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Acta Crystallogr Sect E Struct Rep Online. 2010 August 1; 66(Pt 8): m871.
Published online 2010 July 3. doi:  10.1107/S1600536810025171
PMCID: PMC3007391

(Perchlorato-κO)tris­(triphenyl­phosphine-κP)silver(I)

Abstract

In the title complex, [Ag(C18H15P)3(ClO4)], the silver coord­ination environment is dominated by the distorted P3AgO tetra­hedron in which Ag—O = 2.608 (12) Å and the Ag—P bond lengths are 2.5663 (17), 2.5076(16) and 2.5450 (17) Å. The perchlorate O-atoms are disordered over two positions in a 0.584 (14):0.416 (14) ratio.

Related literature

For similar compounds, see: Awaleh et al. (2005 [triangle]); Effendy et al. (2007a [triangle],b [triangle],c [triangle]); Jin et al. (2010 [triangle]); Di Nicola et al. (2007 [triangle]); Pettinari et al. (2007 [triangle]).

An external file that holds a picture, illustration, etc.
Object name is e-66-0m871-scheme1.jpg

Experimental

Crystal data

  • [Ag(C18H15P)3(ClO4)]
  • M r = 994.13
  • Monoclinic, An external file that holds a picture, illustration, etc.
Object name is e-66-0m871-efi1.jpg
  • a = 18.066 (2) Å
  • b = 13.7779 (16) Å
  • c = 19.064 (2) Å
  • β = 94.132 (2)°
  • V = 4733.0 (9) Å3
  • Z = 4
  • Mo Kα radiation
  • μ = 0.63 mm−1
  • T = 298 K
  • 0.19 × 0.18 × 0.17 mm

Data collection

  • Bruker SMART CCD area-detector diffractometer
  • Absorption correction: multi-scan (SADABS; Sheldrick, 2008 [triangle]) T min = 0.890, T max = 0.901
  • 23792 measured reflections
  • 8339 independent reflections
  • 4010 reflections with I > 2σ(I)
  • R int = 0.069

Refinement

  • R[F 2 > 2σ(F 2)] = 0.057
  • wR(F 2) = 0.128
  • S = 1.03
  • 8339 reflections
  • 605 parameters
  • H-atom parameters constrained
  • Δρmax = 0.85 e Å−3
  • Δρmin = −1.07 e Å−3

Data collection: SMART (Bruker, 2007 [triangle]); cell refinement: SAINT (Bruker, 2007 [triangle]); data reduction: SAINT; 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 angles (°)

Supplementary Material

Crystal structure: contains datablocks global, I. DOI: 10.1107/S1600536810025171/su2189sup1.cif

Structure factors: contains datablocks I. DOI: 10.1107/S1600536810025171/su2189Isup2.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 grants Nos. 2007CB310408 & 2006CB302901, and the Funding Project for Academic Human Resources Development in Institutions of Higher Learning under the jurisdiction of Beijing Municipality, and 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

Reports concerning with the structural and kinetic features of silver(I)-phosphine complexes are growing in number as the participation of these compounds in biological processes are discovered. A recent report (Effendy et al., 2007a) described a series of complexes of silver perchlorate and nitrate, tertiary phosphine ligand and oligodentate N-base adducts of the form AgX:dpex:L(2:1:2). In these complexes, the perchlorate acts either as a counteranion or as a ligand coordinating to silver(I) by one oxygen atom in a monodentate mode or by two oxygen atoms in a bidentate-chelating mode. We have studied the catalytic function of some nitrogen heterocyclic ligands (Jin et al., 2010), and herein we report on the new title complex, which was synthesized under catalysis of 2-aminopyrimidine.

The molecular structure of the title complex is depicted in Fig. 1. The silver atom is four coordinated by three phosphorus atoms from PPh3 groups and one oxygen atom from the ClO4 anion. The Ag—P distances are 2.5641 (14), 2.5047 (13) Å and 2.5415 (13) Å. The Ag—O distance [2.668 (14) Å] is slightly longer than that in adducts of AgClO4:dppe:bpy [2.539 (2) Å] (Effendy et al., 2007a). The angles P—Ag—P are in the range of 114.70 (4) - 119.17 (5)°, while angles P—Ag—O are in the range of 87.1 (4) - 118.1 (4) °, which comfirms the distorted tetrahedral environment around the silver atom.

