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Acta Crystallogr Sect E Struct Rep Online. 2010 October 1; 66(Pt 10): m1237–m1238.
Published online 2010 September 11. doi:  10.1107/S1600536810035622
PMCID: PMC2983356

catena-Poly[silver(I)-bis­[μ-bis­(diphenyl­phosphino)methane-κ2 P:P′]-μ-thio­cyanato-κ2 S:S-silver(I)-μ-thio­cyanato-κ2 S:N]

Abstract

The title compound, [Ag(NCS)(C25H22P2)]n, contains two Ag+ ions, two thio­cyanate ions and two bis­(diphenyl­phosphino)methane (dppm) ligands in the asymmetric unit. One of the thiocyanate ions bridges the two Ag+ ions in a μ2-mode from its S atom and the two dppm ligands bridge the silver ions in a μ11 mode. The remaining SCN ion bridges the binuclear units via its N and S atoms, generating a one-dimensional polymer propagating in [An external file that holds a picture, illustration, etc.
Object name is e-66-m1237-efi1.jpg01]: the resulting AgP2SN and AgP2S2 coordination geometries could be described as distorted tetra­hedral.

Related literature

For general background to silver(I) complexes, see: Awaleh et al. (2007 [triangle]); Liu et al. (2008 [triangle]). For silver(I) complexes containing phosphine ligands and coordinated anions, see: Jin, Song et al. (2010 [triangle]); Jin, Hu et al. (2010 [triangle]). For related structures, see: Jin et al. (2008 [triangle]); Cingolani et al. (2005 [triangle]).

An external file that holds a picture, illustration, etc.
Object name is e-66-m1237-scheme1.jpg

Experimental

Crystal data

  • [Ag(NCS)(C25H22P2)]
  • M r = 550.32
  • Monoclinic, An external file that holds a picture, illustration, etc.
Object name is e-66-m1237-efi2.jpg
  • a = 13.0712 (14) Å
  • b = 23.080 (2) Å
  • c = 15.6340 (16) Å
  • β = 93.470 (1)°
  • V = 4708.0 (8) Å3
  • Z = 8
  • Mo Kα radiation
  • μ = 1.10 mm−1
  • T = 298 K
  • 0.43 × 0.34 × 0.32 mm

Data collection

  • Bruker SMART CCD area-detector diffractometer
  • Absorption correction: multi-scan (SADABS; Bruker, 2007 [triangle]) T min = 0.650, T max = 0.721
  • 23675 measured reflections
  • 8306 independent reflections
  • 4539 reflections with I > 2σ(I)
  • R int = 0.056

Refinement

  • R[F 2 > 2σ(F 2)] = 0.059
  • wR(F 2) = 0.168
  • S = 1.02
  • 8306 reflections
  • 559 parameters
  • 1 restraint
  • H-atom parameters constrained
  • Δρmax = 1.34 e Å−3
  • Δρmin = −1.31 e Å−3

Data collection: SMART (Bruker, 2007 [triangle]); cell refinement: SAINT-Plus (Bruker, 2007 [triangle]); data reduction: SAINT-Plus; program(s) used to solve structure: SHELXS97 (Sheldrick, 2008 [triangle]); program(s) used to refine structure: SHELXL97 (Sheldrick, 2008 [triangle]); molecular graphics: SHELXTL (Sheldrick, 2008 [triangle]); software used to prepare material for publication: SHELXTL.

Table 1
Selected bond lengths (Å)

Supplementary Material

Crystal structure: contains datablocks global, I. DOI: 10.1107/S1600536810035622/hb5620sup1.cif

Structure factors: contains datablocks I. DOI: 10.1107/S1600536810035622/hb5620Isup2.hkl

Additional supplementary materials: crystallographic information; 3D view; checkCIF report

Acknowledgments

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.

supplementary crystallographic information

Comment

Many research efforts have been devoted to the silver(I) complexes due to their fascinating structures and potential applications in the field of photo-sensitizer, semi-conducting or catalytic devices (Awaleh et al., 2007, Liu et al., 2008). Recently, we have found some silver(I) complexes containing phosphine ligands and coordinated anions (Jin, Song et al., 2010, Jin, Hu et al., 2010). Continuing these efforts, we obtain a new one-dimensional polymer [Ag2(dppm)2(SCN)2] by using AgSCN, dppm and 1,10-Phenanthroline(phen).

The crystal structural analysis shows that SCN- bridges the [Ag2(dppm)2(SCN)] binuclear units to give rise to a one-dimensional polymer. In the binclear unit, two dppm ligands lock two silver atoms to form a circular dimer, where S atom of SCN- behaving as bridging ligand links two silver atoms. Two silver atoms are four-coordinated. Ag1 is coordinated by two P-atoms from two dppm ligands, two S atoms from two thiocyanide anions while Ag2 is coordinated by two P-atoms from two dppm ligands, one S-atom and one N-atom from two thiocyanide anions. In the title compound, the P—Ag1—S angles are in the range 104.55 (9)–108.67 (8)°, and the P—Ag1—P angle is 127.18 (8)°, S—Ag1—S is 99.11 (8)°; while N—Ag2—P are in the range 101.4 (2)–113.2 (2)°, P—Ag2—P is 126.43 (8)°, N—Ag2—S are in the range 101.5 (3)–106.66 (8)°. This confirms the distored tetrahedral environment around two silver (I) atoms. The distance of the two silver atoms (3.484 Å) is 0.048 Å longer than the sum of the covalent radii(3.44 Å), which indicates that there exists weak Ag···Ag interaction. The bond lengths of S1—Ag1 and S1—Ag2 are 2.670 and 2.668 Å, respectively.The angles of N1—C1—S1 and N2—C2—S2 are 179.55 and 165.33°, respectively. The angle of Ag1—S1—Ag2 are 10.92° shorter than that reported for [Ag2(dpam)2(SCN)2](92.39°) (Cingolani et al., 2005).

