supplementary materials


dn2590 scheme

Acta Cryst. (2010). E66, m1185-m1186    [ doi:10.1107/S1600536810034197 ]

A tetrasilver(I)ditungsten(VI) cluster with sulfide and bis(diphenylphosphino)methane ligands

R. Wang, L.-L. Song, K.-Y. Hu, Q.-H. Jin and C.-L. Zhang

Abstract top

The asymmetric unit of the title complex, [Ag4W2S8(C25H22P2)3]·2C3H7NO, tris[[mu]2-bis(diphenylphosphino)methane]-3:6[kappa]2P:P';4:5[kappa]2P:P';5:6[kappa]2P:P'-[mu]5-sulfido-2:3:4:5:6[kappa]5S-[mu]3-sulfido-1:3:4[kappa]3S-tetra-[mu]2-sulfido-1:3[kappa]2S;1:4[kappa]2S;2:5[kappa]2S;2:6[kappa]2S-disulfido-1[kappa]S,2[kappa]S-tetrasilver(I)ditungsten(VI) N,N-dimethylformamide disolvate, contains two [WS4]2- anions, four silver cations, three bidentate-bridging bis(diphenylphosphino)methane (dppm) ligands and two N,N-dimethylformamide (DMF) solvent molecules. The coordination geometry of each Ag atom is distorted tetrahedral. Two Ag ions are coordinated by [mu]2-S and [mu]5-S atoms, and by two P atoms from two dppm ligands, while the other two Ag atoms are coordinated by [mu]2-S, [mu]3-S and [mu]5-S atoms, and by one P atom from a dppm ligand.

Comment top

In the recent years, Mo(W)—Cu(Ag)—S clusters derived from the well known synthons tetrathiotungstate and tetrathiomolybdate([MS4]2-(M=Mo, W)) have been extensively investigated due to their rich structural chemistry (Zhang et al., 2000; Zhang et al., 2004; Lang et al., 2006; Ren et al., 2006) and potential applications in biological systems (George et al., 2000; George et al. 2003), and optical materials (Shi et al., 1995; Hong et al., 1997; Niu et al., 2005). Herein a new complex [(WS4)2Ag4(dppm)3].2DMF (1) [dppm=bis(diphenylphosphino)methane,DMF=N,N-dimethylformamide] is reported.

The asymmetric unit contains two [WS4]2- anions, four silver cations, three bridging dppm ligands and two DMF solvent molecules(Fig. 1). One [WS4]2- anion bridges two Ag atoms whereas the other [WS4]2- anion bridges four Ag atoms. In both anions three sulfur atoms are coordinating to silver atoms whereas the W=S unit remaining intact. There are three kinds of bridging S atom: µ2-S (atoms S1, S3, S6 and S7, each is bonded to one W and one Ag atom), µ3-S (S2, bonded to W1, Ag1 and Ag2) and µ5-S (S5, bonded to W2 and four Ag atoms).

In complex 1, Ag1 and Ag2 are coordinated by one P atom from one dppm ligand, one µ2-S atom, one µ3-S atom and one µ5-S, while Ag3 and Ag4 are coordinated by two P atoms from two dppm ligands, one µ2-S atom and one µ5-S atom. It is noticeable that the coordination mode of µ5-S bonding to mixed metal ions is unique.

In two [WS4]2- units, the average length of W-µ2-S (2.2085 Å) is longer than that of W=S (2.1496 Å), but is shorter than those of W-µ3-S of (2.273 Å) and W-µ5-S (2.7102 Å). The Ag—S bond distances are in the range of 2.5140 (12)–2.8409 (12) Å. The average distance of Ag1(Ag2)—P (2.3919 Å) is shorter than that of Ag3(Ag4)—P.

Interestingly, the fragment [(WS4)2Ag4(dppm)3] in the title complex I is an isomer of [(WS4)2Ag4(dppm)3](II)(Yu et al., 2001) (Figure 2). The main difference being the occurence of the µ5-S in complex I. Consequently, in complex I each Ag atom is four-coordinated, while in complex II two Ag atoms are three-coordinated, the other two Ag atoms are four-coordinated. The mean distance of W—S(2.086 Å) in I is shorter than that observed in complex II (2.136 Å). The average W—Ag length in complex I (3.0356 Å) is similar to that in complex II (3.0406 Å).

The formation of this two isomers may be related to the choice of the solvent. Complex I was synthesized in the mixed solvents DMF and MeCN, while complex II is obtained in CH2Cl2. In this paper, complex I was prepared by using different Ag salts as starting materials: AgBF4 or AgNO3. From this we know, the fragment [(WS4)2Ag4(dppm)3] may be easily obtained because of its stable structure with high symmetry.

Related literature top

For related structures, see: Yu et al. (2001). For general background to Mo(W)—Cu(Ag)—S clusters derived from tetrathiotungstate and tetrathiomolybdate [MS4]2-(M = Mo, W) synthons, see: George et al.(2000, 2003); Hong et al. (1997); Lang et al. (2006); Niu et al. (2005); Ren et al. (2006); Shi et al. (1995); Yu et al. (2001); Zhang et al. (2000, 2004).

Experimental top

The title complex was prepared by the reaction of AgNO3, bis(diphenylphosphino)methane(dppm), (NH4)2WS4 and Phen (phenathroline) in molar ratio of 2:4:1:0.5 in the mixed solvents MeCN and DMF(10 ml,V/V=1/1). The mixture was stirred at room temperature for 8 h, then filtered. Subsequent slow evaporation of the filtrate resulted in the formation of yellow crystals of the title complex. Crystals suitable for single-crystal X-ray diffraction were selected directly from the sample as prepared. Analysis found(percentage): C 41.33, H 3.40, N 1.18; calculated: C 41.31, H 3.42, N 1.19.

Alternative method to synthesize complex 1 is using AgBF4 in place of AgNO3 in the starting materials.

Refinement top

Metal atom centers were located from the E-maps and other non-hydrogen atoms were located in successive difference Fourier syntheses. The final refinements were performed by full matrix least-squares methods with anisotropic thermal parameters for non-hydrogen atoms on F2.

The final refinements were performed with isotropic thermal parameters. All hydrogen atoms were located in the calculated sites and included in the final refinement in the riding model approximation with displacement parameters derived from the parent atoms to which they were bonded.

Computing details top

Data collection: RAPID-AUTO (Rigaku, 2004); cell refinement: RAPID-AUTO (Rigaku, 2004); data reduction: RAPID-AUTO (Rigaku, 2004); program(s) used to solve structure: SHELXS97 (Sheldrick, 2008); program(s) used to refine structure: SHELXL97 (Sheldrick, 2008); molecular graphics: ORTEPIII (Burnett & Johnson, 1996) and ORTEP-3 for Windows (Farrugia, 1997); software used to prepare material for publication: SHELXL97 (Sheldrick, 2008).