The crystal structure data show little differences between the title complex and other AgX:PPh3:L, where X is a simple inorganic or organic anion, for example, nitrate (Di Nicola et al., 2007), nitrite (Pettinari et al., 2007), acetate (Effendy et al., 2007b), perchlorate (Effendy et al., 2007c) or trifluoroacetate (Awaleh et al., 2005).

Experimental

A mixture of AgClO4, PPh3 and 2-aminopyrimidine, in the molar ratio 1:1:2, in CH2Cl2 and MeOH (10 ml, V/V=1/1) was stirred for 2 h at ambient temperature, then filtered. Subsequent slow evaporation of the filtrate resulted in the formation of colorless crystals of the title complex. Crystals suitable for single-crystal X-ray diffraction were selected directly from the sample as prepared. Analysis found: C 65.40%, H 5.07%; calculated: C 65.19%, H 4.35%.

Refinement

The perchlorate O-atoms are disordered over two positions: refined occupancies O/O' = 0.584 (14)/0.416 (14). The H-atoms were included in calculated positions and treated as riding atoms: C-H = 0.93 Å with Uiso(H) = 1.2Ueq(parent C-atom).

Figures

Fig. 1.
A view of a basic unit of the title complex. Displacement ellipsoids are drawn at the 50% probability level and H-atoms have been omitted for clarity.

Crystal data

[Ag(C18H15P)3(ClO4)]F(000) = 2040
Mr = 994.13Dx = 1.395 Mg m3
Monoclinic, P21/nMo Kα radiation, λ = 0.71073 Å
Hall symbol: -P 2ynCell parameters from 2750 reflections
a = 18.066 (2) Åθ = 2.7–19.5°
b = 13.7779 (16) ŵ = 0.63 mm1
c = 19.064 (2) ÅT = 298 K
β = 94.132 (2)°Block, colourless
V = 4733.0 (9) Å30.19 × 0.18 × 0.17 mm
Z = 4

Data collection

Bruker SMART CCD area-detector diffractometer8339 independent reflections
Radiation source: fine-focus sealed tube4010 reflections with I > 2σ(I)
graphiteRint = 0.069
phi and ω scansθmax = 25.0°, θmin = 1.5°
Absorption correction: multi-scan (SADABS; Sheldrick, 2008)h = −21→19
Tmin = 0.890, Tmax = 0.901k = −13→16
23792 measured reflectionsl = −22→22