The similar compound [Ag4(SCN)4(dppm)2] (Jin et al.,2008) is prepared by the similar reaction by using quinoline in place of phen. Though both quinoline and phen don't take part in coordination, this two ligands effect the final structures of the products. This confirms again that different nitrogen heterocyclic ligands lead to different structures due to the subtle interation of the nitrogen heterocyclic ligands with silver ions. (Jin, Hu et al., 2010).

Experimental

A mixture of AgSCN (0.0332 g, 0.2 mmol), 1,10-Phenanthroline (0.0792, 0.4 mmol) and bis(diphenylphosphino)methane (0.1532 g, 0.4 mmol) in the molar ratio 1:2:2 in CH3OH/CH2Cl2 was stirred for 5 h at ambient temperature. After filtration, the filtrate was allowed to stand still. Slow evaportation of the solvent yielded colourless blocks of (I). Analysis found(percentage): C 56.70, H 4.00, N 2.54; calculated: C 56.21, H 3.72, N 2.24.

Refinement

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.

Figures

Fig. 1.
Perspective view of a basic unit of the title complex. Hydrogen atoms are omitted for clarity.
Fig. 2.
Perspective view of a one-dimensional polymer of the title complex.

Crystal data

[Ag(NCS)(C25H22P2)]F(000) = 2224
Mr = 550.32Dx = 1.553 Mg m3Dm = 1.553 Mg m3Dm measured by not measured
Monoclinic, P21/nMo Kα radiation, λ = 0.71073 Å
Hall symbol: -P 2ynCell parameters from 4221 reflections
a = 13.0712 (14) Åθ = 2.3–23.1°
b = 23.080 (2) ŵ = 1.10 mm1
c = 15.6340 (16) ÅT = 298 K
β = 93.470 (1)°Block, colourless
V = 4708.0 (8) Å30.43 × 0.34 × 0.32 mm
Z = 8

Data collection

Bruker SMART CCD area-detector diffractometer8306 independent reflections
Radiation source: fine-focus sealed tube4539 reflections with I > 2σ(I)
graphiteRint = 0.056
phi and ω scansθmax = 25.0°, θmin = 1.6°
Absorption correction: multi-scan (SADABS; Bruker, 2007)h = −15→15
Tmin = 0.650, Tmax = 0.721k = −27→22
23675 measured reflectionsl = −15→18

Refinement

Refinement on F2Primary atom site location: structure-invariant direct methods
Least-squares matrix: fullSecondary atom site location: difference Fourier map
R[F2 > 2σ(F2)] = 0.059Hydrogen site location: inferred from neighbouring sites
wR(F2) = 0.168H-atom parameters constrained
S = 1.02w = 1/[σ2(Fo2) + (0.0414P)2 + 37.553P] where P = (Fo2 + 2Fc2)/3
8306 reflections(Δ/σ)max = 0.001
559 parametersΔρmax = 1.34 e Å3
1 restraintΔρmin = −1.31 e Å3

Special details

Geometry. All e.s.d.'s (except the e.s.d. in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell e.s.d.'s are taken into account individually in the estimation of e.s.d.'s in distances, angles and torsion angles; correlations between e.s.d.'s in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell e.s.d.'s is used for estimating e.s.d.'s involving l.s. planes.
Refinement. Refinement 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)

