metal-organic compounds
Bis[1,3(η3)-allyl][μ-2(η4)-1,3-bis(diphenylphosphino)-2,4-diphenylcyclobuta-1,3-diene-1:3κ2P:P′]dichlorido-1κCl,3κCl-[2(η5)-isopropylcyclopentadienyl]-2-cobalt(I)-1,3-dipalladium(II) dichloromethane solvate
aDepartment of Chemistry, National Chung Hsing University, Taichung 402, Taiwan
*Correspondence e-mail: fehong@dragon.nchu.edu.tw
In the title complex, [CoPd2(C3H5)2(C8H11)Cl2(C40H30P2)]·CH2Cl2, the CoI atom is sandwiched between the cyclopentadienyl and cyclobutadiene rings. The two diphenylphosphine substituents of the cyclobutadiene ring are situated opposite to each other and bind two PdII atoms, which are additionally coordinated by a chloride ion and the three C atoms of an allyl ligand, forming a distorted planar coordination environment. The Cl atoms of the dichloromethane solvent molecule (equal occupancies) and one C atom and its attached H atom of each of the allyl ligands (occupancies 0.55:0.45) are disordered.
Related literature
For applications of cobalt-containing phosphine-coordinated palladium complexes, see: Chang & Hong (2005).
Experimental
Crystal data
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Refinement
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Data collection: SMART (Bruker, 1999); cell SAINT (Bruker, 1999); data reduction: SAINT; program(s) used to solve structure: SHELXS97 (Sheldrick, 2008); program(s) used to refine structure: SHELXL97 (Sheldrick, 2008); molecular graphics: SHELXTL (Sheldrick, 2008); software used to prepare material for publication: SHELXTL.
Supporting information
10.1107/S1600536809018133/gk2195sup1.cif
contains datablocks global, I. DOI:Structure factors: contains datablock I. DOI: 10.1107/S1600536809018133/gk2195Isup2.hkl
A 100 ml round-bottomed Schlenk flask equipped with a magnetic stirbar and a rubber septum was charged with allylpalladium(II) chloride dimer (0.05 g, 0.15 mmol), (η5-C5H4iPr)Co(η4-1,3-Ph2-2,4-(PPh2)2C4)(0.11 g, 0.15 mmol) and 10 ml CH2Cl2. After stirring at room temperature for 1 h, the solvent was removed under reduced pressure. The yellow-colored residue was purified by CTLC (Chromatotron, Harrison model 8924) employed EA/CH2Cl2=1:1 mixed solvent. The isolated product was identified as the title compound by spectroscopic methods. 1H NMR (CDCl3, 400 MHz): δ 7.02–8.01 (m, 30H), 5.41 (m, 1H), 4.06 (d, 2H), 2.98 (d, 2H), 0.31 (d, 6H) p.p.m. 13C{1H} NMR (CDCl3, 100 MHz): δ 127.5–132.9, 135.6, 82.0, 80.4, 24.3, 22.0 p.p.m. 31P{1H} NMR (CDCl3, 100 MHz): δ8.6 p.p.m. LRMS: m/s = 1027 [M—Cl]+, [C57H59Cl2CoP2Pd2]. The yield was 53% (0.09 g, 0.08 mmol).
All H atoms were placed in geometrically idealized positions and constrained to ride on their parent atoms with C—H distances in the range 0.93–0.98 Å and Uiso(H) = 1.2Ueq(C). The two allyl groups and the dichloromethane molecule are disordered over two positions with the occupancy factors ratio of 55:45 for the allyl groups and 50:50 for the solvent molecule.
Data collection: SMART (Bruker, 1999); cell
SAINT (Bruker, 1999); data reduction: SAINT (Bruker, 1999); program(s) used to solve structure: SHELXS97 (Sheldrick, 2008); program(s) used to refine structure: SHELXL97 (Sheldrick, 2008); molecular graphics: SHELXTL (Sheldrick, 2008); software used to prepare material for publication: SHELXTL (Sheldrick, 2008).Fig. 1. A view of the molecular structure of the title compound with displacement ellipsoids shown at the 40% probability level. Hydrogen atoms have been omitted for clarity. |
[CoPd2(C3H5)2(C8H11)Cl2(C40H30P2)]·CH2Cl2 | Z = 2 |
Mr = 1189.44 | F(000) = 1198 |
Triclinic, P1 | Dx = 1.536 Mg m−3 |
Hall symbol: -P 1 | Mo Kα radiation, λ = 0.71073 Å |
a = 10.889 (4) Å | Cell parameters from 4357 reflections |
b = 12.499 (4) Å | θ = 2.2–25.4° |
c = 21.746 (8) Å | µ = 1.32 mm−1 |
α = 94.617 (7)° | T = 298 K |