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)] = 0.057Hydrogen site location: inferred from neighbouring sites
wR(F2) = 0.128H-atom parameters constrained
S = 1.03w = 1/[σ2(Fo2) + (0.0375P)2] where P = (Fo2 + 2Fc2)/3
8339 reflections(Δ/σ)max = 0.001
605 parametersΔρmax = 0.85 e Å3
0 restraintsΔρmin = −1.07 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*/UeqOcc. (<1)
Ag10.24335 (3)0.81327 (3)0.01311 (2)0.05196 (17)
P10.34225 (9)0.68176 (12)0.00117 (8)0.0493 (4)
P20.17377 (9)0.80044 (11)0.12190 (8)0.0477 (4)
P30.26351 (10)0.98099 (11)−0.03809 (8)0.0519 (5)
Cl10.09855 (15)0.72401 (17)−0.11116 (12)0.0802 (6)
O10.1224 (7)0.8041 (13)−0.0700 (9)0.089 (5)0.584 (14)
O20.0255 (6)0.7017 (6)−0.0998 (4)0.080 (4)0.584 (14)
O30.1416 (7)0.6407 (8)−0.0977 (5)0.080 (4)0.584 (14)
O40.1075 (10)0.7556 (15)−0.1821 (10)0.105 (6)0.584 (14)
O1'0.1765 (8)0.7147 (13)−0.0977 (7)0.097 (6)0.416 (14)
O2'0.0779 (9)0.6317 (10)−0.0900 (7)0.080 (6)0.416 (14)
O3'0.0800 (10)0.8015 (17)−0.0690 (12)0.080 (6)0.416 (14)
O4'0.0664 (14)0.728 (2)−0.1794 (14)0.105 (9)0.416 (14)
C10.3718 (4)0.6630 (5)−0.0865 (3)0.0579 (18)
C20.3609 (4)0.7343 (5)−0.1358 (4)0.084 (2)
H20.33760.7916−0.12410.101*
C30.3840 (5)0.7227 (6)−0.2031 (4)0.102 (3)
H30.37560.7721−0.23600.123*
C40.4186 (5)0.6403 (6)−0.2217 (4)0.088 (2)
H40.43550.6342−0.26640.106*
C50.4285 (4)0.5664 (6)−0.1743 (4)0.095 (3)
H50.45080.5088−0.18700.114*
C60.4050 (4)0.5775 (5)−0.1071 (4)0.082 (2)
H60.41160.5267−0.07510.099*
C70.3143 (4)0.5609 (5)0.0251 (4)0.0632 (19)
C80.2590 (5)0.5177 (6)−0.0159 (4)0.096 (3)
H80.23710.5520−0.05400.115*
C90.2338 (5)0.4246 (7)−0.0034 (5)0.117 (3)
H90.19870.3953−0.03460.141*
C100.2612 (6)0.3772 (7)0.0549 (5)0.111 (3)
H100.24000.31870.06750.133*
C110.3199 (7)0.4149 (7)0.0955 (5)0.127 (4)
H110.34250.37900.13240.153*
C120.3457 (5)0.5080 (6)0.0809 (4)0.100 (3)
H120.38460.53450.10920.120*
C130.4285 (4)0.6985 (5)0.0558 (3)0.0600 (18)
C140.4977 (4)0.6821 (5)0.0321 (4)0.083 (2)
H140.50150.6629−0.01420.100*
C150.5622 (4)0.6935 (6)0.0762 (5)0.098 (3)
H150.60850.68300.05940.117*
C160.5561 (5)0.7207 (5)0.1453 (4)0.079 (2)
H160.59850.72640.17570.095*
C170.4898 (5)0.7387 (5)0.1686 (4)0.081 (2)
H170.48610.75830.21490.097*
C180.4253 (4)0.7284 (5)0.1235 (4)0.072 (2)
H180.37940.74220.14030.086*
C190.2416 (3)0.7986 (5)0.1960 (3)0.0549 (17)
C200.2915 (4)0.8770 (5)0.2022 (3)0.069 (2)