xyzUiso*/Ueq
Ag10.67704 (5)0.24042 (3)0.55934 (5)0.0460 (2)
Ag20.49477 (5)0.24103 (3)0.71296 (4)0.0422 (2)
N10.7422 (7)0.1363 (5)0.7966 (7)0.090 (3)
N20.9491 (8)0.2412 (4)0.3589 (6)0.084 (3)
P10.60071 (16)0.33099 (9)0.50436 (14)0.0342 (5)
P20.43500 (16)0.33225 (9)0.64005 (14)0.0343 (5)
P30.61866 (16)0.14163 (9)0.52595 (14)0.0336 (5)
P40.45647 (17)0.14001 (9)0.66334 (15)0.0379 (5)
S10.69887 (17)0.24681 (11)0.73000 (16)0.0488 (6)
S20.8817 (2)0.24072 (14)0.5231 (2)0.0715 (8)
C10.7242 (7)0.1814 (5)0.7699 (7)0.054 (3)
C20.9092 (8)0.2425 (4)0.4226 (7)0.052 (2)
C30.4656 (6)0.3405 (4)0.5286 (5)0.040 (2)
H3A0.44400.37890.50970.048*
H3B0.42480.31280.49460.048*
C40.5943 (7)0.3337 (4)0.3880 (6)0.044 (2)
C50.6844 (8)0.3277 (4)0.3492 (7)0.059 (3)
H50.74590.32560.38220.071*
C60.6847 (8)0.3246 (5)0.2606 (7)0.069 (3)
H60.74650.32110.23460.083*
C70.5942 (8)0.3266 (5)0.2106 (7)0.066 (3)
H70.59470.32440.15130.079*
C80.5053 (8)0.3316 (4)0.2487 (6)0.058 (3)
H80.44380.33200.21560.069*
C90.5049 (7)0.3363 (4)0.3366 (6)0.049 (2)
H90.44280.34130.36180.059*
C100.6664 (7)0.3976 (4)0.5373 (6)0.041 (2)
C110.7642 (7)0.3934 (4)0.5762 (6)0.056 (3)
H110.79460.35720.58370.067*
C120.8174 (8)0.4423 (4)0.6041 (7)0.063 (3)
H120.88310.43880.63000.076*
C130.7733 (8)0.4958 (4)0.5936 (7)0.061 (3)
H130.80820.52870.61370.073*
C140.6787 (8)0.5008 (4)0.5539 (7)0.061 (3)
H140.64940.53730.54600.073*
C150.6250 (7)0.4521 (4)0.5250 (6)0.051 (2)
H150.56060.45620.49710.061*
C160.2954 (7)0.3366 (4)0.6316 (6)0.045 (2)
C170.2480 (7)0.3291 (4)0.7076 (7)0.058 (3)
H170.28700.32470.75900.070*
C180.1413 (8)0.3280 (5)0.7065 (8)0.073 (3)
H180.10860.32230.75710.088*
C190.0856 (9)0.3353 (5)0.6317 (9)0.072 (3)
H190.01440.33520.63170.086*
C200.1301 (8)0.3428 (5)0.5569 (8)0.072 (3)
H200.09020.34670.50600.086*
C210.2356 (7)0.3445 (4)0.5569 (7)0.060 (3)
H210.26680.35100.50590.072*
C220.4750 (7)0.4014 (4)0.6861 (6)0.041 (2)
C230.5642 (7)0.4043 (4)0.7378 (6)0.051 (2)
H230.59980.37060.75290.062*
C240.6009 (8)0.4577 (4)0.7673 (7)0.064 (3)
H240.66140.45950.80170.077*
C250.5495 (9)0.5072 (5)0.7463 (7)0.063 (3)
H250.57580.54280.76490.076*
C260.4596 (8)0.5049 (4)0.6982 (6)0.056 (3)
H260.42320.53870.68560.067*
C270.4220 (7)0.4523 (4)0.6680 (6)0.048 (2)
H270.36040.45100.63510.058*
C280.5626 (7)0.1018 (4)0.6134 (6)0.047 (2)
H28A0.61620.09380.65740.056*
H28B0.53720.06480.59140.056*
C290.7291 (7)0.0990 (4)0.4987 (6)0.044 (2)
C300.8073 (7)0.0897 (4)0.5609 (7)0.057 (3)
H300.79580.09730.61800.068*
C310.9021 (8)0.0694 (5)0.5398 (8)0.069 (3)
H310.95470.06480.58210.083*
C320.9181 (9)0.0561 (5)0.4572 (8)0.069 (3)
H320.98120.04150.44290.082*
C330.8420 (9)0.0641 (5)0.3955 (7)0.069 (3)
H330.85310.05460.33900.083*
C340.7467 (8)0.0864 (4)0.4158 (7)0.059 (3)
H340.69560.09250.37280.071*
C350.5264 (7)0.1321 (4)0.4371 (6)0.048 (2)
C360.4939 (8)0.0789 (5)0.4059 (7)0.068 (3)
H360.52270.04530.42960.081*
C370.4185 (9)0.0750 (5)0.3393 (8)0.087 (4)
H370.39710.03870.31920.104*
C380.3753 (8)0.1241 (5)0.3028 (7)0.072 (3)
H380.32280.12130.26010.087*
C390.4105 (8)0.1773 (5)0.3301 (7)0.064 (3)
H390.38410.21080.30420.077*
C400.4854 (7)0.1809 (4)0.3963 (6)0.055 (3)
H400.50890.21730.41410.066*
C410.3476 (7)0.1354 (4)0.5868 (6)0.050 (2)
C420.3018 (8)0.1858 (4)0.5572 (6)0.057 (3)
H420.32960.22080.57650.069*
C430.2166 (8)0.1872 (5)0.5002 (7)0.068 (3)
H430.18830.22250.48280.082*
C440.1741 (8)0.1366 (5)0.4695 (8)0.075 (3)
H440.11360.13690.43490.090*
C450.2227 (10)0.0855 (6)0.4910 (9)0.093 (4)
H450.19650.05050.46980.111*
C460.3107 (9)0.0863 (5)0.5444 (8)0.080 (4)
H460.34740.05200.55220.096*
C470.4310 (8)0.0900 (4)0.7463 (7)0.058 (3)
C480.4558 (10)0.1033 (5)0.8299 (8)0.086 (4)
H480.48510.13940.84190.103*
C490.4401 (11)0.0665 (6)0.8987 (9)0.101 (5)
H490.45870.07860.95420.121*
C500.3977 (10)0.0128 (5)0.8854 (8)0.086 (4)
H500.3875−0.01220.93070.103*
C510.3709 (12)−0.0023 (6)0.8029 (10)0.108 (5)
H510.3412−0.03830.79080.130*
C520.3882 (11)0.0358 (5)0.7370 (9)0.095 (4)
H520.36900.02370.68160.114*

Atomic displacement parameters (Å2)