Figures top
[Figure 1] Fig. 1. Molecular view of compound I with the atom labeling scheme. Ellipsoids are drawn at the 30% probability level. H atoms have been omitted for clarity.
[Figure 2] Fig. 2. Comparison of the two isomers [(WS4)2Ag4(dppm)3] I and II.
tris[µ2-bis(diphenylphosphino)methane]- 3:6κ2P:P';4:5κ2P:P'; 5:6κ2P:P'-µ5-sulfido-2:3:4:5:6κ5S- µ3-sulfido-1:3:4κ3S- tetra-µ2-sulfido-1:3κ2S;1:4κ2S; 2:5κ2S;2:6κ2S-disulfido-1κS,2κS- tetrasilver(I)ditungsten(VI) N,N-dimethylformamide disolvate top
Crystal data top
[Ag4W2S8(C25H22P2)3]·2C3H7NOF(000) = 4600
Mr = 2354.95Dx = 1.826 Mg m3
Monoclinic, P21/cMo Kα radiation, λ = 0.71073 Å
Hall symbol: -P 2ybcCell parameters from 27248 reflections
a = 22.931 (2) Åθ = 3.0–27.5°
b = 14.0395 (12) ŵ = 3.93 mm1
c = 27.855 (3) ÅT = 93 K
β = 107.224 (1)°Block, yellow
V = 8565.6 (14) Å30.47 × 0.43 × 0.43 mm
Z = 4
Data collection top
Rigaku R-AXIS RAPID
diffractometer
19520 independent reflections
Radiation source: Rotating Anode18777 reflections with I > 2σ(I)
graphiteRint = 0.045
ω scansθmax = 27.5°, θmin = 3.0°
Absorption correction: multi-scan
(ABSCOR; Higashi, 1995)
h = 2920
Tmin = 0.262, Tmax = 0.281k = 1818
69256 measured reflectionsl = 3536
Refinement top
Refinement on F2Primary atom site location: structure-invariant direct methods
Least-squares matrix: fullSecondary atom site location: difference Fourier map
R[F2 > 2σ(F2)] = 0.039Hydrogen site location: inferred from neighbouring sites
wR(F2) = 0.089H-atom parameters constrained
S = 1.14 w = 1/[σ2(Fo2) + (0.0341P)2 + 13.8363P]
where P = (Fo2 + 2Fc2)/3
19520 reflections(Δ/σ)max = 0.009
950 parametersΔρmax = 1.20 e Å3
0 restraintsΔρmin = 1.36 e Å3
Crystal data top
[Ag4W2S8(C25H22P2)3]·2C3H7NOV = 8565.6 (14) Å3
Mr = 2354.95Z = 4
Monoclinic, P21/cMo Kα radiation
a = 22.931 (2) ŵ = 3.93 mm1
b = 14.0395 (12) ÅT = 93 K
c = 27.855 (3) Å0.47 × 0.43 × 0.43 mm
β = 107.224 (1)°
Data collection top
Rigaku R-AXIS RAPID
diffractometer
19520 independent reflections
Absorption correction: multi-scan
(ABSCOR; Higashi, 1995)
18777 reflections with I > 2σ(I)
Tmin = 0.262, Tmax = 0.281Rint = 0.045
69256 measured reflectionsθmax = 27.5°
Refinement top
R[F2 > 2σ(F2)] = 0.039 w = 1/[σ2(Fo2) + (0.0341P)2 + 13.8363P]
where P = (Fo2 + 2Fc2)/3
wR(F2) = 0.089Δρmax = 1.20 e Å3
S = 1.14Δρmin = 1.36 e Å3
19520 reflectionsAbsolute structure: ?
950 parametersFlack parameter: ?
0 restraintsRogers parameter: ?
H-atom parameters constrained
Special details top

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.

Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top
xyzUiso*/Ueq
W10.685156 (8)0.527538 (12)0.590934 (6)0.00959 (5)
W20.828154 (8)0.329261 (13)0.458854 (7)0.01383 (5)
Ag10.701283 (16)0.55717 (2)0.490031 (13)0.01578 (7)
Ag20.797387 (15)0.41531 (2)0.598751 (13)0.01418 (7)
Ag30.776781 (15)0.20725 (2)0.532723 (12)0.01373 (7)
Ag40.693052 (15)0.34050 (2)0.401396 (12)0.01168 (7)
S10.60897 (5)0.52790 (8)0.52055 (4)0.0157 (2)
S20.77015 (5)0.59208 (8)0.57931 (4)0.0129 (2)
S30.70064 (5)0.37936 (8)0.62017 (4)0.0136 (2)
S40.65859 (5)0.61359 (8)0.64489 (4)0.0154 (2)
S50.75460 (5)0.37745 (8)0.49394 (4)0.0136 (2)
S60.84065 (6)0.17432 (9)0.46535 (5)0.0247 (3)
S70.79958 (5)0.36970 (9)0.37903 (4)0.0156 (2)
S80.91157 (6)0.40177 (12)0.49661 (5)0.0332 (3)
P10.70165 (5)0.64377 (8)0.41615 (4)0.0122 (2)
P20.90214 (5)0.37198 (8)0.63471 (4)0.0119 (2)
P30.86722 (5)0.16721 (8)0.60311 (4)0.0123 (2)
P40.68282 (5)0.11687 (8)0.49608 (4)0.0110 (2)
P50.65584 (5)0.17597 (8)0.38414 (4)0.0100 (2)
P60.64487 (5)0.47428 (8)0.34787 (4)0.0112 (2)
C10.7730 (2)0.7088 (3)0.42479 (17)0.0187 (10)
C20.8271 (2)0.6582 (4)0.4461 (2)0.0272 (12)
H20.82550.59420.45670.033*
C30.8832 (3)0.7019 (5)0.4518 (2)0.0370 (15)
H30.92000.66730.46550.044*
C40.8853 (3)0.7961 (5)0.4374 (2)0.0437 (18)
H40.92360.82580.44120.052*
C50.8326 (3)0.8468 (5)0.4178 (2)0.0433 (17)
H50.83450.91180.40900.052*
C60.7761 (3)0.8030 (4)0.4107 (2)0.0288 (12)
H60.73960.83770.39620.035*
C70.6402 (2)0.7312 (3)0.39761 (17)0.0153 (9)
C80.6100 (2)0.7549 (3)0.43287 (19)0.0203 (10)
H80.62200.72560.46510.024*
C90.5629 (3)0.8202 (4)0.4214 (2)0.0282 (12)
H90.54310.83700.44570.034*
C100.5449 (2)0.8609 (4)0.3743 (2)0.0281 (12)
H100.51210.90510.36610.034*
C110.5742 (3)0.8380 (4)0.3387 (2)0.0257 (11)
H110.56120.86650.30640.031*
C120.6221 (2)0.7741 (3)0.35032 (18)0.0191 (10)
H120.64260.75940.32620.023*
C130.6964 (2)0.5780 (3)0.35824 (16)0.0130 (9)
H13A0.73780.55600.35920.016*
H13B0.68200.62200.32930.016*
C140.5696 (2)0.5181 (3)0.34616 (17)0.0141 (9)
C150.5491 (2)0.5052 (3)0.38825 (17)0.0155 (9)
H150.57480.47520.41740.019*
C160.4916 (2)0.5358 (3)0.38777 (19)0.0201 (10)
H160.47860.52780.41680.024*
C170.4532 (2)0.5778 (3)0.3455 (2)0.0224 (11)
H170.41360.59780.34530.027*
C180.4728 (2)0.5907 (4)0.30313 (19)0.0236 (11)
H180.44640.61930.27380.028*
C190.5311 (2)0.5619 (3)0.30380 (19)0.0196 (10)
H190.54460.57220.27510.024*
C200.6363 (2)0.4418 (3)0.28259 (18)0.0152 (9)
C210.6730 (2)0.4792 (3)0.25509 (17)0.0169 (9)
H210.70170.52780.26940.020*
C220.6680 (2)0.4458 (4)0.20679 (19)0.0234 (11)
H220.69280.47190.18820.028*
C230.6265 (2)0.3743 (4)0.18612 (19)0.0256 (11)
H230.62300.35150.15330.031*
C240.5905 (3)0.3362 (4)0.21297 (19)0.0269 (12)
H240.56300.28600.19890.032*
C250.5941 (2)0.3709 (3)0.26080 (18)0.0201 (10)
H250.56780.34620.27850.024*
C260.57227 (19)0.1766 (3)0.36167 (16)0.0112 (8)
C270.5416 (2)0.2602 (3)0.36530 (18)0.0173 (9)
H270.56440.31440.38070.021*
C280.4787 (2)0.2666 (4)0.3470 (2)0.0244 (11)
H280.45870.32480.34960.029*
C290.4448 (2)0.1873 (4)0.32495 (19)0.0215 (10)
H290.40160.19130.31180.026*
C300.4751 (2)0.1017 (3)0.32236 (18)0.0189 (10)
H300.45220.04650.30870.023*
C310.5378 (2)0.0973 (3)0.33959 (17)0.0173 (9)
H310.55800.03950.33640.021*
C320.6776 (2)0.1222 (3)0.33224 (16)0.0114 (8)
C330.6938 (2)0.1824 (3)0.29875 (17)0.0162 (9)
H330.69650.24910.30490.019*
C340.7063 (2)0.1462 (4)0.25613 (18)0.0201 (10)
H340.71690.18800.23330.024*
C350.7029 (2)0.0485 (4)0.24736 (18)0.0209 (10)
H350.71130.02360.21840.025*
C360.6874 (2)0.0127 (3)0.28086 (18)0.0200 (10)
H360.68480.07930.27470.024*
C370.6757 (2)0.0242 (3)0.32364 (18)0.0183 (10)
H370.66640.01780.34710.022*
C380.6761 (2)0.0792 (3)0.43110 (16)0.0134 (9)
H38A0.71540.05110.43040.016*
H38B0.64460.02880.42120.016*
C390.6064 (2)0.1611 (3)0.49084 (16)0.0119 (8)
C400.5981 (2)0.2566 (3)0.50130 (18)0.0187 (10)
H400.63240.29700.51430.022*
C410.5393 (2)0.2920 (4)0.4926 (2)0.0233 (11)
H410.53350.35680.49980.028*
C420.4894 (2)0.2340 (4)0.4736 (2)0.0248 (11)
H420.44940.25940.46720.030*
C430.4970 (2)0.1386 (4)0.46372 (18)0.0193 (10)
H430.46240.09850.45130.023*
C440.5557 (2)0.1020 (3)0.47208 (17)0.0159 (9)