H200.28760.92720.16950.083*
C210.3461 (4)0.8798 (6)0.2567 (4)0.087 (2)
H210.37780.93290.26180.105*
C220.3534 (4)0.8046 (7)0.3030 (4)0.086 (2)
H220.39090.80650.33900.104*
C230.3075 (5)0.7275 (6)0.2978 (4)0.087 (2)
H230.31370.67700.33010.105*
C240.2503 (4)0.7230 (5)0.2438 (4)0.071 (2)
H240.21860.66980.24020.085*
C250.1121 (3)0.8980 (4)0.1440 (3)0.0477 (16)
C260.0521 (4)0.9169 (4)0.0966 (3)0.0610 (18)
H260.04590.88110.05520.073*
C270.0013 (4)0.9883 (5)0.1101 (4)0.070 (2)
H27−0.03930.99930.07830.084*
C280.0105 (4)1.0430 (5)0.1701 (4)0.069 (2)
H28−0.02371.09100.17910.083*
C290.0696 (4)1.0266 (5)0.2160 (4)0.069 (2)
H290.07671.06500.25610.082*
C300.1202 (4)0.9529 (5)0.2045 (3)0.0609 (18)
H300.15940.94080.23760.073*
C310.1149 (3)0.6960 (4)0.1318 (3)0.0524 (16)
C320.0666 (4)0.6891 (5)0.1848 (4)0.0699 (19)
H320.06600.73790.21850.084*
C330.0191 (4)0.6104 (6)0.1885 (4)0.082 (2)
H33−0.01270.60620.22460.098*
C340.0192 (4)0.5392 (6)0.1388 (5)0.082 (2)
H34−0.01350.48720.14050.099*
C350.0671 (5)0.5438 (5)0.0865 (4)0.088 (2)
H350.06780.49440.05340.105*
C360.1148 (4)0.6225 (5)0.0831 (4)0.070 (2)
H360.14710.62540.04740.083*
C370.1963 (4)1.0789 (4)−0.0370 (3)0.0534 (17)
C380.1552 (4)1.0904 (5)0.0203 (4)0.0644 (19)
H380.16141.04700.05760.077*
C390.1041 (4)1.1663 (5)0.0236 (4)0.070 (2)
H390.07681.17300.06280.084*
C400.0943 (4)1.2308 (5)−0.0310 (4)0.067 (2)
H400.06101.2820−0.02860.080*
C410.1332 (4)1.2192 (5)−0.0882 (4)0.074 (2)
H410.12541.2619−0.12570.089*
C420.1845 (4)1.1457 (5)−0.0922 (3)0.0660 (19)
H420.21141.1403−0.13180.079*
C430.3407 (4)1.0289 (5)0.0146 (3)0.0617 (19)
C440.3482 (5)1.1219 (6)0.0385 (4)0.103 (3)
H440.31181.16690.02420.123*
C450.4078 (6)1.1526 (7)0.0834 (5)0.121 (3)
H450.41101.21690.09820.145*
C460.4611 (5)1.0881 (8)0.1054 (4)0.109 (3)
H460.50061.10770.13610.131*
C470.4567 (5)0.9952 (8)0.0826 (5)0.127 (4)
H470.49370.95080.09640.152*
C480.3963 (5)0.9671 (6)0.0385 (4)0.101 (3)
H480.39330.90260.02420.121*
C490.2882 (4)0.9838 (4)−0.1286 (3)0.0586 (18)
C500.2438 (4)0.9347 (5)−0.1780 (4)0.073 (2)
H500.20440.8975−0.16410.088*
C510.2574 (5)0.9402 (6)−0.2484 (4)0.089 (2)
H510.22640.9072−0.28140.106*
C520.3145 (5)0.9924 (6)−0.2702 (4)0.091 (3)
H520.32320.9946−0.31770.109*
C530.3594 (4)1.0416 (5)−0.2222 (4)0.083 (2)
H530.39881.0780−0.23680.099*
C540.3465 (4)1.0378 (5)−0.1515 (4)0.071 (2)
H540.37741.0718−0.11900.086*