U11U22U33U12U13U23
Ag10.0510 (4)0.0350 (4)0.0509 (5)0.0026 (3)−0.0054 (3)0.0020 (3)
Ag20.0420 (4)0.0364 (4)0.0477 (4)−0.0003 (3)−0.0025 (3)0.0017 (3)
N10.071 (7)0.083 (8)0.114 (9)0.002 (6)−0.006 (6)0.033 (7)
N20.109 (8)0.087 (7)0.062 (7)−0.013 (6)0.052 (6)−0.016 (5)
P10.0366 (12)0.0327 (12)0.0335 (13)0.0025 (10)0.0034 (10)0.0027 (9)
P20.0357 (12)0.0317 (12)0.0360 (13)0.0029 (10)0.0056 (10)0.0000 (9)
P30.0361 (12)0.0326 (12)0.0320 (13)−0.0006 (10)0.0018 (10)0.0012 (9)
P40.0375 (12)0.0330 (11)0.0441 (14)−0.0037 (10)0.0097 (11)−0.0011 (10)
S10.0394 (12)0.0609 (16)0.0453 (14)−0.0077 (11)−0.0038 (10)−0.0030 (12)
S20.0556 (16)0.094 (2)0.0655 (19)−0.0031 (16)0.0120 (14)−0.0011 (16)
C10.039 (5)0.060 (7)0.062 (7)0.001 (5)−0.002 (5)0.010 (5)
C20.060 (6)0.042 (6)0.057 (7)−0.003 (5)0.012 (5)−0.002 (5)
C30.044 (5)0.038 (5)0.038 (5)−0.001 (4)0.003 (4)−0.002 (4)
C40.046 (5)0.048 (6)0.039 (5)0.000 (4)0.008 (4)0.002 (4)
C50.054 (6)0.077 (8)0.047 (7)−0.005 (5)0.010 (5)0.003 (5)
C60.058 (7)0.101 (9)0.051 (7)−0.007 (6)0.018 (6)−0.004 (6)
C70.068 (7)0.085 (8)0.044 (7)−0.004 (6)0.009 (6)0.001 (6)
C80.055 (6)0.074 (7)0.044 (6)0.001 (5)0.001 (5)−0.002 (5)
C90.047 (6)0.060 (6)0.041 (6)0.004 (5)0.007 (5)0.001 (5)
C100.050 (6)0.036 (5)0.038 (5)−0.005 (4)0.006 (4)0.002 (4)
C110.058 (6)0.049 (6)0.059 (7)−0.003 (5)−0.008 (5)0.000 (5)
C120.061 (7)0.056 (7)0.070 (8)−0.014 (6)−0.011 (6)−0.002 (6)
C130.071 (8)0.048 (7)0.062 (7)−0.014 (6)0.001 (6)−0.010 (5)
C140.074 (8)0.042 (6)0.067 (8)−0.006 (5)0.006 (6)0.003 (5)
C150.055 (6)0.043 (6)0.055 (7)−0.001 (5)0.002 (5)0.006 (5)
C160.038 (5)0.041 (5)0.058 (7)0.002 (4)0.005 (5)0.001 (4)
C170.045 (6)0.064 (7)0.066 (7)0.001 (5)0.008 (5)−0.005 (5)
C180.053 (7)0.084 (9)0.085 (10)−0.001 (6)0.021 (7)−0.007 (7)
C190.045 (6)0.078 (8)0.092 (10)0.005 (6)0.007 (7)−0.011 (7)
C200.048 (7)0.080 (8)0.085 (9)0.010 (6)−0.009 (6)−0.005 (7)
C210.049 (6)0.063 (7)0.068 (8)0.004 (5)−0.001 (5)−0.002 (6)
C220.045 (5)0.038 (5)0.042 (6)0.001 (4)0.006 (4)0.001 (4)
C230.060 (6)0.044 (6)0.049 (6)−0.002 (5)−0.004 (5)−0.001 (5)
C240.069 (7)0.056 (7)0.065 (8)−0.007 (6)−0.010 (6)−0.009 (6)
C250.081 (8)0.051 (7)0.057 (7)−0.014 (6)0.008 (6)−0.006 (5)
C260.077 (8)0.038 (6)0.053 (7)0.003 (5)0.008 (6)−0.001 (5)
C270.057 (6)0.042 (6)0.046 (6)0.002 (5)0.003 (5)−0.001 (4)
C280.050 (6)0.043 (5)0.048 (6)−0.003 (4)0.003 (5)0.003 (4)
C290.045 (5)0.047 (6)0.041 (6)0.004 (4)0.006 (5)−0.002 (4)
C300.051 (6)0.064 (7)0.055 (7)0.011 (5)0.005 (5)−0.007 (5)
C310.055 (7)0.080 (8)0.073 (9)0.011 (6)0.002 (6)−0.010 (6)
C320.059 (7)0.075 (8)0.073 (9)0.012 (6)0.014 (6)0.001 (6)
C330.077 (8)0.074 (8)0.059 (8)0.016 (6)0.020 (6)−0.007 (6)
C340.060 (7)0.065 (7)0.052 (7)0.015 (5)0.005 (5)0.004 (5)
C350.046 (5)0.046 (6)0.049 (6)0.000 (4)−0.008 (5)0.003 (4)
C360.072 (7)0.059 (7)0.069 (8)−0.005 (6)−0.025 (6)0.009 (6)
C370.089 (9)0.076 (9)0.089 (10)−0.013 (7)−0.035 (8)0.004 (7)
C380.061 (7)0.081 (9)0.071 (8)−0.002 (6)−0.022 (6)0.011 (7)
C390.060 (7)0.072 (8)0.059 (7)0.016 (6)−0.013 (6)0.010 (6)
C400.052 (6)0.057 (7)0.054 (7)0.007 (5)−0.006 (5)0.006 (5)
C410.046 (6)0.048 (6)0.055 (6)−0.006 (5)−0.003 (5)−0.001 (5)
C420.061 (7)0.049 (6)0.060 (7)−0.004 (5)−0.010 (5)−0.002 (5)
C430.065 (7)0.068 (8)0.070 (8)0.002 (6)−0.014 (6)0.000 (6)
C440.058 (7)0.076 (9)0.087 (9)0.000 (6)−0.021 (6)−0.004 (7)
C450.083 (9)0.080 (9)0.110 (11)−0.014 (7)−0.033 (8)−0.005 (8)
C460.081 (9)0.065 (8)0.090 (10)−0.004 (6)−0.022 (7)0.000 (7)
C470.075 (7)0.045 (6)0.055 (7)−0.015 (5)0.016 (6)−0.001 (5)
C480.114 (11)0.071 (8)0.070 (9)−0.033 (7)−0.012 (8)0.020 (7)
C490.143 (13)0.088 (10)0.071 (9)−0.031 (9)−0.012 (9)0.023 (7)
C500.115 (11)0.073 (9)0.070 (9)−0.022 (8)0.009 (8)0.024 (7)
C510.158 (15)0.080 (10)0.089 (11)−0.050 (9)0.024 (10)0.015 (8)
C520.134 (12)0.076 (9)0.076 (9)−0.034 (8)0.013 (9)0.006 (7)

