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The title compound, [Pd(C19H17NO4)I(C18H15P)], crystallizes with four independent mol­ecules in the asymmetric unit. The main difference between the mol­ecules is the disposition of the PPh3 ligand, for which in each mol­ecule one ring is perpendicular to the ligand plane, but may be directed in either direction away from the plane; of the four mol­ecules, two represent each possible direction. The independent mol­ecules are arranged to form a chain parallel to [101] with an approximate translation of (a+c)/4 between successive mol­ecules, excluding the PPh3 rings. This leads to a systematic weakness of the reflections with h + l ≠ 4n.

Supporting information

cif

Crystallographic Information File (CIF) https://doi.org/10.1107/S0108270106051870/gd3068sup1.cif
Contains datablocks I, global

hkl

Structure factor file (CIF format) https://doi.org/10.1107/S0108270106051870/gd3068Isup2.hkl
Contains datablock I

CCDC reference: 634875

Comment top

The title compound, (I), was synthesized during a study of aryl palladium complexes bearing functionalized susbtituents on the ortho-position. In these investigations, oxidative addition of Pd0 precursors to aryl halides yields organometallic compounds that are models of intermediates in palladium-catalysed organic syntheses (Vicente et al., 2005) and may lead to new coordination modes for the ligands. There are a large number of known palladium–diimine complexes; a search of the Cambridge Structural Database (CSD, Version?; Allen, 2002) revealed 106 hits for α-diimine complexes of palladium, e.g. de Pater et al. (2005). However, the double bond in the imine group of (I) does not form part of the heterocycle.

Compound (I) crystallizes solvent-free with four independent molecules in the asymmetric unit. Molecules 1 and 3 are shown in Figs. 1 and 2, respectively; a similar numbering scheme was used for all the molecules, replacing the first digit `1' in molecule 1 with the appropriate molecule number 2, 3 or 4. In all four molecules, the Pd atom shows the expected planar four-coordination, albeit with slight but significant deviations from planarity (r.m.s. deviations of the five atoms Pd, I, P, N and C from their least-squares plane are 0.01, 0.04, 0.05 and 0.08 Å, respectively, for molecules 1–4). The bond lengths at Pd are consistent over all four molecules (see below for one possible exception). The bite of the C,N-ligand is constant at ca 82° (important molecular dimensions are given in Table 1). The chelate rings display a configuration whereby the atoms Pdn, Cn01, Cn02 and Cn12 are coplanar (r.m.s. deviations 0.02 Å for all four molecules), and the other two atoms Nn and Cn11 are displaced from this plane to the same side. The double-bond positions Cn01 Cn02 are unambiguously established by the bond lengths. The carboxylate groups are disposed such that the absolute torsion angles Cn02 Cn01—Cn03On01 lie in the range 9–17° and Cn01Cn02—Cn04On02 in the range 90–97°.

Despite the above-mentioned similarities, the molecules differ in one important respect, namely the disposition of the triphenylphosphine ligand. For each molecule, one phenyl ring of PPh3 is approximately perpendicular to the coordination plane (cf. torsion angles I—Pd—P—Cipso in Table 1; in each case, there is one ring with an absolute value ca 90°). However, in molecules 1 and 4, the ring at Cn31 points out of the coordination plane to the same side as ring Cn11, whereas in molecules 2 and 3 (Fig. 2), the ring at Cn51 points to the other side of the plane from Cn11, the same side as Cn21. The differing Pd—P bond lengths (slightly longer for molecules 2 and 3) and the markedly irregular Pd—P—C bond angles for molecules 1 and 4, with wide angles of ca 120° to Cn41 to avoid closer contact between the phenyl ring and the methoxycarbonyl group at Cn01, also reflect these differences. Even within this loose classification as two pairs of similar molecules, there are considerable differences in the I—Pd—P—C and Pd—P—C—C torsion angles for either given pair.

In the CSD (Version?), there are 25 examples of palladium complexes with a coordination sphere of C/N(chelating)/P/I. However, the bond lengths at Pd vary over a very wide range (e.g. Pd—N = 2.09–2.32 Å), making generalization difficult, and the iodo ligand may be trans to C or P. There are no examples with P trans to C for this ligand set; consistent with the great extent of P/C `transphobia' (Vicente et al., 1997, 2002, 2006), the P and C donors are mutually cis in (I) and in the other literature examples.

The molecular packing of (I) is noteworthy. The molecules are associated into chains parallel to [101] (Fig. 3), in which neighbouring molecules, except for the PPh3 phenyl groups as noted above, adopt positions related by the non-crystallographic translation of (a + c)/4. This pseudosymmetry is responsible for the fact that reflections with h + l ≠ 4n are systematically weak. However, the seven non-classical (`weak') hydrogen-bonding interactions (Desiraju & Steiner, 1999; Table 2), of which five involve para-H atoms of the PPh3 ligands, are not formed within the chains.

Experimental top

Under a dinitrogen atmosphere, dimethyl acetylenedicarboxylate (DMAD) (94 µl, 0.7 mmol) was added to a solution of trans-[(C6H4N CH2Ph-2)I(PPh3)2Pd] (Vicente et al., 1999) (125 mg, 0.13 mmol) in degassed CH2Cl2 (5 ml), and the reaction mixture was stirred overnight (16 h). The solvent was removed and the residue was treated with diethyl ether (5 ml). The solid was collected by filtration, washed with diethyl ether (3 × 3 ml) and dried in air to yield complex (I) as a yellow powder (yield 80 mg, 73%). Single crystals were obtained by slow diffusion of Et2O into a solution of complex (I) in CDCl3. Spectroscopic analysis: IR (Nujol, ν, cm−1): 1726(CO); 1H NMR (300 MHz, CDCl3, δ, p.p.m.): 8.70 (d, 3JH,H = 7 Hz, 2H), 8.40 (d, 1JH,H = 13.5 Hz, 1H), 7.68–7.33 (several m, 22H, 4Ph + 2Harom), 3.69 (s, 3H, OMe), 3.06 (s, 3H, OMe); 31P{1H} NMR (121 MHz, CDCl3, δ, p.p.m.): 31.44 (PPh3). Analysis, calculated for C37H31INO4PPd: C 54.33, H 3.82, N 1.71%; found: C 54.53, H 3.86, N 1.67%.

Refinement top

Because of the large number of parameters, full-matrix refinement was not possible and the refinement was therefore split into two blocks consisting of molecules 1 and 2, and molecules 3 and 4, respectively. Methyl H atoms were identified in difference syntheses, idealized and refined as rigid groups allowed to rotate but not tip. Other H atoms were included using a riding model. C—H bond lengths were fixed at 0.98 (methyl) or 0.95 Å (sp2-C), and methyl H—C—H angles were fixed at 109.5°. Uiso(H) values were fixed at 1.2 times Ueq of the parent atom. The maximum residual electron density of 1.3 e Å−3 is associated with the methoxy group at C401, and may indicate slight disorder of this group. The next five difference peaks (down to 0.8 e Å−3) all lie close to Pd or I atoms.

Computing details top

Data collection: SMART (Bruker, 1998); cell refinement: SAINT (Bruker, 1998); data reduction: SAINT; program(s) used to solve structure: SHELXS97 (Sheldrick, 1997); program(s) used to refine structure: SHELXL97 (Sheldrick, 1997); molecular graphics: XP (Siemens, 1994); software used to prepare material for publication: SHELXL97.

Figures top
[Figure 1] Fig. 1. The first independent molecule of compound (I), showing the atom-numbering scheme. Displacement ellipsoids are drawn at the 30% probability level and H atoms are shown as small spheres of arbitrary radii.
[Figure 2] Fig. 2. The third independent molecule of compound (I), showing the atom-numbering scheme. Displacement ellipsoids are drawn at the 30% probability level and H atoms are shown as small spheres of arbitrary radii.
[Figure 3] Fig. 3. The four independent molecules of (I) in the unit cell, running in order from molecule 1 (bottom right) to molecule 4 (top left). H atoms have been omitted.
{2-[2-(benzylideneamino)phenyl]-1,2-bis(methoxycarbonyl)ethenyl- κ2C1,N}iodo(triphenylphosphine-κP)palladium(II) top
Crystal data top
[Pd(C19H17NO4)I(C18H15P)]F(000) = 6496
Mr = 817.90Dx = 1.611 Mg m3
Monoclinic, P21/cMo Kα radiation, λ = 0.71073 Å
Hall symbol: -P 2ybcCell parameters from 7465 reflections
a = 16.6938 (11) Åθ = 2.2–30.4°
b = 22.1074 (15) ŵ = 1.55 mm1
c = 36.666 (3) ÅT = 133 K
β = 94.460 (4)°Prism, yellow
V = 13490.8 (17) Å30.38 × 0.22 × 0.20 mm
Z = 16
Data collection top
Bruker SMART 1000 CCD area-detector
diffractometer
39449 independent reflections
Radiation source: fine-focus sealed tube27970 reflections with I > 2σ(I)
Graphite monochromatorRint = 0.050
Detector resolution: 8.192 pixels mm-1θmax = 30.0°, θmin = 1.1°
ω and ϕ scansh = 2323
Absorption correction: multi-scan
(SADABS; Bruker, 1998)
k = 3131
Tmin = 0.653, Tmax = 0.733l = 5151
261441 measured reflections
Refinement top
Refinement on F2Primary atom site location: structure-invariant direct methods
Least-squares matrix: blockedSecondary atom site location: difference Fourier map
R[F2 > 2σ(F2)] = 0.030Hydrogen site location: inferred from neighbouring sites
wR(F2) = 0.070H-atom parameters constrained
S = 0.95 w = 1/[σ2(Fo2) + (0.033P)2]
where P = (Fo2 + 2Fc2)/3
39449 reflections(Δ/σ)max = 0.006
1629 parametersΔρmax = 1.26 e Å3
0 restraintsΔρmin = 0.90 e Å3
Crystal data top
[Pd(C19H17NO4)I(C18H15P)]V = 13490.8 (17) Å3
Mr = 817.90Z = 16
Monoclinic, P21/cMo Kα radiation
a = 16.6938 (11) ŵ = 1.55 mm1
b = 22.1074 (15) ÅT = 133 K
c = 36.666 (3) Å0.38 × 0.22 × 0.20 mm
β = 94.460 (4)°
Data collection top
Bruker SMART 1000 CCD area-detector
diffractometer
39449 independent reflections
Absorption correction: multi-scan
(SADABS; Bruker, 1998)
27970 reflections with I > 2σ(I)
Tmin = 0.653, Tmax = 0.733Rint = 0.050
261441 measured reflections
Refinement top
R[F2 > 2σ(F2)] = 0.0300 restraints
wR(F2) = 0.070H-atom parameters constrained
S = 0.95Δρmax = 1.26 e Å3
39449 reflectionsΔρmin = 0.90 e Å3
1629 parameters
Special details top

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.

Least-squares planes (x,y,z in crystal coordinates) and deviations from them (* indicates atom used to define plane)

14.7418 (0.0033) x − 5.0256 (0.0092) y + 12.4878 (0.0147) z = 21.5065 (0.0130)

* 0.1632 (0.0006) Pd1 * 0.0094 (0.0007) I1 * −0.0905 (0.0007) P1 * −0.1009 (0.0009) N1 * 0.0188 (0.0010) C101

Rms deviation of fitted atoms = 0.0954

15.0095 (0.0033) x − 1.7365 (0.0096) y + 13.1780 (0.0148) z = 16.5883 (0.0097)

Angle to previous plane (with approximate e.s.d.) = 8.66 (0.05)

* 0.0586 (0.0006) Pd2 * −0.0316 (0.0008) I2 * 0.0045 (0.0007) P2 * 0.0110 (0.0009) N2 * −0.0425 (0.0011) C201

Rms deviation of fitted atoms = 0.0357

14.7183 (0.0032) x − 3.9781 (0.0094) y + 13.4320 (0.0140) z = 8.6350 (0.0071)

Angle to previous plane (with approximate e.s.d.) = 5.91 (0.05)

* 0.0976 (0.0006) Pd3 * −0.0088 (0.0007) I3 * −0.0400 (0.0007) P3 * −0.0422 (0.0009) N3 * −0.0066 (0.0010) C301

Rms deviation of fitted atoms = 0.0510

14.9765 (0.0034) x − 3.9957 (0.0092) y + 12.1773 (0.0159) z = 1.8093 (0.0043)

Angle to previous plane (with approximate e.s.d.) = 2.09 (0.05)

* 0.1503 (0.0007) Pd4 * −0.0036 (0.0008) I4 * −0.0687 (0.0007) P4 * −0.0749 (0.0009) N4 * −0.0031 (0.0011) C401

Rms deviation of fitted atoms = 0.0812

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.

Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top
xyzUiso*/Ueq
Pd10.796745 (10)0.375719 (7)0.945921 (5)0.01348 (3)
I10.843117 (10)0.373141 (7)0.877823 (4)0.02187 (3)
P10.74891 (3)0.28041 (3)0.943714 (17)0.01581 (12)
N10.81094 (11)0.46893 (8)0.94552 (5)0.0162 (4)
O1010.75687 (10)0.37302 (8)1.05905 (5)0.0256 (4)
O1020.59533 (10)0.43949 (8)1.03806 (5)0.0293 (4)
O1030.85616 (9)0.33959 (7)1.02611 (4)0.0215 (4)
O1040.70211 (10)0.50135 (8)1.04600 (5)0.0261 (4)
C1010.75195 (13)0.39345 (10)0.99438 (6)0.0161 (4)
C1020.69726 (13)0.43760 (10)0.99500 (6)0.0165 (5)
C1030.78569 (14)0.36773 (10)1.02993 (7)0.0182 (5)
C1040.65883 (14)0.45703 (10)1.02895 (6)0.0191 (5)
C1050.89563 (15)0.31522 (12)1.05950 (7)0.0310 (6)
H10A0.90120.34711.07810.037*
H10B0.94900.30011.05460.037*
H10C0.86340.28201.06830.037*
C1060.67101 (18)0.52434 (14)1.07891 (8)0.0467 (8)
H10D0.61650.53991.07320.056*
H10E0.70570.55711.08890.056*
H10F0.66970.49171.09690.056*
C1110.73098 (13)0.49189 (9)0.93840 (6)0.0165 (5)
C1120.67252 (13)0.47421 (9)0.96204 (6)0.0162 (5)
C1130.59354 (13)0.49370 (10)0.95415 (7)0.0204 (5)
H1130.55370.48360.97030.024*
C1140.57254 (14)0.52776 (11)0.92295 (7)0.0247 (5)
H1140.51840.54020.91760.030*
C1150.63086 (15)0.54342 (11)0.89975 (7)0.0248 (5)
H1150.61610.56610.87830.030*
C1160.71021 (14)0.52656 (10)0.90740 (7)0.0218 (5)
H1160.75000.53850.89170.026*
C1200.87250 (13)0.50353 (10)0.94601 (6)0.0191 (5)
H1200.86380.54550.94190.023*
C1210.95556 (13)0.48246 (10)0.95249 (6)0.0187 (5)
C1220.97554 (14)0.42587 (10)0.96752 (7)0.0218 (5)
H1220.93450.39930.97430.026*
C1231.05532 (14)0.40861 (11)0.97247 (7)0.0266 (6)
H1231.06880.37010.98270.032*
C1241.11571 (14)0.44686 (12)0.96271 (7)0.0271 (6)
H1241.17020.43440.96600.033*
C1251.09680 (14)0.50327 (12)0.94813 (7)0.0268 (6)
H1251.13820.52970.94160.032*
C1261.01656 (14)0.52107 (10)0.94314 (7)0.0223 (5)
H1261.00340.55990.93330.027*
C1310.64508 (14)0.28215 (11)0.92515 (7)0.0233 (5)
C1320.59983 (16)0.22845 (14)0.92396 (8)0.0370 (7)
H1320.62300.19210.93370.044*
C1330.52255 (19)0.22875 (18)0.90875 (9)0.0545 (10)
H1330.49230.19230.90780.065*
C1340.48798 (17)0.28125 (19)0.89481 (9)0.0549 (10)
H1340.43450.28070.88390.066*
C1350.53073 (17)0.33442 (17)0.89663 (8)0.0459 (8)
H1350.50630.37070.88750.055*
C1360.61026 (15)0.33520 (13)0.91189 (7)0.0293 (6)
H1360.64000.37190.91310.035*
C1410.74156 (13)0.23749 (10)0.98569 (6)0.0174 (5)
C1420.78883 (15)0.18728 (10)0.99548 (7)0.0232 (5)
H1420.82750.17350.97970.028*
C1430.77989 (16)0.15708 (11)1.02820 (7)0.0274 (6)
H1430.81270.12311.03470.033*
C1440.72385 (15)0.17622 (11)1.05120 (7)0.0270 (6)
H1440.71810.15541.07350.032*
C1450.67580 (15)0.22559 (11)1.04203 (7)0.0247 (5)
H1450.63670.23851.05780.030*
C1460.68495 (14)0.25630 (10)1.00965 (7)0.0207 (5)
H1460.65240.29061.00360.025*
C1510.80130 (14)0.23159 (10)0.91323 (7)0.0201 (5)
C1520.76378 (16)0.21055 (10)0.88036 (7)0.0263 (6)
H1520.70790.21720.87490.032*
C1530.80808 (18)0.17976 (11)0.85552 (8)0.0341 (7)
H1530.78250.16590.83300.041*
C1540.88927 (18)0.16941 (11)0.86368 (8)0.0361 (7)
H1540.91940.14810.84690.043*
C1550.92629 (16)0.18996 (11)0.89607 (8)0.0313 (6)
H1550.98190.18230.90170.038*
C1560.88339 (15)0.22175 (10)0.92058 (7)0.0253 (6)
H1560.91000.23690.94250.030*
Pd20.538204 (10)0.380564 (8)0.700376 (5)0.01514 (3)
I20.589372 (9)0.368171 (7)0.633627 (4)0.02137 (3)
P20.51620 (4)0.27958 (3)0.708030 (17)0.01812 (12)
N20.54975 (11)0.47396 (8)0.69592 (5)0.0183 (4)
O2010.49096 (11)0.38376 (9)0.81226 (5)0.0338 (4)
O2020.33118 (11)0.44883 (9)0.78774 (5)0.0366 (5)
O2030.59251 (10)0.34861 (8)0.78148 (5)0.0246 (4)
O2040.43934 (10)0.50794 (8)0.80042 (5)0.0304 (4)
C2010.49247 (13)0.40369 (10)0.74784 (7)0.0198 (5)
C2020.43748 (14)0.44826 (11)0.74723 (7)0.0213 (5)
C2030.52263 (14)0.37823 (11)0.78393 (7)0.0231 (5)
C2040.39649 (15)0.46641 (12)0.78065 (7)0.0251 (5)
C2050.62881 (16)0.32296 (13)0.81525 (7)0.0339 (6)
H20A0.64270.35550.83270.041*
H20B0.67760.30080.81020.041*
H20C0.59070.29530.82560.041*
C2060.41044 (18)0.52275 (15)0.83537 (8)0.0428 (8)
H20D0.35560.53860.83170.051*
H20E0.44550.55340.84760.051*
H20F0.41060.48630.85060.051*
C2110.47125 (14)0.49976 (10)0.68966 (7)0.0206 (5)
C2120.41362 (14)0.48473 (10)0.71408 (7)0.0216 (5)
C2130.33618 (15)0.50865 (12)0.70729 (7)0.0285 (6)
H2130.29630.49960.72360.034*
C2140.31679 (16)0.54499 (12)0.67743 (8)0.0345 (7)
H2140.26360.56000.67300.041*
C2150.37468 (16)0.55979 (12)0.65375 (8)0.0340 (7)
H2150.36140.58550.63340.041*
C2160.45181 (15)0.53705 (11)0.65983 (7)0.0272 (6)
H2160.49150.54700.64360.033*
C2200.61233 (14)0.50798 (10)0.69645 (6)0.0207 (5)
H2200.60400.54970.69120.025*
C2210.69519 (13)0.48772 (10)0.70450 (7)0.0193 (5)
C2220.71439 (14)0.43646 (10)0.72559 (7)0.0218 (5)
H2220.67280.41300.73480.026*
C2230.79356 (14)0.41970 (11)0.73319 (7)0.0249 (5)
H2230.80620.38470.74750.030*
C2240.85488 (15)0.45385 (11)0.71992 (7)0.0260 (6)
H2240.90930.44210.72510.031*
C2250.83644 (15)0.50515 (11)0.69916 (7)0.0269 (6)
H2250.87830.52840.69000.032*
C2260.75698 (14)0.52270 (11)0.69174 (7)0.0250 (5)
H2260.74460.55840.67800.030*
C2310.45588 (14)0.26153 (11)0.74600 (7)0.0216 (5)
C2320.47919 (15)0.21951 (11)0.77306 (7)0.0254 (5)
H2320.52790.19760.77180.030*
C2330.43159 (16)0.20945 (12)0.80195 (7)0.0328 (6)
H2330.44800.18080.82030.039*
C2340.36065 (17)0.24087 (13)0.80406 (8)0.0379 (7)
H2340.32830.23380.82380.045*
C2350.33675 (16)0.28287 (13)0.77729 (8)0.0353 (7)
H2350.28780.30440.77860.042*
C2360.38406 (14)0.29341 (11)0.74863 (7)0.0267 (6)
H2360.36770.32260.73050.032*
C2410.46614 (14)0.24023 (10)0.66870 (7)0.0221 (5)
C2420.38290 (15)0.23293 (11)0.66502 (7)0.0274 (6)
H2420.35160.24530.68430.033*
C2430.34558 (17)0.20787 (12)0.63353 (8)0.0368 (7)
H2430.28880.20360.63110.044*
C2440.39024 (19)0.18913 (12)0.60582 (8)0.0395 (7)
H2440.36410.17250.58410.047*
C2450.47333 (19)0.19426 (12)0.60920 (8)0.0367 (7)
H2450.50430.18030.59020.044*
C2460.51082 (17)0.21998 (11)0.64070 (7)0.0305 (6)
H2460.56770.22370.64310.037*
C2510.60865 (14)0.23718 (10)0.71730 (7)0.0202 (5)
C2520.60983 (15)0.17382 (11)0.71719 (8)0.0293 (6)
H2520.56210.15200.71010.035*
C2530.67992 (17)0.14272 (12)0.72725 (8)0.0366 (7)
H2530.67990.09970.72730.044*
C2540.74994 (16)0.17391 (12)0.73724 (8)0.0342 (7)
H2540.79780.15250.74450.041*
C2550.75003 (15)0.23643 (12)0.73658 (8)0.0308 (6)
H2550.79830.25790.74310.037*
C2560.67966 (14)0.26805 (11)0.72644 (7)0.0227 (5)
H2560.68030.31100.72580.027*
Pd30.285302 (10)0.383534 (7)0.451097 (5)0.01380 (3)
I30.333230 (10)0.363351 (7)0.384679 (4)0.02327 (4)
P30.23960 (4)0.28945 (3)0.463069 (17)0.01722 (12)
N30.30802 (10)0.47445 (8)0.44273 (5)0.0144 (4)
O3010.24010 (11)0.40795 (8)0.56272 (5)0.0335 (4)
O3020.08907 (10)0.47496 (9)0.53539 (5)0.0368 (5)
O3030.33343 (10)0.35695 (8)0.53505 (5)0.0292 (4)
O3040.20057 (10)0.53170 (7)0.54413 (5)0.0249 (4)
C3010.24433 (13)0.41582 (10)0.49781 (6)0.0165 (5)
C3020.19418 (13)0.46345 (10)0.49479 (6)0.0171 (5)
C3030.27009 (14)0.39374 (10)0.53524 (7)0.0193 (5)
C3040.15482 (14)0.48875 (10)0.52710 (7)0.0217 (5)
C3050.36437 (19)0.33452 (14)0.57034 (8)0.0440 (8)
H30A0.38090.36870.58620.053*
H30B0.41080.30830.56730.053*
H30C0.32250.31130.58140.053*
C3060.17105 (18)0.55475 (13)0.57742 (8)0.0396 (7)
H30D0.11600.56960.57230.048*
H30E0.20550.58800.58690.048*
H30F0.17160.52230.59570.048*
C3110.23120 (13)0.50254 (9)0.43444 (6)0.0160 (5)
C3120.17253 (13)0.49447 (10)0.45951 (7)0.0176 (5)
C3130.09587 (14)0.51870 (10)0.45081 (7)0.0226 (5)
H3130.05560.51460.46760.027*
C3140.07828 (14)0.54859 (11)0.41785 (7)0.0265 (6)
H3140.02570.56390.41190.032*
C3150.13685 (15)0.55618 (11)0.39364 (7)0.0264 (6)
H3150.12460.57720.37130.032*
C3160.21394 (14)0.53318 (10)0.40182 (7)0.0206 (5)
H3160.25420.53850.38520.025*
C3200.37335 (13)0.50396 (10)0.44128 (6)0.0174 (5)
H3200.36990.54510.43390.021*
C3210.45362 (13)0.47823 (10)0.45035 (6)0.0175 (5)
C3220.46646 (14)0.42909 (10)0.47398 (7)0.0200 (5)
H3220.42230.41060.48450.024*
C3230.54326 (14)0.40732 (11)0.48210 (7)0.0249 (5)
H3230.55170.37380.49820.030*
C3240.60816 (14)0.43403 (11)0.46698 (7)0.0275 (6)
H3240.66080.41870.47260.033*
C3250.59619 (14)0.48303 (11)0.44373 (7)0.0255 (6)
H3250.64060.50130.43330.031*
C3260.51955 (14)0.50546 (11)0.43564 (7)0.0222 (5)
H3260.51160.53950.42000.027*
C3310.15587 (14)0.29443 (10)0.49180 (7)0.0199 (5)
C3320.15166 (15)0.26441 (11)0.52496 (7)0.0255 (6)
H3320.19380.23800.53370.031*
C3330.08532 (16)0.27316 (12)0.54545 (8)0.0323 (6)
H3330.08270.25270.56810.039*
C3340.02382 (16)0.31120 (12)0.53302 (8)0.0344 (7)
H3340.02120.31670.54700.041*
C3350.02753 (15)0.34141 (12)0.50014 (8)0.0300 (6)
H3350.01500.36760.49150.036*
C3360.09316 (14)0.33349 (11)0.47976 (7)0.0243 (5)
H3360.09570.35480.45740.029*
C3410.20054 (14)0.24257 (10)0.42460 (7)0.0208 (5)
C3420.11919 (15)0.22943 (11)0.41714 (7)0.0276 (6)
H3420.08090.24520.43250.033*
C3430.09359 (17)0.19327 (12)0.38732 (8)0.0354 (7)
H3430.03800.18490.38220.042*
C3440.14890 (18)0.16980 (11)0.36528 (8)0.0347 (7)
H3440.13130.14610.34460.042*
C3450.23001 (18)0.18060 (11)0.37308 (8)0.0346 (7)