Atomic displacement parameters (Å2)

U11U22U33U12U13U23
Ag10.0555 (3)0.0565 (3)0.0441 (3)−0.0045 (3)0.0050 (2)−0.0010 (3)
P10.0562 (11)0.0492 (10)0.0425 (9)−0.0009 (9)0.0046 (8)−0.0011 (8)
P20.0503 (11)0.0525 (11)0.0405 (9)−0.0021 (8)0.0053 (8)−0.0001 (8)
P30.0540 (12)0.0500 (11)0.0511 (10)−0.0032 (8)−0.0011 (9)0.0055 (8)
Cl10.0718 (19)0.0748 (17)0.0907 (17)0.0112 (14)−0.0162 (14)−0.0081 (13)
O10.066 (10)0.110 (9)0.087 (7)−0.031 (11)−0.029 (9)−0.029 (6)
O20.072 (8)0.075 (7)0.091 (7)0.011 (5)−0.016 (5)−0.008 (5)
O30.072 (9)0.075 (8)0.091 (7)0.011 (7)−0.016 (6)−0.008 (5)
O40.126 (16)0.123 (13)0.058 (8)0.007 (10)−0.042 (11)−0.014 (7)
O1'0.072 (11)0.097 (14)0.116 (11)0.001 (9)−0.028 (8)−0.033 (9)
O2'0.072 (13)0.075 (11)0.091 (10)0.011 (9)−0.016 (9)−0.008 (7)
O3'0.072 (13)0.075 (12)0.091 (10)0.011 (12)−0.016 (12)−0.008 (8)
O4'0.13 (2)0.123 (18)0.058 (11)0.007 (14)−0.042 (15)−0.014 (10)
C10.072 (5)0.058 (5)0.045 (4)0.008 (4)0.011 (3)−0.002 (3)
C20.114 (7)0.081 (6)0.060 (5)0.024 (5)0.021 (5)−0.005 (4)
C30.151 (9)0.099 (7)0.060 (5)0.025 (6)0.026 (5)0.016 (5)
C40.120 (7)0.093 (6)0.056 (5)0.020 (5)0.036 (5)0.001 (5)
C50.122 (8)0.100 (7)0.066 (5)0.036 (5)0.033 (5)−0.007 (5)
C60.105 (7)0.082 (6)0.062 (5)0.025 (5)0.020 (5)0.003 (4)
C70.084 (6)0.053 (5)0.053 (4)0.006 (4)0.010 (4)−0.004 (4)
C80.099 (7)0.072 (6)0.113 (7)−0.011 (5)−0.020 (6)0.009 (5)
C90.130 (9)0.082 (8)0.139 (9)−0.028 (6)0.002 (7)−0.006 (6)
C100.148 (10)0.078 (7)0.111 (8)−0.039 (7)0.037 (7)0.001 (6)
C110.195 (12)0.096 (8)0.090 (7)−0.023 (7)0.006 (7)0.009 (6)
C120.150 (9)0.072 (6)0.075 (6)−0.030 (6)−0.009 (6)0.003 (5)
C130.057 (5)0.067 (5)0.055 (4)0.010 (4)0.002 (4)0.001 (4)
C140.075 (6)0.111 (6)0.062 (5)0.012 (5)−0.004 (4)−0.016 (5)
C150.059 (6)0.133 (7)0.100 (7)0.012 (5)0.000 (5)−0.006 (6)
C160.066 (6)0.095 (6)0.074 (6)0.002 (4)−0.019 (5)0.003 (4)
C170.072 (6)0.101 (6)0.068 (5)0.002 (5)−0.009 (5)−0.006 (4)
C180.068 (6)0.083 (5)0.064 (5)0.005 (4)0.000 (4)−0.014 (4)
C190.055 (5)0.066 (5)0.044 (4)0.003 (4)0.008 (3)−0.001 (3)
C200.065 (5)0.082 (5)0.058 (5)−0.006 (4)−0.004 (4)−0.001 (4)
C210.077 (6)0.109 (7)0.074 (6)−0.010 (5)−0.011 (5)−0.016 (5)
C220.074 (6)0.120 (8)0.062 (5)0.014 (6)−0.013 (4)−0.005 (5)
C230.093 (7)0.102 (7)0.066 (5)0.013 (5)−0.004 (5)0.005 (5)
C240.068 (5)0.083 (6)0.062 (5)0.010 (4)0.000 (4)0.001 (4)
C250.052 (5)0.045 (4)0.046 (4)−0.004 (3)0.007 (3)0.002 (3)
C260.065 (5)0.058 (5)0.059 (4)0.001 (4)0.000 (4)−0.006 (3)
C270.064 (5)0.069 (5)0.077 (5)0.001 (4)0.002 (4)0.003 (4)
C280.073 (6)0.059 (5)0.078 (5)0.007 (4)0.022 (4)0.000 (4)
C290.084 (6)0.063 (5)0.060 (5)0.004 (4)0.013 (4)−0.008 (4)
C300.068 (5)0.062 (5)0.053 (4)0.005 (4)0.007 (4)0.002 (4)
C310.054 (4)0.052 (4)0.051 (4)0.003 (3)0.003 (3)0.004 (3)
C320.078 (5)0.062 (5)0.071 (5)−0.008 (4)0.015 (4)−0.002 (4)
C330.076 (6)0.075 (6)0.097 (6)−0.013 (5)0.025 (5)0.018 (5)
C340.079 (7)0.065 (6)0.101 (7)−0.017 (4)−0.004 (5)0.012 (5)
C350.096 (7)0.066 (6)0.100 (7)−0.011 (5)0.001 (6)−0.010 (5)
C360.073 (6)0.063 (5)0.074 (5)−0.007 (4)0.013 (4)−0.002 (4)
C370.059 (5)0.048 (4)0.052 (4)−0.007 (3)−0.003 (4)0.001 (3)
C380.067 (5)0.060 (5)0.066 (5)−0.002 (4)0.001 (4)0.002 (4)
C390.072 (6)0.065 (5)0.071 (5)−0.001 (4)0.005 (4)−0.006 (4)
C400.067 (5)0.059 (5)0.072 (5)0.009 (4)−0.003 (4)−0.007 (4)
C410.087 (6)0.064 (5)0.071 (5)0.012 (4)−0.004 (5)0.010 (4)
C420.073 (5)0.065 (5)0.060 (5)0.007 (4)0.005 (4)0.004 (4)
C430.062 (5)0.061 (5)0.061 (4)−0.004 (4)−0.007 (4)0.014 (4)
C440.085 (7)0.095 (7)0.123 (8)−0.004 (5)−0.024 (6)−0.014 (6)
C450.108 (9)0.109 (8)0.140 (9)−0.016 (6)−0.028 (7)−0.040 (7)
C460.096 (8)0.128 (9)0.098 (7)−0.027 (7)−0.037 (6)0.006 (6)
C470.098 (8)0.125 (9)0.149 (9)−0.010 (7)−0.050 (7)0.025 (7)
C480.086 (7)0.088 (7)0.122 (7)−0.012 (5)−0.031 (6)0.002 (5)
C490.066 (5)0.054 (4)0.055 (4)0.001 (4)−0.002 (4)0.006 (3)
C500.080 (6)0.079 (5)0.062 (5)−0.014 (4)0.007 (4)0.001 (4)
C510.097 (7)0.104 (6)0.063 (5)−0.010 (5)−0.011 (5)−0.003 (5)
C520.104 (8)0.103 (7)0.067 (6)−0.001 (5)0.011 (6)0.006 (5)
C530.083 (6)0.092 (6)0.076 (6)−0.009 (5)0.025 (5)0.017 (5)
C540.073 (6)0.076 (5)0.066 (5)−0.007 (4)0.005 (4)0.005 (4)

