Literature DB >> 21580540

Di-μ-chlorido-bis-{[μ-1,8-bis-(diisopropyl-phosphan-yl)-9,10-dihydro-9,10-ethano-anthracene-κP:P']-μ-chlorido-μ-methyl-idene-dipalladium(II)} tetra-hydro-furan penta-solvate.

Thomas Schnetz1, Frank Rominger, Peter Hofmann.   

Abstract

The title compound, [Pd(4)(CH(2))(2)Cl(4)(C(28)H(40)P(2))(2)]·5C(4)H(8)O, possesses a tetra-nuclear palladium core with four bridging chlorido ligands and two bridging methyl-ene units, as well as two bridging anthracene-based bis-phosphine ligands. This tetra-nuclear complex can be considered as being composed of two μ-chlorido-bridged LPd(2) units. The structural motif of these LPd(2) units shows two doubly bridged palladium centers between the P atoms of the bis-phosphine ligand. One of these bridges is a μ-Cl atom, the other a μ-methyl-ene group. The coordination environment around each palladium center is essentially square planar. We ascribe the oxidation state +II to the palladium centers and do not assume Pd-Pd bonds [shortest distances 2.8110 (5) and 2.8109 (6) Å]. Co-crystallized with the palladium complex we found five non-coordinating tetra-hydro-furan solvent mol-ecules, one of which is disordered over two positions in a 0.429 (9):0.571 (8) ratio.

Entities:  

Year:  2010        PMID: 21580540      PMCID: PMC2984049          DOI: 10.1107/S1600536810010263

Source DB:  PubMed          Journal:  Acta Crystallogr Sect E Struct Rep Online        ISSN: 1600-5368


Related literature

For the synthesis of the Pd(0) precursor, see: Schnetz et al. (2008 ▶). The structural motif of a doubly brigded dinuclear Pd(II) complex with anthraceno-based bis-phosphines was reported by Warth (1999 ▶) and Grossman et al. (2006 ▶). Related palladium structures with a bridging μ2-methyl­ene group were reported by Brownie et al. (2003 ▶) and Klopfenstein et al. (1996 ▶). For a recent example of a tetra­nuclear Pd platform with bridging μ2-methyl­ene units, see: Sachse et al. (2010 ▶).

Experimental

Crystal data

[Pd4(CH2)2Cl4(C28H40P2)2]·5C4H8O M = 1833.05 Triclinic, a = 12.5799 (1) Å b = 17.2830 (3) Å c = 19.7558 (2) Å α = 79.877 (1)° β = 74.703 (1)° γ = 80.717 (1)° V = 4048.61 (9) Å3 Z = 2 Mo Kα radiation μ = 1.13 mm−1 T = 200 K 0.18 × 0.18 × 0.06 mm

Data collection

Bruker SMART CCD diffractometer Absorption correction: multi-scan (SADABS; Sheldrick, 2008a ▶) T min = 0.822, T max = 0.935 36611 measured reflections 15292 independent reflections 9483 reflections with I > 2σ(I) R int = 0.056