H3450.26820.16320.35830.041*
C3460.25542 (16)0.21699 (11)0.40257 (7)0.0298 (6)
H3460.31120.22450.40780.036*
C3510.31475 (14)0.23824 (10)0.48401 (7)0.0210 (5)
C3520.29510 (16)0.17890 (11)0.49255 (7)0.0300 (6)
H3520.24050.16630.49000.036*
C3530.35409 (18)0.13821 (11)0.50466 (8)0.0351 (7)
H3530.34000.09810.51080.042*
C3540.43355 (18)0.15594 (12)0.50785 (8)0.0370 (7)
H3540.47420.12790.51600.044*
C3550.45400 (16)0.21421 (13)0.49919 (8)0.0351 (7)
H3550.50880.22620.50140.042*
C3560.39543 (15)0.25559 (11)0.48724 (7)0.0265 (6)
H3560.41010.29570.48120.032*
Pd40.066901 (10)0.356189 (7)0.195515 (5)0.01439 (3)
I40.110728 (9)0.349090 (7)0.126646 (4)0.02136 (3)
P40.02612 (3)0.25843 (2)0.195618 (16)0.01488 (12)
N40.07953 (11)0.44889 (8)0.19191 (5)0.0159 (4)
O4010.03121 (12)0.36790 (8)0.30896 (5)0.0359 (5)
O4020.13308 (11)0.42279 (9)0.28668 (5)0.0371 (5)
O4030.12015 (11)0.32003 (8)0.27687 (5)0.0294 (4)
O4040.03408 (10)0.49141 (7)0.29189 (5)0.0257 (4)
C4010.02333 (14)0.37831 (10)0.24377 (6)0.0198 (5)
C4020.03203 (14)0.42270 (10)0.24332 (7)0.0195 (5)
C4030.05632 (17)0.35546 (11)0.27972 (7)0.0285 (6)
C4040.07186 (15)0.44352 (11)0.27693 (7)0.0228 (5)
C4050.14865 (19)0.29337 (16)0.31145 (9)0.0531 (9)
H40A0.17190.32490.32780.064*
H40B0.18970.26290.30740.064*
H40C0.10370.27420.32260.064*
C4060.06815 (17)0.51513 (13)0.32414 (8)0.0405 (8)
H40D0.12440.52640.31800.049*
H40E0.03780.55090.33290.049*
H40F0.06530.48420.34330.049*
C4110.00079 (13)0.47172 (9)0.18471 (6)0.0164 (5)
C4120.05776 (13)0.45695 (10)0.20975 (7)0.0182 (5)
C4130.13658 (14)0.47832 (10)0.20239 (7)0.0236 (5)
H4130.17550.47080.21940.028*
C4140.15815 (15)0.51007 (11)0.17087 (8)0.0285 (6)
H4140.21210.52330.16600.034*
C4150.10157 (15)0.52281 (11)0.14611 (7)0.0256 (6)
H4150.11700.54440.12430.031*
C4160.02255 (14)0.50406 (10)0.15323 (7)0.0198 (5)
H4160.01640.51340.13650.024*
C4200.14023 (13)0.48357 (10)0.19184 (6)0.0183 (5)
H4200.13080.52510.18640.022*
C4210.22355 (14)0.46401 (10)0.19955 (7)0.0195 (5)
C4220.24407 (14)0.41019 (10)0.21787 (7)0.0236 (5)
H4220.20310.38430.22540.028*
C4230.32432 (16)0.39456 (12)0.22505 (8)0.0309 (6)
H4230.33820.35790.23750.037*
C4240.38426 (15)0.43228 (12)0.21405 (8)0.0309 (6)
H4240.43910.42140.21890.037*
C4250.36441 (15)0.48588 (12)0.19592 (7)0.0285 (6)
H4250.40560.51160.18840.034*
C4260.28440 (14)0.50194 (11)0.18885 (7)0.0236 (5)
H4260.27090.53890.17670.028*
C4310.07410 (13)0.25386 (10)0.17227 (6)0.0176 (5)
C4320.11664 (14)0.19931 (10)0.17137 (7)0.0222 (5)
H4320.09210.16380.18170.027*
C4330.19451 (14)0.19710 (11)0.15540 (7)0.0268 (6)
H4330.22300.15990.15440.032*
C4340.23098 (15)0.24881 (12)0.14096 (7)0.0279 (6)
H4340.28450.24710.13010.033*
C4350.19001 (15)0.30285 (12)0.14220 (7)0.0277 (6)
H4350.21540.33840.13240.033*
C4360.11164 (14)0.30567 (11)0.15779 (7)0.0222 (5)
H4360.08360.34310.15860.027*
C4410.01077 (13)0.21703 (9)0.23762 (6)0.0156 (4)
C4420.04409 (14)0.15998 (10)0.24537 (6)0.0200 (5)
H4420.07930.14250.22920.024*
C4430.02615 (14)0.12862 (10)0.27662 (7)0.0231 (5)
H4430.04930.09000.28160.028*
C4440.02470 (14)0.15323 (10)0.30019 (7)0.0220 (5)
H4440.03660.13160.32150.026*
C4450.05884 (14)0.20957 (10)0.29312 (7)0.0215 (5)
H4450.09430.22650.30940.026*
C4460.04091 (13)0.24119 (10)0.26206 (6)0.0192 (5)
H4460.06420.27990.25730.023*
C4510.09132 (13)0.20774 (10)0.17218 (6)0.0173 (5)
C4520.06777 (14)0.17750 (10)0.13994 (6)0.0191 (5)
H4520.01470.18280.12900.023*
C4530.12053 (14)0.13967 (10)0.12343 (7)0.0226 (5)
H4530.10420.12010.10100.027*
C4540.19715 (15)0.13054 (11)0.13978 (7)0.0236 (5)
H4540.23300.10380.12890.028*
C4550.22136 (14)0.16037 (11)0.17193 (7)0.0262 (6)
H4550.27380.15380.18330.031*
C4560.16943 (14)0.19991 (11)0.18773 (7)0.0242 (5)
H4560.18720.22170.20920.029*
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
Pd10.01342 (8)0.01423 (8)0.01315 (9)0.00032 (6)0.00329 (6)0.00024 (6)
I10.02859 (8)0.02103 (8)0.01725 (8)0.00036 (6)0.00976 (6)0.00114 (6)
P10.0165 (3)0.0168 (3)0.0144 (3)0.0025 (2)0.0026 (2)0.0008 (2)
N10.0165 (9)0.0159 (9)0.0164 (10)0.0017 (7)0.0032 (8)0.0004 (7)
O1010.0292 (10)0.0338 (10)0.0145 (9)0.0060 (8)0.0056 (7)0.0033 (7)
O1020.0205 (9)0.0401 (11)0.0287 (11)0.0059 (8)0.0107 (8)0.0077 (8)
O1030.0200 (8)0.0261 (9)0.0182 (9)0.0040 (7)0.0001 (7)0.0021 (7)
O1040.0263 (9)0.0303 (9)0.0225 (10)0.0047 (7)0.0082 (8)0.0113 (8)
C1010.0154 (11)0.0174 (11)0.0159 (12)0.0035 (8)0.0044 (9)0.0001 (8)
C1020.0130 (11)0.0201 (11)0.0166 (12)0.0028 (8)0.0026 (9)0.0029 (9)
C1030.0196 (12)0.0166 (11)0.0185 (13)0.0035 (9)0.0015 (9)0.0006 (9)
C1040.0221 (12)0.0210 (12)0.0142 (12)0.0023 (9)0.0014 (10)0.0020 (9)
C1050.0293 (14)0.0388 (15)0.0242 (15)0.0092 (12)0.0030 (12)0.0045 (12)
C1060.0480 (19)0.061 (2)0.0334 (18)0.0110 (16)0.0198 (15)0.0290 (15)
C1110.0166 (11)0.0144 (10)0.0188 (12)0.0014 (8)0.0025 (9)0.0031 (9)
C1120.0167 (11)0.0149 (10)0.0171 (12)0.0006 (8)0.0023 (9)0.0026 (8)
C1130.0166 (11)0.0240 (12)0.0207 (13)0.0015 (9)0.0030 (10)0.0047 (10)
C1140.0195 (12)0.0291 (13)0.0250 (14)0.0073 (10)0.0008 (10)0.0037 (10)
C1150.0293 (14)0.0232 (12)0.0216 (14)0.0081 (10)0.0000 (11)0.0017 (10)
C1160.0254 (13)0.0195 (12)0.0209 (13)0.0001 (10)0.0053 (10)0.0005 (9)
C1200.0228 (12)0.0174 (11)0.0175 (13)0.0028 (9)0.0045 (10)0.0002 (9)
C1210.0158 (11)0.0232 (12)0.0172 (12)0.0037 (9)0.0017 (9)0.0041 (9)
C1220.0189 (12)0.0241 (12)0.0223 (14)0.0035 (9)0.0013 (10)0.0003 (10)
C1230.0229 (13)0.0277 (13)0.0288 (15)0.0003 (10)0.0004 (11)0.0002 (11)
C1240.0170 (12)0.0364 (15)0.0278 (15)0.0002 (10)0.0014 (11)0.0063 (11)
C1250.0203 (13)0.0351 (14)0.0258 (15)0.0083 (11)0.0062 (11)0.0069 (11)
C1260.0231 (13)0.0209 (12)0.0231 (14)0.0054 (10)0.0031 (10)0.0036 (10)
C1310.0186 (12)0.0365 (14)0.0152 (13)0.0057 (10)0.0042 (10)0.0030 (10)
C1320.0326 (16)0.0514 (18)0.0272 (16)0.0212 (13)0.0026 (12)0.0037 (13)
C1330.0378 (18)0.092 (3)0.0338 (19)0.0348 (19)0.0024 (15)0.0031 (18)
C1340.0181 (15)0.121 (3)0.0255 (18)0.0130 (18)0.0003 (13)0.0054 (19)
C1350.0278 (16)0.089 (3)0.0209 (16)0.0152 (16)0.0009 (12)0.0044 (16)
C1360.0213 (13)0.0501 (17)0.0164 (13)0.0028 (12)0.0005 (10)0.0007 (11)
C1410.0206 (12)0.0161 (11)0.0159 (12)0.0044 (9)0.0040 (9)0.0002 (9)
C1420.0278 (13)0.0207 (12)0.0217 (14)0.0010 (10)0.0067 (11)0.0012 (10)
C1430.0365 (15)0.0194 (12)0.0262 (15)0.0026 (11)0.0023 (12)0.0047 (10)
C1440.0371 (15)0.0243 (13)0.0200 (14)0.0055 (11)0.0050 (11)0.0045 (10)
C1450.0269 (13)0.0300 (13)0.0180 (13)0.0045 (10)0.0064 (10)0.0005 (10)
C1460.0209 (12)0.0209 (12)0.0207 (13)0.0012 (9)0.0031 (10)0.0016 (9)
C1510.0278 (13)0.0134 (11)0.0202 (13)0.0049 (9)0.0090 (10)0.0003 (9)
C1520.0385 (15)0.0191 (12)0.0221 (14)0.0065 (11)0.0071 (11)0.0009 (10)
C1530.060 (2)0.0215 (13)0.0223 (15)0.0063 (13)0.0138 (14)0.0043 (11)
C1540.056 (2)0.0199 (13)0.0363 (18)0.0034 (12)0.0303 (15)0.0013 (11)
C1550.0324 (15)0.0228 (13)0.0414 (18)0.0010 (11)0.0208 (13)0.0018 (12)
C1560.0269 (13)0.0197 (12)0.0305 (15)0.0036 (10)0.0094 (11)0.0001 (10)
Pd20.01432 (8)0.01828 (8)0.01301 (9)0.00177 (6)0.00220 (6)0.00209 (6)
I20.02390 (8)0.02360 (8)0.01737 (8)0.00297 (6)0.00649 (6)0.00256 (6)
P20.0166 (3)0.0205 (3)0.0173 (3)0.0008 (2)0.0016 (2)0.0036 (2)
N20.0205 (10)0.0201 (10)0.0144 (10)0.0039 (8)0.0024 (8)0.0008 (8)
O2010.0373 (11)0.0499 (12)0.0150 (10)0.0094 (9)0.0079 (8)0.0052 (8)
O2020.0241 (10)0.0558 (13)0.0312 (12)0.0022 (9)0.0114 (9)0.0054 (10)
O2030.0212 (9)0.0352 (10)0.0172 (9)0.0039 (7)0.0002 (7)0.0055 (7)
O2040.0272 (10)0.0419 (11)0.0228 (10)0.0018 (8)0.0076 (8)0.0062 (8)
C2010.0184 (12)0.0237 (12)0.0177 (13)0.0002 (9)0.0046 (9)0.0011 (9)
C2020.0173 (12)0.0300 (13)0.0170 (13)0.0000 (10)0.0035 (10)0.0007 (10)
C2030.0232 (13)0.0265 (13)0.0200 (13)0.0023 (10)0.0037 (10)0.0009 (10)
C2040.0222 (13)0.0356 (14)0.0179 (13)0.0077 (11)0.0040 (10)0.0028 (11)
C2050.0307 (15)0.0520 (18)0.0183 (14)0.0087 (13)0.0011 (11)0.0096 (12)
C2060.0417 (17)0.065 (2)0.0229 (16)0.0044 (15)0.0115 (13)0.0119 (14)
C2110.0197 (12)0.0224 (12)0.0197 (13)0.0070 (9)0.0012 (10)0.0005 (9)
C2120.0214 (12)0.0252 (12)0.0180 (13)0.0040 (10)0.0009 (10)0.0010 (10)
C2130.0217 (13)0.0362 (15)0.0278 (15)0.0085 (11)0.0031 (11)0.0026 (11)
C2140.0250 (14)0.0415 (16)0.0367 (18)0.0173 (12)0.0004 (12)0.0041 (13)
C2150.0376 (16)0.0376 (16)0.0268 (16)0.0156 (12)0.0034 (13)0.0089 (12)
C2160.0295 (14)0.0277 (13)0.0245 (15)0.0062 (11)0.0034 (11)0.0036 (11)
C2200.0263 (13)0.0188 (11)0.0169 (13)0.0027 (9)0.0012 (10)0.0005 (9)
C2210.0191 (12)0.0202 (11)0.0188 (13)0.0012 (9)0.0019 (10)0.0027 (9)
C2220.0215 (12)0.0214 (12)0.0221 (13)0.0022 (9)0.0003 (10)0.0014 (10)
C2230.0261 (13)0.0211 (12)0.0265 (14)0.0018 (10)0.0038 (11)0.0005 (10)
C2240.0210 (13)0.0269 (13)0.0295 (15)0.0018 (10)0.0015 (11)0.0055 (11)
C2250.0222 (13)0.0305 (14)0.0285 (15)0.0062 (10)0.0046 (11)0.0009 (11)
C2260.0265 (13)0.0215 (12)0.0270 (15)0.0030 (10)0.0016 (11)0.0029 (10)
C2310.0178 (12)0.0269 (13)0.0201 (13)0.0052 (10)0.0022 (10)0.0034 (10)
C2320.0241 (13)0.0277 (13)0.0240 (14)0.0005 (10)0.0001 (11)0.0061 (10)
C2330.0391 (16)0.0363 (15)0.0234 (15)0.0041 (12)0.0041 (12)0.0130 (12)