Geometric parameters (Å, °)

Ag1—P22.5076 (16)C22—C231.347 (9)
Ag1—P32.5450 (17)C22—H220.9300
Ag1—P12.5663 (17)C23—C241.407 (9)
Ag1—O12.608 (12)C23—H230.9300
P1—C71.809 (7)C24—H240.9300
P1—C11.809 (6)C25—C301.378 (7)
P1—C131.826 (6)C25—C261.386 (7)
P2—C191.803 (6)C26—C271.382 (8)
P2—C311.808 (6)C26—H260.9300
P2—C251.815 (6)C27—C281.369 (8)
P3—C431.785 (7)C27—H270.9300
P3—C491.814 (7)C28—C291.351 (8)
P3—C371.815 (6)C28—H280.9300
Cl1—O21.386 (10)C29—C301.393 (8)
Cl1—O4'1.39 (2)C29—H290.9300
Cl1—O3'1.39 (2)C30—H300.9300
Cl1—O2'1.393 (14)C31—C361.373 (8)
Cl1—O31.400 (10)C31—C321.386 (8)
Cl1—O11.403 (16)C32—C331.388 (9)
Cl1—O1'1.419 (14)C32—H320.9300
Cl1—O41.44 (2)C33—C341.363 (9)
C1—C21.364 (8)C33—H330.9300
C1—C61.391 (8)C34—C351.368 (10)
C2—C31.388 (9)C34—H340.9300
C2—H20.9300C35—C361.389 (9)
C3—C41.354 (9)C35—H350.9300
C3—H30.9300C36—H360.9300
C4—C51.365 (9)C37—C381.374 (8)
C4—H40.9300C37—C421.403 (8)
C5—C61.386 (9)C38—C391.399 (8)
C5—H50.9300C38—H380.9300
C6—H60.9300C39—C401.369 (8)
C7—C81.361 (9)C39—H390.9300
C7—C121.377 (9)C40—C411.349 (9)
C8—C91.386 (10)C40—H400.9300
C8—H80.9300C41—C421.378 (8)
C9—C101.351 (11)C41—H410.9300
C9—H90.9300C42—H420.9300
C10—C111.370 (11)C43—C441.363 (9)
C10—H100.9300C43—C481.370 (9)
C11—C121.399 (10)C44—C451.392 (10)
C11—H110.9300C44—H440.9300
C12—H120.9300C45—C461.354 (11)
C13—C181.359 (8)C45—H450.9300
C13—C141.378 (9)C46—C471.353 (11)
C14—C151.395 (9)C46—H460.9300
C14—H140.9300C47—C481.384 (10)
C15—C161.382 (9)C47—H470.9300
C15—H150.9300C48—H480.9300
C16—C171.330 (9)C49—C501.370 (8)
C16—H160.9300C49—C541.386 (8)
C17—C181.405 (8)C50—C511.385 (9)
C17—H170.9300C50—H500.9300
C18—H180.9300C51—C521.348 (10)
C19—C241.385 (8)C51—H510.9300
C19—C201.406 (8)C52—C531.360 (9)
C20—C211.382 (8)C52—H520.9300
C20—H200.9300C53—C541.384 (8)
C21—C221.360 (9)C53—H530.9300
C21—H210.9300C54—H540.9300
P2—Ag1—P3118.38 (6)C24—C19—P2124.3 (5)
P2—Ag1—P1114.66 (5)C20—C19—P2116.7 (5)
P3—Ag1—P1119.17 (6)C21—C20—C19120.2 (7)
P2—Ag1—O192.9 (4)C21—C20—H20119.9
P3—Ag1—O187.0 (4)C19—C20—H20119.9
P1—Ag1—O1118.0 (4)C22—C21—C20119.8 (7)
C7—P1—C1102.0 (3)C22—C21—H21120.1
C7—P1—C13102.4 (3)C20—C21—H21120.1