β = 102.136 (7)° | Parallelepiped, yellow |
γ = 115.166 (7)° | 0.25 × 0.20 × 0.15 mm |
V = 2570.1 (16) Å3 |
Bruker SMART 1000 CCD diffractometer | 10003 independent reflections |
Radiation source: fine-focus sealed tube | 6379 reflections with I > 2σ(I) |
Graphite monochromator | Rint = 0.033 |
Detector resolution: 0 pixels mm-1 | θmax = 26.1°, θmin = 2.0° |
ϕ and ω scans | h = −13→9 |
Absorption correction: multi-scan (SADABS; Sheldrick, 1996) | k = −15→14 |
Tmin = 0.734, Tmax = 0.827 | l = −24→26 |
14882 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)] = 0.047 | Hydrogen site location: inferred from neighbouring sites |
wR(F2) = 0.126 | H-atom parameters constrained |
S = 0.98 | w = 1/[σ2(Fo2) + (0.06P)2] where P = (Fo2 + 2Fc2)/3 |
10003 reflections | (Δ/σ)max < 0.001 |
608 parameters | Δρmax = 0.60 e Å−3 |
0 restraints | Δρmin = −0.59 e Å−3 |
[CoPd2(C3H5)2(C8H11)Cl2(C40H30P2)]·CH2Cl2 | γ = 115.166 (7)° |
Mr = 1189.44 | V = 2570.1 (16) Å3 |
Triclinic, P1 | Z = 2 |
a = 10.889 (4) Å | Mo Kα radiation |
b = 12.499 (4) Å | µ = 1.32 mm−1 |
c = 21.746 (8) Å | T = 298 K |
α = 94.617 (7)° | 0.25 × 0.20 × 0.15 mm |
β = 102.136 (7)° |
Bruker SMART 1000 CCD diffractometer | 10003 independent reflections |
Absorption correction: multi-scan (SADABS; Sheldrick, 1996) | 6379 reflections with I > 2σ(I) |
Tmin = 0.734, Tmax = 0.827 | Rint = 0.033 |
14882 measured reflections |
R[F2 > 2σ(F2)] = 0.047 | 0 restraints |
wR(F2) = 0.126 | H-atom parameters constrained |
S = 0.98 | Δρmax = 0.60 e Å−3 |
10003 reflections | Δρmin = −0.59 e Å−3 |
608 parameters |
Geometry. All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. |
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 > 2sigma(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) | |
Pd1 | 0.72416 (5) | 0.71604 (4) | 0.45564 (2) | 0.04002 (13) | |
Co1 | 0.45423 (7) | 0.73312 (6) | 0.26318 (3) | 0.03195 (17) | |
P1 | 0.76022 (14) | 0.84931 (11) | 0.38561 (6) | 0.0323 (3) | |
C1 | 0.3718 (7) | 0.8474 (6) | 0.2772 (3) | 0.0563 (17) | |
H1 | 0.4224 | 0.9308 | 0.2840 | 0.068* | |
Pd2 | 0.53088 (5) | 0.78107 (4) | 0.06221 (2) | 0.04233 (13) | |
P2 | 0.51015 (14) | 0.63486 (11) | 0.12431 (6) | 0.0331 (3) | |
C2 | 0.2990 (6) | 0.7701 (6) | 0.2175 (3) | 0.0592 (18) | |
H2 | 0.2927 | 0.7934 | 0.1779 | 0.071* | |
C3 | 0.2363 (6) | 0.6497 (6) | 0.2280 (3) | 0.0530 (15) | |
H3 | 0.1843 | 0.5807 | 0.1963 | 0.064* | |
C4 | 0.2667 (5) | 0.6531 (5) | 0.2947 (3) | 0.0430 (13) | |
C5 | 0.3551 (6) | 0.7764 (5) | 0.3256 (3) | 0.0476 (14) | |
H5 | 0.3946 | 0.8050 | 0.3694 | 0.057* | |
C6 | 0.6348 (5) | 0.8196 (4) | 0.2430 (2) | 0.0310 (11) | |
C7 | 0.6545 (5) | 0.7806 (4) | 0.3037 (2) | 0.0301 (11) | |
C8 | 0.5800 (5) | 0.6533 (4) | 0.2708 (2) | 0.0315 (11) | |
C9 | 0.5603 (5) | 0.6945 (4) | 0.2091 (2) | 0.0313 (11) | |
C10 | 0.6979 (6) | 0.9356 (4) | 0.2197 (2) | 0.0351 (12) | |
C11 | 0.8424 (6) | 0.9924 (5) | 0.2267 (3) | 0.0501 (15) | |
H11 | 0.8976 | 0.9571 | 0.2448 | 0.060* | |
C12 | 0.9045 (7) | 1.1006 (6) | 0.2071 (3) | 0.0649 (19) | |
H12 | 1.0014 | 1.1380 | 0.2124 | 0.078* | |
C13 | 0.8247 (8) | 1.1533 (5) | 0.1798 (3) | 0.071 (2) | |
H13 | 0.8669 | 1.2257 | 0.1662 | 0.085* | |
C14 | 0.6823 (7) | 1.0987 (5) | 0.1727 (3) | 0.0618 (18) | |
H14 | 0.6279 | 1.1350 | 0.1551 | 0.074* | |
C15 | 0.6191 (6) | 0.9894 (5) | 0.1917 (3) | 0.0481 (14) | |
H15 | 0.5220 | 0.9518 | 0.1855 | 0.058* | |
C16 | 0.5674 (5) | 0.5406 (4) | 0.2916 (2) | 0.0329 (11) | |
C17 | 0.5024 (6) | 0.5014 (5) | 0.3394 (3) | 0.0457 (14) | |
H17 | 0.4671 | 0.5471 | 0.3587 | 0.055* | |
C18 | 0.4891 (7) | 0.3958 (6) | 0.3589 (3) | 0.0638 (18) | |
H18 | 0.4443 | 0.3701 | 0.3907 | 0.077* | |
C19 | 0.5425 (8) | 0.3279 (6) | 0.3310 (4) | 0.070 (2) | |
H19 | 0.5308 | 0.2553 | 0.3431 | 0.084* | |
C20 | 0.6126 (8) | 0.3672 (6) | 0.2853 (3) | 0.072 (2) | |
H20 | 0.6516 | 0.3230 | 0.2677 | 0.086* | |
