Supporting information
Crystallographic Information File (CIF) https://doi.org/10.1107/S1600536801007589/bt6044sup1.cif | |
Structure factor file (CIF format) https://doi.org/10.1107/S1600536801007589/bt6044Isup2.hkl |
CCDC reference: 170275
Key indicators
- Single-crystal X-ray study
- T = 150 K
- Mean (C-C) = 0.009 Å
- R factor = 0.041
- wR factor = 0.080
- Data-to-parameter ratio = 21.1
checkCIF results
No syntax errors found ADDSYM reports no extra symmetry General Notes
REFLT_03 From the CIF: _diffrn_reflns_theta_max 27.50 From the CIF: _reflns_number_total 5903 From the CIF: _diffrn_reflns_limit_ max hkl 12. 27. 20. From the CIF: _diffrn_reflns_limit_ min hkl -12. -27. -20. TEST1: Expected hkl limits for theta max Calculated maximum hkl 12. 25. 18. Calculated minimum hkl -12. -25. -18. ALERT: Expected hkl max differ from CIF values
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(C26H24P2)] | F(000) = 1448 |
Mr = 758.59 | Dx = 1.962 Mg m−3 |
Monoclinic, P21/n | Mo Kα radiation, λ = 0.71073 Å |
a = 9.465 (1) Å | Cell parameters from 432 reflections |
b = 19.821 (1) Å | θ = 12–20° |
c = 14.208 (1) Å | µ = 3.26 mm−1 |
β = 105.51 (1)° | T = 150 K |
V = 2568.4 (4) Å3 | Plate, yellow |
Z = 4 | 0.30 × 0.12 × 0.06 mm |
SMART 1K CCD area-detector diffractometer | 5903 independent reflections |
Radiation source: fine-focus sealed tube | 4690 reflections with I > 2σ(I) |
Graphite monochromator | Rint = 0.056 |
ω scans | θmax = 27.5°, θmin = 1.8° |
Absorption correction: integration (XPREP SHELXTL; Siemens, 1995), Rint = 0.107 before correction | h = −12→12 |
Tmin = 0.355, Tmax = 0.832 | k = −27→27 |
18477 measured reflections | l = −20→20 |
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)] = 0.041 | Hydrogen site location: inferred from neighbouring sites |
wR(F2) = 0.080 | H-atom parameters constrained |
S = 1.16 | w = 1/[σ2(Fo2) + (0.0102P)2 + 11.804P] where P = (Fo2 + 2Fc2)/3 |
5903 reflections | (Δ/σ)max < 0.001 |
280 parameters | Δρmax = 0.66 e Å−3 |
0 restraints | Δρmin = −1.05 e Å−3 |
Experimental. The data collection nominally covered over a hemisphere of reciprocal space, by a combination of 4 sets of ω scans; each set at different φ and/or 2θ angles and each scan (10 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 279 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 97 with very negative F2. 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 | ||