Refinement

R[F 2 > 2σ(F 2)] = 0.047 wR(F 2) = 0.106 S = 1.01 15292 reflections 915 parameters 434 restraints H atoms treated by a mixture of independent and constrained refinement Δρmax = 0.82 e Å−3 Δρmin = −0.73 e Å−3 Data collection: SMART (Siemens, 1996 ▶); cell refinement: SAINT (Siemens, 1996 ▶); data reduction: SAINT; program(s) used to solve structure: SHELXTL (Sheldrick, 2008b ▶); program(s) used to refine structure: SHELXTL; molecular graphics: SHELXTL; software used to prepare material for publication: SHELXTL. Crystal structure: contains datablocks I, global. DOI: 10.1107/S1600536810010263/hg2653sup1.cif Structure factors: contains datablocks I. DOI: 10.1107/S1600536810010263/hg2653Isup2.hkl Additional supplementary materials: crystallographic information; 3D view; checkCIF report
[Pd4(CH2)2Cl4(C28H40P2)2]·5C4H8OV = 4048.61 (9) Å3
Mr = 1833.05Z = 2
Triclinic, P1F(000) = 1888
Hall symbol: -P 1Dx = 1.504 Mg m3
a = 12.5799 (1) ÅMo Kα radiation, λ = 0.71073 Å
b = 17.2830 (3) ÅCell parameters from 5889 reflections
c = 19.7558 (2) ŵ = 1.13 mm1
α = 79.877 (1)°T = 200 K
β = 74.703 (1)°Polyhedron, colourless
γ = 80.717 (1)°0.18 × 0.18 × 0.06 mm
Bruker SMART CCD diffractometer15292 independent reflections
Radiation source: fine-focus sealed tube9483 reflections with I > 2σ(I)
graphiteRint = 0.056
ω scansθmax = 25.7°, θmin = 1.7°
Absorption correction: multi-scan (SADABS; Sheldrick, 2008a)h = −15→15
Tmin = 0.822, Tmax = 0.935k = −21→21
36611 measured reflectionsl = −24→24
Refinement on F2Primary atom site location: structure-invariant direct methods
Least-squares matrix: fullSecondary atom site location: difference Fourier map
R[F2 > 2σ(F2)] = 0.047Hydrogen site location: inferred from neighbouring sites
wR(F2) = 0.106H atoms treated by a mixture of independent and constrained refinement
S = 1.01w = 1/[σ2(Fo2) + (0.0417P)2 + 0.8053P] where P = (Fo2 + 2Fc2)/3
15292 reflections(Δ/σ)max = 0.001
915 parametersΔρmax = 0.82 e Å3
434 restraintsΔρmin = −0.73 e Å3
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 > 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.
xyzUiso*/UeqOcc. (<1)
Pd10.47930 (3)0.21727 (2)0.34085 (2)0.02319 (11)
Pd20.24625 (3)0.22887 (3)0.38000 (2)0.02516 (11)
Pd30.47029 (3)0.30751 (2)0.14456 (2)0.02341 (11)
Pd40.23706 (3)0.32848 (3)0.18531 (2)0.02701 (12)
Cl10.36596 (11)0.16459 (9)0.28118 (7)0.0361 (4)
Cl20.35972 (11)0.38581 (9)0.23512 (8)0.0430 (4)
Cl30.59914 (10)0.25954 (9)0.22297 (7)0.0339 (4)
Cl40.11979 (11)0.29472 (11)0.30539 (7)0.0504 (5)
C130.3675 (4)0.1783 (3)0.4288 (3)0.0288 (13)
H13A0.373 (4)0.1221 (15)0.430 (2)0.020 (6)*
H13B0.368 (4)0.190 (3)0.4733 (16)0.020 (6)*
C140.3510 (4)0.3541 (3)0.0940 (3)0.0251 (13)
H14A0.344 (4)0.332 (2)0.0546 (18)0.020 (6)*
H14B0.357 (4)0.4093 (15)0.085 (2)0.020 (6)*
P10.59170 (11)0.24153 (8)0.40365 (7)0.0233 (3)
P20.12809 (11)0.25216 (8)0.48211 (7)0.0234 (3)
P30.58086 (11)0.25881 (8)0.04890 (7)0.0220 (3)
P40.11326 (11)0.30836 (9)0.12971 (7)0.0258 (3)
C10.5481 (4)0.2807 (3)0.4894 (3)0.0237 (12)
C20.6275 (4)0.2669 (3)0.5296 (3)0.0298 (13)
H20.69150.23010.51630.036*
C30.6167 (5)0.3044 (4)0.5876 (3)0.0357 (15)
H30.67240.29280.61360.043*
C40.5254 (4)0.3586 (3)0.6083 (3)0.0284 (13)
H40.51920.38690.64650.034*
C50.1723 (5)0.3546 (3)0.6725 (3)0.0369 (15)
H50.17140.38180.71050.044*
C60.0989 (4)0.2990 (4)0.6812 (3)0.0359 (15)
H60.05150.28470.72640.043*
C70.0959 (4)0.2652 (3)0.6240 (3)0.0319 (14)
H70.04370.22890.63040.038*
C80.1666 (4)0.2818 (3)0.5564 (3)0.0241 (12)
C90.3453 (4)0.3529 (3)0.4850 (3)0.0210 (12)
H90.34910.32410.44460.025*
C100.3352 (4)0.4230 (3)0.5926 (3)0.0294 (13)
H100.33210.44800.63510.035*
C110.3217 (5)0.4861 (3)0.5282 (3)0.0371 (15)
H11A0.24860.51860.53950.045*
H11B0.38030.52150.51690.045*
C120.3306 (4)0.4437 (3)0.4638 (3)0.0308 (13)
H12A0.26270.45990.44600.037*
H12B0.39480.45950.42520.037*
C170.4513 (4)0.3315 (3)0.5133 (3)0.0217 (12)
C180.4433 (4)0.3705 (3)0.5715 (3)0.0274 (13)
C190.2483 (4)0.3315 (3)0.5492 (3)0.0230 (12)
C200.2466 (4)0.3694 (3)0.6072 (3)0.0275 (13)
C210.6853 (4)0.3135 (3)0.3499 (3)0.0307 (14)
H210.71420.29580.30220.037*
C220.6176 (5)0.3940 (3)0.3385 (3)0.0430 (16)
H22A0.55310.38790.32170.064*
H22B0.66380.42990.30310.064*
H22C0.59220.41610.38330.064*
C230.7874 (5)0.3200 (4)0.3761 (3)0.0456 (17)
H23A0.82860.26730.38350.068*
H23B0.76360.34210.42090.068*
H23C0.83530.35470.34070.068*
C250.6822 (4)0.1773 (3)0.0762 (3)0.0274 (13)
H250.71170.19680.11160.033*
C260.6233 (5)0.1063 (3)0.1158 (3)0.0389 (15)
H26A0.55990.12350.15320.058*
H26B0.67510.06710.13700.058*
H26C0.59700.08240.08270.058*
C270.7842 (4)0.1526 (4)0.0180 (3)0.0414 (16)
H27A0.82080.1993−0.00620.062*
H27B0.76060.1288−0.01630.062*
H27C0.83630.11400.03950.062*
C310.6835 (4)0.1482 (3)0.4194 (3)0.0321 (14)
H310.73970.15940.44290.038*
C320.6169 (5)0.0855 (3)0.4689 (3)0.0501 (18)
H32A0.57950.10540.51380.075*
H32B0.66700.03730.47800.075*
H32C0.56130.07350.44690.075*
C330.7457 (5)0.1193 (4)0.3483 (3)0.0468 (17)
H33A0.78850.16070.31810.070*
H33B0.69200.10770.32460.070*
H33C0.79620.07130.35710.070*
C350.6651 (5)0.3376 (3)−0.0035 (3)0.0330 (14)
H350.72420.3138−0.04150.040*
C360.5920 (5)0.4037 (3)−0.0393 (3)0.0535 (18)
H36A0.55800.3813−0.06950.080*
H36B0.63790.4440−0.06830.080*
H36C0.53370.4281−0.00290.080*
C370.7210 (5)0.3691 (4)0.0435 (3)0.056 (2)
H37A0.76640.32550.06540.084*
H37B0.66430.39370.08060.084*
H37C0.76840.40870.01490.084*
C410.0125 (4)0.3310 (3)0.4693 (3)0.0301 (13)
H41−0.01660.31770.43090.036*
C420.0557 (5)0.4103 (3)0.4422 (3)0.0423 (16)