C21 | 0.9370 (5) | 0.9072 (4) | 0.3733 (2) | 0.0331 (11) | |
C22 | 0.9643 (6) | 0.8345 (5) | 0.3321 (3) | 0.0444 (13) | |
H22 | 0.8929 | 0.7583 | 0.3117 | 0.053* | |
C23 | 1.0946 (6) | 0.8727 (5) | 0.3208 (3) | 0.0526 (15) | |
H23 | 1.1117 | 0.8222 | 0.2938 | 0.063* | |
C24 | 1.1996 (6) | 0.9865 (6) | 0.3500 (3) | 0.0676 (19) | |
H24 | 1.2869 | 1.0141 | 0.3413 | 0.081* | |
C25 | 1.1763 (6) | 1.0592 (6) | 0.3916 (3) | 0.0650 (19) | |
H25 | 1.2480 | 1.1352 | 0.4120 | 0.078* | |
C26 | 1.0448 (6) | 1.0188 (5) | 0.4032 (3) | 0.0496 (15) | |
H26 | 1.0294 | 1.0681 | 0.4318 | 0.060* | |
C27 | 0.7412 (5) | 0.9859 (4) | 0.4061 (2) | 0.0371 (12) | |
C28 | 0.6891 (6) | 0.9970 (5) | 0.4581 (3) | 0.0567 (17) | |
H28 | 0.6639 | 0.9354 | 0.4813 | 0.068* | |
C29 | 0.6744 (7) | 1.0980 (6) | 0.4754 (4) | 0.070 (2) | |
H29 | 0.6399 | 1.1048 | 0.5104 | 0.084* | |
C30 | 0.7105 (7) | 1.1895 (6) | 0.4411 (4) | 0.069 (2) | |
H30 | 0.6979 | 1.2569 | 0.4521 | 0.083* | |
C31 | 0.7647 (8) | 1.1807 (6) | 0.3910 (3) | 0.0651 (18) | |
H31 | 0.7924 | 1.2436 | 0.3687 | 0.078* | |
C32 | 0.7787 (7) | 1.0783 (5) | 0.3731 (3) | 0.0548 (16) | |
H32 | 0.8141 | 1.0724 | 0.3383 | 0.066* | |
C33 | 0.3390 (5) | 0.5024 (4) | 0.1043 (2) | 0.0382 (12) | |
C34 | 0.2326 (6) | 0.4928 (5) | 0.0537 (3) | 0.0612 (17) | |
H34 | 0.2496 | 0.5536 | 0.0299 | 0.073* | |
C35 | 0.0994 (7) | 0.3932 (6) | 0.0373 (4) | 0.078 (2) | |
H35 | 0.0281 | 0.3888 | 0.0035 | 0.093* | |
C36 | 0.0750 (7) | 0.3034 (6) | 0.0711 (3) | 0.0667 (19) | |
H36 | −0.0130 | 0.2365 | 0.0601 | 0.080* | |
C37 | 0.1786 (7) | 0.3106 (6) | 0.1209 (3) | 0.0675 (19) | |
H37 | 0.1606 | 0.2489 | 0.1442 | 0.081* | |
C38 | 0.3102 (6) | 0.4083 (5) | 0.1375 (3) | 0.0559 (16) | |
H38 | 0.3806 | 0.4110 | 0.1713 | 0.067* | |
C39 | 0.6377 (5) | 0.5762 (5) | 0.1229 (2) | 0.0382 (12) | |
C40 | 0.7772 (6) | 0.6478 (5) | 0.1557 (3) | 0.0477 (14) | |
H40 | 0.8041 | 0.7249 | 0.1775 | 0.057* | |
C41 | 0.8782 (6) | 0.6077 (6) | 0.1572 (3) | 0.0610 (17) | |
H41 | 0.9717 | 0.6577 | 0.1795 | 0.073* | |
C42 | 0.8399 (8) | 0.4940 (7) | 0.1257 (3) | 0.070 (2) | |
H42 | 0.9069 | 0.4660 | 0.1276 | 0.084* | |
C43 | 0.7029 (8) | 0.4219 (6) | 0.0914 (3) | 0.070 (2) | |
H43 | 0.6773 | 0.3456 | 0.0692 | 0.084* | |
C44 | 0.6018 (7) | 0.4626 (5) | 0.0898 (3) | 0.0535 (15) | |
H44 | 0.5090 | 0.4132 | 0.0664 | 0.064* | |
C52 | 0.2038 (6) | 0.5526 (5) | 0.3285 (3) | 0.0533 (15) | |
H52 | 0.2789 | 0.5580 | 0.3645 | 0.064* | |
C53 | 0.6248 (7) | 0.4743 (5) | 0.2656 (3) | 0.0511 (15) | |
H53 | 0.6721 | 0.5012 | 0.2347 | 0.061* | |
C54 | 0.0937 (8) | 0.5682 (8) | 0.3559 (4) | 0.101 (3) | |
H54A | 0.1362 | 0.6455 | 0.3837 | 0.151* | |
H54B | 0.0567 | 0.5060 | 0.3797 | 0.151* | |
H54C | 0.0186 | 0.5630 | 0.3215 | 0.151* | |
C55 | 0.1415 (8) | 0.4290 (6) | 0.2856 (4) | 0.089 (2) | |
H55A | 0.0682 | 0.4218 | 0.2496 | 0.133* | |
H55B | 0.1031 | 0.3674 | 0.3095 | 0.133* | |
H55C | 0.2141 | 0.4200 | 0.2705 | 0.133* | |
Cl1 | 0.51400 (16) | 0.70395 (13) | 0.47871 (7) | 0.0526 (4) | |
Cl2 | 0.31495 (17) | 0.79401 (14) | 0.05176 (8) | 0.0607 (4) | |
C48 | 0.7290 (7) | 0.8105 (6) | 0.0497 (3) | 0.073 (2) | |
H48A | 0.6757 | 0.7633 | 0.0768 | 0.087* | |
H48B | 0.8215 | 0.8157 | 0.0525 | 0.087* | |
C47 | 0.7535 (9) | 0.5996 (7) | 0.5217 (4) | 0.090 (3) | |
H47A | 0.6787 | 0.6237 | 0.5140 | 0.107* | |
H47B | 0.7554 | 0.5520 | 0.5546 | 0.107* | |
C49 | 0.6587 (12) | 0.8395 (9) | −0.0045 (5) | 0.042 (3) | 0.55 |
H49A | 0.7139 | 0.8581 | −0.0358 | 0.050* | 0.55 |
C49' | 0.697 (3) | 0.886 (2) | 0.0259 (12) | 0.105 (9)* | 0.45 |
H49B | 0.7839 | 0.9417 | 0.0169 | 0.126* | 0.45 |
C46 | 0.8156 (14) | 0.5940 (10) | 0.4751 (6) | 0.052 (3) | 0.55 |
H46 | 0.8562 | 0.5379 | 0.4815 | 0.063* | 0.55 |
C46' | 0.862 (2) | 0.6582 (17) | 0.5070 (10) | 0.078 (5)* | 0.45 |
H46' | 0.9363 | 0.6459 | 0.5348 | 0.093* | 0.45 |