Pd | 0.18303 (4) | 0.326237 (19) | 0.21618 (3) | 0.01517 (9) | |
I1 | 0.05634 (4) | 0.213028 (18) | 0.13280 (3) | 0.02293 (9) | |
I2 | −0.06742 (4) | 0.387890 (19) | 0.21131 (3) | 0.02568 (10) | |
P1 | 0.40705 (14) | 0.28443 (7) | 0.21606 (10) | 0.0165 (3) | |
P2 | 0.31003 (15) | 0.41505 (7) | 0.29652 (10) | 0.0178 (3) | |
C1 | 0.5489 (6) | 0.3438 (3) | 0.2838 (4) | 0.0234 (12) | |
H1A | 0.6384 | 0.3184 | 0.3172 | 0.030* | |
H1B | 0.5747 | 0.3757 | 0.2375 | 0.030* | |
C2 | 0.4926 (6) | 0.3828 (3) | 0.3592 (4) | 0.0212 (11) | |
H2A | 0.5597 | 0.4206 | 0.3861 | 0.028* | |
H2B | 0.4867 | 0.3528 | 0.4138 | 0.028* | |
C11 | 0.4493 (5) | 0.2046 (2) | 0.2801 (4) | 0.0164 (10) | |
C12 | 0.4064 (7) | 0.1959 (3) | 0.3658 (4) | 0.0283 (13) | |
H12 | 0.3560 | 0.2313 | 0.3884 | 0.034* | |
C13 | 0.4355 (7) | 0.1362 (3) | 0.4185 (4) | 0.0366 (15) | |
H13 | 0.4068 | 0.1311 | 0.4773 | 0.044* | |
C14 | 0.5075 (6) | 0.0843 (3) | 0.3855 (4) | 0.0300 (14) | |
H14 | 0.5259 | 0.0431 | 0.4210 | 0.036* | |
C15 | 0.5518 (7) | 0.0920 (3) | 0.3016 (5) | 0.0328 (14) | |
H15 | 0.6015 | 0.0563 | 0.2794 | 0.039* | |
C16 | 0.5237 (7) | 0.1524 (3) | 0.2488 (4) | 0.0281 (13) | |
H16 | 0.5556 | 0.1576 | 0.1912 | 0.034* | |
C21 | 0.4477 (6) | 0.2758 (3) | 0.0986 (4) | 0.0181 (11) | |
C22 | 0.5951 (6) | 0.2674 (3) | 0.0975 (4) | 0.0221 (11) | |
H22 | 0.6704 | 0.2662 | 0.1571 | 0.026* | |
C23 | 0.6307 (6) | 0.2609 (3) | 0.0093 (4) | 0.0268 (13) | |
H23 | 0.7300 | 0.2551 | 0.0086 | 0.032* | |
C24 | 0.5215 (7) | 0.2628 (3) | −0.0777 (4) | 0.0282 (13) | |
H24 | 0.5456 | 0.2571 | −0.1379 | 0.034* | |
C25 | 0.3774 (7) | 0.2732 (3) | −0.0771 (4) | 0.0288 (13) | |
H25 | 0.3035 | 0.2761 | −0.1372 | 0.035* | |
C26 | 0.3395 (6) | 0.2790 (3) | 0.0104 (4) | 0.0219 (11) | |
H26 | 0.2399 | 0.2853 | 0.0101 | 0.026* | |
C31 | 0.2524 (6) | 0.4582 (3) | 0.3927 (4) | 0.0223 (12) | |
C32 | 0.2213 (6) | 0.5271 (3) | 0.3899 (5) | 0.0301 (13) | |
H32 | 0.2269 | 0.5532 | 0.3349 | 0.036* | |
C33 | 0.1832 (6) | 0.5575 (3) | 0.4675 (5) | 0.0347 (15) | |
H33 | 0.1627 | 0.6044 | 0.4651 | 0.042* | |
C34 | 0.1738 (6) | 0.5204 (4) | 0.5478 (5) | 0.0398 (17) | |
H34 | 0.1457 | 0.5415 | 0.6001 | 0.048* | |