C1—P1—C13104.4 (3)C23—C22—C21121.5 (8)
C7—P1—Ag1114.7 (2)C23—C22—H22119.2
C1—P1—Ag1115.9 (2)C21—C22—H22119.2
C13—P1—Ag1115.6 (2)C22—C23—C24120.2 (8)
C19—P2—C31106.2 (3)C22—C23—H23119.9
C19—P2—C25102.8 (3)C24—C23—H23119.9
C31—P2—C25101.0 (3)C19—C24—C23119.4 (7)
C19—P2—Ag1107.2 (2)C19—C24—H24120.3
C31—P2—Ag1118.4 (2)C23—C24—H24120.3
C25—P2—Ag1119.49 (19)C30—C25—C26118.2 (6)
C43—P3—C49107.0 (3)C30—C25—P2124.9 (5)
C43—P3—C37102.4 (3)C26—C25—P2116.9 (5)
C49—P3—C37101.8 (3)C27—C26—C25120.7 (6)
C43—P3—Ag1104.3 (2)C27—C26—H26119.6
C49—P3—Ag1115.9 (2)C25—C26—H26119.6
C37—P3—Ag1123.8 (2)C28—C27—C26120.4 (7)
O2—Cl1—O4'79.4 (12)C28—C27—H27119.8
O2—Cl1—O3'79.0 (9)C26—C27—H27119.8
O4'—Cl1—O3'113.9 (16)C29—C28—C27119.5 (7)
O2—Cl1—O2'58.4 (7)C29—C28—H28120.3
O4'—Cl1—O2'102.1 (12)C27—C28—H28120.3
O3'—Cl1—O2'116.9 (11)C28—C29—C30121.0 (6)
O2—Cl1—O3108.2 (7)C28—C29—H29119.5
O4'—Cl1—O3113.4 (14)C30—C29—H29119.5
O3'—Cl1—O3132.6 (9)C25—C30—C29120.1 (6)
O2'—Cl1—O349.8 (6)C25—C30—H30119.9
O2—Cl1—O1110.2 (7)C29—C30—H30119.9
O4'—Cl1—O1125.5 (14)C36—C31—C32118.1 (6)
O3'—Cl1—O131.9 (7)C36—C31—P2119.3 (5)
O2'—Cl1—O1129.3 (9)C32—C31—P2122.5 (5)
O3—Cl1—O1113.5 (8)C31—C32—C33121.0 (7)
O2—Cl1—O1'153.5 (8)C31—C32—H32119.5
O4'—Cl1—O1'121.1 (14)C33—C32—H32119.5
O3'—Cl1—O1'104.0 (8)C34—C33—C32119.7 (8)
O2'—Cl1—O1'98.5 (9)C34—C33—H33120.1
O3—Cl1—O1'50.4 (7)C32—C33—H33120.1
O1—Cl1—O1'73.1 (7)C33—C34—C35120.4 (7)
O2—Cl1—O4112.7 (7)C33—C34—H34119.8
O4'—Cl1—O434.4 (10)C35—C34—H34119.8
O3'—Cl1—O4111.0 (13)C34—C35—C36119.8 (7)
O2'—Cl1—O4126.7 (9)C34—C35—H35120.1
O3—Cl1—O4108.7 (11)C36—C35—H35120.1
O1—Cl1—O4103.7 (11)C31—C36—C35121.0 (7)
O1'—Cl1—O491.1 (10)C31—C36—H36119.5
Cl1—O1—Ag1126.0 (10)C35—C36—H36119.5
C2—C1—C6117.3 (6)C38—C37—C42117.2 (6)
C2—C1—P1119.7 (5)C38—C37—P3119.7 (5)
C6—C1—P1123.0 (5)C42—C37—P3123.0 (5)
C1—C2—C3121.1 (7)C37—C38—C39121.2 (6)
C1—C2—H2119.5C37—C38—H38119.4
C3—C2—H2119.5C39—C38—H38119.4
C4—C3—C2120.9 (7)C40—C39—C38120.1 (7)
C4—C3—H3119.6C40—C39—H39120.0
C2—C3—H3119.6C38—C39—H39120.0
C3—C4—C5119.5 (7)C41—C40—C39119.4 (7)
C3—C4—H4120.2C41—C40—H40120.3
C5—C4—H4120.2C39—C40—H40120.3
C4—C5—C6119.7 (7)C40—C41—C42121.6 (7)