H440.56120.03700.46500.019*
C450.6863 (2)0.0014 (3)0.52730 (17)0.0144 (9)
C460.7188 (2)0.0738 (3)0.51465 (18)0.0198 (10)
H460.73710.06620.48850.024*
C470.7243 (3)0.1603 (4)0.54060 (19)0.0254 (11)
H470.74600.21170.53180.030*
C480.6979 (2)0.1708 (4)0.57924 (19)0.0245 (11)
H480.70160.22950.59680.029*
C490.6666 (2)0.0966 (4)0.59207 (19)0.0246 (11)
H490.64860.10440.61850.030*
C500.6608 (2)0.0102 (4)0.56679 (18)0.0204 (10)
H500.63950.04100.57630.024*
C510.9045 (2)0.0612 (3)0.58746 (16)0.0156 (9)
C520.8728 (3)0.0241 (4)0.5823 (2)0.0297 (12)
H520.83450.02650.58900.036*
C530.8965 (3)0.1062 (4)0.5675 (2)0.0377 (15)
H530.87440.16430.56380.045*
C540.9519 (3)0.1034 (4)0.5582 (2)0.0327 (13)
H540.96820.15970.54830.039*
C550.9841 (3)0.0190 (4)0.5631 (2)0.0297 (12)
H551.02230.01710.55630.036*
C560.9603 (2)0.0633 (4)0.5781 (2)0.0246 (11)
H560.98260.12120.58190.030*
C570.8633 (2)0.1414 (3)0.66613 (17)0.0137 (9)
C580.9155 (2)0.1100 (3)0.70346 (17)0.0182 (10)
H580.95180.09620.69500.022*
C590.9142 (2)0.0992 (4)0.75240 (18)0.0200 (10)
H590.94960.07770.77750.024*
C600.8614 (2)0.1197 (4)0.76500 (18)0.0209 (10)
H600.86100.11320.79890.025*
C610.8097 (2)0.1492 (3)0.72898 (19)0.0188 (10)
H610.77370.16280.73790.023*
C620.8100 (2)0.1593 (3)0.67889 (18)0.0170 (9)
H620.77390.17830.65380.020*
C630.92682 (19)0.2589 (3)0.61403 (16)0.0116 (8)
H63A0.96380.23600.63990.014*
H63B0.93770.26950.58260.014*
C640.9232 (2)0.3680 (3)0.70338 (17)0.0138 (9)
C650.9833 (2)0.3707 (4)0.73330 (18)0.0212 (10)
H651.01530.37000.71810.025*
C660.9974 (2)0.3745 (4)0.78542 (19)0.0251 (11)
H661.03880.37870.80550.030*
C670.9514 (3)0.3723 (4)0.80778 (19)0.0286 (12)
H670.96120.37390.84340.034*
C680.8912 (3)0.3677 (4)0.77874 (19)0.0277 (12)
H680.85950.36580.79430.033*
C690.8771 (2)0.3658 (3)0.72647 (18)0.0191 (10)
H690.83570.36300.70650.023*
C700.9557 (2)0.4595 (3)0.62351 (17)0.0142 (9)
C711.0132 (2)0.4363 (3)0.61976 (17)0.0153 (9)
H711.02640.37180.62270.018*
C721.0514 (2)0.5073 (3)0.61178 (17)0.0173 (9)
H721.09040.49130.60870.021*
C731.0329 (2)0.6012 (4)0.60827 (18)0.0205 (10)
H731.05930.64960.60300.025*
C740.9756 (2)0.6252 (4)0.61239 (19)0.0226 (11)
H740.96330.69000.61080.027*
C750.9368 (2)0.5540 (3)0.61882 (19)0.0193 (10)
H750.89700.56990.62000.023*
O10.71217 (18)0.7272 (3)0.26992 (15)0.0286 (9)
N10.78968 (19)0.6532 (3)0.24912 (16)0.0215 (9)
C760.7377 (2)0.7023 (3)0.2391 (2)0.0230 (11)
H760.71880.71960.20500.028*
C770.8220 (2)0.6244 (4)0.3001 (2)0.0287 (12)
H77A0.80740.66210.32390.043*
H77B0.86590.63500.30650.043*
H77C0.81450.55670.30440.043*
C780.8173 (3)0.6276 (4)0.2097 (2)0.0303 (12)
H78A0.79210.65250.17730.045*
H78B0.81990.55810.20780.045*
H78C0.85830.65500.21770.045*
O20.9365 (2)0.6952 (4)0.83007 (18)0.0508 (13)
N20.8745 (2)0.6405 (3)0.75669 (18)0.0266 (10)
C790.8866 (3)0.6654 (4)0.8036 (2)0.0352 (14)
H790.85460.66040.81860.042*
C800.9225 (3)0.6454 (5)0.7310 (3)0.0405 (15)
H80A0.95870.67720.75300.061*
H80B0.90720.68150.69970.061*
H80C0.93340.58080.72350.061*
C810.8168 (3)0.6078 (5)0.7255 (3)0.0424 (16)
H81A0.78740.60680.74480.064*
H81B0.82130.54340.71350.064*
H81C0.80210.65070.69660.064*
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
W10.00959 (9)0.01051 (8)0.00897 (8)0.00050 (6)0.00322 (7)0.00076 (6)
W20.01041 (9)0.02124 (10)0.00953 (9)0.00198 (7)0.00248 (7)0.00324 (7)
Ag10.01769 (18)0.01876 (17)0.01144 (16)0.00004 (13)0.00515 (13)0.00419 (13)
Ag20.00979 (16)0.01623 (16)0.01571 (17)0.00196 (12)0.00253 (13)0.00284 (13)
Ag30.01196 (17)0.01387 (16)0.01320 (16)0.00216 (12)0.00038 (13)0.00199 (12)
Ag40.01172 (16)0.01111 (15)0.01114 (15)0.00089 (12)0.00175 (12)0.00073 (12)
S10.0119 (5)0.0230 (6)0.0107 (5)0.0008 (4)0.0009 (4)0.0018 (4)
S20.0118 (5)0.0124 (5)0.0151 (5)0.0015 (4)0.0049 (4)0.0014 (4)
S30.0149 (5)0.0121 (5)0.0154 (5)0.0014 (4)0.0069 (4)0.0030 (4)
S40.0166 (6)0.0149 (5)0.0165 (5)0.0016 (4)0.0077 (4)0.0022 (4)
S50.0178 (6)0.0134 (5)0.0100 (5)0.0002 (4)0.0047 (4)0.0002 (4)
S60.0313 (7)0.0250 (6)0.0236 (6)0.0131 (5)0.0168 (6)0.0079 (5)
S70.0139 (6)0.0241 (6)0.0093 (5)0.0017 (4)0.0043 (4)0.0032 (4)
S80.0199 (7)0.0608 (10)0.0151 (6)0.0208 (6)0.0006 (5)0.0056 (6)