H42A0.11800.40540.40070.063*
H42B0.08070.42760.47950.063*
H42C−0.00370.44940.42910.063*
C43−0.0856 (5)0.3370 (4)0.5334 (3)0.0494 (18)
H43A−0.11260.28520.54980.074*
H43B−0.14520.37580.52020.074*
H43C−0.06210.35380.57150.074*
C450.0110 (4)0.2437 (3)0.1876 (3)0.0341 (14)
H45−0.01660.26550.23360.041*
C460.0685 (5)0.1603 (4)0.2042 (3)0.0510 (18)
H46A0.13360.16330.22160.077*
H46B0.09200.13500.16110.077*
H46C0.01680.12910.24050.077*
C47−0.0916 (5)0.2408 (4)0.1605 (3)0.0503 (18)
H47A−0.12790.29470.15060.075*
H47B−0.14350.20940.19650.075*
H47C−0.06890.21630.11690.075*
C510.0572 (4)0.1624 (3)0.5190 (3)0.0297 (13)
H51−0.00460.17480.56070.036*
C520.1377 (5)0.0938 (3)0.5439 (3)0.0471 (17)
H52A0.16820.10940.57960.071*
H52B0.19830.08040.50340.071*
H52C0.09810.04750.56470.071*
C530.0074 (5)0.1400 (4)0.4633 (3)0.0445 (16)
H53A−0.04420.18460.44840.067*
H53B−0.03250.09380.48360.067*
H53C0.06700.12720.42210.067*
C550.0288 (4)0.4056 (3)0.1131 (3)0.0326 (14)
H55−0.03220.39680.09260.039*
C560.0986 (5)0.4633 (3)0.0601 (3)0.0433 (16)
H56A0.13100.44070.01590.065*
H56B0.15820.47360.07950.065*
H56C0.05190.51310.05040.065*
C57−0.0237 (5)0.4382 (4)0.1828 (3)0.0507 (18)
H57A−0.06880.39980.21570.076*
H57B−0.07090.48800.17400.076*
H57C0.03480.44780.20350.076*
C610.5362 (4)0.2169 (3)−0.0176 (3)0.0208 (12)
C620.6145 (5)0.2129 (3)−0.0826 (3)0.0335 (14)
H620.67780.2402−0.09220.040*
C630.6036 (5)0.1707 (3)−0.1339 (3)0.0371 (15)
H630.65820.1697−0.17750.045*
C640.5121 (4)0.1301 (3)−0.1204 (3)0.0316 (14)
H640.50440.0994−0.15390.038*
C650.1548 (5)0.1827 (4)−0.0661 (3)0.0404 (16)
H650.15520.1531−0.10240.049*
C660.0753 (5)0.2472 (4)−0.0516 (3)0.0433 (16)
H660.02370.2641−0.08030.052*
C670.0705 (4)0.2866 (3)0.0037 (3)0.0318 (14)
H670.01360.32930.01360.038*
C680.1480 (4)0.2657 (3)0.0465 (3)0.0247 (12)
C690.3374 (4)0.1758 (3)0.0579 (3)0.0239 (12)
H690.34180.20770.09450.029*
C700.3274 (5)0.0963 (3)−0.0395 (3)0.0360 (15)
H700.32280.0681−0.07840.043*
C710.3235 (5)0.0396 (3)0.0305 (3)0.0395 (15)
H71A0.3852−0.00390.02350.047*
H71B0.25270.01630.04560.047*
C720.3337 (5)0.0862 (3)0.0879 (3)0.0335 (14)
H72A0.40230.06460.10390.040*
H72B0.26960.08000.12930.040*
C770.4402 (4)0.1786 (3)−0.0054 (3)0.0240 (12)
C780.4326 (4)0.1349 (3)−0.0579 (3)0.0255 (12)
C790.2347 (4)0.2052 (3)0.0281 (3)0.0252 (13)
C800.2345 (4)0.1623 (3)−0.0263 (3)0.0326 (14)
O800.1835 (5)0.6705 (3)0.1947 (3)0.0915 (19)
C810.2354 (8)0.6670 (5)0.2510 (5)0.095 (3)
H81A0.19240.70420.28400.114*
H81B0.31120.68240.23190.114*
C820.2408 (6)0.5849 (4)0.2891 (4)0.075 (2)
H82A0.22850.58450.34080.090*
H82B0.31300.55370.27120.090*
C830.1470 (6)0.5538 (4)0.2719 (4)0.066 (2)
H83A0.16130.49570.27210.080*
H83B0.07540.56690.30590.080*
C840.1476 (7)0.5960 (4)0.1998 (4)0.078 (3)
H84A0.19840.56530.16380.094*
H84B0.07210.60290.19160.094*
O850.2286 (6)−0.1162 (4)0.3862 (3)0.132 (3)
C860.2504 (10)−0.1239 (5)0.3145 (4)0.121 (4)
H86A0.1959−0.15450.30640.146*
H86B0.3258−0.15190.29850.146*
C870.2416 (8)−0.0422 (5)0.2748 (4)0.089 (3)
H87A0.3159−0.02470.25360.106*
H87B0.2025−0.03920.23680.106*
C880.1768 (7)0.0059 (4)0.3300 (4)0.080 (2)
H88A0.19430.06120.31860.096*
H88B0.09600.00570.33690.096*
C890.2148 (8)−0.0357 (5)0.3923 (4)0.096 (3)
H89A0.2859−0.01870.39320.116*
H89B0.1591−0.02460.43650.116*
O900.0116 (9)−0.1175 (5)0.2291 (6)0.174 (4)
C910.0593 (9)−0.1076 (9)0.1565 (6)0.184 (8)
H91A0.0489−0.15350.13620.220*
H91B0.1401−0.10610.14840.220*
C920.0106 (9)−0.0350 (7)0.1205 (5)0.120 (4)
H92A−0.0069−0.04450.07680.144*
H92B0.06060.00680.10820.144*
C93−0.0921 (7)−0.0134 (5)0.1748 (5)0.089 (3)
H93A−0.10550.04440.17560.107*
H93B−0.1575−0.03070.16530.107*
C94−0.0704 (8)−0.0555 (8)0.2414 (5)0.135 (4)
H94A−0.0475−0.01870.26650.162*
H94B−0.1391−0.07560.27200.162*
O950.7300 (10)0.5637 (7)0.2061 (7)0.079 (4)0.429 (8)
C960.680 (2)0.6400 (9)0.1905 (16)0.090 (6)0.429 (8)
H96A0.73560.67260.15790.107*0.429 (8)
H96B0.65030.66440.23450.107*0.429 (8)
C970.591 (2)0.6369 (12)0.1573 (17)0.112 (6)0.429 (8)
H97A0.58890.68040.11760.134*0.429 (8)
H97B0.51780.64000.19210.134*0.429 (8)
C980.620 (2)0.5577 (13)0.1312 (16)0.102 (7)0.429 (8)
H98A0.55440.52790.14600.122*0.429 (8)
H98B0.64450.56450.07890.122*0.429 (8)
C990.7080 (17)0.5161 (9)0.1624 (11)0.071 (5)0.429 (8)
H99A0.68560.46540.19050.085*0.429 (8)
H99B0.77540.50420.12480.085*0.429 (8)
O95B0.5847 (12)0.5705 (7)0.2323 (5)0.133 (5)0.571 (8)
C96B0.612 (2)0.6465 (9)0.2023 (8)0.102 (6)0.571 (8)
H96C0.65510.66550.23000.123*0.571 (8)
H96D0.54370.68400.20170.123*0.571 (8)
C97B0.678 (2)0.6408 (10)0.1300 (8)0.114 (6)0.571 (8)
H97C0.75310.65580.12370.137*0.571 (8)
H97D0.64180.67580.09520.137*0.571 (8)
C98B0.6847 (17)0.5567 (10)0.1210 (9)0.107 (6)0.571 (8)
H98C0.67320.55200.07430.129*0.571 (8)
H98D0.75750.52740.12550.129*0.571 (8)
C99B0.5943 (15)0.5271 (9)0.1789 (8)0.090 (5)0.571 (8)
H99C0.52420.53480.16330.108*0.571 (8)
H99D0.61260.47000.19470.108*0.571 (8)
O1000.6310 (6)−0.0810 (3)0.2290 (3)0.094 (2)
C1010.6399 (8)−0.1579 (4)0.2635 (4)0.091 (3)
H10A0.7157−0.18480.24670.109*
H10B0.5864−0.18790.25350.109*
C1020.6167 (7)−0.1553 (5)0.3389 (4)0.089 (3)
H10C0.6824−0.17880.35740.107*
H10D0.5536−0.18500.36470.107*
C1030.5893 (10)−0.0716 (5)0.3481 (4)0.130 (4)
H10E0.5153−0.06240.38080.156*
H10F0.6451−0.05440.36750.156*
C1040.5895 (8)−0.0291 (4)0.2784 (4)0.089 (3)
H10G0.5131−0.00580.27620.107*
H10H0.63630.01450.26800.107*
U11U22U33U12U13U23
Pd10.0153 (2)0.0337 (3)0.0231 (2)−0.00019 (18)−0.00609 (18)−0.01090 (19)
Pd20.0153 (2)0.0391 (3)0.0236 (2)−0.00203 (19)−0.00592 (18)−0.0102 (2)
