1408 (5) | 0.8136 (10) | 0.032 (3) | |
C2 | 0.0614 (5) | 0.0740 (5) | 0.7868 (9) | 0.029 (2) | |
C3 | 0.0809 (5) | 0.0164 (6) | 0.6974 (10) | 0.042 (3) | |
H8 | 0.1241 | 0.0214 | 0.6475 | 0.050* | |
C4 | 0.0364 (5) | −0.0477 (6) | 0.6827 (11) | 0.049 (3) | |
H9 | 0.0504 | −0.0868 | 0.6238 | 0.058* | |
C5 | −0.0474 (5) | −0.0013 (6) | 0.8343 (10) | 0.041 (3) | |
H10 | −0.0916 | −0.0076 | 0.8811 | 0.049* | |
C6 | −0.0047 (5) | 0.0649 (6) | 0.8532 (10) | 0.036 (3) | |
H11 | −0.0207 | 0.1037 | 0.9112 | 0.043* | |
C7 | −0.0708 (5) | −0.1290 (5) | 0.7344 (11) | 0.064 (4) | |
H14 | −0.0658 | −0.1605 | 0.8125 | 0.096* | |
H12 | −0.0532 | −0.1579 | 0.6592 | 0.096* | |
H13 | −0.1222 | −0.1156 | 0.7219 | 0.096* |
U11 | U22 | U33 | U12 | U13 | U23 | |
Pt1 | 0.0360 (3) | 0.0274 (3) | 0.0314 (3) | 0.000 | 0.0042 (3) | 0.000 |
Pt2 | 0.0367 (3) | 0.0287 (3) | 0.0286 (3) | 0.000 | 0.0001 (3) | 0.000 |
Cl1 | 0.0616 (19) | 0.0376 (16) | 0.0356 (16) | 0.0049 (16) | 0.0014 (17) | −0.0004 (13) |
Cl2 | 0.095 (4) | 0.064 (3) | 0.034 (3) | 0.000 | 0.013 (3) | 0.000 |
Cl3 | 0.043 (2) | 0.051 (3) | 0.037 (2) | 0.000 | −0.003 (2) | 0.000 |
O1 | 0.043 (4) | 0.061 (5) | 0.036 (4) | −0.012 (4) | −0.001 (4) | −0.005 (4) |
O2 | 0.114 (7) | 0.113 (7) | 0.031 (5) | 0.038 (5) | 0.016 (5) | 0.024 (4) |
O3 | 0.080 (6) | 0.072 (6) | 0.077 (6) | −0.028 (5) | −0.004 (5) | −0.001 (5) |
O4 | 0.102 (7) | 0.048 (5) | 0.107 (8) | 0.010 (5) | −0.002 (6) | −0.040 (5) |
O5 | 0.067 (6) | 0.084 (6) | 0.065 (6) | 0.014 (5) | −0.013 (5) | 0.015 (5) |
O6 | 0.184 (15) | 0.139 (13) | 0.065 (11) | 0.000 | −0.003 (11) | 0.000 |
O7 | 0.189 (19) | 0.178 (19) | 0.21 (2) | 0.000 | 0.043 (18) | 0.000 |
O8 | 0.283 (15) | 0.145 (11) | 0.140 (10) | 0.057 (11) | −0.018 (11) | 0.101 (9) |
O9 | 0.069 (7) | 0.075 (7) | 0.017 (6) | 0.000 | 0.009 (5) | 0.000 |
N1 | 0.052 (5) | 0.033 (5) | 0.056 (6) | −0.001 (4) | 0.002 (5) | −0.002 (4) |
N2 | 0.044 (6) | 0.037 (5) | 0.043 (5) | −0.006 (4) | 0.005 (5) | 0.003 (4) |
N3 | 0.040 (5) | 0.034 (5) | 0.023 (5) | −0.008 (4) | 0.004 (4) | −0.007 (4) |