P10.0146 (6)0.0116 (5)0.0102 (5)0.0019 (4)0.0036 (4)0.0007 (4)
P20.0103 (5)0.0127 (5)0.0118 (5)0.0002 (4)0.0019 (4)0.0012 (4)
P30.0126 (6)0.0123 (5)0.0105 (5)0.0008 (4)0.0012 (4)0.0014 (4)
P40.0119 (5)0.0107 (5)0.0099 (5)0.0015 (4)0.0026 (4)0.0009 (4)
P50.0110 (5)0.0100 (5)0.0089 (5)0.0003 (4)0.0027 (4)0.0002 (4)
P60.0111 (6)0.0112 (5)0.0111 (5)0.0000 (4)0.0032 (4)0.0017 (4)
C10.024 (3)0.021 (2)0.014 (2)0.0047 (19)0.0099 (19)0.0057 (19)
C20.020 (3)0.031 (3)0.030 (3)0.004 (2)0.006 (2)0.009 (2)
C30.021 (3)0.056 (4)0.034 (3)0.010 (3)0.007 (2)0.016 (3)
C40.039 (4)0.067 (5)0.032 (3)0.035 (3)0.020 (3)0.021 (3)
C50.050 (4)0.041 (4)0.040 (4)0.030 (3)0.016 (3)0.005 (3)
C60.034 (3)0.027 (3)0.025 (3)0.015 (2)0.009 (2)0.003 (2)
C70.018 (2)0.011 (2)0.017 (2)0.0027 (17)0.0049 (19)0.0010 (17)
C80.025 (3)0.016 (2)0.021 (2)0.0004 (19)0.010 (2)0.0008 (19)
C90.032 (3)0.022 (3)0.036 (3)0.004 (2)0.019 (3)0.004 (2)
C100.024 (3)0.022 (3)0.039 (3)0.004 (2)0.009 (2)0.005 (2)
C110.029 (3)0.019 (2)0.029 (3)0.002 (2)0.008 (2)0.006 (2)
C120.028 (3)0.015 (2)0.015 (2)0.0009 (19)0.008 (2)0.0018 (18)
C130.014 (2)0.014 (2)0.010 (2)0.0012 (17)0.0027 (17)0.0031 (17)
C140.015 (2)0.014 (2)0.015 (2)0.0031 (17)0.0063 (18)0.0027 (17)
C150.015 (2)0.015 (2)0.016 (2)0.0023 (17)0.0044 (18)0.0044 (18)
C160.018 (3)0.024 (3)0.019 (2)0.0012 (19)0.008 (2)0.003 (2)
C170.015 (2)0.020 (2)0.034 (3)0.0037 (19)0.009 (2)0.001 (2)
C180.020 (3)0.026 (3)0.021 (3)0.004 (2)0.000 (2)0.004 (2)
C190.019 (3)0.021 (2)0.021 (2)0.0055 (19)0.008 (2)0.006 (2)
C200.014 (2)0.010 (2)0.020 (2)0.0033 (17)0.0036 (18)0.0031 (18)
C210.013 (2)0.022 (2)0.015 (2)0.0022 (18)0.0031 (18)0.0002 (18)
C220.023 (3)0.032 (3)0.016 (2)0.009 (2)0.007 (2)0.001 (2)
C230.031 (3)0.028 (3)0.014 (2)0.003 (2)0.001 (2)0.003 (2)
C240.042 (3)0.015 (2)0.017 (2)0.005 (2)0.002 (2)0.0003 (19)
C250.025 (3)0.016 (2)0.016 (2)0.0064 (19)0.000 (2)0.0033 (18)
C260.009 (2)0.017 (2)0.0078 (19)0.0001 (16)0.0029 (16)0.0040 (16)
C270.018 (2)0.016 (2)0.019 (2)0.0002 (18)0.0084 (19)0.0023 (18)
C280.019 (3)0.020 (2)0.037 (3)0.005 (2)0.012 (2)0.000 (2)
C290.011 (2)0.033 (3)0.022 (3)0.002 (2)0.0048 (19)0.002 (2)
C300.018 (2)0.021 (2)0.017 (2)0.0063 (19)0.0049 (19)0.0068 (19)
C310.019 (2)0.018 (2)0.014 (2)0.0008 (18)0.0030 (19)0.0003 (18)
C320.013 (2)0.012 (2)0.0088 (19)0.0016 (16)0.0031 (16)0.0014 (16)
C330.018 (2)0.014 (2)0.017 (2)0.0010 (17)0.0056 (19)0.0008 (18)
C340.020 (3)0.026 (3)0.017 (2)0.003 (2)0.010 (2)0.002 (2)
C350.024 (3)0.027 (3)0.013 (2)0.000 (2)0.007 (2)0.004 (2)
C360.028 (3)0.011 (2)0.020 (2)0.0032 (19)0.006 (2)0.0052 (18)
C370.025 (3)0.017 (2)0.014 (2)0.0002 (19)0.007 (2)0.0025 (18)
C380.016 (2)0.012 (2)0.012 (2)0.0024 (17)0.0048 (18)0.0011 (17)
C390.011 (2)0.017 (2)0.0081 (19)0.0030 (16)0.0038 (16)0.0013 (16)
C400.018 (2)0.017 (2)0.019 (2)0.0022 (18)0.0034 (19)0.0039 (19)
C410.023 (3)0.017 (2)0.033 (3)0.003 (2)0.013 (2)0.002 (2)
C420.018 (3)0.033 (3)0.025 (3)0.003 (2)0.009 (2)0.003 (2)
C430.015 (2)0.023 (2)0.019 (2)0.0064 (19)0.0053 (19)0.005 (2)
C440.017 (2)0.017 (2)0.015 (2)0.0040 (18)0.0071 (18)0.0027 (18)
C450.013 (2)0.018 (2)0.012 (2)0.0051 (17)0.0032 (17)0.0018 (17)
C460.028 (3)0.017 (2)0.015 (2)0.0001 (19)0.006 (2)0.0006 (18)
C470.037 (3)0.017 (2)0.018 (2)0.000 (2)0.001 (2)0.001 (2)
C480.030 (3)0.018 (2)0.019 (3)0.006 (2)0.003 (2)0.002 (2)
C490.027 (3)0.030 (3)0.017 (2)0.006 (2)0.007 (2)0.009 (2)
C500.024 (3)0.024 (2)0.015 (2)0.001 (2)0.007 (2)0.0054 (19)
C510.019 (2)0.014 (2)0.010 (2)0.0035 (18)0.0017 (18)0.0002 (17)
C520.028 (3)0.023 (3)0.037 (3)0.000 (2)0.008 (3)0.003 (2)
C530.044 (4)0.015 (3)0.051 (4)0.004 (2)0.008 (3)0.012 (3)
C540.050 (4)0.024 (3)0.020 (3)0.011 (3)0.003 (3)0.008 (2)
C550.034 (3)0.027 (3)0.029 (3)0.013 (2)0.011 (2)0.004 (2)
C560.027 (3)0.020 (2)0.029 (3)0.004 (2)0.011 (2)0.003 (2)
C570.014 (2)0.013 (2)0.013 (2)0.0018 (17)0.0026 (17)0.0019 (17)
C580.015 (2)0.026 (2)0.014 (2)0.0007 (19)0.0050 (18)0.0014 (19)
C590.019 (3)0.025 (3)0.013 (2)0.001 (2)0.0019 (19)0.0066 (19)
C600.026 (3)0.024 (2)0.014 (2)0.002 (2)0.009 (2)0.0015 (19)
C610.018 (2)0.018 (2)0.024 (3)0.0007 (18)0.013 (2)0.0030 (19)
C620.014 (2)0.015 (2)0.022 (2)0.0009 (17)0.0066 (19)0.0015 (18)