C45 | 0.9043 (8) | 0.6902 (7) | 0.4564 (4) | 0.082 (2) | |
H45A | 0.9942 | 0.6959 | 0.4530 | 0.099* | |
H45B | 0.8674 | 0.7363 | 0.4315 | 0.099* | |
C50 | 0.6146 (9) | 0.9242 (7) | 0.0062 (4) | 0.092 (3) | |
H50A | 0.6436 | 0.9933 | −0.0145 | 0.110* | |
H50B | 0.5329 | 0.9045 | 0.0226 | 0.110* | |
Cl4' | 1.3448 (8) | 1.1123 (8) | 0.1784 (6) | 0.137 (3) | 0.50 |
Cl3' | 1.0857 (6) | 0.9245 (8) | 0.1500 (5) | 0.175 (3) | 0.50 |
Cl3 | 1.0708 (6) | 0.9902 (5) | 0.0675 (4) | 0.160 (3) | 0.50 |
Cl4 | 1.276 (3) | 1.067 (2) | 0.1853 (10) | 0.376 (15) | 0.50 |
C56 | 1.2044 (18) | 0.9887 (15) | 0.1210 (8) | 0.181 (7) | |
H56A | 1.1709 | 1.0175 | 0.0841 | 0.217* | |
H56B | 1.2380 | 0.9332 | 0.1066 | 0.217* |
U11 | U22 | U33 | U12 | U13 | U23 | |
Pd1 | 0.0423 (3) | 0.0414 (2) | 0.0371 (2) | 0.0195 (2) | 0.01012 (19) | 0.00980 (18) |
Co1 | 0.0251 (3) | 0.0379 (4) | 0.0374 (4) | 0.0164 (3) | 0.0113 (3) | 0.0112 (3) |
P1 | 0.0309 (7) | 0.0332 (7) | 0.0332 (7) | 0.0155 (6) | 0.0088 (6) | 0.0039 (6) |
C1 | 0.050 (4) | 0.052 (4) | 0.092 (5) | 0.034 (3) | 0.041 (4) | 0.028 (4) |
Pd2 | 0.0447 (3) | 0.0415 (3) | 0.0407 (3) | 0.0177 (2) | 0.0134 (2) | 0.01344 (19) |
P2 | 0.0294 (7) | 0.0344 (7) | 0.0332 (7) | 0.0123 (6) | 0.0085 (6) | 0.0065 (6) |
C2 | 0.038 (3) | 0.098 (5) | 0.069 (5) | 0.047 (4) | 0.025 (3) | 0.043 (4) |
C3 | 0.024 (3) | 0.072 (4) | 0.056 (4) | 0.016 (3) | 0.011 (3) | 0.010 (3) |
C4 | 0.026 (3) | 0.056 (4) | 0.052 (4) | 0.019 (3) | 0.019 (3) | 0.016 (3) |
C5 | 0.044 (3) | 0.060 (4) | 0.053 (4) | 0.031 (3) | 0.026 (3) | 0.014 (3) |
C6 | 0.028 (3) | 0.031 (3) | 0.038 (3) | 0.016 (2) | 0.011 (2) | 0.006 (2) |
C7 | 0.026 (3) | 0.031 (3) | 0.037 (3) | 0.015 (2) | 0.012 (2) | 0.007 (2) |
C8 | 0.027 (3) | 0.036 (3) | 0.034 (3) | 0.016 (2) | 0.009 (2) | 0.005 (2) |
C9 | 0.025 (3) | 0.037 (3) | 0.032 (3) | 0.013 (2) | 0.010 (2) | 0.006 (2) |
C10 | 0.042 (3) | 0.029 (3) | 0.032 (3) | 0.013 (2) | 0.012 (2) | 0.004 (2) |
C11 | 0.038 (3) | 0.048 (3) | 0.055 (4) | 0.010 (3) | 0.014 (3) | 0.013 (3) |
C12 | 0.055 (4) | 0.056 (4) | 0.066 (4) | 0.003 (4) | 0.026 (4) | 0.024 (3) |
C13 | 0.078 (5) | 0.037 (3) | 0.081 (5) | 0.007 (4) | 0.027 (4) | 0.024 (3) |
C14 | 0.070 (5) | 0.048 (4) | 0.065 (4) | 0.024 (4) | 0.014 (4) | 0.022 (3) |
C15 | 0.051 (4) | 0.043 (3) | 0.055 (4) | 0.022 (3) | 0.019 (3) | 0.020 (3) |
C16 | 0.030 (3) | 0.034 (3) | 0.031 (3) | 0.014 (2) | 0.000 (2) | 0.004 (2) |
C17 | 0.041 (3) | 0.053 (3) | 0.050 (3) | 0.026 (3) | 0.014 (3) | 0.020 (3) |
C18 | 0.062 (4) | 0.066 (4) | 0.067 (4) | 0.025 (4) | 0.024 (4) | 0.032 (4) |
C19 | 0.081 (5) | 0.044 (4) | 0.083 (5) | 0.032 (4) | 0.008 (4) | 0.023 (4) |
C20 | 0.105 (6) | 0.061 (4) | 0.078 (5) | 0.060 (5) | 0.028 (5) | 0.022 (4) |
C21 | 0.029 (3) | 0.036 (3) | 0.034 (3) | 0.018 (2) | 0.003 (2) | 0.003 (2) |
C22 | 0.031 (3) | 0.045 (3) | 0.057 (4) | 0.019 (3) | 0.011 (3) | 0.005 (3) |
C23 | 0.039 (3) | 0.059 (4) | 0.059 (4) | 0.024 (3) | 0.013 (3) | −0.003 (3) |
C24 | 0.030 (3) | 0.087 (5) | 0.079 (5) | 0.021 (4) | 0.018 (3) | 0.003 (4) |
C25 | 0.036 (3) | 0.053 (4) | 0.082 (5) | 0.003 (3) | 0.015 (3) | −0.011 (3) |
C26 | 0.033 (3) | 0.051 (4) | 0.053 (4) | 0.013 (3) | 0.008 (3) | −0.005 (3) |
C27 | 0.039 (3) | 0.039 (3) | 0.037 (3) | 0.023 (3) | 0.007 (2) | 0.003 (2) |
C28 | 0.062 (4) | 0.042 (3) | 0.072 (4) | 0.022 (3) | 0.038 (4) | 0.004 (3) |
C29 | 0.074 (5) | 0.064 (4) | 0.085 (5) | 0.036 (4) | 0.041 (4) | 0.000 (4) |
C30 | 0.075 (5) | 0.053 (4) | 0.087 (5) | 0.046 (4) | 0.007 (4) | −0.006 (4) |
C31 | 0.087 (5) | 0.056 (4) | 0.065 (4) | 0.046 (4) | 0.014 (4) | 0.017 (3) |
C32 | 0.077 (5) | 0.053 (4) | 0.044 (3) | 0.040 (4) | 0.014 (3) | 0.004 (3) |
C33 | 0.035 (3) | 0.034 (3) | 0.038 (3) | 0.008 (2) | 0.012 (2) | 0.001 (2) |
C34 | 0.043 (4) | 0.049 (4) | 0.071 (4) | 0.010 (3) | 0.000 (3) | 0.013 (3) |
C35 | 0.047 (4) | 0.062 (4) | 0.084 (5) | 0.005 (4) | −0.017 (4) | 0.008 (4) |