Pd30.0175 (2)0.0314 (3)0.0243 (2)−0.00120 (18)−0.00655 (18)−0.01135 (19)
Pd40.0174 (2)0.0401 (3)0.0253 (3)0.00263 (19)−0.00767 (19)−0.0111 (2)
Cl10.0238 (7)0.0553 (10)0.0362 (9)−0.0054 (7)−0.0060 (6)−0.0261 (7)
Cl20.0267 (8)0.0601 (11)0.0519 (10)0.0057 (7)−0.0123 (7)−0.0394 (8)
Cl30.0186 (7)0.0640 (10)0.0220 (8)−0.0036 (7)−0.0059 (6)−0.0136 (7)
Cl40.0196 (8)0.1063 (14)0.0236 (8)0.0052 (8)−0.0084 (6)−0.0112 (9)
C130.022 (3)0.035 (3)0.030 (3)−0.003 (3)−0.007 (3)−0.006 (3)
C140.023 (3)0.024 (3)0.031 (3)−0.002 (2)−0.008 (3)−0.009 (3)
P10.0143 (7)0.0337 (9)0.0235 (8)−0.0005 (6)−0.0064 (6)−0.0081 (6)
P20.0138 (7)0.0324 (9)0.0249 (8)0.0005 (6)−0.0062 (6)−0.0067 (6)
P30.0185 (7)0.0271 (8)0.0217 (8)−0.0038 (6)−0.0051 (6)−0.0060 (6)
P40.0188 (7)0.0350 (9)0.0242 (8)−0.0015 (6)−0.0081 (6)−0.0026 (7)
C10.024 (3)0.028 (3)0.021 (3)−0.007 (2)−0.008 (2)−0.004 (2)
C20.022 (3)0.043 (4)0.024 (3)0.003 (3)−0.008 (2)−0.006 (3)
C30.026 (3)0.059 (4)0.025 (3)−0.011 (3)−0.008 (3)−0.006 (3)
C40.027 (3)0.043 (4)0.020 (3)−0.010 (3)−0.006 (2)−0.012 (3)
C50.030 (3)0.050 (4)0.029 (4)0.006 (3)−0.002 (3)−0.017 (3)
C60.025 (3)0.058 (4)0.020 (3)−0.004 (3)0.004 (2)−0.006 (3)
C70.024 (3)0.047 (4)0.026 (3)−0.008 (3)−0.006 (3)−0.005 (3)
C80.016 (3)0.032 (3)0.023 (3)0.004 (2)−0.005 (2)−0.006 (2)
C90.014 (3)0.030 (3)0.020 (3)0.000 (2)−0.006 (2)−0.005 (2)
C100.031 (3)0.028 (3)0.034 (3)0.002 (3)−0.011 (3)−0.015 (3)
C110.043 (4)0.031 (3)0.040 (4)−0.005 (3)−0.011 (3)−0.010 (3)
C120.030 (3)0.031 (3)0.028 (3)0.000 (3)−0.008 (3)0.001 (3)
C170.016 (3)0.029 (3)0.020 (3)−0.004 (2)−0.005 (2)−0.001 (2)
C180.028 (3)0.031 (3)0.023 (3)−0.011 (3)−0.004 (2)0.000 (2)
C190.020 (3)0.025 (3)0.023 (3)0.007 (2)−0.009 (2)−0.003 (2)
C200.021 (3)0.030 (3)0.032 (3)0.005 (2)−0.009 (3)−0.010 (3)
C210.024 (3)0.052 (4)0.019 (3)−0.014 (3)−0.003 (2)−0.006 (3)
C220.048 (4)0.048 (4)0.037 (4)−0.021 (3)−0.009 (3)−0.006 (3)
C230.032 (4)0.080 (5)0.032 (4)−0.022 (3)−0.005 (3)−0.014 (3)
C250.021 (3)0.036 (3)0.028 (3)0.000 (2)−0.007 (2)−0.010 (3)
C260.038 (4)0.036 (4)0.043 (4)0.008 (3)−0.016 (3)−0.007 (3)
C270.024 (3)0.060 (4)0.040 (4)0.010 (3)−0.008 (3)−0.019 (3)
C310.025 (3)0.038 (4)0.037 (4)0.008 (3)−0.015 (3)−0.012 (3)
C320.049 (4)0.037 (4)0.056 (5)0.014 (3)−0.015 (4)−0.003 (3)
C330.042 (4)0.053 (4)0.043 (4)0.022 (3)−0.013 (3)−0.021 (3)
C350.033 (3)0.037 (4)0.029 (3)−0.013 (3)−0.001 (3)−0.007 (3)
C360.054 (4)0.036 (4)0.060 (5)−0.010 (3)−0.003 (4)0.008 (3)
C370.054 (4)0.075 (5)0.048 (4)−0.045 (4)−0.002 (3)−0.015 (4)
C410.026 (3)0.038 (4)0.027 (3)0.002 (3)−0.010 (3)−0.008 (3)
C420.038 (4)0.035 (4)0.056 (4)0.004 (3)−0.023 (3)−0.005 (3)
C430.031 (4)0.076 (5)0.037 (4)0.022 (3)−0.012 (3)−0.018 (3)
C450.022 (3)0.050 (4)0.028 (3)−0.008 (3)−0.004 (3)0.001 (3)
C460.036 (4)0.054 (4)0.053 (4)−0.016 (3)0.001 (3)0.012 (3)
C470.026 (3)0.081 (5)0.045 (4)−0.019 (3)−0.008 (3)0.000 (4)
C510.020 (3)0.035 (3)0.030 (3)−0.005 (2)0.001 (2)−0.004 (3)
C520.045 (4)0.032 (4)0.063 (5)−0.008 (3)−0.016 (3)0.003 (3)
C530.043 (4)0.043 (4)0.057 (4)−0.013 (3)−0.023 (3)−0.010 (3)
C550.028 (3)0.036 (4)0.037 (4)0.003 (3)−0.018 (3)−0.002 (3)
C560.048 (4)0.034 (4)0.050 (4)−0.003 (3)−0.022 (3)0.004 (3)
C570.053 (4)0.049 (4)0.048 (4)0.014 (3)−0.015 (3)−0.016 (3)
C610.018 (3)0.023 (3)0.021 (3)0.001 (2)−0.006 (2)−0.004 (2)
C620.031 (3)0.041 (4)0.028 (3)−0.011 (3)−0.003 (3)−0.005 (3)
C630.035 (4)0.052 (4)0.023 (3)−0.002 (3)−0.002 (3)−0.012 (3)
C640.034 (3)0.034 (3)0.030 (3)0.005 (3)−0.011 (3)−0.017 (3)
C650.043 (4)0.050 (4)0.040 (4)−0.010 (3)−0.020 (3)−0.019 (3)
C660.031 (4)0.063 (5)0.043 (4)−0.005 (3)−0.020 (3)−0.010 (3)
C670.020 (3)0.048 (4)0.028 (3)0.000 (3)−0.009 (3)−0.007 (3)
C680.021 (3)0.029 (3)0.026 (3)−0.006 (2)−0.009 (2)−0.003 (2)
C690.023 (3)0.022 (3)0.030 (3)−0.005 (2)−0.011 (2)−0.004 (2)
C700.040 (4)0.036 (4)0.040 (4)−0.004 (3)−0.018 (3)−0.016 (3)
C710.035 (4)0.029 (3)0.056 (4)−0.011 (3)−0.007 (3)−0.009 (3)
C720.033 (3)0.030 (3)0.038 (4)−0.008 (3)−0.012 (3)0.001 (3)
C770.026 (3)0.018 (3)0.028 (3)0.002 (2)−0.012 (2)0.000 (2)
C780.026 (3)0.030 (3)0.024 (3)−0.001 (2)−0.011 (3)−0.009 (2)
C790.023 (3)0.034 (3)0.023 (3)−0.012 (3)−0.007 (2)−0.004 (2)
C800.029 (3)0.034 (3)0.040 (4)−0.011 (3)−0.013 (3)−0.004 (3)
O800.132 (5)0.070 (4)0.068 (4)−0.040 (4)−0.005 (4)−0.001 (3)
C810.107 (8)0.091 (8)0.086 (7)−0.048 (6)−0.003 (6)−0.005 (6)
C820.078 (6)0.053 (5)0.083 (6)−0.003 (4)0.003 (5)−0.025 (5)
C830.055 (5)0.045 (5)0.078 (6)−0.002 (4)0.016 (4)−0.006 (4)
C840.087 (6)0.076 (6)0.066 (6)−0.035 (5)0.020 (5)−0.030 (5)
O850.192 (8)0.086 (5)0.080 (5)0.053 (5)−0.016 (5)0.000 (4)
C860.216 (13)0.072 (7)0.062 (6)0.029 (7)−0.023 (7)−0.030 (5)
C870.125 (8)0.086 (7)0.050 (5)0.005 (6)−0.023 (5)−0.010 (5)
C880.088 (7)0.067 (6)0.091 (7)−0.003 (5)−0.042 (6)−0.008 (5)
C890.124 (9)0.084 (7)0.081 (7)0.006 (6)−0.035 (6)−0.016 (6)
O900.161 (9)0.121 (7)0.222 (11)−0.004 (6)−0.038 (8)−0.003 (7)
C910.090 (9)0.36 (2)0.109 (10)0.087 (11)−0.025 (8)−0.158 (13)
C920.101 (9)0.169 (12)0.092 (8)−0.061 (8)0.008 (7)−0.032 (8)
C930.072 (7)0.078 (6)0.125 (9)−0.013 (5)−0.036 (7)−0.012 (6)
C940.070 (8)0.192 (14)0.117 (10)0.002 (8)0.009 (7)−0.018 (10)
O950.079 (9)0.079 (8)0.098 (10)0.016 (7)−0.055 (8)−0.037 (7)
C960.117 (15)0.074 (9)0.090 (15)−0.010 (10)−0.058 (12)0.003 (10)
C970.142 (14)0.099 (11)0.117 (14)0.035 (11)−0.096 (11)−0.023 (11)
C980.110 (16)0.103 (13)0.114 (16)0.025 (12)−0.081 (12)−0.026 (12)
C990.093 (12)0.077 (10)0.052 (11)0.005 (9)−0.049 (9)−0.004 (8)
O95B0.203 (14)0.092 (8)0.075 (7)−0.028 (8)0.022 (8)−0.010 (6)