C630.008 (2)0.016 (2)0.012 (2)0.0002 (16)0.0050 (16)0.0009 (17)
C640.017 (2)0.0093 (19)0.013 (2)0.0019 (17)0.0017 (18)0.0012 (16)
C650.018 (3)0.027 (3)0.016 (2)0.002 (2)0.0018 (19)0.001 (2)
C660.020 (3)0.030 (3)0.019 (2)0.002 (2)0.005 (2)0.001 (2)
C670.035 (3)0.036 (3)0.011 (2)0.002 (2)0.001 (2)0.005 (2)
C680.034 (3)0.036 (3)0.017 (3)0.005 (2)0.013 (2)0.006 (2)
C690.018 (2)0.021 (2)0.018 (2)0.0015 (19)0.0045 (19)0.0052 (19)
C700.012 (2)0.017 (2)0.012 (2)0.0031 (17)0.0015 (17)0.0004 (17)
C710.013 (2)0.017 (2)0.014 (2)0.0020 (17)0.0021 (18)0.0007 (18)
C720.016 (2)0.024 (2)0.015 (2)0.0050 (19)0.0088 (19)0.0020 (19)
C730.021 (3)0.023 (2)0.016 (2)0.008 (2)0.004 (2)0.0018 (19)
C740.021 (3)0.017 (2)0.027 (3)0.0029 (19)0.004 (2)0.004 (2)
C750.010 (2)0.018 (2)0.028 (3)0.0020 (18)0.0035 (19)0.001 (2)
O10.031 (2)0.0237 (19)0.035 (2)0.0058 (16)0.0170 (18)0.0087 (17)
N10.020 (2)0.022 (2)0.023 (2)0.0003 (17)0.0074 (18)0.0044 (18)
C760.021 (3)0.017 (2)0.031 (3)0.0007 (19)0.009 (2)0.012 (2)
C770.022 (3)0.034 (3)0.026 (3)0.001 (2)0.001 (2)0.008 (2)
C780.029 (3)0.028 (3)0.037 (3)0.006 (2)0.014 (3)0.004 (2)
O20.026 (2)0.071 (3)0.043 (3)0.006 (2)0.008 (2)0.016 (3)
N20.017 (2)0.028 (2)0.032 (3)0.0030 (18)0.0038 (19)0.007 (2)
C790.029 (3)0.043 (4)0.032 (3)0.004 (3)0.005 (3)0.001 (3)
C800.039 (4)0.045 (4)0.043 (4)0.001 (3)0.020 (3)0.006 (3)
C810.027 (3)0.034 (3)0.056 (4)0.002 (3)0.003 (3)0.016 (3)
Geometric parameters (Å, °) top
W1—S42.1523 (11)C32—C331.390 (6)
W1—S12.2062 (11)C32—C371.395 (6)
W1—S32.2240 (11)C33—C341.396 (6)
W1—S22.2579 (11)C33—H330.9500
W1—Ag22.9701 (4)C34—C351.391 (7)
W1—Ag12.9707 (5)C34—H340.9500
W2—S82.1470 (13)C35—C361.390 (7)
W2—S62.1945 (13)C35—H350.9500
W2—S72.1985 (11)C36—C371.396 (6)
W2—S52.2878 (11)C36—H360.9500
W2—Ag43.0410 (4)C37—H370.9500
W2—Ag33.1609 (4)C38—H38A0.9900
Ag1—P12.3924 (12)C38—H38B0.9900
Ag1—S12.5374 (12)C39—C401.396 (6)
Ag1—S22.5677 (12)C39—C441.398 (6)
Ag1—S52.7919 (12)C40—C411.390 (7)
Ag2—P22.3914 (12)C40—H400.9500
Ag2—S32.5132 (11)C41—C421.376 (7)
Ag2—S22.5772 (11)C41—H410.9500
Ag2—S52.8412 (12)C42—C431.389 (7)
Ag3—P42.4478 (12)C42—H420.9500
Ag3—P32.4602 (12)C43—C441.394 (7)
Ag3—S52.6096 (12)C43—H430.9500
Ag3—S62.7403 (13)C44—H440.9500
Ag4—P62.4485 (12)C45—C461.396 (7)
Ag4—P52.4601 (11)C45—C501.400 (6)
Ag4—S52.5984 (12)C46—C471.400 (7)
Ag4—S72.7248 (12)C46—H460.9500
P1—C11.826 (5)C47—C481.390 (8)
P1—C71.824 (5)C47—H470.9500
P1—C131.831 (4)C48—C491.371 (8)
P2—C701.829 (5)C48—H480.9500
P2—C641.830 (5)C49—C501.389 (7)
P2—C631.835 (4)C49—H490.9500
P3—C571.820 (5)C50—H500.9500
P3—C511.831 (5)C51—C561.380 (7)
P3—C631.836 (4)C51—C521.387 (7)
P4—C391.823 (5)C52—C531.390 (8)
P4—C451.830 (5)C52—H520.9500
P4—C381.848 (4)C53—C541.369 (9)
P5—C321.826 (4)C53—H530.9500
P5—C261.832 (4)C54—C551.381 (8)
P5—C381.847 (4)C54—H540.9500
P6—C141.820 (5)C55—C561.394 (7)
P6—C201.828 (5)C55—H550.9500
P6—C131.844 (4)C56—H560.9500
C1—C61.387 (7)C57—C621.395 (6)
C1—C21.399 (7)C57—C581.403 (6)
C2—C31.392 (8)C58—C591.381 (6)
C2—H20.9500C58—H580.9500
C3—C41.386 (10)C59—C601.387 (7)
C3—H30.9500C59—H590.9500
C4—C51.369 (10)C60—C611.371 (7)
C4—H40.9500C60—H600.9500
C5—C61.394 (8)C61—C621.404 (7)
C5—H50.9500C61—H610.9500
C6—H60.9500C62—H620.9500
C7—C121.395 (6)C63—H63A0.9900
C7—C81.400 (6)C63—H63B0.9900
C8—C91.380 (7)C64—C691.389 (6)
C8—H80.9500C64—C651.385 (7)
C9—C101.376 (8)C65—C661.392 (7)
C9—H90.9500C65—H650.9500
C10—C111.388 (8)C66—C671.375 (8)
C10—H100.9500C66—H660.9500
C11—C121.381 (7)C67—C681.380 (8)
C11—H110.9500C67—H670.9500
C12—H120.9500C68—C691.395 (7)
C13—H13A0.9900C68—H680.9500
C13—H13B0.9900C69—H690.9500
C14—C191.390 (7)C70—C711.392 (6)
C14—C151.399 (6)C70—C751.390 (6)
C15—C161.381 (7)C71—C721.388 (6)
C15—H150.9500C71—H710.9500
C16—C171.376 (7)C72—C731.378 (7)
C16—H160.9500C72—H720.9500
C17—C181.394 (7)C73—C741.394 (7)
C17—H170.9500C73—H730.9500
C18—C191.390 (7)C74—C751.385 (6)
C18—H180.9500C74—H740.9500
C19—H190.9500C75—H750.9500
C20—C211.398 (6)O1—C761.224 (6)
C20—C251.396 (6)N1—C761.333 (6)
C21—C221.397 (6)N1—C771.452 (6)
C21—H210.9500N1—C781.465 (7)
C22—C231.384 (8)C76—H760.9500
C22—H220.9500C77—H77A0.9800
