Supporting information
Crystallographic Information File (CIF) https://doi.org/10.1107/S1600536801007541/bt6043sup1.cif | |
Structure factor file (CIF format) https://doi.org/10.1107/S1600536801007541/bt6043Isup2.hkl |
CCDC reference: 170274
Key indicators
- Single-crystal X-ray study
- T = 150 K
- Mean (C-C) = 0.007 Å
- Disorder in solvent or counterion
- R factor = 0.036
- wR factor = 0.073
- Data-to-parameter ratio = 20.6
checkCIF results
No syntax errors found ADDSYM reports no extra symmetry
Alert Level C:
PLAT_202 Alert C Isotropic non-H Atoms in Anion/Solvent = 1 PLAT_302 Alert C Anion/Solvent Disorder ....................... 17.00 Perc.
0 Alert Level A = Potentially serious problem
0 Alert Level B = Potential problem
2 Alert Level C = Please check
Data collection: SMART (Siemens, 1995); cell refinement: SMART; data reduction: SAINT (Siemens, 1995); program(s) used to solve structure: SHELXS86 (Sheldrick, 1990); program(s) used to refine structure: SHELXL93 (Sheldrick, 1993); molecular graphics: SHELXTL (Siemens, 1995); software used to prepare material for publication: SHELXTL.
[PdI2(C18H15P)2]·2C4H8O | F(000) = 1016 |
Mr = 1028.95 | Dx = 1.630 Mg m−3 |
Monoclinic, P21/c | Mo Kα radiation, λ = 0.71073 Å |
a = 12.011 (3) Å | Cell parameters from 512 reflections |
b = 20.234 (4) Å | θ = 12–20° |
c = 8.625 (2) Å | µ = 2.03 mm−1 |
β = 90.35 (1)° | T = 150 K |
V = 2096.1 (8) Å3 | Block, orange |
Z = 2 | 0.20 × 0.15 × 0.12 mm |
SMART 1K CCD area-detector diffractometer | 4806 independent reflections |
Radiation source: fine-focus sealed tube | 4029 reflections with I > 2σ(I) |
Graphite monochromator | Rint = 0.056 |
ω scans | θmax = 27.5°, θmin = 1.0° |
Absorption correction: integration (XPREP SHELXTL; Siemens, 1995), Rint = 0.061 before correction | h = −11→16 |
Tmin = 0.709, Tmax = 0.795 | k = −25→28 |
15358 measured reflections | l = −12→12 |
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)] = 0.036 | H-atom parameters constrained |
wR(F2) = 0.073 | w = 1/[σ2(Fo2) + 5.8022P] where P = (Fo2 + 2Fc2)/3 |
S = 1.14 | (Δ/σ)max = 0.002 |
4806 reflections | Δρmax = 0.64 e Å−3 |
233 parameters | Δρmin = −0.52 e Å−3 |
2 restraints | Extinction correction: SHELXL, Fc*=kFc[1+0.001xFc2λ3/sin(2θ)]-1/4 |
Primary atom site location: structure-invariant direct methods | Extinction coefficient: 0.0007 (1) |