C35 | 0.2059 (7) | 0.4519 (4) | 0.5512 (5) | 0.0412 (17) | |
H35 | 0.2013 | 0.4263 | 0.6068 | 0.049* | |
C36 | 0.2446 (7) | 0.4207 (3) | 0.4747 (4) | 0.0307 (14) | |
H36 | 0.2659 | 0.3738 | 0.4778 | 0.037* | |
C41 | 0.3480 (6) | 0.4757 (3) | 0.2123 (4) | 0.0197 (11) | |
C42 | 0.4484 (6) | 0.5287 (3) | 0.2444 (4) | 0.0260 (12) | |
H42 | 0.4892 | 0.5357 | 0.3124 | 0.031* | |
C43 | 0.4887 (7) | 0.5708 (3) | 0.1776 (5) | 0.0338 (14) | |
H43 | 0.5573 | 0.6061 | 0.2001 | 0.041* | |
C44 | 0.4278 (7) | 0.5615 (3) | 0.0778 (5) | 0.0354 (15) | |
H44 | 0.4557 | 0.5902 | 0.0322 | 0.043* | |
C45 | 0.3277 (7) | 0.5106 (3) | 0.0452 (4) | 0.0320 (14) | |
H45 | 0.2853 | 0.5049 | −0.0229 | 0.038* | |
C46 | 0.2879 (6) | 0.4672 (3) | 0.1112 (4) | 0.0245 (12) | |
H46 | 0.2197 | 0.4319 | 0.0878 | 0.029* |
U11 | U22 | U33 | U12 | U13 | U23 | |
Pd | 0.01245 (19) | 0.01539 (19) | 0.01755 (18) | −0.00116 (15) | 0.00381 (14) | −0.00207 (16) |
I1 | 0.02370 (19) | 0.01948 (18) | 0.02451 (18) | −0.00400 (15) | 0.00452 (14) | −0.00343 (15) |
I2 | 0.01920 (18) | 0.0271 (2) | 0.0311 (2) | 0.00150 (15) | 0.00725 (15) | −0.00585 (16) |
P1 | 0.0140 (6) | 0.0167 (6) | 0.0192 (6) | 0.0001 (5) | 0.0049 (5) | −0.0001 (5) |
P2 | 0.0165 (7) | 0.0172 (7) | 0.0191 (7) | −0.0006 (5) | 0.0037 (5) | −0.0024 (5) |
C1 | 0.016 (3) | 0.025 (3) | 0.029 (3) | −0.002 (2) | 0.006 (2) | −0.001 (2) |
C2 | 0.020 (3) | 0.020 (3) | 0.021 (3) | −0.002 (2) | 0.000 (2) | −0.002 (2) |
C11 | 0.015 (2) | 0.016 (3) | 0.018 (2) | −0.001 (2) | 0.003 (2) | 0.000 (2) |
C12 | 0.035 (3) | 0.027 (3) | 0.026 (3) | 0.002 (3) | 0.013 (3) | 0.002 (2) |
C13 | 0.045 (4) | 0.042 (4) | 0.024 (3) | −0.002 (3) | 0.012 (3) | 0.006 (3) |
C14 | 0.025 (3) | 0.027 (3) | 0.032 (3) | −0.005 (3) | −0.002 (3) | 0.010 (3) |
C15 | 0.040 (4) | 0.017 (3) | 0.043 (4) | 0.009 (3) | 0.013 (3) | 0.001 (3) |
C16 | 0.036 (3) | 0.021 (3) | 0.030 (3) | 0.004 (3) | 0.014 (3) | 0.001 (2) |
C21 | 0.017 (3) | 0.019 (3) | 0.019 (2) | 0.001 (2) | 0.006 (2) | 0.001 (2) |
C22 | 0.019 (3) | 0.024 (3) | 0.024 (3) | 0.002 (2) | 0.008 (2) | 0.006 (2) |
C23 | 0.025 (3) | 0.029 (3) | 0.031 (3) | 0.007 (2) | 0.016 (3) | 0.006 (3) |
C24 | 0.039 (4) | 0.024 (3) | 0.026 (3) | −0.002 (3) | 0.016 (3) | 0.003 (2) |
C25 | 0.030 (3) | 0.030 (3) | 0.023 (3) | −0.011 (3) | 0.001 (2) | 0.002 (2) |