C36 | 0.039 (4) | 0.052 (4) | 0.082 (5) | 0.002 (3) | 0.009 (4) | 0.002 (4) |
C37 | 0.058 (4) | 0.053 (4) | 0.071 (5) | 0.003 (4) | 0.021 (4) | 0.020 (3) |
C38 | 0.047 (4) | 0.053 (4) | 0.057 (4) | 0.015 (3) | 0.006 (3) | 0.017 (3) |
C39 | 0.036 (3) | 0.040 (3) | 0.038 (3) | 0.015 (3) | 0.014 (2) | 0.006 (2) |
C40 | 0.041 (3) | 0.054 (4) | 0.050 (4) | 0.024 (3) | 0.014 (3) | 0.007 (3) |
C41 | 0.039 (3) | 0.077 (5) | 0.069 (4) | 0.030 (4) | 0.014 (3) | 0.002 (4) |
C42 | 0.067 (5) | 0.101 (6) | 0.065 (5) | 0.061 (5) | 0.017 (4) | 0.004 (4) |
C43 | 0.080 (5) | 0.072 (5) | 0.071 (5) | 0.051 (4) | 0.015 (4) | −0.008 (4) |
C44 | 0.050 (4) | 0.058 (4) | 0.049 (4) | 0.027 (3) | 0.003 (3) | 0.000 (3) |
C52 | 0.038 (3) | 0.061 (4) | 0.062 (4) | 0.019 (3) | 0.020 (3) | 0.025 (3) |
C53 | 0.068 (4) | 0.056 (4) | 0.046 (3) | 0.039 (3) | 0.023 (3) | 0.018 (3) |
C54 | 0.079 (6) | 0.121 (7) | 0.146 (8) | 0.051 (5) | 0.085 (6) | 0.080 (6) |
C55 | 0.077 (6) | 0.067 (5) | 0.097 (6) | 0.009 (4) | 0.021 (5) | 0.024 (4) |
Cl1 | 0.0488 (9) | 0.0544 (9) | 0.0561 (9) | 0.0202 (8) | 0.0234 (7) | 0.0133 (7) |
Cl2 | 0.0568 (10) | 0.0636 (10) | 0.0678 (10) | 0.0341 (9) | 0.0130 (8) | 0.0171 (8) |
C48 | 0.042 (4) | 0.103 (6) | 0.096 (6) | 0.033 (4) | 0.049 (4) | 0.060 (5) |
C47 | 0.096 (6) | 0.110 (6) | 0.110 (7) | 0.074 (6) | 0.042 (5) | 0.079 (5) |
C49 | 0.050 (7) | 0.036 (6) | 0.037 (6) | 0.006 (5) | 0.035 (5) | 0.012 (5) |
C46 | 0.073 (8) | 0.045 (7) | 0.053 (7) | 0.045 (7) | 0.004 (7) | 0.015 (6) |
C45 | 0.077 (5) | 0.113 (6) | 0.111 (6) | 0.078 (5) | 0.042 (5) | 0.065 (5) |
C50 | 0.099 (6) | 0.098 (6) | 0.120 (7) | 0.049 (5) | 0.081 (6) | 0.082 (6) |
Cl4' | 0.096 (4) | 0.098 (4) | 0.166 (8) | 0.042 (3) | −0.037 (4) | −0.031 (4) |
Cl3' | 0.082 (4) | 0.233 (8) | 0.229 (8) | 0.060 (5) | 0.078 (5) | 0.115 (7) |
Cl3 | 0.067 (3) | 0.119 (4) | 0.253 (8) | 0.008 (3) | 0.058 (4) | −0.015 (5) |
Cl4 | 0.64 (4) | 0.56 (3) | 0.214 (15) | 0.53 (3) | 0.08 (2) | 0.11 (2) |
C56 | 0.239 (18) | 0.266 (18) | 0.162 (14) | 0.200 (16) | 0.111 (14) | 0.064 (13) |
Pd1—C46' | 2.09 (2) | C25—H25 | 0.9300 |
Pd1—C45 | 2.116 (6) | C26—H26 | 0.9300 |
Pd1—C46 | 2.171 (10) | C27—C32 | 1.368 (7) |
Pd1—C47 | 2.195 (6) | C27—C28 | 1.389 (7) |
Pd1—P1 | 2.3132 (15) | C28—C29 | 1.372 (8) |
Pd1—Cl1 | 2.3901 (17) | C28—H28 | 0.9300 |
Co1—C6 | 1.964 (5) | C29—C30 | 1.378 (9) |
Co1—C7 | 1.973 (5) | C29—H29 | 0.9300 |
Co1—C9 | 1.976 (5) | C30—C31 | 1.361 (9) |
Co1—C8 | 1.998 (5) | C30—H30 | 0.9300 |
Co1—C1 | 2.018 (5) | C31—C32 | 1.387 (8) |
Co1—C2 | 2.022 (5) | C31—H31 | 0.9300 |
Co1—C5 | 2.072 (5) | C32—H32 | 0.9300 |
Co1—C3 | 2.075 (5) | C33—C34 | 1.376 (8) |
Co1—C4 | 2.146 (5) | C33—C38 | 1.386 (7) |
P1—C7 | 1.813 (5) | C34—C35 | 1.399 (8) |
P1—C21 | 1.835 (5) | C34—H34 | 0.9300 |
P1—C27 | 1.837 (5) | C35—C36 | 1.354 (9) |
C1—C2 | 1.400 (9) | C35—H35 | 0.9300 |
C1—C5 | 1.421 (8) | C36—C37 | 1.355 (9) |
C1—H1 | 0.9300 | C36—H36 | 0.9300 |
Pd2—C48 | 2.110 (6) | C37—C38 | 1.378 (8) |
Pd2—C49' | 2.09 (3) | C37—H37 | 0.9300 |
Pd2—C49 | 2.174 (9) | C38—H38 | 0.9300 |
Pd2—C50 | 2.223 (6) | C39—C40 | 1.380 (7) |
Pd2—P2 | 2.3215 (15) | C39—C44 | 1.389 (7) |
Pd2—Cl2 | 2.3897 (18) | C40—C41 | 1.384 (8) |
P2—C9 | 1.806 (5) | C40—H40 | 0.9300 |
P2—C33 | 1.823 (5) | C41—C42 | 1.372 (9) |
P2—C39 | 1.830 (5) | C41—H41 | 0.9300 |
C2—C3 | 1.424 (8) | C42—C43 | 1.369 (9) |
C2—H2 | 0.9300 | C42—H42 | 0.9300 |
C3—C4 | 1.412 (8) | C43—C44 | 1.391 (8) |
C3—H3 | 0.9300 | C43—H43 | 0.9300 |
C4—C5 | 1.433 (8) | C44—H44 | 0.9300 |
C4—C52 | 1.489 (7) | C52—C54 | 1.520 (8) |
C5—H5 | 0.9300 | C52—C55 | 1.526 (9) |
C6—C7 | 1.449 (6) | C52—H52 | 0.9800 |
C6—C9 | 1.460 (6) | C53—H53 | 0.9300 |
C6—C10 | 1.500 (6) | C54—H54A | 0.9600 |
C7—C8 | 1.475 (6) | C54—H54B | 0.9600 |
C8—C16 | 1.473 (7) | C54—H54C | 0.9600 |
C8—C9 | 1.482 (6) | C55—H55A | 0.9600 |