Experimental. The data collection nominally covered a hemisphere of reciprocal space, by a combination of 5 sets of ω scans; each set at different φ and/or 2θ angles and each scan (12 sec exposure) covering 0.3° in ω. Crystal to detector distance 4.51 cm. Crystal decay was monitored by repeating 50 initial frames at the end of data collection and comparing 286 duplicate reflections. |
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 on F2 for ALL reflections except for 50 with very negative F2 or flagged by the user for potential systematic errors. Weighted R-factors wR and all goodnesses of fit S are based on F2, conventional R-factors R are based on F, with F set to zero for negative F2. The observed criterion of F2 > σ(F2) is used only for calculating _R_factor_gt etc. and is not relevant to the choice of reflections for refinement. |
x | y | z | Uiso*/Ueq | Occ. (<1) | |
I | 0.59876 (2) | 0.612148 (12) | 0.44335 (3) | 0.02307 (8) | |
Pd | 0.5000 | 0.5000 | 0.5000 | 0.01538 (10) | |
P | 0.64544 (9) | 0.43845 (5) | 0.39338 (12) | 0.0175 (2) | |
C11 | 0.7618 (3) | 0.48191 (19) | 0.3002 (5) | 0.0227 (9) | |
C12 | 0.8411 (4) | 0.5116 (2) | 0.3946 (6) | 0.0292 (10) | |
H12 | 0.8365 | 0.5086 | 0.5043 | 0.035* | |
C13 | 0.9297 (4) | 0.5464 (2) | 0.3289 (7) | 0.0389 (12) | |
H13 | 0.9837 | 0.5671 | 0.3936 | 0.047* | |
C14 | 0.9379 (4) | 0.5519 (3) | 0.1699 (7) | 0.0421 (13) | |
H14 | 0.9988 | 0.5755 | 0.1269 | 0.050* | |
C15 | 0.8594 (4) | 0.5223 (3) | 0.0760 (7) | 0.0420 (13) | |
H15 | 0.8662 | 0.5264 | −0.0333 | 0.050* | |
C16 | 0.7715 (4) | 0.4873 (2) | 0.1405 (6) | 0.0291 (10) | |
H16 | 0.7169 | 0.4679 | 0.0747 | 0.035* | |
C21 | 0.7204 (3) | 0.3875 (2) | 0.5338 (5) | 0.0200 (8) | |
C22 | 0.8110 (3) | 0.3485 (2) | 0.4864 (5) | 0.0225 (9) | |
H22 | 0.8295 | 0.3464 | 0.3796 | 0.027* | |
C23 | 0.8705 (4) | 0.3115 (2) | 0.5953 (5) | 0.0269 (10) | |
H23 | 0.9320 | 0.2857 | 0.5621 | 0.032* | |
C24 | 0.8424 (4) | 0.3143 (2) | 0.7509 (6) | 0.0298 (10) | |
H24 | 0.8824 | 0.2882 | 0.8239 | 0.036* | |
C25 | 0.7543 (4) | 0.3537 (2) | 0.8003 (5) | 0.0302 (10) | |
H25 | 0.7356 | 0.3560 | 0.9070 | 0.036* | |
C26 | 0.6932 (4) | 0.3901 (2) | 0.6908 (5) | 0.0246 (9) | |
H26 | 0.6328 | 0.4169 | 0.7235 | 0.029* | |
C31 | 0.5899 (3) | 0.3863 (2) | 0.2394 (5) | 0.0197 (8) | |
C32 | 0.6119 (4) | 0.31897 (19) | 0.2232 (5) | 0.0222 (9) | |
H32 | 0.6589 | 0.2974 | 0.2964 | 0.027* | |
C33 | 0.5657 (4) | 0.2831 (2) | 0.1016 (5) | 0.0287 (10) | |
H33 | 0.5803 | 0.2371 | 0.0915 | 0.034* | |
C34 | 0.4968 (4) | 0.3137 (2) | −0.0057 (5) | 0.0309 (10) | |
H34 | 0.4655 | 0.2889 | −0.0887 | 0.037* | |
C35 | 0.4727 (4) | 0.3808 (2) | 0.0095 (5) | 0.0290 (10) | |