C2340.0361 (16)0.0536 (19)0.0257 (16)0.0033 (14)0.0136 (13)0.0108 (13)
C2350.0237 (14)0.0499 (18)0.0332 (17)0.0027 (12)0.0089 (12)0.0073 (13)
C2360.0223 (13)0.0348 (14)0.0230 (14)0.0010 (11)0.0026 (11)0.0073 (11)
C2410.0260 (13)0.0191 (12)0.0206 (13)0.0020 (10)0.0010 (10)0.0040 (9)
C2420.0260 (13)0.0253 (13)0.0302 (15)0.0027 (10)0.0019 (11)0.0010 (11)
C2430.0328 (16)0.0331 (15)0.0420 (19)0.0079 (12)0.0128 (14)0.0004 (13)
C2440.058 (2)0.0251 (14)0.0327 (17)0.0092 (13)0.0139 (15)0.0007 (12)
C2450.057 (2)0.0283 (14)0.0252 (16)0.0070 (13)0.0034 (14)0.0048 (11)
C2460.0362 (15)0.0286 (14)0.0269 (15)0.0033 (11)0.0031 (12)0.0014 (11)
C2510.0186 (12)0.0230 (12)0.0191 (13)0.0018 (9)0.0017 (10)0.0042 (9)
C2520.0277 (14)0.0226 (13)0.0377 (17)0.0020 (10)0.0037 (12)0.0032 (11)
C2530.0417 (17)0.0224 (13)0.0461 (19)0.0075 (12)0.0055 (14)0.0088 (12)
C2540.0293 (15)0.0363 (15)0.0366 (17)0.0133 (12)0.0001 (13)0.0091 (13)
C2550.0190 (13)0.0355 (15)0.0373 (17)0.0034 (11)0.0023 (12)0.0017 (12)
C2560.0196 (12)0.0231 (12)0.0253 (14)0.0010 (9)0.0012 (10)0.0044 (10)
Pd30.01376 (8)0.01384 (8)0.01392 (9)0.00039 (6)0.00187 (6)0.00049 (6)
I30.02867 (9)0.02536 (8)0.01612 (8)0.00733 (6)0.00394 (6)0.00150 (6)
P30.0178 (3)0.0152 (3)0.0183 (3)0.0015 (2)0.0009 (2)0.0005 (2)
N30.0153 (9)0.0156 (9)0.0126 (10)0.0015 (7)0.0035 (7)0.0003 (7)
O3010.0449 (12)0.0350 (11)0.0223 (11)0.0115 (9)0.0124 (9)0.0052 (8)
O3020.0198 (9)0.0544 (13)0.0379 (13)0.0059 (9)0.0133 (9)0.0145 (10)
O3030.0314 (10)0.0385 (10)0.0177 (10)0.0126 (8)0.0016 (8)0.0048 (8)
O3040.0290 (10)0.0247 (9)0.0223 (10)0.0036 (7)0.0098 (8)0.0079 (7)
C3010.0158 (11)0.0178 (11)0.0163 (12)0.0039 (8)0.0047 (9)0.0026 (9)
C3020.0130 (11)0.0179 (11)0.0209 (13)0.0044 (8)0.0041 (9)0.0039 (9)
C3030.0233 (12)0.0175 (11)0.0170 (12)0.0040 (9)0.0018 (10)0.0010 (9)
C3040.0198 (12)0.0231 (12)0.0225 (14)0.0027 (9)0.0045 (10)0.0020 (10)
C3050.054 (2)0.0523 (19)0.0252 (16)0.0210 (15)0.0016 (14)0.0118 (14)
C3060.0526 (19)0.0374 (16)0.0309 (17)0.0028 (14)0.0160 (14)0.0156 (13)
C3110.0147 (11)0.0130 (10)0.0201 (13)0.0005 (8)0.0003 (9)0.0030 (9)
C3120.0146 (11)0.0154 (11)0.0228 (13)0.0001 (8)0.0015 (9)0.0034 (9)
C3130.0149 (11)0.0250 (13)0.0281 (15)0.0007 (9)0.0025 (10)0.0019 (10)
C3140.0181 (12)0.0285 (13)0.0323 (16)0.0057 (10)0.0027 (11)0.0017 (11)
C3150.0291 (14)0.0235 (13)0.0254 (14)0.0034 (10)0.0056 (11)0.0034 (10)
C3160.0202 (12)0.0187 (11)0.0228 (13)0.0000 (9)0.0014 (10)0.0004 (9)
C3200.0197 (12)0.0160 (11)0.0170 (12)0.0007 (9)0.0045 (9)0.0006 (9)
C3210.0150 (11)0.0185 (11)0.0190 (13)0.0007 (9)0.0013 (9)0.0035 (9)
C3220.0173 (11)0.0211 (12)0.0214 (13)0.0022 (9)0.0001 (10)0.0006 (9)
C3230.0236 (13)0.0232 (12)0.0271 (15)0.0018 (10)0.0031 (11)0.0002 (10)
C3240.0168 (12)0.0304 (14)0.0349 (16)0.0028 (10)0.0004 (11)0.0084 (11)
C3250.0167 (12)0.0317 (14)0.0290 (15)0.0046 (10)0.0069 (10)0.0058 (11)
C3260.0203 (12)0.0238 (12)0.0229 (14)0.0022 (10)0.0044 (10)0.0012 (10)
C3310.0212 (12)0.0176 (11)0.0211 (13)0.0056 (9)0.0027 (10)0.0016 (9)
C3320.0301 (14)0.0214 (12)0.0250 (14)0.0045 (10)0.0016 (11)0.0005 (10)
C3330.0403 (16)0.0342 (15)0.0237 (15)0.0120 (12)0.0100 (12)0.0017 (11)
C3340.0312 (15)0.0346 (15)0.0389 (18)0.0099 (12)0.0136 (13)0.0055 (13)
C3350.0220 (13)0.0295 (14)0.0390 (17)0.0028 (11)0.0051 (12)0.0034 (12)
C3360.0226 (13)0.0240 (12)0.0261 (14)0.0035 (10)0.0011 (11)0.0017 (10)
C3410.0257 (13)0.0160 (11)0.0202 (13)0.0021 (9)0.0023 (10)0.0001 (9)
C3420.0261 (13)0.0261 (13)0.0297 (15)0.0034 (10)0.0028 (11)0.0009 (11)
C3430.0359 (16)0.0305 (15)0.0372 (18)0.0097 (12)0.0129 (13)0.0014 (12)
C3440.0544 (19)0.0218 (13)0.0256 (15)0.0063 (12)0.0111 (14)0.0021 (11)
C3450.0490 (18)0.0240 (14)0.0307 (16)0.0005 (12)0.0026 (14)0.0073 (11)
C3460.0307 (14)0.0281 (14)0.0303 (16)0.0025 (11)0.0011 (12)0.0066 (11)
C3510.0255 (13)0.0200 (12)0.0170 (13)0.0036 (10)0.0024 (10)0.0000 (9)
C3520.0347 (15)0.0200 (12)0.0336 (16)0.0008 (11)0.0071 (12)0.0012 (11)
C3530.0488 (18)0.0195 (13)0.0357 (17)0.0069 (12)0.0053 (14)0.0026 (11)
C3540.0452 (17)0.0344 (16)0.0305 (16)0.0214 (13)0.0034 (13)0.0019 (12)
C3550.0245 (14)0.0417 (17)0.0387 (18)0.0108 (12)0.0004 (12)0.0033 (13)
C3560.0263 (13)0.0259 (13)0.0271 (15)0.0039 (10)0.0006 (11)0.0025 (11)
Pd40.01743 (8)0.01292 (8)0.01295 (9)0.00208 (6)0.00197 (7)0.00009 (6)
I40.02720 (8)0.02062 (7)0.01697 (8)0.00082 (6)0.00621 (6)0.00045 (6)
P40.0174 (3)0.0140 (3)0.0132 (3)0.0012 (2)0.0013 (2)0.0000 (2)
N40.0183 (10)0.0165 (9)0.0131 (10)0.0010 (7)0.0029 (8)0.0000 (7)
O4010.0604 (14)0.0302 (10)0.0177 (10)0.0008 (9)0.0074 (9)0.0003 (8)
O4020.0373 (11)0.0461 (12)0.0305 (12)0.0206 (9)0.0183 (9)0.0137 (9)
O4030.0361 (11)0.0349 (10)0.0163 (10)0.0027 (8)0.0032 (8)0.0052 (8)
O4040.0266 (9)0.0238 (9)0.0279 (11)0.0077 (7)0.0095 (8)0.0103 (7)
C4010.0256 (12)0.0188 (11)0.0153 (12)0.0090 (9)0.0043 (10)0.0002 (9)
C4020.0229 (12)0.0166 (11)0.0200 (13)0.0091 (9)0.0069 (10)0.0052 (9)
C4030.0435 (16)0.0174 (12)0.0243 (15)0.0108 (11)0.0006 (12)0.0012 (10)
C4040.0265 (13)0.0230 (12)0.0198 (13)0.0047 (10)0.0067 (10)0.0035 (10)
C4050.045 (2)0.076 (2)0.037 (2)0.0180 (17)0.0022 (16)0.0144 (17)
C4060.0455 (18)0.0442 (18)0.0339 (18)0.0045 (14)0.0163 (14)0.0232 (14)
C4110.0176 (11)0.0132 (10)0.0186 (12)0.0018 (8)0.0028 (9)0.0046 (8)
C4120.0206 (12)0.0140 (11)0.0205 (13)0.0047 (9)0.0053 (10)0.0047 (9)
C4130.0215 (12)0.0224 (12)0.0281 (15)0.0036 (10)0.0085 (11)0.0050 (10)
C4140.0211 (13)0.0285 (14)0.0353 (17)0.0028 (10)0.0005 (11)0.0057 (11)
C4150.0283 (14)0.0230 (13)0.0249 (14)0.0046 (10)0.0025 (11)0.0020 (10)
C4160.0233 (12)0.0172 (11)0.0191 (13)0.0014 (9)0.0031 (10)0.0017 (9)
C4200.0225 (12)0.0163 (11)0.0162 (12)0.0012 (9)0.0027 (9)0.0005 (9)
C4210.0210 (12)0.0192 (11)0.0185 (13)0.0012 (9)0.0019 (10)0.0030 (9)
C4220.0225 (13)0.0215 (12)0.0262 (14)0.0023 (10)0.0027 (10)0.0000 (10)
C4230.0320 (15)0.0283 (14)0.0313 (16)0.0049 (11)0.0047 (12)0.0007 (11)
C4240.0201 (13)0.0392 (16)0.0327 (16)0.0053 (11)0.0020 (11)0.0096 (12)
C4250.0220 (13)0.0347 (15)0.0295 (16)0.0067 (11)0.0062 (11)0.0066 (11)
C4260.0221 (13)0.0240 (12)0.0249 (14)0.0034 (10)0.0036 (10)0.0022 (10)
C4310.0164 (11)0.0226 (12)0.0137 (12)0.0023 (9)0.0012 (9)0.0030 (9)
C4320.0214 (12)0.0211 (12)0.0240 (14)0.0034 (9)0.0003 (10)0.0019 (10)
C4330.0230 (13)0.0294 (14)0.0281 (15)0.0076 (10)0.0028 (11)0.0061 (11)
C4340.0192 (12)0.0452 (16)0.0191 (14)0.0029 (11)0.0002 (10)0.0033 (11)
C4350.0262 (14)0.0335 (14)0.0229 (14)0.0037 (11)0.0018 (11)0.0049 (11)
C4360.0225 (12)0.0240 (12)0.0199 (13)0.0024 (10)0.0005 (10)0.0046 (10)
C4410.0168 (11)0.0161 (10)0.0137 (12)0.0039 (8)0.0006 (9)0.0006 (8)
C4420.0252 (13)0.0183 (11)0.0169 (12)0.0010 (9)0.0041 (10)0.0003 (9)
C4430.0257 (13)0.0191 (12)0.0247 (14)0.0003 (10)0.0033 (10)0.0024 (10)
C4440.0272 (13)0.0225 (12)0.0164 (12)0.0057 (10)0.0033 (10)0.0033 (9)
C4450.0201 (12)0.0259 (13)0.0192 (13)0.0044 (10)0.0055 (10)0.0027 (10)
C4460.0206 (12)0.0179 (11)0.0192 (13)0.0004 (9)0.0015 (10)0.0002 (9)
C4510.0203 (11)0.0155 (11)0.0167 (12)0.0037 (9)0.0050 (9)0.0005 (9)
C4520.0217 (12)0.0215 (12)0.0141 (12)0.0007 (9)0.0015 (9)0.0005 (9)
C4530.0266 (13)0.0226 (12)0.0190 (13)0.0048 (10)0.0047 (10)0.0036 (9)
C4540.0258 (13)0.0240 (12)0.0225 (14)0.0009 (10)0.0110 (11)0.0033 (10)
C4550.0185 (12)0.0321 (14)0.0281 (15)0.0006 (10)0.0028 (11)0.0028 (11)
C4560.0238 (13)0.0271 (13)0.0216 (14)0.0029 (10)0.0017 (10)0.0063 (10)
Geometric parameters (Å, º) top
Pd1—C1012.019 (2)O403—C4031.333 (3)
Pd1—N12.0744 (18)O403—C4051.445 (3)
Pd1—P12.2524 (6)O404—C4041.329 (3)
Pd1—I12.6716 (3)O404—C4061.450 (3)
C101—C1021.338 (3)C401—C4031.478 (3)
Pd2—C2012.020 (2)C402—C4121.480 (3)
Pd2—N22.0813 (19)C402—C4041.517 (3)
Pd2—P22.2833 (6)C411—C4161.382 (3)
Pd2—I22.6683 (3)C411—C4121.411 (3)
C201—C2021.346 (3)C412—C4131.404 (3)
Pd3—C3012.023 (2)C413—C4141.376 (4)
Pd3—N32.0727 (17)C414—C4151.389 (4)
Pd3—P32.2700 (6)C415—C4161.388 (3)
Pd3—I32.6595 (3)C420—C4211.463 (3)
C301—C3021.344 (3)C421—C4221.396 (3)
Pd4—C4012.024 (2)C421—C4261.397 (3)
Pd4—N42.0654 (18)C422—C4231.389 (3)
Pd4—P42.2660 (6)C423—C4241.386 (4)
Pd4—I42.6877 (3)C424—C4251.386 (4)
C401—C4021.347 (3)C425—C4261.387 (3)
P1—C1311.813 (2)C431—C4361.391 (3)
P1—C1411.820 (2)C431—C4321.399 (3)
P1—C1511.825 (2)C432—C4331.384 (3)
N1—C1201.280 (3)C433—C4341.381 (3)
N1—C1111.433 (3)C434—C4351.376 (3)
O101—C1031.211 (3)C435—C4361.388 (3)
O102—C1041.200 (3)C441—C4461.397 (3)
O103—C1031.348 (3)C441—C4421.399 (3)
O103—C1051.448 (3)C442—C4431.392 (3)
O104—C1041.343 (3)C443—C4441.370 (3)
O104—C1061.443 (3)C444—C4451.386 (3)
C101—C1031.492 (3)C445—C4461.389 (3)
C102—C1121.486 (3)C451—C4521.388 (3)
C102—C1041.506 (3)C451—C4561.393 (3)
C111—C1161.392 (3)C452—C4531.387 (3)
C111—C1121.410 (3)C453—C4541.384 (3)
C112—C1131.396 (3)C454—C4551.384 (3)
C113—C1141.392 (3)C455—C4561.389 (3)
C114—C1151.386 (3)C105—H10A0.9800
C115—C1161.384 (3)C105—H10B0.9800
C120—C1211.464 (3)C105—H10C0.9800
C121—C1261.392 (3)C106—H10D0.9800
C121—C1221.397 (3)C106—H10E0.9800
C122—C1231.384 (3)C106—H10F0.9800
C123—C1241.384 (3)C113—H1130.9500