C23—C241.376 (8)C77—H77B0.9800
C23—H230.9500C77—H77C0.9800
C24—C251.398 (7)C78—H78A0.9800
C24—H240.9500C78—H78B0.9800
C25—H250.9500C78—H78C0.9800
C26—C271.387 (6)O2—C791.237 (7)
C26—C311.399 (6)N2—C791.300 (7)
C27—C281.383 (7)N2—C811.427 (7)
C27—H270.9500N2—C801.481 (7)
C28—C291.392 (7)C79—H790.9500
C28—H280.9500C80—H80A0.9800
C29—C301.401 (7)C80—H80B0.9800
C29—H290.9500C80—H80C0.9800
C30—C311.376 (7)C81—H81A0.9800
C30—H300.9500C81—H81B0.9800
C31—H310.9500C81—H81C0.9800
S4—W1—S1107.81 (4)C25—C24—H24119.8
S4—W1—S3108.47 (4)C20—C25—C24120.0 (5)
S1—W1—S3109.03 (4)C20—C25—H25120.0
S4—W1—S2108.04 (4)C24—C25—H25120.0
S1—W1—S2111.20 (4)C27—C26—C31118.3 (4)
S3—W1—S2112.14 (4)C27—C26—P5118.7 (3)
S4—W1—Ag2131.67 (3)C31—C26—P5123.0 (3)
S1—W1—Ag2120.49 (3)C28—C27—C26121.5 (5)
S3—W1—Ag255.67 (3)C28—C27—H27119.2
S2—W1—Ag257.14 (3)C26—C27—H27119.2
S4—W1—Ag1136.25 (3)C27—C28—C29119.8 (5)
S1—W1—Ag156.40 (3)C27—C28—H28120.1
S3—W1—Ag1115.24 (3)C29—C28—H28120.1
S2—W1—Ag156.88 (3)C28—C29—C30119.2 (5)
Ag2—W1—Ag178.214 (10)C28—C29—H29120.4
S8—W2—S6110.73 (6)C30—C29—H29120.4
S8—W2—S7109.18 (5)C31—C30—C29120.2 (4)
S6—W2—S7109.38 (5)C31—C30—H30119.9
S8—W2—S5108.25 (5)C29—C30—H30119.9
S6—W2—S5110.66 (4)C30—C31—C26120.9 (4)
S7—W2—S5108.61 (4)C30—C31—H31119.5
S8—W2—Ag4148.67 (5)C26—C31—H31119.5
S6—W2—Ag4100.53 (4)C33—C32—C37119.0 (4)
S7—W2—Ag460.14 (3)C33—C32—P5118.1 (3)
S5—W2—Ag456.25 (3)C37—C32—P5122.8 (3)
S8—W2—Ag3112.82 (4)C32—C33—C34120.8 (4)
S6—W2—Ag358.26 (3)C32—C33—H33119.6
S7—W2—Ag3137.85 (3)C34—C33—H33119.6
S5—W2—Ag354.42 (3)C33—C34—C35119.6 (4)
Ag4—W2—Ag381.533 (11)C33—C34—H34120.2
P1—Ag1—S1125.90 (4)C35—C34—H34120.2
P1—Ag1—S2125.34 (4)C36—C35—C34120.2 (4)
S1—Ag1—S292.36 (4)C36—C35—H35119.9
P1—Ag1—S5112.32 (4)C34—C35—H35119.9
S1—Ag1—S5103.87 (4)C35—C36—C37119.7 (4)
S2—Ag1—S589.89 (3)C35—C36—H36120.2
P1—Ag1—W1156.66 (3)C37—C36—H36120.2
S1—Ag1—W146.40 (3)C32—C37—C36120.6 (4)
S2—Ag1—W147.43 (2)C32—C37—H37119.7
S5—Ag1—W190.70 (2)C36—C37—H37119.7
P2—Ag2—S3134.21 (4)P5—C38—P4114.5 (2)
P2—Ag2—S2118.94 (4)P5—C38—H38A108.6
S3—Ag2—S293.86 (4)P4—C38—H38A108.6
P2—Ag2—S5112.41 (4)P5—C38—H38B108.6
S3—Ag2—S598.39 (4)P4—C38—H38B108.6
S2—Ag2—S588.61 (3)H38A—C38—H38B107.6
P2—Ag2—W1155.06 (3)C40—C39—C44119.8 (4)
S3—Ag2—W146.95 (3)C40—C39—P4119.9 (3)
S2—Ag2—W147.38 (2)C44—C39—P4120.1 (3)
S5—Ag2—W189.76 (2)C41—C40—C39119.5 (4)
P4—Ag3—P3130.09 (4)C41—C40—H40120.3
P4—Ag3—S5105.22 (4)C39—C40—H40120.3
P3—Ag3—S5123.65 (4)C42—C41—C40120.6 (5)
P4—Ag3—S6102.12 (4)C42—C41—H41119.7
P3—Ag3—S690.68 (4)C40—C41—H41119.7
S5—Ag3—S687.08 (4)C41—C42—C43120.5 (5)
P4—Ag3—W2117.46 (3)C41—C42—H42119.8
P3—Ag3—W2104.71 (3)C43—C42—H42119.8
S5—Ag3—W245.48 (2)C42—C43—C44119.6 (4)
S6—Ag3—W242.93 (3)C42—C43—H43120.2
P6—Ag4—P5122.24 (4)C44—C43—H43120.2
P6—Ag4—S5117.74 (4)C39—C44—C43120.0 (4)
P5—Ag4—S5115.87 (4)C39—C44—H44120.0
P6—Ag4—S791.08 (4)C43—C44—H44120.0
P5—Ag4—S7112.28 (4)C46—C45—C50119.2 (4)
S5—Ag4—S786.36 (4)C46—C45—P4120.1 (3)
P6—Ag4—W2124.47 (3)C50—C45—P4120.5 (4)
P5—Ag4—W2107.12 (3)C45—C46—C47119.9 (5)
S5—Ag4—W247.06 (3)C45—C46—H46120.0
S7—Ag4—W244.41 (2)C47—C46—H46120.0
W1—S1—Ag177.20 (4)C48—C47—C46119.9 (5)
W1—S2—Ag175.69 (3)C48—C47—H47120.0
W1—S2—Ag275.48 (3)C46—C47—H47120.0
Ag1—S2—Ag293.50 (4)C49—C48—C47120.2 (5)
W1—S3—Ag277.39 (3)C49—C48—H48119.9
W2—S5—Ag476.69 (3)C47—C48—H48119.9
W2—S5—Ag380.10 (3)C48—C49—C50120.7 (5)
Ag4—S5—Ag3102.12 (4)C48—C49—H49119.7
W2—S5—Ag1128.34 (4)C50—C49—H49119.7
Ag4—S5—Ag192.22 (4)C49—C50—C45120.0 (5)
Ag3—S5—Ag1150.82 (5)C49—C50—H50120.0
W2—S5—Ag2114.86 (4)C45—C50—H50120.0
Ag4—S5—Ag2167.86 (5)C56—C51—C52119.1 (5)
Ag3—S5—Ag277.31 (3)C56—C51—P3123.5 (4)
Ag1—S5—Ag283.40 (3)C52—C51—P3117.4 (4)
W2—S6—Ag378.81 (4)C51—C52—C53120.6 (6)
W2—S7—Ag475.45 (3)C51—C52—H52119.7
C1—P1—C7106.7 (2)C53—C52—H52119.7
C1—P1—C13101.0 (2)C54—C53—C52119.9 (5)
C7—P1—C13104.3 (2)C54—C53—H53120.0
C1—P1—Ag1111.83 (16)C52—C53—H53120.0
C7—P1—Ag1112.73 (15)C53—C54—C55120.3 (5)
C13—P1—Ag1119.05 (14)C53—C54—H54119.8
C70—P2—C64102.5 (2)C55—C54—H54119.8
C70—P2—C63104.0 (2)C56—C55—C54119.7 (6)
C64—P2—C63106.9 (2)C56—C55—H55120.1
C70—P2—Ag2113.57 (15)C54—C55—H55120.1