C96B0.162 (16)0.072 (8)0.075 (10)−0.012 (10)−0.027 (11)−0.021 (7)
C97B0.142 (14)0.100 (10)0.090 (11)−0.063 (11)0.010 (10)0.001 (9)
C98B0.124 (14)0.107 (10)0.079 (10)0.020 (11)−0.007 (9)−0.037 (9)
C99B0.137 (13)0.071 (9)0.082 (10)−0.040 (9)−0.062 (9)0.017 (7)
O1000.168 (6)0.062 (4)0.072 (4)−0.023 (4)−0.059 (4)−0.006 (3)
C1010.140 (9)0.049 (6)0.091 (7)0.003 (5)−0.048 (6)−0.015 (5)
C1020.105 (7)0.086 (7)0.071 (7)−0.033 (6)−0.020 (5)0.024 (5)
C1030.232 (14)0.077 (7)0.057 (7)−0.033 (8)0.010 (7)−0.004 (5)
C1040.128 (8)0.053 (5)0.086 (7)0.011 (5)−0.037 (6)−0.011 (5)
Pd1—C132.014 (6)C52—H52B0.9800
Pd1—P12.2393 (13)C52—H52C0.9800
Pd1—Cl12.4360 (13)C53—H53A0.9800
Pd1—Cl32.4767 (14)C53—H53B0.9800
Pd1—Pd22.8110 (5)C53—H53C0.9800
Pd2—C132.017 (5)C55—C561.515 (7)
Pd2—P22.2251 (14)C55—C571.524 (7)
Pd2—Cl12.4465 (14)C55—H551.0000
Pd2—Cl42.4621 (14)C56—H56A0.9800
Pd3—C142.004 (5)C56—H56B0.9800
Pd3—P32.2380 (14)C56—H56C0.9800
Pd3—Cl22.4284 (14)C57—H57A0.9800
Pd3—Cl32.4807 (13)C57—H57B0.9800
Pd3—Pd42.8109 (6)C57—H57C0.9800
Pd4—C142.016 (5)C61—C621.402 (7)
Pd4—P42.2281 (14)C61—C771.416 (7)
Pd4—Cl22.4429 (14)C62—C631.394 (7)
Pd4—Cl42.4676 (15)C62—H620.9500
C13—H13A0.96 (2)C63—C641.386 (7)
C13—H13B0.94 (2)C63—H630.9500
C14—H14A0.95 (2)C64—C781.374 (7)
C14—H14B0.95 (2)C64—H640.9500
P1—C211.847 (5)C65—C661.387 (8)
P1—C11.850 (5)C65—C801.397 (7)
P1—C311.856 (5)C65—H650.9500
P2—C81.836 (5)C66—C671.370 (7)
P2—C511.854 (5)C66—H660.9500
P2—C411.862 (5)C67—C681.418 (7)
P3—C251.848 (5)C67—H670.9500
P3—C611.850 (5)C68—C791.405 (7)
P3—C351.854 (5)C69—C791.536 (7)
P4—C681.838 (5)C69—C771.544 (7)
P4—C451.857 (5)C69—C721.562 (7)
P4—C551.864 (5)C69—H691.0000
C1—C21.400 (7)C70—C801.500 (8)
C1—C171.406 (7)C70—C781.508 (7)
C2—C31.381 (7)C70—C711.541 (8)
C2—H20.9500C70—H701.0000
C3—C41.379 (7)C71—C721.544 (7)
C3—H30.9500C71—H71A0.9900
C4—C181.382 (7)C71—H71B0.9900
C4—H40.9500C72—H72A0.9900
C5—C201.389 (7)C72—H72B0.9900
C5—C61.396 (8)C77—C781.416 (7)
C5—H50.9500C79—C801.408 (7)
C6—C71.372 (7)O80—C841.410 (7)
C6—H60.9500O80—C811.419 (8)
C7—C81.407 (7)C81—C821.485 (8)
C7—H70.9500C81—H81A0.9900
C8—C191.407 (7)C81—H81B0.9900
C9—C171.545 (6)C82—C831.509 (8)
C9—C121.545 (7)C82—H82A0.9900
C9—C191.549 (7)C82—H82B0.9900
C9—H91.0000C83—C841.481 (8)
C10—C201.501 (7)C83—H83A0.9900
C10—C181.510 (7)C83—H83B0.9900
C10—C111.550 (7)C84—H84A0.9900
C10—H101.0000C84—H84B0.9900
C11—C121.546 (7)O85—C861.396 (8)
C11—H11A0.9900O85—C891.398 (8)
C11—H11B0.9900C86—C871.493 (9)
C12—H12A0.9900C86—H86A0.9900
C12—H12B0.9900C86—H86B0.9900
C17—C181.406 (7)C87—C881.476 (8)
C19—C201.409 (7)C87—H87A0.9900
C21—C221.524 (8)C87—H87B0.9900
C21—C231.531 (7)C88—C891.466 (8)
C21—H211.0000C88—H88A0.9900
C22—H22A0.9800C88—H88B0.9900
C22—H22B0.9800C89—H89A0.9900
C22—H22C0.9800C89—H89B0.9900
C23—H23A0.9800O90—C941.368 (9)
C23—H23B0.9800O90—C911.392 (10)
C23—H23C0.9800C91—C921.459 (11)
C25—C261.524 (7)C91—H91A0.9900
C25—C271.539 (7)C91—H91B0.9900
C25—H251.0000C92—C931.488 (9)
C26—H26A0.9800C92—H92A0.9900
C26—H26B0.9800C92—H92B0.9900
C26—H26C0.9800C93—C941.458 (10)
C27—H27A0.9800C93—H93A0.9900
C27—H27B0.9800C93—H93B0.9900
C27—H27C0.9800C94—H94A0.9900
C31—C321.523 (8)C94—H94B0.9900
C31—C331.541 (7)O95—C961.386 (12)
C31—H311.0000O95—C991.395 (12)
C32—H32A0.9800C96—C971.457 (13)
C32—H32B0.9800C96—H96A0.9900
C32—H32C0.9800C96—H96B0.9900
C33—H33A0.9800C97—C981.503 (14)
C33—H33B0.9800C97—H97A0.9900
C33—H33C0.9800C97—H97B0.9900
C35—C371.517 (7)C98—C991.442 (13)
C35—C361.540 (8)C98—H98A0.9900
C35—H351.0000C98—H98B0.9900
C36—H36A0.9800C99—H99A0.9900
C36—H36B0.9800C99—H99B0.9900
C36—H36C0.9800O95B—C99B1.369 (11)
C37—H37A0.9800O95B—C96B1.400 (12)
C37—H37B0.9800C96B—C97B1.462 (13)
C37—H37C0.9800C96B—H96C0.9900
C41—C421.513 (7)C96B—H96D0.9900
C41—C431.523 (7)C97B—C98B1.481 (13)
C41—H411.0000C97B—H97C0.9900
C42—H42A0.9800C97B—H97D0.9900
C42—H42B0.9800C98B—C99B1.469 (13)
C42—H42C0.9800C98B—H98C0.9900
C43—H43A0.9800C98B—H98D0.9900
C43—H43B0.9800C99B—H99C0.9900
C43—H43C0.9800C99B—H99D0.9900
C45—C461.526 (8)O100—C1011.385 (7)
C45—C471.533 (7)O100—C1041.386 (7)
C45—H451.0000C101—C1021.449 (8)
C46—H46A0.9800C101—H10A0.9900
C46—H46B0.9800C101—H10B0.9900
C46—H46C0.9800C102—C1031.463 (9)
C47—H47A0.9800C102—H10C0.9900
C47—H47B0.9800C102—H10D0.9900
C47—H47C0.9800C103—C1041.441 (8)
C51—C531.532 (7)C103—H10E0.9900
C51—C521.532 (7)C103—H10F0.9900
C51—H511.0000C104—H10G0.9900
C52—H52A0.9800C104—H10H0.9900
C13—Pd1—P192.48 (16)H47B—C47—H47C109.5
C13—Pd1—Cl183.25 (16)C53—C51—C52110.9 (5)
P1—Pd1—Cl1169.09 (5)C53—C51—P2109.8 (4)
C13—Pd1—Cl3171.59 (16)C52—C51—P2110.7 (4)
P1—Pd1—Cl395.90 (5)C53—C51—H51108.4
Cl1—Pd1—Cl388.39 (5)C52—C51—H51108.4
C13—Pd1—Pd245.84 (15)P2—C51—H51108.4
P1—Pd1—Pd2127.42 (4)C51—C52—H52A109.5
Cl1—Pd1—Pd255.02 (3)C51—C52—H52B109.5
Cl3—Pd1—Pd2127.57 (3)H52A—C52—H52B109.5
C13—Pd2—P292.22 (16)C51—C52—H52C109.5
C13—Pd2—Cl182.90 (16)H52A—C52—H52C109.5
P2—Pd2—Cl1163.70 (6)H52B—C52—H52C109.5
C13—Pd2—Cl4171.82 (16)C51—C53—H53A109.5
P2—Pd2—Cl495.20 (5)C51—C53—H53B109.5
Cl1—Pd2—Cl490.85 (5)H53A—C53—H53B109.5
C13—Pd2—Pd145.73 (16)C51—C53—H53C109.5
P2—Pd2—Pd1130.03 (4)H53A—C53—H53C109.5
Cl1—Pd2—Pd154.67 (3)H53B—C53—H53C109.5
Cl4—Pd2—Pd1126.13 (4)C56—C55—C57111.5 (5)
C14—Pd3—P392.96 (16)C56—C55—P4110.9 (4)
C14—Pd3—Cl283.43 (15)C57—C55—P4109.9 (4)
P3—Pd3—Cl2168.52 (6)C56—C55—H55108.2
C14—Pd3—Cl3171.08 (16)C57—C55—H55108.2
P3—Pd3—Cl395.94 (5)P4—C55—H55108.2
Cl2—Pd3—Cl387.73 (5)C55—C56—H56A109.5
C14—Pd3—Pd445.81 (15)C55—C56—H56B109.5
P3—Pd3—Pd4128.42 (4)H56A—C56—H56B109.5