C124—C1251.384 (4)C114—H1140.9500
C125—C1261.394 (3)C115—H1150.9500
C131—C1361.381 (3)C116—H1160.9500
C131—C1321.406 (3)C120—H1200.9500
C132—C1331.365 (4)C122—H1220.9500
C133—C1341.377 (5)C123—H1230.9500
C134—C1351.374 (5)C124—H1240.9500
C135—C1361.400 (4)C125—H1250.9500
C141—C1421.393 (3)C126—H1260.9500
C141—C1461.403 (3)C132—H1320.9500
C142—C1431.391 (3)C133—H1330.9500
C143—C1441.374 (3)C134—H1340.9500
C144—C1451.380 (3)C135—H1350.9500
C145—C1461.386 (3)C136—H1360.9500
C151—C1561.393 (3)C142—H1420.9500
C151—C1521.394 (3)C143—H1430.9500
C152—C1531.394 (3)C144—H1440.9500
C153—C1541.384 (4)C145—H1450.9500
C154—C1551.373 (4)C146—H1460.9500
C155—C1561.384 (3)C152—H1520.9500
P2—C2511.815 (2)C153—H1530.9500
P2—C2311.825 (2)C154—H1540.9500
P2—C2411.829 (2)C155—H1550.9500
N2—C2201.286 (3)C156—H1560.9500
N2—C2111.431 (3)C205—H20A0.9800
O201—C2031.208 (3)C205—H20B0.9800
O202—C2041.205 (3)C205—H20C0.9800
O203—C2031.347 (3)C206—H20D0.9800
O203—C2051.451 (3)C206—H20E0.9800
O204—C2041.341 (3)C206—H20F0.9800
O204—C2061.442 (3)C213—H2130.9500
C201—C2031.489 (3)C214—H2140.9500
C202—C2121.487 (3)C215—H2150.9500
C202—C2041.504 (3)C216—H2160.9500
C211—C2161.388 (3)C220—H2200.9500
C211—C2121.404 (3)C222—H2220.9500
C212—C2131.401 (3)C223—H2230.9500
C213—C2141.376 (4)C224—H2240.9500
C214—C2151.388 (4)C225—H2250.9500
C215—C2161.384 (3)C226—H2260.9500
C220—C2211.462 (3)C232—H2320.9500
C221—C2221.395 (3)C233—H2330.9500
C221—C2261.398 (3)C234—H2340.9500
C222—C2231.380 (3)C235—H2350.9500
C223—C2241.390 (3)C236—H2360.9500
C224—C2251.387 (3)C242—H2420.9500
C225—C2261.389 (3)C243—H2430.9500
C231—C2321.392 (3)C244—H2440.9500
C231—C2361.401 (3)C245—H2450.9500
C232—C2331.391 (3)C246—H2460.9500
C233—C2341.380 (4)C252—H2520.9500
C234—C2351.387 (4)C253—H2530.9500
C235—C2361.382 (4)C254—H2540.9500
C241—C2461.389 (4)C255—H2550.9500
C241—C2421.395 (3)C256—H2560.9500
C242—C2431.384 (4)C305—H30A0.9800
C243—C2441.370 (4)C305—H30B0.9800
C244—C2451.388 (4)C305—H30C0.9800
C245—C2461.392 (4)C306—H30D0.9800
C251—C2561.386 (3)C306—H30E0.9800
C251—C2521.401 (3)C306—H30F0.9800
C252—C2531.382 (3)C313—H3130.9500
C253—C2541.382 (4)C314—H3140.9500
C254—C2551.382 (4)C315—H3150.9500
C255—C2561.393 (3)C316—H3160.9500
P3—C3511.815 (2)C320—H3200.9500
P3—C3311.818 (2)C322—H3220.9500
P3—C3411.829 (2)C323—H3230.9500
N3—C3201.276 (3)C324—H3240.9500
N3—C3111.436 (3)C325—H3250.9500
O301—C3031.201 (3)C326—H3260.9500
O302—C3041.201 (3)C332—H3320.9500
O303—C3031.334 (3)C333—H3330.9500
O303—C3051.443 (3)C334—H3340.9500
O304—C3041.342 (3)C335—H3350.9500
O304—C3061.444 (3)C336—H3360.9500
C301—C3031.488 (3)C342—H3420.9500
C302—C3121.484 (3)C343—H3430.9500
C302—C3041.506 (3)C344—H3440.9500
C311—C3161.385 (3)C345—H3450.9500
C311—C3121.406 (3)C346—H3460.9500
C312—C3131.401 (3)C352—H3520.9500
C313—C3141.389 (3)C353—H3530.9500
C314—C3151.381 (4)C354—H3540.9500
C315—C3161.394 (3)C355—H3550.9500
C320—C3211.470 (3)C356—H3560.9500
C321—C3221.396 (3)C405—H40A0.9800
C321—C3261.399 (3)C405—H40B0.9800
C322—C3231.380 (3)C405—H40C0.9800
C323—C3241.387 (3)C406—H40D0.9800
C324—C3251.383 (4)C406—H40E0.9800
C325—C3261.383 (3)C406—H40F0.9800
C331—C3321.392 (3)C413—H4130.9500
C331—C3361.402 (3)C414—H4140.9500
C332—C3331.399 (4)C415—H4150.9500
C333—C3341.377 (4)C416—H4160.9500
C334—C3351.384 (4)C420—H4200.9500
C335—C3361.385 (3)C422—H4220.9500
C341—C3461.388 (3)C423—H4230.9500
C341—C3421.395 (3)C424—H4240.9500
C342—C3431.395 (4)C425—H4250.9500
C343—C3441.375 (4)C426—H4260.9500
C344—C3451.383 (4)C432—H4320.9500
C345—C3461.387 (3)C433—H4330.9500
C351—C3521.394 (3)C434—H4340.9500
C351—C3561.397 (3)C435—H4350.9500
C352—C3531.381 (3)C436—H4360.9500
C353—C3541.379 (4)C442—H4420.9500
C354—C3551.376 (4)C443—H4430.9500
C355—C3561.385 (3)C444—H4440.9500
P4—C4311.822 (2)C445—H4450.9500
P4—C4511.823 (2)C446—H4460.9500
P4—C4411.827 (2)C452—H4520.9500
N4—C4201.271 (3)C453—H4530.9500
N4—C4111.438 (3)C454—H4540.9500
O401—C4031.213 (3)C455—H4550.9500
O402—C4041.200 (3)C456—H4560.9500
C101—Pd1—N182.16 (8)C434—C433—C432120.3 (2)
C101—Pd1—P193.37 (6)C435—C434—C433120.2 (2)
N1—Pd1—P1165.77 (5)C434—C435—C436120.2 (2)
C101—Pd1—I1168.71 (6)C435—C436—C431120.2 (2)
N1—Pd1—I188.46 (5)C446—C441—C442118.0 (2)
P1—Pd1—I194.253 (17)C446—C441—P4118.89 (17)
C131—P1—Pd1108.64 (8)C442—C441—P4122.91 (18)
C141—P1—Pd1120.28 (7)C443—C442—C441120.6 (2)
C151—P1—Pd1112.94 (7)C444—C443—C442120.3 (2)
C201—Pd2—N281.95 (8)C443—C444—C445120.3 (2)
C201—Pd2—P293.81 (7)C444—C445—C446119.6 (2)
N2—Pd2—P2175.10 (5)C445—C446—C441121.1 (2)
C201—Pd2—I2170.30 (7)C452—C451—C456118.9 (2)
N2—Pd2—I289.52 (5)C452—C451—P4123.89 (18)
P2—Pd2—I294.495 (17)C456—C451—P4117.23 (18)
C231—P2—Pd2114.28 (8)C453—C452—C451121.0 (2)
C241—P2—Pd2115.85 (8)C454—C453—C452119.7 (2)
C251—P2—Pd2112.67 (8)C455—C454—C453119.9 (2)
C301—Pd3—N382.01 (8)C454—C455—C456120.3 (2)
C301—Pd3—P391.08 (6)C455—C456—C451120.2 (2)
N3—Pd3—P3170.16 (5)O103—C105—H10A109.5
C301—Pd3—I3168.52 (6)O103—C105—H10B109.5
N3—Pd3—I387.45 (5)H10A—C105—H10B109.5
P3—Pd3—I398.796 (17)O103—C105—H10C109.5
C331—P3—Pd3109.98 (7)H10A—C105—H10C109.5
C341—P3—Pd3118.36 (8)H10B—C105—H10C109.5
C351—P3—Pd3114.94 (8)O104—C106—H10D109.5
C401—Pd4—N482.05 (8)O104—C106—H10E109.5
C401—Pd4—P495.77 (6)H10D—C106—H10E109.5
N4—Pd4—P4168.13 (5)O104—C106—H10F109.5
C401—Pd4—I4167.88 (7)H10D—C106—H10F109.5
N4—Pd4—I487.77 (5)H10E—C106—H10F109.5
P4—Pd4—I492.847 (16)C114—C113—H113119.6
C431—P4—Pd4108.49 (8)C112—C113—H113119.6
C441—P4—Pd4122.76 (7)C115—C114—H114120.1
C451—P4—Pd4113.26 (7)C113—C114—H114120.1
C131—P1—C141101.72 (11)C116—C115—H115119.5
C131—P1—C151105.81 (11)C114—C115—H115119.5
C141—P1—C151106.05 (10)C115—C116—H116120.4
C120—N1—C111121.76 (19)C111—C116—H116120.4
C120—N1—Pd1133.28 (16)N1—C120—H120117.9
C111—N1—Pd1104.35 (13)C121—C120—H120117.9
C103—O103—C105115.30 (19)C123—C122—H122120.1
C104—O104—C106115.5 (2)C121—C122—H122120.1
C102—C101—C103118.4 (2)C122—C123—H123119.6
C102—C101—Pd1117.17 (17)C124—C123—H123119.6
C103—C101—Pd1123.67 (16)C125—C124—H124119.9
C101—C102—C112122.0 (2)C123—C124—H124119.9
C101—C102—C104123.9 (2)C124—C125—H125120.2
C112—C102—C104114.03 (19)C126—C125—H125120.2
O101—C103—O103123.1 (2)C121—C126—H126119.7
O101—C103—C101125.8 (2)C125—C126—H126119.7
O103—C103—C101111.0 (2)C133—C132—H132120.1
O102—C104—O104124.1 (2)C131—C132—H132120.1
O102—C104—C102125.5 (2)C132—C133—H133119.6
O104—C104—C102110.15 (19)C134—C133—H133119.6
C116—C111—C112120.9 (2)C135—C134—H134119.9
C116—C111—N1120.9 (2)C133—C134—H134119.9
C112—C111—N1118.0 (2)C134—C135—H135119.9
C113—C112—C111118.3 (2)C136—C135—H135119.9
C113—C112—C102122.3 (2)C131—C136—H136120.3
C111—C112—C102119.28 (19)C135—C136—H136120.3
C114—C113—C112120.7 (2)C143—C142—H142119.7
C115—C114—C113119.7 (2)C141—C142—H142119.7
C116—C115—C114121.0 (2)C144—C143—H143119.8
C115—C116—C111119.2 (2)C142—C143—H143119.8
N1—C120—C121124.1 (2)C143—C144—H144119.9
C126—C121—C122119.3 (2)C145—C144—H144119.9
C126—C121—C120117.8 (2)C144—C145—H145120.2
C122—C121—C120122.9 (2)C146—C145—H145120.2
C123—C122—C121119.8 (2)C145—C146—H146119.5
C122—C123—C124120.7 (2)C141—C146—H146119.5
C125—C124—C123120.1 (2)C151—C152—H152119.9
C124—C125—C126119.5 (2)C153—C152—H152119.9
C121—C126—C125120.6 (2)C154—C153—H153120.0
C136—C131—C132119.7 (2)C152—C153—H153120.0
C136—C131—P1120.96 (19)C155—C154—H154120.0
C132—C131—P1119.3 (2)C153—C154—H154120.0
C133—C132—C131119.8 (3)C154—C155—H155119.7
C132—C133—C134120.8 (3)C156—C155—H155119.7
C135—C134—C133120.1 (3)C155—C156—H156119.8
C134—C135—C136120.2 (3)C151—C156—H156119.8
C131—C136—C135119.4 (3)O203—C205—H20A109.5
C142—C141—C146118.1 (2)O203—C205—H20B109.5
C142—C141—P1124.02 (18)H20A—C205—H20B109.5
C146—C141—P1117.92 (17)O203—C205—H20C109.5
C143—C142—C141120.6 (2)H20A—C205—H20C109.5
C144—C143—C142120.3 (2)H20B—C205—H20C109.5
C143—C144—C145120.3 (2)O204—C206—H20D109.5
C144—C145—C146119.7 (2)O204—C206—H20E109.5
C145—C146—C141121.1 (2)H20D—C206—H20E109.5
C156—C151—C152119.0 (2)O204—C206—H20F109.5
C156—C151—P1119.00 (19)H20D—C206—H20F109.5
C152—C151—P1121.48 (19)H20E—C206—H20F109.5
C151—C152—C153120.1 (3)C214—C213—H213119.4
C154—C153—C152120.0 (3)C212—C213—H213119.4
C155—C154—C153120.0 (3)C213—C214—H214119.9
C154—C155—C156120.6 (3)C215—C214—H214119.9
C155—C156—C151120.3 (3)C216—C215—H215120.1
C251—P2—C231104.82 (11)C214—C215—H215120.1
C251—P2—C241103.40 (11)C215—C216—H216120.0
C231—P2—C241104.60 (11)C211—C216—H216120.0
C220—N2—C211120.1 (2)N2—C220—H220117.3
C220—N2—Pd2131.22 (16)C221—C220—H220117.3
C211—N2—Pd2108.58 (14)C223—C222—H222119.8
C203—O203—C205116.06 (19)C221—C222—H222119.8
C204—O204—C206115.7 (2)C222—C223—H223119.9
C202—C201—C203118.3 (2)C224—C223—H223119.9
C202—C201—Pd2118.29 (18)C225—C224—H224120.1
C203—C201—Pd2123.07 (17)C223—C224—H224120.1
C201—C202—C212123.4 (2)C224—C225—H225119.9
C201—C202—C204122.3 (2)C226—C225—H225119.9
C212—C202—C204114.3 (2)C225—C226—H226120.1
O201—C203—O203123.1 (2)C221—C226—H226120.1
O201—C203—C201125.8 (2)C233—C232—H232119.8
O203—C203—C201111.0 (2)C231—C232—H232119.8
O202—C204—O204123.9 (2)C234—C233—H233119.8