C26 | 0.017 (3) | 0.026 (3) | 0.022 (3) | −0.004 (2) | 0.004 (2) | 0.001 (2) |
C31 | 0.016 (3) | 0.030 (3) | 0.020 (3) | −0.003 (2) | 0.003 (2) | −0.008 (2) |
C32 | 0.024 (3) | 0.031 (3) | 0.034 (3) | −0.002 (3) | 0.006 (3) | −0.010 (3) |
C33 | 0.025 (3) | 0.036 (4) | 0.042 (4) | −0.003 (3) | 0.007 (3) | −0.023 (3) |
C34 | 0.018 (3) | 0.071 (5) | 0.032 (3) | −0.010 (3) | 0.009 (3) | −0.021 (3) |
C35 | 0.036 (4) | 0.063 (5) | 0.025 (3) | −0.007 (3) | 0.009 (3) | −0.006 (3) |
C36 | 0.033 (3) | 0.034 (3) | 0.026 (3) | −0.007 (3) | 0.010 (3) | 0.002 (3) |
C41 | 0.019 (3) | 0.019 (3) | 0.023 (3) | 0.002 (2) | 0.008 (2) | −0.002 (2) |
C42 | 0.026 (3) | 0.025 (3) | 0.026 (3) | −0.005 (2) | 0.006 (2) | −0.001 (2) |
C43 | 0.034 (3) | 0.027 (3) | 0.041 (4) | −0.011 (3) | 0.011 (3) | −0.003 (3) |
C44 | 0.051 (4) | 0.021 (3) | 0.043 (4) | −0.003 (3) | 0.028 (3) | 0.001 (3) |
C45 | 0.042 (4) | 0.031 (3) | 0.023 (3) | −0.001 (3) | 0.009 (3) | 0.004 (3) |
C46 | 0.029 (3) | 0.023 (3) | 0.022 (3) | −0.002 (2) | 0.008 (2) | −0.001 (2) |
Pd—P2 | 2.2612 (14) | C23—C24 | 1.384 (8) |
Pd—P1 | 2.2769 (14) | C23—H23 | 0.9504 |
Pd—I2 | 2.6514 (6) | C24—C25 | 1.381 (8) |
Pd—I1 | 2.6678 (5) | C24—H24 | 0.9505 |
P1—C11 | 1.815 (5) | C25—C26 | 1.387 (8) |
P1—C21 | 1.818 (5) | C25—H25 | 0.9503 |
P1—C1 | 1.850 (6) | C26—H26 | 0.9503 |
P2—C41 | 1.798 (5) | C31—C32 | 1.394 (8) |
P2—C31 | 1.815 (5) | C31—C36 | 1.402 (8) |
P2—C2 | 1.834 (5) | C32—C33 | 1.386 (8) |
C1—C2 | 1.528 (7) | C32—H32 | 0.9502 |
C1—H1A | 0.9901 | C33—C34 | 1.381 (9) |
C1—H1B | 0.9902 | C33—H33 | 0.9499 |
C2—H2A | 0.9899 | C34—C35 | 1.390 (10) |
C2—H2B | 0.9902 | C34—H34 | 0.9504 |
C11—C16 | 1.391 (7) | C35—C36 | 1.381 (9) |
C11—C12 | 1.394 (7) | C35—H35 | 0.9503 |
C12—C13 | 1.389 (8) | C36—H36 | 0.9497 |
C12—H12 | 0.9500 | C41—C46 | 1.407 (7) |
C13—C14 | 1.383 (9) | C41—C42 | 1.408 (8) |
C13—H13 | 0.9506 | C42—C43 | 1.392 (8) |
C14—C15 | 1.374 (9) | C42—H42 | 0.9503 |
C14—H14 | 0.9500 | C43—C44 | 1.393 (9) |
C15—C16 | 1.400 (8) | C43—H43 | 0.9500 |
C15—H15 | 0.9501 | C44—C45 | 1.378 (9) |
C16—H16 | 0.9504 | C44—H44 | 0.9502 |
C21—C26 | 1.392 (7) | C45—C46 | 1.396 (8) |
C21—C22 | 1.410 (7) | C45—H45 | 0.9503 |
C22—C23 | 1.386 (7) | C46—H46 | 0.9500 |
C22—H22 | 0.9502 | ||
P2—Pd—P1 | 85.08 (5) | C23—C22—C21 | 120.1 (5) |
P2—Pd—I2 | 90.30 (4) | C23—C22—H22 | 119.9 |