Geometric parameters (Å, °)

Ag1—P12.450 (2)C21—H210.9300
Ag1—P32.451 (2)C22—C231.379 (12)
Ag1—S12.670 (3)C22—C271.384 (12)
Ag1—S22.768 (3)C23—C241.392 (13)
Ag2—N2i2.429 (9)C23—H230.9300
Ag2—P22.497 (2)C24—C251.355 (14)
Ag2—P42.498 (2)C24—H240.9300
Ag2—S12.668 (2)C25—C261.357 (14)
N1—C11.142 (12)C25—H250.9300
N2—C21.153 (12)C26—C271.382 (12)
N2—Ag2ii2.429 (9)C26—H260.9300
P1—C41.817 (9)C27—H270.9300
P1—C101.819 (9)C28—H28A0.9700
P1—C31.842 (8)C28—H28B0.9700
P2—C221.815 (9)C29—C341.361 (13)
P2—C31.821 (9)C29—C301.384 (12)
P2—C161.825 (9)C30—C311.385 (13)
P3—C351.797 (9)C30—H300.9300
P3—C291.819 (9)C31—C321.355 (14)
P3—C281.838 (9)C31—H310.9300
P4—C471.783 (10)C32—C331.356 (14)
P4—C411.806 (9)C32—H320.9300
P4—C281.855 (9)C33—C341.402 (13)
S1—C11.659 (11)C33—H330.9300
S2—C21.633 (11)C34—H340.9300
C3—H3A0.9700C35—C361.379 (13)
C3—H3B0.9700C35—C401.386 (12)
C4—C51.364 (13)C36—C371.393 (14)
C4—C91.380 (12)C36—H360.9300
C5—C61.387 (13)C37—C381.375 (15)
C5—H50.9300C37—H370.9300
C6—C71.378 (14)C38—C391.370 (14)
C6—H60.9300C38—H380.9300
C7—C81.342 (13)C39—C401.384 (13)
C7—H70.9300C39—H390.9300
C8—C91.378 (13)C40—H400.9300
C8—H80.9300C41—C421.375 (13)
C9—H90.9300C41—C461.385 (14)
C10—C151.378 (12)C42—C431.383 (13)
C10—C111.386 (12)C42—H420.9300
C11—C121.382 (13)C43—C441.367 (14)
C11—H110.9300C43—H430.9300
C12—C131.369 (13)C44—C451.373 (15)
C12—H120.9300C44—H440.9300
C13—C141.355 (13)C45—C461.379 (15)
C13—H130.9300C45—H450.9300
C14—C151.388 (13)C46—H460.9300
C14—H140.9300C47—C481.363 (15)
C15—H150.9300C47—C521.374 (14)
C16—C211.377 (13)C48—C491.396 (15)
C16—C171.383 (13)C48—H480.9300
C17—C181.394 (13)C49—C501.368 (16)
C17—H170.9300C49—H490.9300
C18—C191.351 (15)C50—C511.362 (17)
C18—H180.9300C50—H500.9300
C19—C201.348 (15)C51—C521.383 (16)
C19—H190.9300C51—H510.9300
C20—C211.380 (14)C52—H520.9300
C20—H200.9300
P1—Ag1—P3127.18 (8)C16—C21—C20120.8 (11)
P1—Ag1—S1108.67 (8)C16—C21—H21119.6
P3—Ag1—S1106.10 (8)C20—C21—H21119.6
P1—Ag1—S2107.71 (9)C23—C22—C27118.3 (8)
P3—Ag1—S2104.55 (9)C23—C22—P2119.2 (7)
S1—Ag1—S299.11 (8)C27—C22—P2122.4 (7)
N2i—Ag2—P2101.4 (2)C22—C23—C24119.9 (9)
N2i—Ag2—P4113.2 (2)C22—C23—H23120.0
P2—Ag2—P4126.43 (8)C24—C23—H23120.0
N2i—Ag2—S1101.5 (3)C25—C24—C23120.7 (10)
P2—Ag2—S1106.66 (8)C25—C24—H24119.7
P4—Ag2—S1104.95 (8)C23—C24—H24119.7
C2—N2—Ag2ii163.2 (10)C24—C25—C26120.1 (10)
C4—P1—C10104.3 (4)C24—C25—H25120.0
C4—P1—C3102.5 (4)C26—C25—H25120.0
C10—P1—C3106.5 (4)C25—C26—C27120.1 (10)
C4—P1—Ag1111.9 (3)C25—C26—H26119.9
C10—P1—Ag1116.5 (3)C27—C26—H26119.9
C3—P1—Ag1113.9 (3)C26—C27—C22120.8 (9)
C22—P2—C3102.3 (4)C26—C27—H27119.6
C22—P2—C16104.1 (4)C22—C27—H27119.6
C3—P2—C16101.6 (4)P3—C28—P4114.6 (5)
C22—P2—Ag2119.0 (3)P3—C28—H28A108.6
C3—P2—Ag2116.4 (3)P4—C28—H28A108.6
C16—P2—Ag2111.3 (3)P3—C28—H28B108.6
C35—P3—C29105.0 (4)P4—C28—H28B108.6
C35—P3—C28103.6 (4)H28A—C28—H28B107.6
C29—P3—C28105.2 (4)C34—C29—C30118.4 (9)
C35—P3—Ag1117.6 (3)C34—C29—P3121.4 (7)
C29—P3—Ag1108.1 (3)C30—C29—P3118.8 (7)
C28—P3—Ag1116.1 (3)C29—C30—C31121.2 (10)
C47—P4—C41105.6 (5)C29—C30—H30119.4
C47—P4—C28100.1 (4)C31—C30—H30119.4
C41—P4—C28105.8 (4)C32—C31—C30119.7 (11)
C47—P4—Ag2114.9 (3)C32—C31—H31120.1
C41—P4—Ag2113.3 (3)C30—C31—H31120.1