Cl2—Pd3—Pd455.00 (3)C55—C56—H56C109.5
Cl3—Pd3—Pd4126.99 (3)H56A—C56—H56C109.5
C14—Pd4—P493.15 (15)H56B—C56—H56C109.5
C14—Pd4—Cl282.81 (15)C55—C57—H57A109.5
P4—Pd4—Cl2165.38 (6)C55—C57—H57B109.5
C14—Pd4—Cl4171.78 (15)H57A—C57—H57B109.5
P4—Pd4—Cl494.75 (5)C55—C57—H57C109.5
Cl2—Pd4—Cl490.06 (5)H57A—C57—H57C109.5
C14—Pd4—Pd345.46 (15)H57B—C57—H57C109.5
P4—Pd4—Pd3130.09 (4)C62—C61—C77117.8 (5)
Cl2—Pd4—Pd354.52 (3)C62—C61—P3115.2 (4)
Cl4—Pd4—Pd3126.60 (4)C77—C61—P3126.2 (4)
Pd1—Cl1—Pd270.30 (4)C63—C62—C61122.9 (5)
Pd3—Cl2—Pd470.48 (4)C63—C62—H62118.5
Pd1—Cl3—Pd3105.30 (5)C61—C62—H62118.5
Pd2—Cl4—Pd4106.56 (5)C64—C63—C62119.0 (5)
Pd1—C13—Pd288.4 (2)C64—C63—H63120.5
Pd1—C13—H13A106 (3)C62—C63—H63120.5
Pd2—C13—H13A108 (3)C78—C64—C63119.1 (5)
Pd1—C13—H13B121 (3)C78—C64—H64120.4
Pd2—C13—H13B121 (3)C63—C64—H64120.4
H13A—C13—H13B110 (4)C66—C65—C80118.6 (5)
Pd3—C14—Pd488.7 (2)C66—C65—H65120.7
Pd3—C14—H14A120 (3)C80—C65—H65120.7
Pd4—C14—H14A116 (3)C67—C66—C65120.6 (5)
Pd3—C14—H14B105 (3)C67—C66—H66119.7
Pd4—C14—H14B110 (3)C65—C66—H66119.7
H14A—C14—H14B114 (4)C66—C67—C68122.0 (5)
C21—P1—C1101.1 (2)C66—C67—H67119.0
C21—P1—C31105.4 (3)C68—C67—H67119.0
C1—P1—C31105.2 (2)C79—C68—C67117.6 (5)
C21—P1—Pd1110.04 (17)C79—C68—P4124.9 (4)
C1—P1—Pd1126.30 (17)C67—C68—P4116.7 (4)
C31—P1—Pd1107.06 (18)C79—C69—C77107.3 (4)
C8—P2—C51106.0 (2)C79—C69—C72107.9 (4)
C8—P2—C41101.1 (2)C77—C69—C72105.3 (4)
C51—P2—C41103.6 (2)C79—C69—H69112.0
C8—P2—Pd2124.66 (17)C77—C69—H69112.0
C51—P2—Pd2107.31 (18)C72—C69—H69112.0
C41—P2—Pd2112.23 (17)C80—C70—C78105.5 (4)
C25—P3—C61101.7 (2)C80—C70—C71108.2 (5)
C25—P3—C35105.2 (2)C78—C70—C71108.1 (4)
C61—P3—C35104.6 (2)C80—C70—H70111.6
C25—P3—Pd3109.80 (17)C78—C70—H70111.6
C61—P3—Pd3126.43 (16)C71—C70—H70111.6
C35—P3—Pd3107.38 (18)C70—C71—C72109.1 (4)
C68—P4—C45101.5 (2)C70—C71—H71A109.9
C68—P4—C55105.9 (2)C72—C71—H71A109.9
C45—P4—C55104.2 (3)C70—C71—H71B109.9
C68—P4—Pd4124.74 (17)C72—C71—H71B109.9
C45—P4—Pd4111.81 (18)H71A—C71—H71B108.3
C55—P4—Pd4106.91 (18)C71—C72—C69110.3 (4)
C2—C1—C17117.0 (5)C71—C72—H72A109.6
C2—C1—P1115.6 (4)C69—C72—H72A109.6
C17—C1—P1126.8 (4)C71—C72—H72B109.6
C3—C2—C1122.7 (5)C69—C72—H72B109.6
C3—C2—H2118.6H72A—C72—H72B108.1
C1—C2—H2118.6C78—C77—C61117.8 (5)
C4—C3—C2120.5 (5)C78—C77—C69111.9 (4)
C4—C3—H3119.8C61—C77—C69130.3 (4)
C2—C3—H3119.8C64—C78—C77123.1 (5)
C3—C4—C18117.9 (5)C64—C78—C70123.4 (5)
C3—C4—H4121.1C77—C78—C70113.4 (5)
C18—C4—H4121.1C68—C79—C80119.4 (5)
C20—C5—C6118.7 (5)C68—C79—C69130.0 (4)
C20—C5—H5120.6C80—C79—C69110.6 (5)
C6—C5—H5120.6C65—C80—C79121.4 (5)
C7—C6—C5119.4 (5)C65—C80—C70123.3 (5)
C7—C6—H6120.3C79—C80—C70115.3 (5)
C5—C6—H6120.3C84—O80—C81107.5 (6)
C6—C7—C8123.0 (5)O80—C81—C82108.9 (6)
C6—C7—H7118.5O80—C81—H81A109.9
C8—C7—H7118.5C82—C81—H81A109.9
C19—C8—C7117.6 (5)O80—C81—H81B109.9
C19—C8—P2124.7 (4)C82—C81—H81B109.9
C7—C8—P2116.7 (4)H81A—C81—H81B108.3
C17—C9—C12107.1 (4)C81—C82—C83101.9 (6)
C17—C9—C19105.5 (4)C81—C82—H82A111.4
C12—C9—C19107.9 (4)C83—C82—H82A111.4
C17—C9—H9112.0C81—C82—H82B111.4
C12—C9—H9112.0C83—C82—H82B111.4
C19—C9—H9112.0H82A—C82—H82B109.2
C20—C10—C18105.0 (4)C84—C83—C82102.3 (6)
C20—C10—C11108.4 (4)C84—C83—H83A111.3
C18—C10—C11108.5 (4)C82—C83—H83A111.3
C20—C10—H10111.5C84—C83—H83B111.3
C18—C10—H10111.5C82—C83—H83B111.3
C11—C10—H10111.5H83A—C83—H83B109.2
C12—C11—C10109.0 (4)O80—C84—C83107.8 (6)
C12—C11—H11A109.9O80—C84—H84A110.1
C10—C11—H11A109.9C83—C84—H84A110.1
C12—C11—H11B109.9O80—C84—H84B110.1
C10—C11—H11B109.9C83—C84—H84B110.1
H11A—C11—H11B108.3H84A—C84—H84B108.5
C9—C12—C11110.4 (4)C86—O85—C89108.4 (6)
C9—C12—H12A109.6O85—C86—C87107.0 (6)
C11—C12—H12A109.6O85—C86—H86A110.3
C9—C12—H12B109.6C87—C86—H86A110.3
C11—C12—H12B109.6O85—C86—H86B110.3
H12A—C12—H12B108.1C87—C86—H86B110.3
C1—C17—C18119.1 (4)H86A—C86—H86B108.6
C1—C17—C9129.5 (4)C88—C87—C86103.1 (6)
C18—C17—C9111.4 (4)C88—C87—H87A111.1
C4—C18—C17122.6 (5)C86—C87—H87A111.1
C4—C18—C10123.1 (5)C88—C87—H87B111.1
C17—C18—C10114.2 (4)C86—C87—H87B111.1
C8—C19—C20118.7 (5)H87A—C87—H87B109.1
C8—C19—C9129.7 (4)C89—C88—C87101.5 (6)
C20—C19—C9111.6 (4)C89—C88—H88A111.5
C5—C20—C19122.1 (5)C87—C88—H88A111.5
C5—C20—C10123.9 (5)C89—C88—H88B111.5
C19—C20—C10113.9 (5)C87—C88—H88B111.5
C22—C21—C23111.5 (5)H88A—C88—H88B109.3
C22—C21—P1109.1 (4)O85—C89—C88105.8 (6)
C23—C21—P1116.8 (4)O85—C89—H89A110.6
C22—C21—H21106.3C88—C89—H89A110.6
C23—C21—H21106.3O85—C89—H89B110.6
P1—C21—H21106.3C88—C89—H89B110.6
C21—C22—H22A109.5H89A—C89—H89B108.7
C21—C22—H22B109.5C94—O90—C91106.6 (8)
H22A—C22—H22B109.5O90—C91—C92111.8 (8)
C21—C22—H22C109.5O90—C91—H91A109.3
H22A—C22—H22C109.5C92—C91—H91A109.3
H22B—C22—H22C109.5O90—C91—H91B109.3
C21—C23—H23A109.5C92—C91—H91B109.3
C21—C23—H23B109.5H91A—C91—H91B107.9
H23A—C23—H23B109.5C91—C92—C93102.1 (7)
C21—C23—H23C109.5C91—C92—H92A111.3
H23A—C23—H23C109.5C93—C92—H92A111.3
H23B—C23—H23C109.5C91—C92—H92B111.3
C26—C25—C27111.3 (5)C93—C92—H92B111.3
C26—C25—P3110.2 (4)H92A—C92—H92B109.2
C27—C25—P3116.7 (4)C94—C93—C92104.3 (7)
C26—C25—H25106.0C94—C93—H93A110.9
C27—C25—H25106.0C92—C93—H93A110.9
P3—C25—H25106.0C94—C93—H93B110.9
C25—C26—H26A109.5C92—C93—H93B110.9
C25—C26—H26B109.5H93A—C93—H93B108.9
H26A—C26—H26B109.5O90—C94—C93110.4 (8)
C25—C26—H26C109.5O90—C94—H94A109.6
H26A—C26—H26C109.5C93—C94—H94A109.6
H26B—C26—H26C109.5O90—C94—H94B109.6
C25—C27—H27A109.5C93—C94—H94B109.6
C25—C27—H27B109.5H94A—C94—H94B108.1
H27A—C27—H27B109.5C96—O95—C99108.5 (11)
C25—C27—H27C109.5O95—C96—C97108.8 (12)
H27A—C27—H27C109.5O95—C96—H96A109.9