H35 | 0.4270 | 0.4020 | −0.0658 | 0.035* | |
C36 | 0.5175 (4) | 0.4165 (2) | 0.1319 (5) | 0.0248 (9) | |
H36 | 0.4980 | 0.4617 | 0.1449 | 0.030* | |
O1 | 0.0569 (4) | 0.2825 (3) | 0.2968 (6) | 0.0811 (16) | |
C2A | 0.1011 (8) | 0.3458 (5) | 0.2895 (13) | 0.050 (3)* | 0.60 |
H20A | 0.1188 | 0.3631 | 0.3942 | 0.065* | 0.60 |
H21A | 0.0455 | 0.3755 | 0.2406 | 0.065* | 0.60 |
C2B | 0.0792 (11) | 0.3437 (7) | 0.220 (2) | 0.060 (5)* | 0.40 |
H20B | 0.0558 | 0.3822 | 0.2831 | 0.078* | 0.40 |
H21B | 0.0388 | 0.3446 | 0.1199 | 0.078* | 0.40 |
C3 | 0.2035 (5) | 0.3432 (3) | 0.1912 (8) | 0.0529 (15) | |
H30 | 0.2502 | 0.3772 | 0.2426 | 0.069* | |
H31 | 0.2029 | 0.3515 | 0.0780 | 0.069* | |
C4 | 0.2456 (5) | 0.2751 (3) | 0.2353 (9) | 0.0641 (19) | |
H40 | 0.2950 | 0.2754 | 0.3276 | 0.083* | |
H41 | 0.2868 | 0.2565 | 0.1463 | 0.083* | |
C5 | 0.1434 (6) | 0.2357 (4) | 0.2579 (10) | 0.075 (2) | |
H50 | 0.1212 | 0.2105 | 0.1642 | 0.097* | |
H51 | 0.1556 | 0.2041 | 0.3440 | 0.097* |
U11 | U22 | U33 | U12 | U13 | U23 | |
I | 0.02519 (15) | 0.01400 (12) | 0.03006 (16) | −0.00184 (11) | 0.00310 (11) | 0.00015 (11) |
Pd | 0.0174 (2) | 0.01099 (18) | 0.0177 (2) | 0.00050 (16) | 0.00067 (16) | −0.00094 (15) |
P | 0.0200 (5) | 0.0133 (5) | 0.0192 (5) | 0.0010 (4) | 0.0007 (4) | −0.0003 (4) |
C11 | 0.021 (2) | 0.0108 (17) | 0.036 (3) | 0.0037 (15) | 0.0084 (18) | −0.0017 (16) |
C12 | 0.026 (2) | 0.022 (2) | 0.040 (3) | −0.0021 (18) | −0.001 (2) | 0.0013 (19) |
C13 | 0.024 (3) | 0.026 (2) | 0.067 (4) | −0.0044 (19) | 0.001 (2) | 0.004 (2) |
C14 | 0.035 (3) | 0.033 (3) | 0.059 (4) | −0.005 (2) | 0.020 (3) | 0.006 (3) |
C15 | 0.046 (3) | 0.035 (3) | 0.046 (3) | 0.000 (2) | 0.021 (3) | 0.006 (2) |
C16 | 0.032 (3) | 0.024 (2) | 0.031 (2) | −0.0005 (18) | 0.007 (2) | −0.0005 (19) |
C21 | 0.0159 (19) | 0.0176 (18) | 0.027 (2) | −0.0051 (16) | −0.0037 (16) | −0.0012 (17) |
C22 | 0.023 (2) | 0.023 (2) | 0.021 (2) | 0.0014 (17) | −0.0014 (17) | −0.0019 (17) |
C23 | 0.026 (2) | 0.020 (2) | 0.035 (3) | 0.0041 (17) | −0.0024 (19) | −0.0040 (18) |
C24 | 0.028 (2) | 0.024 (2) | 0.037 (3) | −0.0025 (19) | −0.010 (2) | 0.0074 (19) |
C25 | 0.037 (3) | 0.031 (2) | 0.023 (2) | −0.005 (2) | 0.000 (2) | 0.0055 (19) |
C26 | 0.024 (2) | 0.025 (2) | 0.025 (2) | 0.0002 (18) | −0.0017 (18) | −0.0032 (18) |
C31 | 0.020 (2) | 0.0174 (18) | 0.022 (2) | −0.0018 (16) | 0.0057 (16) | 0.0030 (16) |
C32 | 0.027 (2) | 0.0167 (19) | 0.023 (2) | 0.0002 (17) | 0.0034 (18) | −0.0016 (16) |
C33 | 0.034 (3) | 0.020 (2) | 0.032 (2) | −0.0043 (18) | 0.006 (2) | −0.0063 (18) |