O202—C204—C202124.5 (2)C232—C233—H233119.8
O204—C204—C202111.4 (2)C233—C234—H234120.1
C216—C211—C212120.9 (2)C235—C234—H234120.1
C216—C211—N2121.2 (2)C236—C235—H235120.0
C212—C211—N2117.9 (2)C234—C235—H235120.0
C213—C212—C211117.8 (2)C235—C236—H236119.7
C213—C212—C202122.3 (2)C231—C236—H236119.7
C211—C212—C202119.7 (2)C243—C242—H242119.8
C214—C213—C212121.2 (3)C241—C242—H242119.8
C213—C214—C215120.2 (2)C244—C243—H243119.9
C216—C215—C214119.9 (2)C242—C243—H243119.9
C215—C216—C211120.0 (2)C243—C244—H244119.8
N2—C220—C221125.3 (2)C245—C244—H244119.8
C222—C221—C226119.4 (2)C244—C245—H245120.3
C222—C221—C220122.3 (2)C246—C245—H245120.3
C226—C221—C220118.3 (2)C241—C246—H246119.6
C223—C222—C221120.3 (2)C245—C246—H246119.6
C222—C223—C224120.2 (2)C253—C252—H252119.7
C225—C224—C223119.9 (2)C251—C252—H252119.7
C224—C225—C226120.2 (2)C254—C253—H253119.9
C225—C226—C221119.9 (2)C252—C253—H253119.9
C232—C231—C236118.7 (2)C253—C254—H254120.1
C232—C231—P2123.33 (19)C255—C254—H254120.1
C236—C231—P2117.95 (18)C254—C255—H255119.8
C233—C232—C231120.3 (2)C256—C255—H255119.8
C234—C233—C232120.4 (2)C251—C256—H256119.8
C233—C234—C235119.9 (3)C255—C256—H256119.8
C236—C235—C234120.1 (3)O303—C305—H30A109.5
C235—C236—C231120.7 (2)O303—C305—H30B109.5
C246—C241—C242118.6 (2)H30A—C305—H30B109.5
C246—C241—P2119.81 (19)O303—C305—H30C109.5
C242—C241—P2121.5 (2)H30A—C305—H30C109.5
C243—C242—C241120.5 (3)H30B—C305—H30C109.5
C244—C243—C242120.3 (3)O304—C306—H30D109.5
C243—C244—C245120.5 (3)O304—C306—H30E109.5
C244—C245—C246119.3 (3)H30D—C306—H30E109.5
C241—C246—C245120.8 (3)O304—C306—H30F109.5
C256—C251—C252118.8 (2)H30D—C306—H30F109.5
C256—C251—P2119.33 (18)H30E—C306—H30F109.5
C252—C251—P2121.85 (18)C314—C313—H313119.7
C253—C252—C251120.6 (2)C312—C313—H313119.7
C254—C253—C252120.2 (2)C315—C314—H314119.8
C253—C254—C255119.8 (2)C313—C314—H314119.8
C254—C255—C256120.3 (2)C314—C315—H315119.8
C251—C256—C255120.3 (2)C316—C315—H315119.8
C351—P3—C331109.27 (11)C311—C316—H316120.3
C351—P3—C34199.55 (11)C315—C316—H316120.3
C331—P3—C341103.71 (11)N3—C320—H320118.0
C320—N3—C311121.50 (19)C321—C320—H320118.0
C320—N3—Pd3131.99 (15)C323—C322—H322120.0
C311—N3—Pd3106.26 (13)C321—C322—H322120.0
C303—O303—C305115.7 (2)C322—C323—H323119.8
C304—O304—C306115.1 (2)C324—C323—H323119.8
C302—C301—C303117.8 (2)C325—C324—H324120.0
C302—C301—Pd3117.13 (18)C323—C324—H324120.0
C303—C301—Pd3124.91 (16)C326—C325—H325120.0
C301—C302—C312122.8 (2)C324—C325—H325120.0
C301—C302—C304122.2 (2)C325—C326—H326119.8
C312—C302—C304114.99 (19)C321—C326—H326119.8
O301—C303—O303123.1 (2)C331—C332—H332120.0
O301—C303—C301125.3 (2)C333—C332—H332120.0
O303—C303—C301111.6 (2)C334—C333—H333119.7
O302—C304—O304124.1 (2)C332—C333—H333119.7
O302—C304—C302124.6 (2)C333—C334—H334120.0
O304—C304—C302111.19 (19)C335—C334—H334120.0
C316—C311—C312121.2 (2)C334—C335—H335120.0
C316—C311—N3121.1 (2)C336—C335—H335120.0
C312—C311—N3117.6 (2)C335—C336—H336119.6
C313—C312—C311118.2 (2)C331—C336—H336119.6
C313—C312—C302122.1 (2)C343—C342—H342119.8
C311—C312—C302119.61 (19)C341—C342—H342119.8
C314—C313—C312120.5 (2)C344—C343—H343120.1
C315—C314—C313120.3 (2)C342—C343—H343120.1
C314—C315—C316120.3 (2)C343—C344—H344119.8
C311—C316—C315119.4 (2)C345—C344—H344119.8
N3—C320—C321124.1 (2)C344—C345—H345120.1
C322—C321—C326119.1 (2)C346—C345—H345120.1
C322—C321—C320122.4 (2)C345—C346—H346119.5
C326—C321—C320118.5 (2)C341—C346—H346119.5
C323—C322—C321120.0 (2)C353—C352—H352119.6
C322—C323—C324120.4 (2)C351—C352—H352119.6
C325—C324—C323120.0 (2)C354—C353—H353120.0
C326—C325—C324120.0 (2)C352—C353—H353120.0
C325—C326—C321120.4 (2)C355—C354—H354120.0
C332—C331—C336118.8 (2)C353—C354—H354120.0
C332—C331—P3124.80 (19)C354—C355—H355119.7
C336—C331—P3116.36 (18)C356—C355—H355119.7
C331—C332—C333119.9 (2)C355—C356—H356120.1
C334—C333—C332120.5 (3)C351—C356—H356120.1
C333—C334—C335120.0 (3)O403—C405—H40A109.5
C334—C335—C336120.0 (3)O403—C405—H40B109.5
C335—C336—C331120.7 (2)H40A—C405—H40B109.5
C346—C341—C342118.5 (2)O403—C405—H40C109.5
C346—C341—P3117.88 (18)H40A—C405—H40C109.5
C342—C341—P3123.5 (2)H40B—C405—H40C109.5
C343—C342—C341120.5 (3)O404—C406—H40D109.5
C344—C343—C342119.9 (3)O404—C406—H40E109.5
C343—C344—C345120.3 (3)H40D—C406—H40E109.5
C344—C345—C346119.8 (3)O404—C406—H40F109.5
C345—C346—C341120.9 (3)H40D—C406—H40F109.5
C352—C351—C356118.8 (2)H40E—C406—H40F109.5
C352—C351—P3121.00 (19)C414—C413—H413119.6
C356—C351—P3119.65 (18)C412—C413—H413119.6
C353—C352—C351120.7 (3)C413—C414—H414119.8
C354—C353—C352119.9 (3)C415—C414—H414119.8
C355—C354—C353120.0 (2)C416—C415—H415120.0
C354—C355—C356120.6 (3)C414—C415—H415120.0
C355—C356—C351119.9 (2)C411—C416—H416120.1
C431—P4—C451107.73 (10)C415—C416—H416120.1
C431—P4—C441100.63 (10)N4—C420—H420117.7
C451—P4—C441102.56 (10)C421—C420—H420117.7
C420—N4—C411121.34 (19)C423—C422—H422120.0
C420—N4—Pd4133.17 (16)C421—C422—H422120.0
C411—N4—Pd4105.17 (13)C424—C423—H423119.9
C403—O403—C405112.4 (2)C422—C423—H423119.9
C404—O404—C406114.91 (19)C425—C424—H424119.9
C402—C401—C403117.9 (2)C423—C424—H424119.9
C402—C401—Pd4117.27 (18)C424—C425—H425120.0
C403—C401—Pd4124.25 (18)C426—C425—H425120.0
C401—C402—C412122.5 (2)C425—C426—H426119.8
C401—C402—C404123.7 (2)C421—C426—H426119.8
C412—C402—C404113.8 (2)C433—C432—H432120.0
O401—C403—O403122.4 (2)C431—C432—H432120.0
O401—C403—C401125.5 (3)C434—C433—H433119.9
O403—C403—C401112.1 (2)C432—C433—H433119.9
O402—C404—O404124.7 (2)C435—C434—H434119.9
O402—C404—C402124.3 (2)C433—C434—H434119.9
O404—C404—C402110.68 (19)C434—C435—H435119.9
C416—C411—C412121.1 (2)C436—C435—H435119.9
C416—C411—N4121.0 (2)C435—C436—H436119.9
C412—C411—N4117.8 (2)C431—C436—H436119.9
C413—C412—C411117.8 (2)C443—C442—H442119.7
C413—C412—C402122.6 (2)C441—C442—H442119.7
C411—C412—C402119.5 (2)C444—C443—H443119.8
C414—C413—C412120.9 (2)C442—C443—H443119.8
C413—C414—C415120.4 (2)C443—C444—H444119.8
C416—C415—C414120.1 (2)C445—C444—H444119.8
C411—C416—C415119.7 (2)C444—C445—H445120.2
N4—C420—C421124.6 (2)C446—C445—H445120.2
C422—C421—C426119.4 (2)C445—C446—H446119.4
C422—C421—C420122.6 (2)C441—C446—H446119.4
C426—C421—C420118.0 (2)C453—C452—H452119.5
C423—C422—C421120.0 (2)C451—C452—H452119.5
C424—C423—C422120.2 (2)C454—C453—H453120.1
C425—C424—C423120.2 (2)C452—C453—H453120.1
C424—C425—C426120.0 (2)C455—C454—H454120.1
C425—C426—C421120.3 (2)C453—C454—H454120.1
C436—C431—C432119.2 (2)C454—C455—H455119.8
C436—C431—P4120.24 (17)C456—C455—H455119.8
C432—C431—P4120.33 (18)C455—C456—H456119.9
C433—C432—C431119.9 (2)C451—C456—H456119.9
I1—Pd1—P1—C13187.82 (8)C242—C241—C246—C2451.5 (4)
I1—Pd1—P1—C141155.74 (9)P2—C241—C246—C245174.9 (2)
I1—Pd1—P1—C15129.24 (9)C244—C245—C246—C2410.3 (4)
Pd1—P1—C131—C132174.63 (19)C231—P2—C251—C256111.6 (2)
Pd1—P1—C141—C142111.48 (19)C241—P2—C251—C256139.1 (2)
Pd1—P1—C151—C152110.40 (18)Pd2—P2—C251—C25613.2 (2)
C102—C101—C103—O10117.2 (3)C231—P2—C251—C25265.3 (2)
C101—C102—C104—O10295.5 (3)C241—P2—C251—C25244.0 (2)
I2—Pd2—P2—C231165.59 (9)C256—C251—C252—C2532.3 (4)
I2—Pd2—P2—C24143.87 (9)P2—C251—C252—C253174.7 (2)
I2—Pd2—P2—C25174.91 (9)C251—C252—C253—C2540.6 (4)
Pd2—P2—C231—C232128.6 (2)C252—C253—C254—C2551.0 (5)
Pd2—P2—C241—C24293.2 (2)C253—C254—C255—C2561.0 (4)
Pd2—P2—C251—C252169.81 (19)C252—C251—C256—C2552.3 (4)
C202—C201—C203—O20117.3 (4)P2—C251—C256—C255174.7 (2)
C201—C202—C204—O20297.0 (3)C254—C255—C256—C2510.7 (4)
I3—Pd3—P3—C331148.06 (8)C301—Pd3—P3—C35197.74 (11)
I3—Pd3—P3—C34129.18 (9)C301—Pd3—P3—C33126.05 (11)
I3—Pd3—P3—C35188.14 (9)C301—Pd3—P3—C341144.93 (11)
Pd3—P3—C331—C332125.79 (19)C301—Pd3—N3—C320113.6 (2)
Pd3—P3—C341—C342108.0 (2)I3—Pd3—N3—C32071.0 (2)
Pd3—P3—C351—C352179.46 (19)C301—Pd3—N3—C31172.26 (15)
C302—C301—C303—O30113.1 (4)I3—Pd3—N3—C311103.17 (13)
C301—C302—C304—O30294.4 (3)N3—Pd3—C301—C30248.12 (17)
I4—Pd4—P4—C43180.69 (8)P3—Pd3—C301—C302124.85 (17)
I4—Pd4—P4—C441162.79 (9)N3—Pd3—C301—C303127.22 (19)
I4—Pd4—P4—C45138.86 (8)P3—Pd3—C301—C30359.81 (18)
Pd4—P4—C431—C432174.12 (17)C303—C301—C302—C312171.96 (19)
Pd4—P4—C441—C442129.76 (17)Pd3—C301—C302—C3123.7 (3)
Pd4—P4—C451—C452113.42 (18)C303—C301—C302—C3048.9 (3)
C402—C401—C403—O4019.4 (4)Pd3—C301—C302—C304175.42 (16)
C401—C402—C404—O40290.4 (3)C305—O303—C303—O3010.2 (4)
C101—Pd1—P1—C13183.85 (10)C305—O303—C303—C301178.3 (2)
C101—Pd1—P1—C14132.59 (11)Pd3—C301—C303—O301171.57 (19)
C101—Pd1—P1—C151159.09 (11)C302—C301—C303—O303164.9 (2)
C101—Pd1—N1—C120116.1 (2)Pd3—C301—C303—O30310.4 (3)
I1—Pd1—N1—C12070.2 (2)C306—O304—C304—O3029.3 (4)
C101—Pd1—N1—C11173.15 (15)C306—O304—C304—C302174.6 (2)
I1—Pd1—N1—C111100.56 (13)C312—C302—C304—O30284.8 (3)
N1—Pd1—C101—C10248.52 (17)C301—C302—C304—O30489.6 (3)
P1—Pd1—C101—C102117.91 (17)C312—C302—C304—O30491.2 (2)
N1—Pd1—C101—C103121.01 (18)C320—N3—C311—C31653.4 (3)
P1—Pd1—C101—C10372.56 (17)Pd3—N3—C311—C316121.49 (19)
C103—C101—C102—C112167.51 (19)C320—N3—C311—C312130.6 (2)
Pd1—C101—C102—C1122.6 (3)Pd3—N3—C311—C31254.5 (2)
C103—C101—C102—C1049.0 (3)C316—C311—C312—C3130.5 (3)
Pd1—C101—C102—C104179.13 (16)N3—C311—C312—C313176.46 (19)