H27B—C27—H27C109.5C97—C96—H96A109.9
C32—C31—C33111.6 (5)O95—C96—H96B109.9
C32—C31—P1110.6 (4)C97—C96—H96B109.9
C33—C31—P1110.1 (4)H96A—C96—H96B108.3
C32—C31—H31108.2C96—C97—C98103.2 (12)
C33—C31—H31108.2C96—C97—H97A111.1
P1—C31—H31108.2C98—C97—H97A111.1
C31—C32—H32A109.5C96—C97—H97B111.1
C31—C32—H32B109.5C98—C97—H97B111.1
H32A—C32—H32B109.5H97A—C97—H97B109.1
C31—C32—H32C109.5C99—C98—C97106.3 (11)
H32A—C32—H32C109.5C99—C98—H98A110.5
H32B—C32—H32C109.5C97—C98—H98A110.5
C31—C33—H33A109.5C99—C98—H98B110.5
C31—C33—H33B109.5C97—C98—H98B110.5
H33A—C33—H33B109.5H98A—C98—H98B108.7
C31—C33—H33C109.5O95—C99—C98108.6 (11)
H33A—C33—H33C109.5O95—C99—H99A110.0
H33B—C33—H33C109.5C98—C99—H99A110.0
C37—C35—C36111.8 (5)O95—C99—H99B110.0
C37—C35—P3110.0 (4)C98—C99—H99B110.0
C36—C35—P3110.2 (4)H99A—C99—H99B108.4
C37—C35—H35108.2C99B—O95B—C96B108.7 (10)
C36—C35—H35108.2O95B—C96B—C97B106.9 (10)
P3—C35—H35108.2O95B—C96B—H96C110.3
C35—C36—H36A109.5C97B—C96B—H96C110.3
C35—C36—H36B109.5O95B—C96B—H96D110.3
H36A—C36—H36B109.5C97B—C96B—H96D110.3
C35—C36—H36C109.5H96C—C96B—H96D108.6
H36A—C36—H36C109.5C96B—C97B—C98B105.2 (10)
H36B—C36—H36C109.5C96B—C97B—H97C110.7
C35—C37—H37A109.5C98B—C97B—H97C110.7
C35—C37—H37B109.5C96B—C97B—H97D110.7
H37A—C37—H37B109.5C98B—C97B—H97D110.7
C35—C37—H37C109.5H97C—C97B—H97D108.8
H37A—C37—H37C109.5C99B—C98B—C97B103.5 (10)
H37B—C37—H37C109.5C99B—C98B—H98C111.1
C42—C41—C43110.8 (5)C97B—C98B—H98C111.1
C42—C41—P2110.6 (4)C99B—C98B—H98D111.1
C43—C41—P2115.4 (4)C97B—C98B—H98D111.1
C42—C41—H41106.5H98C—C98B—H98D109.0
C43—C41—H41106.5O95B—C99B—C98B105.4 (11)
P2—C41—H41106.5O95B—C99B—H99C110.7
C41—C42—H42A109.5C98B—C99B—H99C110.7
C41—C42—H42B109.5O95B—C99B—H99D110.7
H42A—C42—H42B109.5C98B—C99B—H99D110.7
C41—C42—H42C109.5H99C—C99B—H99D108.8
H42A—C42—H42C109.5C101—O100—C104109.5 (6)
H42B—C42—H42C109.5O100—C101—C102108.5 (6)
C41—C43—H43A109.5O100—C101—H10A110.0
C41—C43—H43B109.5C102—C101—H10A110.0
H43A—C43—H43B109.5O100—C101—H10B110.0
C41—C43—H43C109.5C102—C101—H10B110.0
H43A—C43—H43C109.5H10A—C101—H10B108.4
H43B—C43—H43C109.5C101—C102—C103106.3 (6)
C46—C45—C47110.6 (5)C101—C102—H10C110.5
C46—C45—P4110.1 (4)C103—C102—H10C110.5
C47—C45—P4115.7 (4)C101—C102—H10D110.5
C46—C45—H45106.6C103—C102—H10D110.5
C47—C45—H45106.6H10C—C102—H10D108.7
P4—C45—H45106.6C104—C103—C102105.8 (6)
C45—C46—H46A109.5C104—C103—H10E110.6
C45—C46—H46B109.5C102—C103—H10E110.6
H46A—C46—H46B109.5C104—C103—H10F110.6
C45—C46—H46C109.5C102—C103—H10F110.6
H46A—C46—H46C109.5H10E—C103—H10F108.7
H46B—C46—H46C109.5O100—C104—C103108.9 (6)
C45—C47—H47A109.5O100—C104—H10G109.9
C45—C47—H47B109.5C103—C104—H10G109.9
H47A—C47—H47B109.5O100—C104—H10H109.9
C45—C47—H47C109.5C103—C104—H10H109.9
H47A—C47—H47C109.5H10G—C104—H10H108.3
P1—Pd1—Pd2—C13−48.2 (2)C11—C10—C18—C17−58.7 (6)
Cl1—Pd1—Pd2—C13118.6 (2)C7—C8—C19—C20−7.6 (7)
Cl3—Pd1—Pd2—C13173.1 (2)P2—C8—C19—C20160.4 (4)
C13—Pd1—Pd2—P241.6 (2)C7—C8—C19—C9172.3 (5)
P1—Pd1—Pd2—P2−6.58 (8)P2—C8—C19—C9−19.7 (8)
Cl1—Pd1—Pd2—P2160.23 (7)C17—C9—C19—C8−124.8 (5)
Cl3—Pd1—Pd2—P2−145.33 (7)C12—C9—C19—C8120.9 (5)
C13—Pd1—Pd2—Cl1−118.6 (2)C17—C9—C19—C2055.1 (5)
P1—Pd1—Pd2—Cl1−166.80 (7)C12—C9—C19—C20−59.2 (5)
Cl3—Pd1—Pd2—Cl154.44 (6)C6—C5—C20—C191.6 (8)
C13—Pd1—Pd2—Cl4−179.0 (2)C6—C5—C20—C10−175.2 (5)
P1—Pd1—Pd2—Cl4132.84 (7)C8—C19—C20—C54.9 (8)
Cl1—Pd1—Pd2—Cl4−60.35 (7)C9—C19—C20—C5−175.0 (5)
Cl3—Pd1—Pd2—Cl4−5.91 (7)C8—C19—C20—C10−178.0 (4)
P3—Pd3—Pd4—C14−47.2 (2)C9—C19—C20—C102.1 (6)
Cl2—Pd3—Pd4—C14119.1 (2)C18—C10—C20—C5118.9 (6)
Cl3—Pd3—Pd4—C14173.1 (2)C11—C10—C20—C5−125.3 (6)
C14—Pd3—Pd4—P443.3 (2)C18—C10—C20—C19−58.1 (6)
P3—Pd3—Pd4—P4−3.91 (8)C11—C10—C20—C1957.7 (6)
Cl2—Pd3—Pd4—P4162.40 (7)C1—P1—C21—C22−66.9 (4)
Cl3—Pd3—Pd4—P4−143.62 (7)C31—P1—C21—C22−176.2 (4)
C14—Pd3—Pd4—Cl2−119.1 (2)Pd1—P1—C21—C2268.7 (4)
P3—Pd3—Pd4—Cl2−166.31 (7)C1—P1—C21—C2360.6 (5)
Cl3—Pd3—Pd4—Cl253.98 (7)C31—P1—C21—C23−48.7 (5)
C14—Pd3—Pd4—Cl4−177.2 (2)Pd1—P1—C21—C23−163.8 (4)
P3—Pd3—Pd4—Cl4135.55 (7)C61—P3—C25—C26−67.4 (4)
Cl2—Pd3—Pd4—Cl4−58.15 (8)C35—P3—C25—C26−176.2 (4)
Cl3—Pd3—Pd4—Cl4−4.16 (8)Pd3—P3—C25—C2668.6 (4)
C13—Pd1—Cl1—Pd239.34 (16)C61—P3—C25—C2760.7 (4)
P1—Pd1—Cl1—Pd2106.8 (3)C35—P3—C25—C27−48.1 (5)
Cl3—Pd1—Cl1—Pd2−139.83 (5)Pd3—P3—C25—C27−163.3 (4)
C13—Pd2—Cl1—Pd1−39.29 (16)C21—P1—C31—C32175.1 (4)
P2—Pd2—Cl1—Pd1−112.65 (17)C1—P1—C31—C3268.7 (4)
Cl4—Pd2—Cl1—Pd1135.41 (5)Pd1—P1—C31—C32−67.8 (4)
C14—Pd3—Cl2—Pd439.11 (16)C21—P1—C31—C33−61.2 (4)
P3—Pd3—Cl2—Pd4111.3 (2)C1—P1—C31—C33−167.5 (4)
Cl3—Pd3—Cl2—Pd4−139.72 (5)Pd1—P1—C31—C3356.0 (4)
C14—Pd4—Cl2—Pd3−38.89 (15)C25—P3—C35—C37−65.2 (5)
P4—Pd4—Cl2—Pd3−113.6 (2)C61—P3—C35—C37−171.9 (4)
Cl4—Pd4—Cl2—Pd3137.01 (5)Pd3—P3—C35—C3751.7 (5)
C13—Pd1—Cl3—Pd333.1 (12)C25—P3—C35—C36171.1 (4)
P1—Pd1—Cl3—Pd3−151.36 (6)C61—P3—C35—C3664.4 (4)
Cl1—Pd1—Cl3—Pd338.70 (6)Pd3—P3—C35—C36−72.0 (4)
Pd2—Pd1—Cl3—Pd3−3.13 (7)C8—P2—C41—C4267.7 (4)
C14—Pd3—Cl3—Pd141.5 (10)C51—P2—C41—C42177.3 (4)
P3—Pd3—Cl3—Pd1−141.93 (6)Pd2—P2—C41—C42−67.2 (4)
Cl2—Pd3—Cl3—Pd148.98 (6)C8—P2—C41—C43−59.1 (5)
Pd4—Pd3—Cl3—Pd17.45 (7)C51—P2—C41—C4350.6 (5)
C13—Pd2—Cl4—Pd43.9 (12)Pd2—P2—C41—C43166.0 (4)
P2—Pd2—Cl4—Pd4158.94 (7)C68—P4—C45—C4668.6 (4)
Cl1—Pd2—Cl4—Pd4−36.21 (7)C55—P4—C45—C46178.4 (4)
Pd1—Pd2—Cl4—Pd48.95 (9)Pd4—P4—C45—C46−66.4 (4)
C14—Pd4—Cl4—Pd2−18.7 (11)C68—P4—C45—C47−57.7 (5)
P4—Pd4—Cl4—Pd2145.37 (7)C55—P4—C45—C4752.2 (5)
Cl2—Pd4—Cl4—Pd2−48.46 (7)Pd4—P4—C45—C47167.3 (4)
Pd3—Pd4—Cl4—Pd2−4.70 (9)C8—P2—C51—C53172.1 (4)
P1—Pd1—C13—Pd2143.68 (16)C41—P2—C51—C5366.1 (4)
Cl1—Pd1—C13—Pd2−46.40 (15)Pd2—P2—C51—C53−52.8 (4)