C10—C15 | 1.377 (7) | C55—H55B | 0.9600 |
C10—C11 | 1.390 (7) | C55—H55C | 0.9600 |
C11—C12 | 1.381 (8) | C48—C49' | 1.25 (3) |
C11—H11 | 0.9300 | C48—C49 | 1.425 (14) |
C12—C13 | 1.369 (9) | C48—H48A | 0.9700 |
C12—H12 | 0.9300 | C48—H48B | 0.9700 |
C13—C14 | 1.370 (9) | C47—C46' | 1.222 (19) |
C13—H13 | 0.9300 | C47—C46 | 1.344 (14) |
C14—C15 | 1.386 (7) | C47—H47A | 0.9700 |
C14—H14 | 0.9300 | C47—H47B | 0.9700 |
C15—H15 | 0.9300 | C49—C49' | 0.75 (2) |
C16—C53 | 1.382 (7) | C49—C50 | 1.358 (13) |
C16—C17 | 1.386 (7) | C49—H49A | 0.9800 |
C17—C18 | 1.377 (8) | C49'—C50 | 1.21 (3) |
C17—H17 | 0.9300 | C49'—H49B | 0.9800 |
C18—C19 | 1.382 (9) | C46—C46' | 0.893 (18) |
C18—H18 | 0.9300 | C46—C45 | 1.342 (13) |
C19—C20 | 1.374 (9) | C46—H46 | 0.9800 |
C19—H19 | 0.9300 | C46'—C45 | 1.31 (2) |
C20—C53 | 1.400 (8) | C46'—H46' | 0.9800 |
C20—H20 | 0.9300 | C45—H45A | 0.9700 |
C21—C26 | 1.374 (7) | C45—H45B | 0.9700 |
C21—C22 | 1.387 (7) | C50—H50A | 0.9700 |
C22—C23 | 1.375 (7) | C50—H50B | 0.9700 |
C22—H22 | 0.9300 | Cl4'—C56 | 1.78 (2) |
C23—C24 | 1.379 (8) | Cl3'—C56 | 1.502 (14) |
C23—H23 | 0.9300 | Cl3—C56 | 1.670 (17) |
C24—C25 | 1.367 (8) | Cl4—C56 | 1.48 (2) |
C24—H24 | 0.9300 | C56—H56A | 0.9700 |
C25—C26 | 1.387 (8) | C56—H56B | 0.9700 |
C46'—Pd1—C45 | 36.2 (5) | C18—C17—C16 | 121.1 (6) |
C46'—Pd1—C46 | 24.1 (5) | C18—C17—H17 | 119.5 |
C45—Pd1—C46 | 36.5 (4) | C16—C17—H17 | 119.5 |
C46'—Pd1—C47 | 33.0 (5) | C17—C18—C19 | 119.8 (6) |
C45—Pd1—C47 | 66.9 (3) | C17—C18—H18 | 120.1 |
C46—Pd1—C47 | 35.9 (4) | C19—C18—H18 | 120.1 |
C46'—Pd1—P1 | 130.0 (5) | C20—C19—C18 | 120.4 (6) |
C45—Pd1—P1 | 96.36 (19) | C20—C19—H19 | 119.8 |
C46—Pd1—P1 | 129.6 (4) | C18—C19—H19 | 119.8 |
C47—Pd1—P1 | 163.0 (2) | C19—C20—C53 | 119.3 (6) |
C46'—Pd1—Cl1 | 126.2 (6) | C19—C20—H20 | 120.3 |
C45—Pd1—Cl1 | 161.9 (2) | C53—C20—H20 | 120.3 |
C46—Pd1—Cl1 | 126.6 (4) | C26—C21—C22 | 118.1 (5) |
C47—Pd1—Cl1 | 94.9 (2) | C26—C21—P1 | 123.4 (4) |
P1—Pd1—Cl1 | 101.77 (5) | C22—C21—P1 | 118.6 (4) |
C6—Co1—C7 | 43.20 (19) | C23—C22—C21 | 121.4 (5) |
C6—Co1—C9 | 43.51 (19) | C23—C22—H22 | 119.3 |
C7—Co1—C9 | 63.05 (19) | C21—C22—H22 | 119.3 |
C6—Co1—C8 | 63.45 (19) | C22—C23—C24 | 119.3 (5) |
C7—Co1—C8 | 43.60 (19) | C22—C23—H23 | 120.3 |
C9—Co1—C8 | 43.78 (19) | C24—C23—H23 | 120.3 |
C6—Co1—C1 | 109.4 (2) | C25—C24—C23 | 120.4 (6) |
C7—Co1—C1 | 120.6 (2) | C25—C24—H24 | 119.8 |
C9—Co1—C1 | 141.4 (2) | C23—C24—H24 | 119.8 |
C8—Co1—C1 | 163.6 (3) | C24—C25—C26 | 119.6 (6) |
C6—Co1—C2 | 114.4 (2) | C24—C25—H25 | 120.2 |
C7—Co1—C2 | 151.5 (2) | C26—C25—H25 | 120.2 |
C9—Co1—C2 | 116.0 (2) | C21—C26—C25 | 121.2 (5) |
C8—Co1—C2 | 155.2 (3) | C21—C26—H26 | 119.4 |
C1—Co1—C2 | 40.5 (3) | C25—C26—H26 | 119.4 |
C6—Co1—C5 | 134.4 (2) | C32—C27—C28 | 118.5 (5) |
C7—Co1—C5 | 112.9 (2) | C32—C27—P1 | 122.7 (4) |
C9—Co1—C5 | 175.9 (2) | C28—C27—P1 | 118.7 (4) |
C8—Co1—C5 | 132.9 (2) | C29—C28—C27 | 120.6 (6) |
C1—Co1—C5 | 40.6 (2) | C29—C28—H28 | 119.7 |
C2—Co1—C5 | 67.9 (2) | C27—C28—H28 | 119.7 |
C6—Co1—C3 | 145.7 (2) | C28—C29—C30 | 120.2 (6) |
C7—Co1—C3 | 167.8 (2) | C28—C29—H29 | 119.9 |
C9—Co1—C3 | 116.7 (2) | C30—C29—H29 | 119.9 |
C8—Co1—C3 | 126.7 (2) | C31—C30—C29 | 119.6 (6) |
C1—Co1—C3 | 68.0 (3) | C31—C30—H30 | 120.2 |
C2—Co1—C3 | 40.7 (2) | C29—C30—H30 | 120.2 |
C5—Co1—C3 | 67.1 (2) | C30—C31—C32 | 120.2 (6) |
C6—Co1—C4 | 173.7 (2) | C30—C31—H31 | 119.9 |
C7—Co1—C4 | 133.2 (2) | C32—C31—H31 | 119.9 |
C9—Co1—C4 | 142.2 (2) | C27—C32—C31 | 120.8 (6) |
C8—Co1—C4 | 118.2 (2) | C27—C32—H32 | 119.6 |
C1—Co1—C4 | 67.2 (2) | C31—C32—H32 | 119.6 |
C2—Co1—C4 | 66.9 (2) | C34—C33—C38 | 117.5 (5) |
C5—Co1—C4 | 39.7 (2) | C34—C33—P2 | 119.6 (4) |
C3—Co1—C4 | 39.0 (2) | C38—C33—P2 | 123.0 (5) |
C7—P1—C21 | 99.7 (2) | C33—C34—C35 | 121.2 (6) |
C7—P1—C27 | 106.7 (2) | C33—C34—H34 | 119.4 |
C21—P1—C27 | 103.7 (2) | C35—C34—H34 | 119.4 |