N4 | 0.032 (5) | 0.029 (5) | 0.051 (7) | −0.001 (4) | −0.006 (5) | −0.008 (5) |
C1 | 0.035 (6) | 0.028 (6) | 0.033 (7) | −0.004 (5) | −0.003 (6) | 0.000 (5) |
C2 | 0.028 (6) | 0.029 (6) | 0.029 (6) | 0.001 (5) | −0.007 (6) | 0.005 (5) |
C3 | 0.031 (6) | 0.042 (6) | 0.053 (7) | −0.006 (5) | 0.013 (6) | −0.011 (6) |
C4 | 0.036 (7) | 0.048 (7) | 0.062 (9) | 0.005 (6) | 0.012 (7) | −0.023 (6) |
C5 | 0.026 (7) | 0.042 (7) | 0.055 (8) | −0.003 (6) | 0.005 (6) | 0.001 (6) |
C6 | 0.036 (6) | 0.032 (6) | 0.040 (7) | 0.009 (5) | 0.009 (6) | −0.013 (6) |
C7 | 0.050 (7) | 0.040 (7) | 0.102 (11) | −0.023 (6) | −0.006 (7) | −0.001 (7) |
Pt1—N3 | 2.007 (7) | Cl2—O6 | 1.351 (13) |
Pt1—N1 | 2.049 (7) | Cl2—O7 | 1.420 (19) |
Pt1—Pt2 | 3.0569 (8) | Cl3—O11A | 1.417 (15) |
Pt2—N2 | 2.025 (6) | Cl3—O9 | 1.432 (9) |
Pt2—O1 | 2.038 (6) | Cl3—O10A | 1.472 (10) |
Pt1—Pt2i | 7.2325 (9) | Cl3—O11B | 1.50 (4) |
O1—C1 | 1.282 (10) | Cl3—O10B | 1.50 (3) |
N3—C1 | 1.260 (10) | N1—H4 | 0.8900 |
N4—C4 | 1.313 (11) | N1—H2 | 0.8900 |
N4—C5 | 1.322 (11) | N1—H3 | 0.8900 |
N4—C7 | 1.498 (10) | N2—H6 | 0.8900 |
C1—C2 | 1.505 (11) | N2—H7 | 0.8900 |
C2—C6 | 1.372 (11) | N2—H5 | 0.8900 |
C2—C3 | 1.381 (12) | N3—H1 | 0.8600 |
C3—C4 | 1.364 (12) | C3—H8 | 0.9300 |
C5—C6 | 1.380 (12) | C4—H9 | 0.9300 |
Cl1—O2 | 1.392 (7) | C5—H10 | 0.9300 |
Cl1—O4 | 1.397 (7) | C6—H11 | 0.9300 |
Cl1—O5 | 1.424 (7) | C7—H14 | 0.9600 |
Cl1—O3 | 1.444 (7) | C7—H12 | 0.9600 |
Cl2—O8 | 1.327 (9) | C7—H13 | 0.9600 |
N3—Pt1—N3ii | 93.0 (4) | O11A—Cl3—O9 | 114.2 (8) |
N3—Pt1—N1ii | 176.2 (3) | O11A—Cl3—O10A | 109.1 (6) |
N3—Pt1—N1 | 87.4 (3) | O9—Cl3—O10A | 108.2 (5) |
N1ii—Pt1—N1 | 91.9 (4) | O10A—Cl3—O10Aii | 108.0 (8) |
N3—Pt1—Pt2 | 76.1 (2) | O9—Cl3—O11B | 111.3 (17) |
N1—Pt1—Pt2 | 107.7 (2) | O9—Cl3—O10B | 105.0 (12) |
N2ii—Pt2—N2 | 87.6 (4) | O11B—Cl3—O10B | 114.1 (13) |
N2ii—Pt2—O1 | 177.0 (3) | O10Bii—Cl3—O10B | 107 (2) |
N2—Pt2—O1 | 91.1 (3) | Pt1—N1—H4 | 109.5 |
O1—Pt2—O1ii | 90.1 (4) | Pt1—N1—H2 | 109.5 |
N2—Pt2—Pt1 | 101.8 (2) | H4—N1—H2 | 109.5 |
O1—Pt2—Pt1 | 81.15 (18) | Pt1—N1—H3 | 109.5 |