P1—Pd—I2 | 173.71 (4) | C21—C22—H22 | 120.0 |
P2—Pd—I1 | 173.81 (4) | C24—C23—C22 | 120.0 (5) |
P1—Pd—I1 | 90.09 (4) | C24—C23—H23 | 119.9 |
I2—Pd—I1 | 94.790 (18) | C22—C23—H23 | 120.0 |
C11—P1—C21 | 107.8 (2) | C25—C24—C23 | 120.1 (5) |
C11—P1—C1 | 105.1 (2) | C25—C24—H24 | 119.9 |
C21—P1—C1 | 103.6 (2) | C23—C24—H24 | 120.0 |
C11—P1—Pd | 113.39 (17) | C24—C25—C26 | 120.6 (5) |
C21—P1—Pd | 117.44 (17) | C24—C25—H25 | 119.6 |
C1—P1—Pd | 108.34 (18) | C26—C25—H25 | 119.7 |
C41—P2—C31 | 109.8 (3) | C25—C26—C21 | 119.9 (5) |
C41—P2—C2 | 103.1 (3) | C25—C26—H26 | 120.1 |
C31—P2—C2 | 103.4 (2) | C21—C26—H26 | 120.0 |
C41—P2—Pd | 110.99 (18) | C32—C31—C36 | 119.1 (5) |
C31—P2—Pd | 121.39 (18) | C32—C31—P2 | 122.9 (4) |
C2—P2—Pd | 106.18 (18) | C36—C31—P2 | 117.9 (5) |
C2—C1—P1 | 110.3 (4) | C33—C32—C31 | 120.1 (6) |
C2—C1—H1A | 109.6 | C33—C32—H32 | 120.0 |
P1—C1—H1A | 109.6 | C31—C32—H32 | 120.0 |
C2—C1—H1B | 109.6 | C34—C33—C32 | 121.0 (6) |
P1—C1—H1B | 109.6 | C34—C33—H33 | 119.6 |
H1A—C1—H1B | 108.1 | C32—C33—H33 | 119.5 |
C1—C2—P2 | 107.2 (4) | C33—C34—C35 | 119.1 (6) |
C1—C2—H2A | 110.2 | C33—C34—H34 | 120.4 |
P2—C2—H2A | 110.3 | C35—C34—H34 | 120.5 |
C1—C2—H2B | 110.3 | C36—C35—C34 | 120.8 (6) |
P2—C2—H2B | 110.3 | C36—C35—H35 | 119.7 |
H2A—C2—H2B | 108.5 | C34—C35—H35 | 119.5 |
C16—C11—C12 | 118.6 (5) | C35—C36—C31 | 120.0 (6) |
C16—C11—P1 | 123.4 (4) | C35—C36—H36 | 120.0 |
C12—C11—P1 | 118.0 (4) | C31—C36—H36 | 120.0 |
C13—C12—C11 | 120.9 (5) | C46—C41—C42 | 118.2 (5) |
C13—C12—H12 | 119.5 | C46—C41—P2 | 120.1 (4) |
C11—C12—H12 | 119.6 | C42—C41—P2 | 121.4 (4) |
C14—C13—C12 | 119.8 (6) | C43—C42—C41 | 120.7 (5) |
C14—C13—H13 | 120.1 | C43—C42—H42 | 119.7 |
C12—C13—H13 | 120.1 | C41—C42—H42 | 119.6 |
C15—C14—C13 | 120.2 (6) | C42—C43—C44 | 120.1 (6) |
C15—C14—H14 | 120.0 | C42—C43—H43 | 119.9 |
C13—C14—H14 | 119.8 | C44—C43—H43 | 120.0 |
C14—C15—C16 | 120.2 (5) | C45—C44—C43 | 119.9 (6) |
C14—C15—H15 | 119.9 | C45—C44—H44 | 120.0 |
C16—C15—H15 | 119.9 | C43—C44—H44 | 120.1 |
C11—C16—C15 | 120.3 (5) | C44—C45—C46 | 120.7 (6) |
C11—C16—H16 | 119.9 | C44—C45—H45 | 119.7 |
C15—C16—H16 | 119.8 | C46—C45—H45 | 119.6 |
C26—C21—C22 | 119.1 (5) | C45—C46—C41 | 120.3 (5) |
C26—C21—P1 | 122.5 (4) | C45—C46—H46 | 119.9 |
C22—C21—P1 | 118.4 (4) | C41—C46—H46 | 119.8 |