C64—P2—Ag2111.52 (15)C51—C56—C55120.4 (5)
C63—P2—Ag2116.97 (15)C51—C56—H56119.8
C57—P3—C51103.1 (2)C55—C56—H56119.8
C57—P3—C63103.1 (2)C62—C57—C58119.2 (4)
C51—P3—C63103.4 (2)C62—C57—P3120.5 (3)
C57—P3—Ag3122.93 (15)C58—C57—P3120.2 (3)
C51—P3—Ag3109.79 (15)C59—C58—C57120.2 (4)
C63—P3—Ag3112.48 (15)C59—C58—H58119.9
C39—P4—C45104.2 (2)C57—C58—H58119.9
C39—P4—C38102.7 (2)C58—C59—C60120.2 (5)
C45—P4—C38101.0 (2)C58—C59—H59119.9
C39—P4—Ag3124.25 (15)C60—C59—H59119.9
C45—P4—Ag3110.63 (15)C61—C60—C59120.5 (4)
C38—P4—Ag3111.39 (15)C61—C60—H60119.7
C32—P5—C26103.6 (2)C59—C60—H60119.7
C32—P5—C38100.7 (2)C60—C61—C62120.1 (4)
C26—P5—C38105.3 (2)C60—C61—H61120.0
C32—P5—Ag4112.51 (15)C62—C61—H61120.0
C26—P5—Ag4109.23 (15)C57—C62—C61119.8 (4)
C38—P5—Ag4123.52 (15)C57—C62—H62120.1
C14—P6—C20103.7 (2)C61—C62—H62120.1
C14—P6—C13107.2 (2)P2—C63—P3112.0 (2)
C20—P6—C13103.2 (2)P2—C63—H63A109.2
C14—P6—Ag4121.93 (15)P3—C63—H63A109.2
C20—P6—Ag4108.08 (14)P2—C63—H63B109.2
C13—P6—Ag4110.97 (15)P3—C63—H63B109.2
C6—C1—C2119.4 (5)H63A—C63—H63B107.9
C6—C1—P1123.9 (4)C69—C64—C65118.7 (4)
C2—C1—P1116.7 (4)C69—C64—P2118.9 (4)
C3—C2—C1119.9 (6)C65—C64—P2122.4 (4)
C3—C2—H2120.1C64—C65—C66120.7 (5)
C1—C2—H2120.1C64—C65—H65119.6
C2—C3—C4119.8 (6)C66—C65—H65119.6
C2—C3—H3120.1C67—C66—C65120.0 (5)
C4—C3—H3120.1C67—C66—H66120.0
C5—C4—C3120.6 (6)C65—C66—H66120.0
C5—C4—H4119.7C66—C67—C68120.3 (5)
C3—C4—H4119.7C66—C67—H67119.9
C4—C5—C6120.1 (6)C68—C67—H67119.9
C4—C5—H5120.0C67—C68—C69119.6 (5)
C6—C5—H5120.0C67—C68—H68120.2
C1—C6—C5120.2 (6)C69—C68—H68120.2
C1—C6—H6119.9C64—C69—C68120.7 (5)
C5—C6—H6119.9C64—C69—H69119.7
C12—C7—C8119.3 (4)C68—C69—H69119.7
C12—C7—P1123.2 (4)C71—C70—C75119.5 (4)
C8—C7—P1117.6 (4)C71—C70—P2123.7 (4)
C9—C8—C7120.7 (5)C75—C70—P2116.8 (3)
C9—C8—H8119.6C70—C71—C72120.0 (4)
C7—C8—H8119.6C70—C71—H71120.0
C8—C9—C10119.4 (5)C72—C71—H71120.0
C8—C9—H9120.3C73—C72—C71120.2 (4)
C10—C9—H9120.3C73—C72—H72119.9
C9—C10—C11120.8 (5)C71—C72—H72119.9
C9—C10—H10119.6C72—C73—C74120.2 (4)
C11—C10—H10119.6C72—C73—H73119.9
C12—C11—C10120.2 (5)C74—C73—H73119.9
C12—C11—H11119.9C75—C74—C73119.6 (5)
C10—C11—H11119.9C75—C74—H74120.2
C11—C12—C7119.7 (5)C73—C74—H74120.2
C11—C12—H12120.2C74—C75—C70120.4 (5)
C7—C12—H12120.2C74—C75—H75119.8
P1—C13—P6114.1 (2)C70—C75—H75119.8
P1—C13—H13A108.7C76—N1—C77121.0 (5)
P6—C13—H13A108.7C76—N1—C78121.9 (4)
P1—C13—H13B108.7C77—N1—C78117.1 (4)
P6—C13—H13B108.7O1—C76—N1125.7 (5)
H13A—C13—H13B107.6O1—C76—H76117.1
C19—C14—C15118.8 (4)N1—C76—H76117.1
C19—C14—P6122.1 (3)N1—C77—H77A109.5
C15—C14—P6119.1 (4)N1—C77—H77B109.5
C16—C15—C14120.5 (4)H77A—C77—H77B109.5
C16—C15—H15119.7N1—C77—H77C109.5
C14—C15—H15119.7H77A—C77—H77C109.5
C17—C16—C15120.6 (5)H77B—C77—H77C109.5
C17—C16—H16119.7N1—C78—H78A109.5
C15—C16—H16119.7N1—C78—H78B109.5
C16—C17—C18119.7 (5)H78A—C78—H78B109.5
C16—C17—H17120.2N1—C78—H78C109.5
C18—C17—H17120.2H78A—C78—H78C109.5
C19—C18—C17120.0 (5)H78B—C78—H78C109.5
C19—C18—H18120.0C79—N2—C81125.7 (5)
C17—C18—H18120.0C79—N2—C80120.2 (5)
C14—C19—C18120.4 (4)C81—N2—C80114.1 (5)
C14—C19—H19119.8O2—C79—N2125.1 (6)
C18—C19—H19119.8O2—C79—H79117.4
C21—C20—C25118.8 (4)N2—C79—H79117.4
C21—C20—P6123.1 (4)N2—C80—H80A109.5
C25—C20—P6117.8 (4)N2—C80—H80B109.5
C22—C21—C20120.7 (5)H80A—C80—H80B109.5
C22—C21—H21119.7N2—C80—H80C109.5
C20—C21—H21119.7H80A—C80—H80C109.5
C23—C22—C21119.7 (5)H80B—C80—H80C109.5
C23—C22—H22120.2N2—C81—H81A109.5
C21—C22—H22120.2N2—C81—H81B109.5
C24—C23—C22120.3 (5)H81A—C81—H81B109.5
C24—C23—H23119.9N2—C81—H81C109.5
C22—C23—H23119.9H81A—C81—H81C109.5
C23—C24—C25120.5 (5)H81B—C81—H81C109.5
C23—C24—H24119.8
Acknowledgements top

This work was supported by the National Keystone Basic Research Program (973 Program) under grant No. 2007CB310408, No. 2006CB302901 and the Funding Project for Academic Human Resources Development in Institutions of Higher Learning Under the Jurisdiction of Beijing Municipality. It was also supported by the State Key Laboratory of Functional Materials for Informatics, Shanghai Institute of Microsystem and Information Technology, Chinese Academy of Sciences.

references
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