C28—P4—Ag2115.7 (3)C31—C32—C33119.8 (11)
C1—S1—Ag299.6 (3)C31—C32—H32120.1
C1—S1—Ag1109.4 (4)C33—C32—H32120.1
Ag2—S1—Ag181.47 (7)C32—C33—C34120.8 (11)
C2—S2—Ag1117.9 (4)C32—C33—H33119.6
N1—C1—S1179.3 (12)C34—C33—H33119.6
N2—C2—S2165.5 (11)C29—C34—C33119.9 (10)
P2—C3—P1116.9 (4)C29—C34—H34120.1
P2—C3—H3A108.1C33—C34—H34120.1
P1—C3—H3A108.1C36—C35—C40117.3 (9)
P2—C3—H3B108.1C36—C35—P3124.0 (7)
P1—C3—H3B108.1C40—C35—P3118.7 (7)
H3A—C3—H3B107.3C35—C36—C37120.8 (10)
C5—C4—C9118.0 (9)C35—C36—H36119.6
C5—C4—P1117.0 (7)C37—C36—H36119.6
C9—C4—P1124.8 (7)C38—C37—C36120.7 (11)
C4—C5—C6120.2 (10)C38—C37—H37119.6
C4—C5—H5119.9C36—C37—H37119.6
C6—C5—H5119.9C39—C38—C37119.2 (10)
C7—C6—C5120.7 (10)C39—C38—H38120.4
C7—C6—H6119.6C37—C38—H38120.4
C5—C6—H6119.6C38—C39—C40119.8 (10)
C8—C7—C6119.2 (10)C38—C39—H39120.1
C8—C7—H7120.4C40—C39—H39120.1
C6—C7—H7120.4C39—C40—C35122.1 (10)
C7—C8—C9120.4 (10)C39—C40—H40118.9
C7—C8—H8119.8C35—C40—H40118.9
C9—C8—H8119.8C42—C41—C46113.5 (9)
C8—C9—C4121.5 (9)C42—C41—P4118.9 (7)
C8—C9—H9119.3C46—C41—P4127.0 (8)
C4—C9—H9119.3C41—C42—C43123.6 (10)
C15—C10—C11117.9 (8)C41—C42—H42118.2
C15—C10—P1123.8 (7)C43—C42—H42118.2
C11—C10—P1118.2 (7)C44—C43—C42120.0 (10)
C12—C11—C10121.0 (9)C44—C43—H43120.0
C12—C11—H11119.5C42—C43—H43120.0
C10—C11—H11119.5C43—C44—C45118.4 (10)
C13—C12—C11119.9 (10)C43—C44—H44120.8
C13—C12—H12120.0C45—C44—H44120.8
C11—C12—H12120.0C44—C45—C46119.6 (11)
C14—C13—C12119.9 (9)C44—C45—H45120.2
C14—C13—H13120.0C46—C45—H45120.2
C12—C13—H13120.0C45—C46—C41123.6 (11)
C13—C14—C15120.6 (10)C45—C46—H46118.2
C13—C14—H14119.7C41—C46—H46118.2
C15—C14—H14119.7C48—C47—C52112.3 (10)
C10—C15—C14120.6 (9)C48—C47—P4120.4 (8)
C10—C15—H15119.7C52—C47—P4127.3 (9)
C14—C15—H15119.7C47—C48—C49124.3 (12)
C21—C16—C17119.0 (9)C47—C48—H48117.9
C21—C16—P2125.6 (8)C49—C48—H48117.9
C17—C16—P2115.4 (7)C50—C49—C48120.8 (13)
C16—C17—C18119.4 (10)C50—C49—H49119.6
C16—C17—H17120.3C48—C49—H49119.6
C18—C17—H17120.3C51—C50—C49117.1 (12)
C19—C18—C17119.7 (11)C51—C50—H50121.5
C19—C18—H18120.2C49—C50—H50121.5
C17—C18—H18120.2C50—C51—C52119.8 (13)
C20—C19—C18121.9 (11)C50—C51—H51120.1
C20—C19—H19119.0C52—C51—H51120.1
C18—C19—H19119.0C47—C52—C51125.8 (13)
C19—C20—C21119.2 (11)C47—C52—H52117.1
C19—C20—H20120.4C51—C52—H52117.1
C21—C20—H20120.4
P3—Ag1—P1—C4−57.1 (3)C3—P2—C16—C21−0.2 (9)
S1—Ag1—P1—C4174.4 (3)Ag2—P2—C16—C21−124.8 (8)
S2—Ag1—P1—C467.9 (3)C22—P2—C16—C17−76.7 (8)
P3—Ag1—P1—C10−176.9 (3)C3—P2—C16—C17177.2 (7)
S1—Ag1—P1—C1054.5 (3)Ag2—P2—C16—C1752.7 (8)
S2—Ag1—P1—C10−52.0 (3)C21—C16—C17—C181.7 (15)
P3—Ag1—P1—C358.6 (3)P2—C16—C17—C18−175.9 (8)
S1—Ag1—P1—C3−70.0 (3)C16—C17—C18—C19−1.1 (16)
S2—Ag1—P1—C3−176.5 (3)C17—C18—C19—C201.1 (18)
N2i—Ag2—P2—C2251.2 (4)C18—C19—C20—C21−1.7 (18)
P4—Ag2—P2—C22−178.4 (3)C17—C16—C21—C20−2.3 (15)
S1—Ag2—P2—C22−54.6 (3)P2—C16—C21—C20175.0 (8)
N2i—Ag2—P2—C3174.4 (4)C19—C20—C21—C162.3 (16)
P4—Ag2—P2—C3−55.1 (3)C3—P2—C22—C23−105.2 (8)
S1—Ag2—P2—C368.6 (3)C16—P2—C22—C23149.2 (8)
N2i—Ag2—P2—C16−69.8 (4)Ag2—P2—C22—C2324.7 (9)
P4—Ag2—P2—C1660.7 (4)C3—P2—C22—C2771.4 (8)
S1—Ag2—P2—C16−175.6 (3)C16—P2—C22—C27−34.1 (9)
P1—Ag1—P3—C3513.1 (4)Ag2—P2—C22—C27−158.7 (7)
S1—Ag1—P3—C35142.7 (4)C27—C22—C23—C24−2.6 (14)