Cl3—Pd1—C13—Pd2−40.7 (13)C8—P2—C51—C52−65.1 (4)
P2—Pd2—C13—Pd1−149.43 (16)C41—P2—C51—C52−171.1 (4)
Cl1—Pd2—C13—Pd146.18 (15)Pd2—P2—C51—C5270.0 (4)
Cl4—Pd2—C13—Pd15.7 (13)C68—P4—C55—C56−67.6 (4)
P3—Pd3—C14—Pd4144.83 (15)C45—P4—C55—C56−174.2 (4)
Cl2—Pd3—C14—Pd4−46.11 (14)Pd4—P4—C55—C5667.2 (4)
Cl3—Pd3—C14—Pd4−38.6 (11)C68—P4—C55—C57168.6 (4)
P4—Pd4—C14—Pd3−148.28 (15)C45—P4—C55—C5762.1 (5)
Cl2—Pd4—C14—Pd345.84 (14)Pd4—P4—C55—C57−56.5 (4)
Cl4—Pd4—C14—Pd315.8 (12)C25—P3—C61—C62−73.1 (4)
C13—Pd1—P1—C21−158.8 (3)C35—P3—C61—C6236.1 (5)
Cl1—Pd1—P1—C21134.6 (3)Pd3—P3—C61—C62161.2 (3)
Cl3—Pd1—P1—C2121.9 (2)C25—P3—C61—C7796.6 (5)
Pd2—Pd1—P1—C21−126.45 (19)C35—P3—C61—C77−154.1 (4)
C13—Pd1—P1—C1−37.3 (3)Pd3—P3—C61—C77−29.0 (5)
Cl1—Pd1—P1—C1−103.9 (3)C77—C61—C62—C63−2.5 (8)
Cl3—Pd1—P1—C1143.3 (2)P3—C61—C62—C63168.2 (5)
Pd2—Pd1—P1—C1−5.0 (2)C61—C62—C63—C64−0.5 (9)
C13—Pd1—P1—C3187.2 (2)C62—C63—C64—C782.2 (8)
Cl1—Pd1—P1—C3120.6 (3)C80—C65—C66—C67−4.3 (9)
Cl3—Pd1—P1—C31−92.19 (19)C65—C66—C67—C682.3 (9)
Pd2—Pd1—P1—C31119.51 (19)C66—C67—C68—C793.4 (8)
C13—Pd2—P2—C837.3 (3)C66—C67—C68—P4−166.7 (5)
Cl1—Pd2—P2—C8109.4 (3)C45—P4—C68—C79−90.5 (5)
Cl4—Pd2—P2—C8−139.2 (2)C55—P4—C68—C79160.9 (4)
Pd1—Pd2—P2—C88.9 (2)Pd4—P4—C68—C7936.5 (5)
C13—Pd2—P2—C51−87.2 (2)C45—P4—C68—C6778.7 (4)
Cl1—Pd2—P2—C51−15.1 (3)C55—P4—C68—C67−29.8 (5)
Cl4—Pd2—P2—C5196.27 (18)Pd4—P4—C68—C67−154.2 (3)
Pd1—Pd2—P2—C51−115.58 (18)C80—C70—C71—C72−58.2 (6)
C13—Pd2—P2—C41159.7 (2)C78—C70—C71—C7255.6 (6)
Cl1—Pd2—P2—C41−128.2 (2)C70—C71—C72—C693.4 (6)
Cl4—Pd2—P2—C41−16.86 (19)C79—C69—C72—C7154.6 (6)
Pd1—Pd2—P2—C41131.30 (19)C77—C69—C72—C71−59.8 (5)
C14—Pd3—P3—C25−158.6 (2)C62—C61—C77—C783.6 (7)
Cl2—Pd3—P3—C25130.1 (3)P3—C61—C77—C78−165.9 (4)
Cl3—Pd3—P3—C2521.90 (18)C62—C61—C77—C69−176.4 (5)
Pd4—Pd3—P3—C25−126.81 (18)P3—C61—C77—C6914.1 (8)
C14—Pd3—P3—C61−36.4 (3)C79—C69—C77—C78−55.4 (5)
Cl2—Pd3—P3—C61−107.7 (3)C72—C69—C77—C7859.4 (5)
Cl3—Pd3—P3—C61144.1 (2)C79—C69—C77—C61124.6 (5)
Pd4—Pd3—P3—C61−4.6 (2)C72—C69—C77—C61−120.6 (5)
C14—Pd3—P3—C3587.5 (2)C63—C64—C78—C77−1.0 (8)
Cl2—Pd3—P3—C3516.2 (3)C63—C64—C78—C70177.0 (5)
Cl3—Pd3—P3—C35−91.94 (19)C61—C77—C78—C64−2.0 (8)
Pd4—Pd3—P3—C35119.34 (18)C69—C77—C78—C64178.0 (5)
C14—Pd4—P4—C6834.1 (3)C61—C77—C78—C70179.8 (4)
Cl2—Pd4—P4—C68107.5 (3)C69—C77—C78—C70−0.2 (6)
Cl4—Pd4—P4—C68−143.6 (2)C80—C70—C78—C64−122.2 (6)
Pd3—Pd4—P4—C684.8 (2)C71—C70—C78—C64122.2 (6)
C14—Pd4—P4—C45156.7 (3)C80—C70—C78—C7756.0 (6)
Cl2—Pd4—P4—C45−129.9 (3)C71—C70—C78—C77−59.6 (6)
Cl4—Pd4—P4—C45−21.0 (2)C67—C68—C79—C80−6.9 (7)
Pd3—Pd4—P4—C45127.4 (2)P4—C68—C79—C80162.2 (4)
C14—Pd4—P4—C55−89.8 (2)C67—C68—C79—C69172.2 (5)
Cl2—Pd4—P4—C55−16.4 (3)P4—C68—C79—C69−18.6 (8)
Cl4—Pd4—P4—C5592.41 (19)C77—C69—C79—C68−126.1 (6)
Pd3—Pd4—P4—C55−119.16 (19)C72—C69—C79—C68120.9 (6)
C21—P1—C1—C2−75.0 (4)C77—C69—C79—C8053.1 (5)
C31—P1—C1—C234.5 (5)C72—C69—C79—C80−59.9 (6)
Pd1—P1—C1—C2159.7 (3)C66—C65—C80—C790.5 (9)
C21—P1—C1—C1795.5 (5)C66—C65—C80—C70−177.1 (5)
C31—P1—C1—C17−155.0 (5)C68—C79—C80—C655.2 (8)
Pd1—P1—C1—C17−29.8 (5)C69—C79—C80—C65−174.2 (5)
C17—C1—C2—C3−4.0 (8)C68—C79—C80—C70−177.0 (5)
P1—C1—C2—C3167.4 (4)C69—C79—C80—C703.6 (7)
C1—C2—C3—C4−0.5 (9)C78—C70—C80—C65119.0 (6)
C2—C3—C4—C183.5 (8)C71—C70—C80—C65−125.5 (6)
C20—C5—C6—C7−5.1 (8)C78—C70—C80—C79−58.8 (6)
C5—C6—C7—C82.2 (9)C71—C70—C80—C7956.7 (6)
C6—C7—C8—C194.2 (8)C84—O80—C81—C825.0 (9)
C6—C7—C8—P2−164.8 (4)O80—C81—C82—C83−24.0 (9)
C51—P2—C8—C19160.6 (4)C81—C82—C83—C8432.6 (8)
C41—P2—C8—C19−91.7 (5)C81—O80—C84—C8316.9 (9)
Pd2—P2—C8—C1935.5 (5)C82—C83—C84—O80−31.4 (8)
C51—P2—C8—C7−31.3 (5)C89—O85—C86—C87−4.0 (12)
C41—P2—C8—C776.4 (4)O85—C86—C87—C88−19.3 (11)
Pd2—P2—C8—C7−156.4 (3)C86—C87—C88—C8933.6 (10)
C20—C10—C11—C12−58.4 (6)C86—O85—C89—C8826.2 (11)
C18—C10—C11—C1255.2 (6)C87—C88—C89—O85−37.3 (9)
C17—C9—C12—C11−58.4 (5)C94—O90—C91—C922.7 (16)
C19—C9—C12—C1154.8 (5)O90—C91—C92—C93−15.2 (15)
C10—C11—C12—C92.3 (6)C91—C92—C93—C9420.8 (12)
C2—C1—C17—C185.4 (7)C91—O90—C94—C9311.8 (14)
P1—C1—C17—C18−165.0 (4)C92—C93—C94—O90−21.1 (13)
C2—C1—C17—C9−174.2 (5)C99—O95—C96—C9722 (4)
P1—C1—C17—C915.4 (8)O95—C96—C97—C98−20 (4)
C12—C9—C17—C1−121.6 (6)C96—C97—C98—C9911 (4)
C19—C9—C17—C1123.6 (5)C96—O95—C99—C98−15 (3)
C12—C9—C17—C1858.7 (5)C97—C98—C99—O952(4)
C19—C9—C17—C18−56.0 (5)C99B—O95B—C96B—C97B−21 (3)
C3—C4—C18—C17−2.0 (8)O95B—C96B—C97B—C98B1(3)
C3—C4—C18—C10174.8 (5)C96B—C97B—C98B—C99B17 (3)
C1—C17—C18—C4−2.5 (8)C96B—O95B—C99B—C98B32 (2)
C9—C17—C18—C4177.2 (5)C97B—C98B—C99B—O95B−30 (3)
C1—C17—C18—C10−179.6 (4)C104—O100—C101—C102−7.5 (10)
C9—C17—C18—C100.1 (6)O100—C101—C102—C1031.9 (11)
C20—C10—C18—C4−120.0 (5)C101—C102—C103—C1044.1 (12)
C11—C10—C18—C4124.3 (5)C101—O100—C104—C10310.3 (11)
C20—C10—C18—C1757.1 (6)C102—C103—C104—O100−8.7 (12)
  3 in total

1.  A short history of SHELX.

Authors:  George M Sheldrick
Journal:  Acta Crystallogr A       Date:  2007-12-21       Impact factor: 2.290

2.  A unique Pd4 platform with CH3 and mu-CH2 groups and its C-C coupling reaction with simple olefins.

Authors:  Anna Sachse; Michael John; Franc Meyer
Journal:  Angew Chem Int Ed Engl       Date:  2010-03-08       Impact factor: 15.336

3.  Isolation and characterization of stable, distinctly bent, trans-chelated bisphosphine palladium(0) species.

Authors:  Thomas Schnetz; Marc Röder; Frank Rominger; Peter Hofmann
Journal:  Dalton Trans       Date:  2008-03-11       Impact factor: 4.390

  3 in total

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