C105—O103—C103—O1010.5 (3)C316—C311—C312—C302177.7 (2)
C105—O103—C103—C101177.49 (19)N3—C311—C312—C3026.4 (3)
Pd1—C101—C103—O101173.42 (18)C301—C302—C312—C313144.9 (2)
C102—C101—C103—O103159.73 (19)C304—C302—C312—C31334.3 (3)
Pd1—C101—C103—O1039.7 (3)C301—C302—C312—C31138.1 (3)
C106—O104—C104—O1025.3 (4)C304—C302—C312—C311142.7 (2)
C106—O104—C104—C102179.5 (2)C311—C312—C313—C3141.5 (3)
C112—C102—C104—O10287.7 (3)C302—C312—C313—C314178.6 (2)
C101—C102—C104—O10490.4 (3)C312—C313—C314—C3151.7 (4)
C112—C102—C104—O10486.4 (2)C313—C314—C315—C3160.9 (4)
C120—N1—C111—C11653.0 (3)C312—C311—C316—C3150.3 (3)
Pd1—N1—C111—C116119.08 (19)N3—C311—C316—C315175.5 (2)
C120—N1—C111—C112132.1 (2)C314—C315—C316—C3110.1 (4)
Pd1—N1—C111—C11255.8 (2)C311—N3—C320—C321178.4 (2)
C116—C111—C112—C1131.7 (3)Pd3—N3—C320—C3218.2 (4)
N1—C111—C112—C113176.57 (19)N3—C320—C321—C32225.2 (4)
C116—C111—C112—C102179.5 (2)N3—C320—C321—C326156.9 (2)
N1—C111—C112—C1025.6 (3)C326—C321—C322—C3231.0 (3)
C101—C102—C112—C113143.1 (2)C320—C321—C322—C323178.9 (2)
C104—C102—C112—C11340.0 (3)C321—C322—C323—C3240.1 (4)
C101—C102—C112—C11139.1 (3)C322—C323—C324—C3250.3 (4)
C104—C102—C112—C111137.7 (2)C323—C324—C325—C3260.2 (4)
C111—C112—C113—C1142.5 (3)C324—C325—C326—C3211.1 (4)
C102—C112—C113—C114179.8 (2)C322—C321—C326—C3251.5 (4)
C112—C113—C114—C1151.1 (4)C320—C321—C326—C325179.4 (2)
C113—C114—C115—C1161.1 (4)C351—P3—C331—C3321.2 (2)
C114—C115—C116—C1111.8 (4)C341—P3—C331—C332106.7 (2)
C112—C111—C116—C1150.4 (3)C351—P3—C331—C336178.64 (17)
N1—C111—C116—C115174.3 (2)C341—P3—C331—C33675.92 (19)
C111—N1—C120—C121178.9 (2)Pd3—P3—C331—C33651.60 (19)
Pd1—N1—C120—C1219.4 (4)C336—C331—C332—C3330.5 (3)
N1—C120—C121—C126163.8 (2)P3—C331—C332—C333177.86 (19)
N1—C120—C121—C12216.3 (4)C331—C332—C333—C3340.2 (4)
C126—C121—C122—C1230.9 (4)C332—C333—C334—C3350.4 (4)
C120—C121—C122—C123179.2 (2)C333—C334—C335—C3360.1 (4)
C121—C122—C123—C1240.1 (4)C334—C335—C336—C3310.9 (4)
C122—C123—C124—C1250.6 (4)C332—C331—C336—C3351.0 (4)
C123—C124—C125—C1260.4 (4)P3—C331—C336—C335178.59 (19)
C122—C121—C126—C1251.0 (4)C351—P3—C341—C34650.8 (2)
C120—C121—C126—C125179.0 (2)C331—P3—C341—C346163.4 (2)
C124—C125—C126—C1210.4 (4)Pd3—P3—C341—C34674.5 (2)
C141—P1—C131—C136133.9 (2)C351—P3—C341—C342126.7 (2)
C151—P1—C131—C136115.5 (2)C331—P3—C341—C34214.1 (2)
Pd1—P1—C131—C1366.0 (2)C346—C341—C342—C3432.5 (4)
C141—P1—C131—C13246.8 (2)P3—C341—C342—C343179.9 (2)
C151—P1—C131—C13263.8 (2)C341—C342—C343—C3440.7 (4)
C136—C131—C132—C1331.9 (4)C342—C343—C344—C3451.7 (4)
P1—C131—C132—C133177.5 (2)C343—C344—C345—C3462.2 (4)
C131—C132—C133—C1340.6 (5)C344—C345—C346—C3410.4 (4)
C132—C133—C134—C1351.1 (5)C342—C341—C346—C3451.9 (4)
C133—C134—C135—C1361.5 (5)P3—C341—C346—C345179.5 (2)
C132—C131—C136—C1351.5 (4)C331—P3—C351—C35256.4 (2)
P1—C131—C136—C135177.9 (2)C341—P3—C351—C35251.9 (2)
C134—C135—C136—C1310.2 (4)C331—P3—C351—C356132.2 (2)
C131—P1—C141—C142128.6 (2)C341—P3—C351—C356119.5 (2)
C151—P1—C141—C14218.1 (2)Pd3—P3—C351—C3568.0 (2)
C131—P1—C141—C14651.6 (2)C356—C351—C352—C3531.2 (4)
C151—P1—C141—C146162.04 (18)P3—C351—C352—C353172.7 (2)
Pd1—P1—C141—C14668.34 (19)C351—C352—C353—C3541.0 (4)
C146—C141—C142—C1430.2 (3)C352—C353—C354—C3550.4 (4)
P1—C141—C142—C143179.60 (19)C353—C354—C355—C3560.0 (4)
C141—C142—C143—C1440.4 (4)C354—C355—C356—C3510.2 (4)
C142—C143—C144—C1450.1 (4)C352—C351—C356—C3550.8 (4)
C143—C144—C145—C1460.7 (4)P3—C351—C356—C355172.4 (2)
C144—C145—C146—C1411.0 (4)C401—Pd4—P4—C43190.78 (10)
C142—C141—C146—C1450.5 (3)C401—Pd4—P4—C451149.67 (11)
P1—C141—C146—C145179.70 (18)C401—Pd4—P4—C44125.74 (11)
C131—P1—C151—C156179.72 (19)C401—Pd4—N4—C420113.8 (2)
C141—P1—C151—C15672.8 (2)I4—Pd4—N4—C42072.8 (2)
Pd1—P1—C151—C15661.0 (2)C401—Pd4—N4—C41172.87 (15)
C131—P1—C151—C1528.3 (2)I4—Pd4—N4—C411100.54 (13)
C141—P1—C151—C152115.8 (2)N4—Pd4—C401—C40248.20 (17)
C156—C151—C152—C1530.5 (3)P4—Pd4—C401—C402120.04 (17)
P1—C151—C152—C153171.91 (19)N4—Pd4—C401—C403122.63 (19)
C151—C152—C153—C1540.8 (4)P4—Pd4—C401—C40369.13 (19)
C152—C153—C154—C1550.6 (4)C403—C401—C402—C412168.1 (2)
C153—C154—C155—C1560.9 (4)Pd4—C401—C402—C4123.3 (3)
C154—C155—C156—C1512.1 (4)C403—C401—C402—C40410.1 (3)
C152—C151—C156—C1552.0 (3)Pd4—C401—C402—C404178.52 (16)
P1—C151—C156—C155173.56 (19)C405—O403—C403—O4016.8 (4)
C201—Pd2—P2—C251110.11 (11)C405—O403—C403—C401175.1 (2)
C201—Pd2—P2—C2319.39 (11)Pd4—C401—C403—O401179.8 (2)
C201—Pd2—P2—C241131.12 (11)C402—C401—C403—O403168.6 (2)
C201—Pd2—N2—C220113.1 (2)Pd4—C401—C403—O4032.2 (3)
I2—Pd2—N2—C22071.5 (2)C406—O404—C404—O4025.6 (4)
C201—Pd2—N2—C21170.01 (16)C406—O404—C404—C402179.5 (2)
I2—Pd2—N2—C211105.35 (14)C401—C402—C404—O40495.6 (3)
N2—Pd2—C201—C20247.04 (19)C412—C402—C404—O40482.7 (2)
P2—Pd2—C201—C202130.49 (18)C420—N4—C411—C41654.6 (3)
N2—Pd2—C201—C203126.5 (2)Pd4—N4—C411—C416119.75 (19)
P2—Pd2—C201—C20355.93 (19)C420—N4—C411—C412129.1 (2)
C203—C201—C202—C212168.7 (2)Pd4—N4—C411—C41256.6 (2)
Pd2—C201—C202—C2125.2 (3)C416—C411—C412—C4132.6 (3)
C203—C201—C202—C2049.6 (4)N4—C411—C412—C413178.87 (19)
Pd2—C201—C202—C204176.49 (18)C416—C411—C412—C402179.5 (2)
C205—O203—C203—O2010.1 (4)N4—C411—C412—C4024.2 (3)
C205—O203—C203—C201178.6 (2)C401—C402—C412—C413146.1 (2)
Pd2—C201—C203—O201169.1 (2)C404—C402—C412—C41335.6 (3)
C202—C201—C203—O203161.2 (2)C401—C402—C412—C41137.2 (3)
Pd2—C201—C203—O20312.4 (3)C404—C402—C412—C411141.2 (2)
C206—O204—C204—O20211.8 (4)C411—C412—C413—C4143.1 (3)
C206—O204—C204—C202172.5 (2)C402—C412—C413—C414179.9 (2)
C201—C202—C204—O20487.2 (3)C412—C413—C414—C4151.5 (4)
C212—C202—C204—O20284.6 (3)C412—C402—C404—O40291.3 (3)
C212—C202—C204—O20491.2 (2)C413—C414—C415—C4160.7 (4)
C220—N2—C211—C21652.0 (3)C412—C411—C416—C4150.5 (3)
Pd2—N2—C211—C216125.3 (2)N4—C411—C416—C415176.6 (2)
C220—N2—C211—C212129.9 (2)C414—C415—C416—C4111.2 (3)
Pd2—N2—C211—C21252.8 (2)C411—N4—C420—C421178.8 (2)
C216—C211—C212—C2130.0 (4)Pd4—N4—C420—C4218.7 (4)
N2—C211—C212—C213178.2 (2)N4—C420—C421—C42219.1 (4)
C216—C211—C212—C202175.7 (2)N4—C420—C421—C426162.6 (2)
N2—C211—C212—C2026.1 (3)C426—C421—C422—C4230.5 (4)
C201—C202—C212—C213148.9 (3)C420—C421—C422—C423178.8 (2)
C204—C202—C212—C21332.7 (3)C421—C422—C423—C4240.0 (4)
C201—C202—C212—C21135.7 (4)C422—C423—C424—C4250.2 (4)
C204—C202—C212—C211142.8 (2)C423—C424—C425—C4260.2 (4)
C211—C212—C213—C2140.9 (4)C424—C425—C426—C4210.7 (4)
C202—C212—C213—C214176.4 (2)C422—C421—C426—C4250.8 (4)
C212—C213—C214—C2151.5 (4)C420—C421—C426—C425179.2 (2)
C213—C214—C215—C2161.1 (4)C451—P4—C431—C436122.4 (2)
C214—C215—C216—C2110.3 (4)C441—P4—C431—C436130.6 (2)
C212—C211—C216—C2150.2 (4)Pd4—P4—C431—C4360.6 (2)
N2—C211—C216—C215177.9 (2)C451—P4—C431—C43262.9 (2)
C211—N2—C220—C221176.5 (2)C441—P4—C431—C43244.1 (2)
Pd2—N2—C220—C2216.9 (4)C436—C431—C432—C4331.5 (4)
N2—C220—C221—C22225.2 (4)P4—C431—C432—C433176.30 (19)
N2—C220—C221—C226157.5 (2)C431—C432—C433—C4341.2 (4)
C226—C221—C222—C2231.3 (4)C432—C433—C434—C4350.3 (4)
C220—C221—C222—C223178.6 (2)C433—C434—C435—C4360.3 (4)
C221—C222—C223—C2240.1 (4)C434—C435—C436—C4310.1 (4)
C222—C223—C224—C2250.4 (4)C432—C431—C436—C4350.9 (4)
C223—C224—C225—C2260.3 (4)P4—C431—C436—C435175.66 (19)
C224—C225—C226—C2211.5 (4)C431—P4—C441—C44665.50 (19)
C222—C221—C226—C2252.0 (4)C451—P4—C441—C446176.55 (17)
C220—C221—C226—C225179.4 (2)Pd4—P4—C441—C44654.8 (2)
C251—P2—C231—C2324.8 (2)C431—P4—C441—C442109.9 (2)
C241—P2—C231—C232103.7 (2)C451—P4—C441—C4421.1 (2)
C251—P2—C231—C236172.70 (19)C446—C441—C442—C4430.2 (3)
C241—P2—C231—C23678.8 (2)P4—C441—C442—C443175.67 (18)
Pd2—P2—C231—C23648.9 (2)C441—C442—C443—C4440.2 (4)
C236—C231—C232—C2330.3 (4)C442—C443—C444—C4450.1 (4)
P2—C231—C232—C233177.8 (2)C443—C444—C445—C4460.3 (4)
C231—C232—C233—C2340.2 (4)C444—C445—C446—C4410.3 (3)
C232—C233—C234—C2350.2 (4)C442—C441—C446—C4450.1 (3)
C233—C234—C235—C2360.3 (5)P4—C441—C446—C445175.59 (17)
C234—C235—C236—C2310.8 (4)C431—P4—C451—C4526.6 (2)
C232—C231—C236—C2350.8 (4)C441—P4—C451—C452112.2 (2)
P2—C231—C236—C235178.4 (2)C431—P4—C451—C456174.09 (18)
C251—P2—C241—C24640.6 (2)C441—P4—C451—C45668.5 (2)
C231—P2—C241—C246150.1 (2)Pd4—P4—C451—C45665.92 (19)
Pd2—P2—C241—C24683.1 (2)C456—C451—C452—C4530.5 (3)
C251—P2—C241—C242143.1 (2)P4—C451—C452—C453179.79 (18)
C231—P2—C241—C24233.6 (2)C451—C452—C453—C4541.8 (4)
C246—C241—C242—C2432.1 (4)C452—C453—C454—C4551.7 (4)
P2—C241—C242—C243174.2 (2)C453—C454—C455—C4560.6 (4)
C241—C242—C243—C2440.9 (4)C454—C455—C456—C4512.9 (4)
C242—C243—C244—C2450.9 (4)C452—C451—C456—C4552.8 (4)
C243—C244—C245—C2461.5 (4)P4—C451—C456—C455177.85 (19)
Hydrogen-bond geometry (Å, º) top
D—H···AD—HH···AD···AD—H···A
C154—H154···O401i0.952.443.325 (3)155
C254—H254···O402i0.952.493.334 (3)148
C313—H313···O302ii0.952.423.170 (3)136
C354—H354···O102iii0.952.593.536 (3)174
C454—H454···O301iii0.952.453.088 (3)124
C133—H133···I3iv0.952.993.805 (3)145
C444—H444···I1v0.952.993.780 (2)141
Symmetry codes: (i) x+1, y+1/2, z+1/2; (ii) x, y+1, z+1; (iii) x, y+1/2, z1/2; (iv) x, y+1/2, z+1/2; (v) x1, y+1/2, z1/2.