C7—P1—Pd1 | 113.91 (16) | C36—C35—C34 | 119.6 (7) |
C21—P1—Pd1 | 112.87 (16) | C36—C35—H35 | 120.2 |
C27—P1—Pd1 | 117.94 (17) | C34—C35—H35 | 120.2 |
C2—C1—C5 | 108.2 (6) | C37—C36—C35 | 120.2 (6) |
C2—C1—Co1 | 69.9 (3) | C37—C36—H36 | 119.9 |
C5—C1—Co1 | 71.7 (3) | C35—C36—H36 | 119.9 |
C2—C1—H1 | 125.9 | C36—C37—C38 | 120.8 (6) |
C5—C1—H1 | 125.9 | C36—C37—H37 | 119.6 |
Co1—C1—H1 | 124.2 | C38—C37—H37 | 119.6 |
C48—Pd2—C49' | 34.6 (7) | C37—C38—C33 | 120.7 (6) |
C48—Pd2—C49 | 38.8 (4) | C37—C38—H38 | 119.6 |
C49'—Pd2—C49 | 20.1 (6) | C33—C38—H38 | 119.6 |
C48—Pd2—C50 | 66.8 (3) | C40—C39—C44 | 117.7 (5) |
C49'—Pd2—C50 | 32.3 (7) | C40—C39—P2 | 119.0 (4) |
C49—Pd2—C50 | 36.0 (3) | C44—C39—P2 | 123.4 (4) |
C48—Pd2—P2 | 96.09 (19) | C39—C40—C41 | 121.6 (6) |
C49'—Pd2—P2 | 130.5 (8) | C39—C40—H40 | 119.2 |
C49—Pd2—P2 | 129.5 (3) | C41—C40—H40 | 119.2 |
C50—Pd2—P2 | 162.7 (2) | C42—C41—C40 | 119.8 (6) |
C48—Pd2—Cl2 | 160.51 (19) | C42—C41—H41 | 120.1 |
C49'—Pd2—Cl2 | 126.2 (8) | C40—C41—H41 | 120.1 |
C49—Pd2—Cl2 | 122.7 (3) | C43—C42—C41 | 120.0 (6) |
C50—Pd2—Cl2 | 93.9 (2) | C43—C42—H42 | 120.0 |
P2—Pd2—Cl2 | 103.31 (5) | C41—C42—H42 | 120.0 |
C9—P2—C33 | 108.3 (2) | C42—C43—C44 | 120.1 (6) |
C9—P2—C39 | 99.4 (2) | C42—C43—H43 | 120.0 |
C33—P2—C39 | 105.3 (2) | C44—C43—H43 | 120.0 |
C9—P2—Pd2 | 112.77 (16) | C39—C44—C43 | 120.9 (6) |
C33—P2—Pd2 | 116.33 (18) | C39—C44—H44 | 119.6 |
C39—P2—Pd2 | 113.17 (17) | C43—C44—H44 | 119.6 |
C1—C2—C3 | 108.2 (6) | C4—C52—C54 | 109.3 (5) |
C1—C2—Co1 | 69.6 (3) | C4—C52—C55 | 112.6 (5) |
C3—C2—Co1 | 71.7 (3) | C54—C52—C55 | 111.2 (6) |
C1—C2—H2 | 125.9 | C4—C52—H52 | 107.9 |
C3—C2—H2 | 125.9 | C54—C52—H52 | 107.9 |
Co1—C2—H2 | 124.5 | C55—C52—H52 | 107.9 |
C4—C3—C2 | 108.3 (6) | C16—C53—C20 | 120.8 (6) |
C4—C3—Co1 | 73.2 (3) | C16—C53—H53 | 119.6 |
C2—C3—Co1 | 67.7 (3) | C20—C53—H53 | 119.6 |
C4—C3—H3 | 125.8 | C52—C54—H54A | 109.5 |
C2—C3—H3 | 125.8 | C52—C54—H54B | 109.5 |
Co1—C3—H3 | 124.9 | H54A—C54—H54B | 109.5 |
C3—C4—C5 | 107.2 (5) | C52—C54—H54C | 109.5 |
C3—C4—C52 | 127.5 (5) | H54A—C54—H54C | 109.5 |
C5—C4—C52 | 124.7 (5) | H54B—C54—H54C | 109.5 |
C3—C4—Co1 | 67.8 (3) | C52—C55—H55A | 109.5 |
C5—C4—Co1 | 67.4 (3) | C52—C55—H55B | 109.5 |
C52—C4—Co1 | 136.6 (4) | H55A—C55—H55B | 109.5 |
C1—C5—C4 | 107.8 (5) | C52—C55—H55C | 109.5 |
C1—C5—Co1 | 67.7 (3) | H55A—C55—H55C | 109.5 |
C4—C5—Co1 | 72.9 (3) | H55B—C55—H55C | 109.5 |
C1—C5—H5 | 126.1 | C49—C48—Pd2 | 73.0 (5) |
C4—C5—H5 | 126.1 | C49—C48—H48A | 119.8 |
Co1—C5—H5 | 124.9 | Pd2—C48—H48A | 49.5 |
C7—C6—C9 | 90.4 (4) | C49—C48—H48B | 119.8 |
C7—C6—C10 | 135.9 (4) | Pd2—C48—H48B | 167.0 |
C9—C6—C10 | 131.5 (4) | H48A—C48—H48B | 117.7 |
C7—C6—Co1 | 68.7 (3) | C46—C47—Pd1 | 71.1 (5) |
C9—C6—Co1 | 68.7 (3) | C46—C47—H47A | 119.4 |
C10—C6—Co1 | 132.3 (3) | Pd1—C47—H47A | 53.1 |
C6—C7—C8 | 90.9 (4) | C46—C47—H47B | 119.4 |
C6—C7—P1 | 136.9 (4) | Pd1—C47—H47B | 169.5 |
C8—C7—P1 | 130.8 (4) | H47A—C47—H47B | 117.0 |
C6—C7—Co1 | 68.1 (3) | C50—C49—C48 | 117.9 (9) |
C8—C7—Co1 | 69.1 (3) | C50—C49—Pd2 | 74.0 (5) |
P1—C7—Co1 | 130.6 (2) | C48—C49—Pd2 | 68.1 (4) |
C16—C8—C7 | 133.0 (4) | C50—C49—H49A | 110.6 |
C16—C8—C9 | 136.7 (4) | C48—C49—H49A | 110.6 |
C7—C8—C9 | 88.6 (4) | Pd2—C49—H49A | 174.8 |
C16—C8—Co1 | 132.3 (3) | C47—C46—C45 | 124.6 (10) |
C7—C8—Co1 | 67.3 (3) | C47—C46—Pd1 | 73.1 (5) |
C9—C8—Co1 | 67.3 (3) | C45—C46—Pd1 | 69.6 (5) |
C6—C9—C8 | 90.2 (4) | C47—C46—H46 | 109.4 |
C6—C9—P2 | 129.4 (4) | C45—C46—H46 | 109.4 |
C8—C9—P2 | 138.9 (4) | Pd1—C46—H46 | 177.1 |
C6—C9—Co1 | 67.8 (3) | Pd1—C46'—H46' | 169.9 |
C8—C9—Co1 | 68.9 (3) | C46—C45—Pd1 | 74.0 (5) |
P2—C9—Co1 | 130.6 (3) | C46—C45—H45A | 119.4 |
C15—C10—C11 | 118.1 (5) | Pd1—C45—H45A | 166.6 |
C15—C10—C6 | 122.9 (5) | C46—C45—H45B | 119.4 |
C11—C10—C6 | 119.0 (5) | Pd1—C45—H45B | 50.4 |