C34 | 0.030 (2) | 0.035 (2) | 0.027 (2) | −0.009 (2) | 0.0020 (19) | −0.013 (2) |
C35 | 0.025 (2) | 0.041 (3) | 0.020 (2) | 0.0057 (19) | 0.0017 (18) | −0.003 (2) |
C36 | 0.029 (2) | 0.021 (2) | 0.024 (2) | 0.0047 (17) | −0.0023 (18) | −0.0025 (17) |
O1 | 0.069 (3) | 0.069 (3) | 0.105 (4) | −0.035 (3) | 0.038 (3) | −0.024 (3) |
C3 | 0.054 (4) | 0.045 (3) | 0.059 (4) | −0.007 (3) | 0.003 (3) | 0.004 (3) |
C4 | 0.051 (4) | 0.045 (4) | 0.096 (5) | −0.004 (3) | −0.012 (4) | −0.001 (4) |
C5 | 0.079 (5) | 0.058 (5) | 0.088 (6) | −0.019 (4) | −0.015 (4) | 0.006 (4) |
I—Pd | 2.6081 (5) | C23—C24 | 1.387 (6) |
Pd—Pi | 2.3384 (11) | C24—C25 | 1.394 (7) |
Pd—P | 2.3384 (11) | C25—C26 | 1.401 (6) |
Pd—Ii | 2.6081 (5) | C31—C32 | 1.394 (5) |
P—C31 | 1.820 (4) | C31—C36 | 1.408 (6) |
P—C21 | 1.824 (4) | C32—C33 | 1.389 (6) |
P—C11 | 1.840 (4) | C33—C34 | 1.385 (7) |
C11—C12 | 1.387 (6) | C34—C35 | 1.393 (6) |
C11—C16 | 1.387 (6) | C35—C36 | 1.386 (6) |
C12—C13 | 1.399 (6) | O1—C2A | 1.389 (10) |
C13—C14 | 1.380 (8) | O1—C2B | 1.429 (13) |
C14—C15 | 1.376 (8) | O1—C5 | 1.446 (9) |
C15—C16 | 1.391 (7) | C2A—C3 | 1.499 (10) |
C21—C26 | 1.396 (6) | C2B—C3 | 1.516 (14) |
C21—C22 | 1.408 (6) | C3—C4 | 1.516 (8) |
C22—C23 | 1.395 (6) | C4—C5 | 1.478 (9) |
Pi—Pd—P | 180.0 | C23—C22—C21 | 119.9 (4) |
Pi—Pd—I | 87.25 (3) | C24—C23—C22 | 120.2 (4) |
P—Pd—I | 92.75 (3) | C23—C24—C25 | 120.6 (4) |
Pi—Pd—Ii | 92.75 (3) | C24—C25—C26 | 119.4 (4) |
P—Pd—Ii | 87.25 (3) | C21—C26—C25 | 120.6 (4) |
I—Pd—Ii | 180.0 | C32—C31—C36 | 118.4 (4) |
C31—P—C21 | 109.51 (18) | C32—C31—P | 124.8 (3) |
C31—P—C11 | 103.56 (19) | C36—C31—P | 116.8 (3) |
C21—P—C11 | 100.76 (19) | C33—C32—C31 | 120.8 (4) |
C31—P—Pd | 108.96 (14) | C34—C33—C32 | 120.3 (4) |
C21—P—Pd | 114.00 (14) | C33—C34—C35 | 119.8 (4) |
C11—P—Pd | 119.24 (13) | C36—C35—C34 | 120.0 (4) |
C12—C11—C16 | 119.2 (4) | C35—C36—C31 | 120.7 (4) |
C12—C11—P | 118.1 (3) | C2A—O1—C2B | 26.7 (8) |
C16—C11—P | 122.7 (3) | C2A—O1—C5 | 108.6 (6) |
C11—C12—C13 | 120.1 (5) | C2B—O1—C5 | 108.9 (7) |
C14—C13—C12 | 120.2 (5) | O1—C2A—C3 | 108.0 (7) |
C15—C14—C13 | 119.8 (5) | O1—C2B—C3 | 105.0 (9) |
C14—C15—C16 | 120.3 (5) | C2A—C3—C4 | 99.4 (6) |
C11—C16—C15 | 120.4 (5) | C2A—C3—C2B | 25.0 (7) |
C26—C21—C22 | 119.2 (4) | C4—C3—C2B | 106.9 (7) |
C26—C21—P | 120.4 (3) | C5—C4—C3 | 104.3 (5) |
C22—C21—P | 120.2 (3) | O1—C5—C4 | 106.0 (6) |
Symmetry code: (i) −x+1, −y+1, −z+1. |
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