C1—O1—Pt2 | 124.0 (6) | H4—N1—H3 | 109.5 |
C1—N3—Pt1 | 132.8 (7) | H2—N1—H3 | 109.5 |
C4—N4—C5 | 120.8 (8) | Pt2—N2—H6 | 109.5 |
C4—N4—C7 | 119.5 (8) | Pt2—N2—H7 | 109.5 |
C5—N4—C7 | 119.7 (8) | H6—N2—H7 | 109.5 |
N3—C1—O1 | 125.8 (9) | Pt2—N2—H5 | 109.5 |
N3—C1—C2 | 118.9 (9) | H6—N2—H5 | 109.5 |
O1—C1—C2 | 115.2 (9) | H7—N2—H5 | 109.5 |
C6—C2—C3 | 117.4 (8) | C1—N3—H1 | 113.6 |
C6—C2—C1 | 122.6 (9) | Pt1—N3—H1 | 113.6 |
C3—C2—C1 | 120.0 (8) | C4—C3—H8 | 120.2 |
C4—C3—C2 | 119.6 (9) | C2—C3—H8 | 120.2 |
N4—C4—C3 | 121.7 (9) | N4—C4—H9 | 119.2 |
N4—C5—C6 | 120.1 (9) | C3—C4—H9 | 119.2 |
C2—C6—C5 | 120.4 (9) | N4—C5—H10 | 119.9 |
O2—Cl1—O4 | 109.5 (5) | C6—C5—H10 | 119.9 |
O2—Cl1—O5 | 110.5 (5) | C2—C6—H11 | 119.8 |
O4—Cl1—O5 | 111.1 (5) | C5—C6—H11 | 119.8 |
O2—Cl1—O3 | 108.6 (5) | N4—C7—H14 | 109.5 |
O4—Cl1—O3 | 107.9 (5) | N4—C7—H12 | 109.5 |
O5—Cl1—O3 | 109.2 (5) | H14—C7—H12 | 109.5 |
O8—Cl2—O8ii | 119.9 (12) | N4—C7—H13 | 109.5 |
O8—Cl2—O6 | 114.4 (6) | H14—C7—H13 | 109.5 |
O8—Cl2—O7 | 101.9 (8) | H12—C7—H13 | 109.5 |
O6—Cl2—O7 | 100.0 (11) | ||
N1—Pt1—Pt2—N2 | 4.0 (3) | C5—N4—C4—C3 | 0.0 (16) |
N3—Pt1—Pt2—O1 | −2.6 (3) | C7—N4—C4—C3 | −177.2 (9) |
N3—C1—C2—C6 | −151.7 (9) | C2—C3—C4—N4 | 1.4 (16) |
O1—C1—C2—C6 | 32.1 (13) | C4—N4—C5—C6 | 0.1 (15) |
N3—C1—C2—C3 | 31.8 (13) | C7—N4—C5—C6 | 177.2 (9) |
O1—C1—C2—C3 | −144.4 (9) | C3—C2—C6—C5 | 2.9 (14) |
C6—C2—C3—C4 | −2.8 (15) | C1—C2—C6—C5 | −173.8 (8) |
C1—C2—C3—C4 | 173.9 (9) | N4—C5—C6—C2 | −1.5 (15) |
Symmetry codes: (i) x, y, z−1; (ii) x, −y+1/2, z. |
D—H···A | D—H | H···A | D···A | D—H···A |
N1—H4···O4 | 0.89 | 2.65 | 3.136 (11) | 116 |
N1—H4···O8 | 0.89 | 2.43 | 3.213 (13) | 146 |
N1—H3···O10A | 0.89 | 2.41 | 3.180 (12) | 146 |
N3—H1···O4 | 0.86 | 2.38 | 3.118 (11) | 143 |
N2—H5···O3iii | 0.89 | 2.52 | 3.058 (11) | 119 |
N2—H6···O2iv | 0.89 | 2.58 | 2.988 (10) | 109 |
N2—H5···O5iii | 0.89 | 2.29 | 3.174 (10) | 171 |
N2—H7···O11Bii | 0.89 | 2.17 | 2.96 (4) | 148 |
Symmetry codes: (ii) x, −y+1/2, z; (iii) −x+1/2, −y, z+1/2; (iv) x, y, z+1. |