S2—Ag1—P3—C35−113.1 (4)P2—C22—C23—C24174.2 (8)
P1—Ag1—P3—C29131.7 (3)C22—C23—C24—C250.5 (16)
S1—Ag1—P3—C29−98.8 (3)C23—C24—C25—C262.0 (17)
S2—Ag1—P3—C295.4 (3)C24—C25—C26—C27−2.2 (16)
P1—Ag1—P3—C28−110.5 (3)C25—C26—C27—C220.0 (15)
S1—Ag1—P3—C2819.1 (3)C23—C22—C27—C262.4 (14)
S2—Ag1—P3—C28123.3 (3)P2—C22—C27—C26−174.3 (7)
N2i—Ag2—P4—C47−14.5 (5)C35—P3—C28—P4−77.0 (6)
P2—Ag2—P4—C47−140.2 (4)C29—P3—C28—P4173.0 (5)
S1—Ag2—P4—C4795.3 (4)Ag1—P3—C28—P453.5 (5)
N2i—Ag2—P4—C41107.1 (5)C47—P4—C28—P3−176.6 (5)
P2—Ag2—P4—C41−18.7 (4)C41—P4—C28—P373.9 (6)
S1—Ag2—P4—C41−143.2 (4)Ag2—P4—C28—P3−52.5 (6)
N2i—Ag2—P4—C28−130.4 (4)C35—P3—C29—C3424.1 (9)
P2—Ag2—P4—C28103.8 (3)C28—P3—C29—C34133.1 (8)
S1—Ag2—P4—C28−20.7 (3)Ag1—P3—C29—C34−102.2 (8)
N2i—Ag2—S1—C179.4 (5)C35—P3—C29—C30−169.4 (8)
P2—Ag2—S1—C1−174.8 (4)C28—P3—C29—C30−60.5 (9)
P4—Ag2—S1—C1−38.6 (4)Ag1—P3—C29—C3064.2 (8)
N2i—Ag2—S1—Ag1−172.2 (2)C34—C29—C30—C311.6 (15)
P2—Ag2—S1—Ag1−66.44 (8)P3—C29—C30—C31−165.3 (8)
P4—Ag2—S1—Ag169.74 (8)C29—C30—C31—C32−2.6 (17)
P1—Ag1—S1—C1166.8 (4)C30—C31—C32—C331.6 (18)
P3—Ag1—S1—C127.2 (4)C31—C32—C33—C340.5 (18)
S2—Ag1—S1—C1−80.9 (4)C30—C29—C34—C330.5 (15)
P1—Ag1—S1—Ag269.48 (8)P3—C29—C34—C33167.0 (8)
P3—Ag1—S1—Ag2−70.11 (8)C32—C33—C34—C29−1.5 (17)
S2—Ag1—S1—Ag2−178.23 (8)C29—P3—C35—C3653.5 (10)
P1—Ag1—S2—C2−62.2 (4)C28—P3—C35—C36−56.6 (10)
P3—Ag1—S2—C275.4 (4)Ag1—P3—C35—C36173.7 (8)
S1—Ag1—S2—C2−175.2 (4)C29—P3—C35—C40−126.1 (8)
Ag2—S1—C1—N1119 (96)C28—P3—C35—C40123.9 (8)
Ag1—S1—C1—N135 (96)Ag1—P3—C35—C40−5.8 (9)
Ag2ii—N2—C2—S2−149 (2)C40—C35—C36—C37−3.5 (17)
Ag1—S2—C2—N2−169 (4)P3—C35—C36—C37176.9 (9)
C22—P2—C3—P178.9 (5)C35—C36—C37—C380(2)
C16—P2—C3—P1−173.7 (5)C36—C37—C38—C393(2)
Ag2—P2—C3—P1−52.6 (5)C37—C38—C39—C40−2.9 (18)
C4—P1—C3—P2173.2 (5)C38—C39—C40—C35−0.3 (17)
C10—P1—C3—P2−77.6 (6)C36—C35—C40—C393.5 (16)
Ag1—P1—C3—P252.2 (5)P3—C35—C40—C39−176.9 (8)
C10—P1—C4—C569.3 (8)C47—P4—C41—C42132.2 (9)
C3—P1—C4—C5−179.9 (8)C28—P4—C41—C42−122.3 (8)
Ag1—P1—C4—C5−57.5 (8)Ag2—P4—C41—C425.5 (10)
C10—P1—C4—C9−116.6 (8)C47—P4—C41—C46−57.0 (11)
C3—P1—C4—C9−5.7 (9)C28—P4—C41—C4648.6 (11)
Ag1—P1—C4—C9116.6 (8)Ag2—P4—C41—C46176.4 (9)
C9—C4—C5—C60.2 (15)C46—C41—C42—C439.5 (16)
P1—C4—C5—C6174.8 (8)P4—C41—C42—C43−178.4 (9)
C4—C5—C6—C7−1.1 (17)C41—C42—C43—C44−0.7 (18)
C5—C6—C7—C80.1 (18)C42—C43—C44—C45−5.3 (19)
C6—C7—C8—C91.7 (17)C43—C44—C45—C462(2)
C7—C8—C9—C4−2.5 (16)C44—C45—C46—C418(2)
C5—C4—C9—C81.5 (14)C42—C41—C46—C45−13.3 (18)
P1—C4—C9—C8−172.6 (8)P4—C41—C46—C45175.4 (10)
C4—P1—C10—C1567.9 (9)C41—P4—C47—C48−140.9 (10)
C3—P1—C10—C15−40.0 (9)C28—P4—C47—C48109.4 (11)
Ag1—P1—C10—C15−168.2 (7)Ag2—P4—C47—C48−15.2 (12)
C4—P1—C10—C11−111.3 (8)C41—P4—C47—C5240.1 (13)
C3—P1—C10—C11140.8 (7)C28—P4—C47—C52−69.6 (12)
Ag1—P1—C10—C1112.6 (9)Ag2—P4—C47—C52165.7 (10)
C15—C10—C11—C121.9 (15)C52—C47—C48—C490(2)
P1—C10—C11—C12−178.8 (8)P4—C47—C48—C49−179.0 (11)
C10—C11—C12—C130.1 (16)C47—C48—C49—C500(2)
C11—C12—C13—C14−1.7 (17)C48—C49—C50—C51−1(2)
C12—C13—C14—C151.1 (17)C49—C50—C51—C521(2)
C11—C10—C15—C14−2.5 (14)C48—C47—C52—C510(2)
P1—C10—C15—C14178.3 (8)P4—C47—C52—C51178.9 (12)
C13—C14—C15—C101.0 (16)C50—C51—C52—C470(3)
C22—P2—C16—C21105.8 (9)