Experimental details

Crystal data
Chemical formula[Pd(C19H17NO4)I(C18H15P)]
Mr817.90
Crystal system, space groupMonoclinic, P21/c
Temperature (K)133
a, b, c (Å)16.6938 (11), 22.1074 (15), 36.666 (3)
β (°) 94.460 (4)
V3)13490.8 (17)
Z16
Radiation typeMo Kα
µ (mm1)1.55
Crystal size (mm)0.38 × 0.22 × 0.20
Data collection
DiffractometerBruker SMART 1000 CCD area-detector
diffractometer
Absorption correctionMulti-scan
(SADABS; Bruker, 1998)
Tmin, Tmax0.653, 0.733
No. of measured, independent and
observed [I > 2σ(I)] reflections
261441, 39449, 27970
Rint0.050
(sin θ/λ)max1)0.704
Refinement
R[F2 > 2σ(F2)], wR(F2), S 0.030, 0.070, 0.95
No. of reflections39449
No. of parameters1629
H-atom treatmentH-atom parameters constrained
Δρmax, Δρmin (e Å3)1.26, 0.90

Computer programs: SMART (Bruker, 1998), SAINT (Bruker, 1998), SAINT, SHELXS97 (Sheldrick, 1997), SHELXL97 (Sheldrick, 1997), XP (Siemens, 1994), SHELXL97.

Selected geometric parameters (Å, º) top
Pd1—C1012.019 (2)Pd3—C3012.023 (2)
Pd1—N12.0744 (18)Pd3—N32.0727 (17)
Pd1—P12.2524 (6)Pd3—P32.2700 (6)
Pd1—I12.6716 (3)Pd3—I32.6595 (3)
C101—C1021.338 (3)C301—C3021.344 (3)
Pd2—C2012.020 (2)Pd4—C4012.024 (2)
Pd2—N22.0813 (19)Pd4—N42.0654 (18)
Pd2—P22.2833 (6)Pd4—P42.2660 (6)
Pd2—I22.6683 (3)Pd4—I42.6877 (3)
C201—C2021.346 (3)C401—C4021.347 (3)
C101—Pd1—N182.16 (8)C301—Pd3—N382.01 (8)
C101—Pd1—P193.37 (6)C301—Pd3—P391.08 (6)
N1—Pd1—P1165.77 (5)N3—Pd3—P3170.16 (5)
C101—Pd1—I1168.71 (6)C301—Pd3—I3168.52 (6)
N1—Pd1—I188.46 (5)N3—Pd3—I387.45 (5)
P1—Pd1—I194.253 (17)P3—Pd3—I398.796 (17)
C131—P1—Pd1108.64 (8)C331—P3—Pd3109.98 (7)
C141—P1—Pd1120.28 (7)C341—P3—Pd3118.36 (8)
C151—P1—Pd1112.94 (7)C351—P3—Pd3114.94 (8)
C201—Pd2—N281.95 (8)C401—Pd4—N482.05 (8)
C201—Pd2—P293.81 (7)C401—Pd4—P495.77 (6)
N2—Pd2—P2175.10 (5)N4—Pd4—P4168.13 (5)
C201—Pd2—I2170.30 (7)C401—Pd4—I4167.88 (7)
N2—Pd2—I289.52 (5)N4—Pd4—I487.77 (5)
P2—Pd2—I294.495 (17)P4—Pd4—I492.847 (16)
C231—P2—Pd2114.28 (8)C431—P4—Pd4108.49 (8)
C241—P2—Pd2115.85 (8)C441—P4—Pd4122.76 (7)
C251—P2—Pd2112.67 (8)C451—P4—Pd4113.26 (7)
I1—Pd1—P1—C13187.82 (8)I3—Pd3—P3—C331148.06 (8)
I1—Pd1—P1—C141155.74 (9)I3—Pd3—P3—C34129.18 (9)
I1—Pd1—P1—C15129.24 (9)I3—Pd3—P3—C35188.14 (9)
Pd1—P1—C131—C132174.63 (19)Pd3—P3—C331—C332125.79 (19)
Pd1—P1—C141—C142111.48 (19)Pd3—P3—C341—C342108.0 (2)
Pd1—P1—C151—C152110.40 (18)Pd3—P3—C351—C352179.46 (19)
C102—C101—C103—O10117.2 (3)C302—C301—C303—O30113.1 (4)
C101—C102—C104—O10295.5 (3)C301—C302—C304—O30294.4 (3)
I2—Pd2—P2—C231165.59 (9)I4—Pd4—P4—C43180.69 (8)
I2—Pd2—P2—C24143.87 (9)I4—Pd4—P4—C441162.79 (9)
I2—Pd2—P2—C25174.91 (9)I4—Pd4—P4—C45138.86 (8)
Pd2—P2—C231—C232128.6 (2)Pd4—P4—C431—C432174.12 (17)
Pd2—P2—C241—C24293.2 (2)Pd4—P4—C441—C442129.76 (17)
Pd2—P2—C251—C252169.81 (19)Pd4—P4—C451—C452113.42 (18)
C202—C201—C203—O20117.3 (4)C402—C401—C403—O4019.4 (4)
C201—C202—C204—O20297.0 (3)C401—C402—C404—O40290.4 (3)
Hydrogen-bond geometry (Å, º) top
D—H···AD—HH···AD···AD—H···A
C154—H154···O401i0.952.443.325 (3)155.3
C254—H254···O402i0.952.493.334 (3)147.8
C313—H313···O302ii0.952.423.170 (3)135.7
C354—H354···O102iii0.952.593.536 (3)174.1
C454—H454···O301iii0.952.453.088 (3)124.1
C133—H133···I3iv0.952.993.805 (3)144.9
C444—H444···I1v0.952.993.780 (2)141.2
Symmetry codes: (i) x+1, y+1/2, z+1/2; (ii) x, y+1, z+1; (iii) x, y+1/2, z1/2; (iv) x, y+1/2, z+1/2; (v) x1, y+1/2, z1/2.
 

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