C12—C11—C10 | 120.6 (6) | H45A—C45—H45B | 117.1 |
C12—C11—H11 | 119.7 | C49—C50—Pd2 | 70.0 (5) |
C10—C11—H11 | 119.7 | C49—C50—H50A | 119.8 |
C13—C12—C11 | 120.5 (6) | Pd2—C50—H50A | 170.2 |
C13—C12—H12 | 119.7 | C49—C50—H50B | 119.8 |
C11—C12—H12 | 119.7 | Pd2—C50—H50B | 53.5 |
C12—C13—C14 | 119.6 (6) | H50A—C50—H50B | 117.6 |
C12—C13—H13 | 120.2 | Cl4—C56—Cl3 | 125.4 (11) |
C14—C13—H13 | 120.2 | Cl3'—C56—Cl4' | 110.1 (11) |
C13—C14—C15 | 120.1 (6) | Cl4—C56—H56A | 121.9 |
C13—C14—H14 | 120.0 | Cl3'—C56—H56A | 109.6 |
C15—C14—H14 | 120.0 | Cl4'—C56—H56A | 109.6 |
C10—C15—C14 | 121.1 (6) | Cl4—C56—H56B | 119.6 |
C10—C15—H15 | 119.5 | Cl3'—C56—H56B | 109.6 |
C14—C15—H15 | 119.5 | Cl3—C56—H56B | 115.0 |
C53—C16—C17 | 118.6 (5) | Cl4'—C56—H56B | 109.6 |
C53—C16—C8 | 120.8 (5) | H56A—C56—H56B | 108.2 |
C17—C16—C8 | 120.6 (5) |
Experimental details
Crystal data | |
Chemical formula | [CoPd2(C3H5)2(C8H11)Cl2(C40H30P2)]·CH2Cl2 |
Mr | 1189.44 |
Crystal system, space group | Triclinic, P1 |
Temperature (K) | 298 |
a, b, c (Å) | 10.889 (4), 12.499 (4), 21.746 (8) |
α, β, γ (°) | 94.617 (7), 102.136 (7), 115.166 (7) |
V (Å3) | 2570.1 (16) |
Z | 2 |
Radiation type | Mo Kα |
µ (mm−1) | 1.32 |
Crystal size (mm) | 0.25 × 0.20 × 0.15 |
Data collection | |
Diffractometer | Bruker SMART 1000 CCD diffractometer |
Absorption correction | Multi-scan (SADABS; Sheldrick, 1996) |
Tmin, Tmax | 0.734, 0.827 |
No. of measured, independent and observed [I > 2σ(I)] reflections | 14882, 10003, 6379 |
Rint | 0.033 |
(sin θ/λ)max (Å−1) | 0.618 |
Refinement | |
R[F2 > 2σ(F2)], wR(F2), S | 0.047, 0.126, 0.98 |
No. of reflections | 10003 |
No. of parameters | 608 |
H-atom treatment | H-atom parameters constrained |
Δρmax, Δρmin (e Å−3) | 0.60, −0.59 |
Computer programs: SMART (Bruker, 1999), SAINT (Bruker, 1999), SHELXS97 (Sheldrick, 2008), SHELXL97 (Sheldrick, 2008), SHELXTL (Sheldrick, 2008).
Pd1—C45 | 2.116 (6) | Pd2—C48 | 2.110 (6) |
Pd1—C46 | 2.171 (10) | Pd2—C49 | 2.174 (9) |
Pd1—C47 | 2.195 (6) | Pd2—C50 | 2.223 (6) |
Pd1—P1 | 2.3132 (15) | Pd2—P2 | 2.3215 (15) |
Pd1—Cl1 | 2.3901 (17) | Pd2—Cl2 | 2.3897 (18) |
Acknowledgements
Financial support from the National Science Council of the Republic of China (NSC-95–2113-M-005–015-MY3) is gratefully appreciated.
References
Bruker (1999). SMART and SAINT. Bruker AXS Inc., Madison, Wisconsin, USA. Google Scholar
Chang, Y.-C. & Hong, F.-E. (2005). Organometallics, 24, 5686–5695. Web of Science CSD CrossRef CAS Google Scholar
Sheldrick, G. M. (1996). SADABS. University of Göttingen, Germany. Google Scholar
Sheldrick, G. M. (2008). Acta Cryst. A64, 112–122. Web of Science CrossRef CAS IUCr Journals Google Scholar
This is an open-access article distributed under the terms of the Creative Commons Attribution (CC-BY) Licence, which permits unrestricted use, distribution, and reproduction in any medium, provided the original authors and source are cited.
Recently, we have synthesized a series of cobalt-containing phosphine-coordinated palladium complexes which have shown high activities in the Suzuki-Miyaura reaction (Chang et al., 2005). We report herein the synthesis and crystal structure of a cobalt-containing phosphine coordinated palladium complex, a potential catalyst for cross-coupling reactions.
The crystal structure of the title compound reveals that it is a CoI sandwich complex (Figure 1) containing two diphenylphosphino-coordinated palladium moieties attached to the cyclobutadiene ring. The two rings sandwiching the Co atom, cyclopentadienyl and cyclobutadiene, are almost parallel to each other [dihedral angle of 8.46 (8)° ]. The cyclopentadienyl ring bears an isopropyl group as a substituent. The palladium atoms are pentacoordinated; they bind to a chloride ion, a phosphorous atom from the diphenylphosphine ligand and three carbon atoms from the disordered allylic group.