Symmetry codes: (i) x−1/2, −y+1/2, z+1/2; (ii) x+1/2, −y+1/2, z−1/2.

Footnotes

Supplementary data and figures for this paper are available from the IUCr electronic archives (Reference: HB5620).

References

  • Awaleh, M. O., Badia, A. & Brisse, F. (2007). Inorg. Chem.46, 3185–3191. [PubMed]
  • Bruker (2007). SMART, SAINT-Plus and SADABS Bruker AXS Inc., Madison, Wisconsin, USA.
  • Cingolani, A., Di Nicola, C., Effendy, Pettinari, C., Skelton, B. W., Somers, N. & White, A. H. (2005). Inorg. Chim. Acta, 358, 748–762.
  • Jin, Q. H., Hu, K. Y., Chen, L. M., Sun, J. J., Yang, L. & Li, P. Z. (2008). Z. Kristallogr. New Cryst. Struct.223, 78–81.
  • Jin, Q. H., Hu, K. Y., Song, L. L., Wang, R., Zhang, C. L., Zuo, X. & Lu, X. M. (2010). Polyhedron, 29, 441–445.
  • Jin, Q. H., Song, L. L., Hu, K. Y., Zhou, L. L., Zhang, Y. Y. & Wang, R. (2010). Inorg. Chem. Commun.13, 62–65.
  • Liu, C. S., Chen, P. Q., Chang, Z., Wang, J. J., Yan, L. F., Sun, H. W., Bu, X. H., Lin, Z. M. & Batten, S. R. (2008). Inorg. Chem. Commun.11, 159–163.
  • Sheldrick, G. M. (2008). Acta Cryst. A64, 112–122. [PubMed]

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