C4—C5—H5120.2C40—C41—H41119.2
C6—C5—H5120.2C42—C41—H41119.2
C5—C6—C1121.4 (7)C41—C42—C37120.5 (7)
C1—C6—H6119.3C41—C42—H42119.8
C8—C7—C12117.1 (7)C37—C42—H42119.8
C8—C7—P1117.7 (6)C44—C43—C48114.9 (7)
C12—C7—P1125.1 (6)C44—C43—P3126.2 (6)
C7—C8—C9122.8 (8)C48—C43—P3118.8 (6)
C7—C8—H8118.6C43—C44—C45123.0 (8)
C9—C8—H8118.6C43—C44—H44118.5
C10—C9—C8119.0 (9)C45—C44—H44118.5
C10—C9—H9120.5C46—C45—C44119.5 (9)
C8—C9—H9120.5C46—C45—H45120.2
C9—C10—C11120.2 (9)C44—C45—H45120.2
C9—C10—H10119.9C47—C46—C45119.8 (9)
C11—C10—H10119.9C47—C46—H46120.1
C10—C11—C12119.3 (9)C45—C46—H46120.1
C10—C11—H11120.3C46—C47—C48119.1 (9)
C12—C11—H11120.3C46—C47—H47120.5
C7—C12—C11121.0 (8)C48—C47—H47120.5
C7—C12—H12119.5C43—C48—C47123.7 (8)
C11—C12—H12119.5C43—C48—H48118.1
C18—C13—C14117.6 (6)C47—C48—H48118.1
C18—C13—P1119.1 (6)C50—C49—C54118.0 (6)
C14—C13—P1123.4 (5)C50—C49—P3118.1 (6)
C13—C14—C15121.4 (7)C54—C49—P3123.8 (5)
C13—C14—H14119.3C49—C50—C51120.2 (7)
C15—C14—H14119.3C49—C50—H50119.9
C16—C15—C14119.0 (8)C51—C50—H50119.9
C16—C15—H15120.5C52—C51—C50121.4 (8)
C14—C15—H15120.5C52—C51—H51119.3
C17—C16—C15120.3 (7)C50—C51—H51119.3
C17—C16—H16119.9C51—C52—C53119.4 (8)
C15—C16—H16119.9C51—C52—H52120.3
C16—C17—C18120.3 (7)C53—C52—H52120.3
C16—C17—H17119.9C52—C53—C54120.2 (7)
C18—C17—H17119.9C52—C53—H53119.9
C13—C18—C17121.4 (7)C54—C53—H53119.9
C13—C18—H18119.3C53—C54—C49120.8 (7)
C17—C18—H18119.3C53—C54—H54119.6
C24—C19—C20118.8 (6)C49—C54—H54119.6
P2—Ag1—P1—C741.9 (3)C31—P2—C19—C20−176.2 (5)
P3—Ag1—P1—C7−169.3 (2)C25—P2—C19—C20−70.6 (5)
O1—Ag1—P1—C7−66.1 (5)Ag1—P2—C19—C2056.2 (5)
P2—Ag1—P1—C1160.5 (2)C24—C19—C20—C21−2.5 (10)
P3—Ag1—P1—C1−50.7 (2)P2—C19—C20—C21−178.6 (5)
O1—Ag1—P1—C152.5 (5)C19—C20—C21—C222.5 (11)
P2—Ag1—P1—C13−77.0 (2)C20—C21—C22—C23−1.2 (13)
P3—Ag1—P1—C1371.8 (2)C21—C22—C23—C240.0 (13)
O1—Ag1—P1—C13175.1 (5)C20—C19—C24—C231.3 (10)
P3—Ag1—P2—C19−94.4 (2)P2—C19—C24—C23177.0 (5)
P1—Ag1—P2—C1954.6 (2)C22—C23—C24—C190.0 (11)
O1—Ag1—P2—C19177.4 (5)C19—P2—C25—C30−0.2 (6)
P3—Ag1—P2—C31145.6 (2)C31—P2—C25—C30109.5 (6)
P1—Ag1—P2—C31−65.4 (2)Ag1—P2—C25—C30−118.7 (5)
O1—Ag1—P2—C3157.4 (4)C19—P2—C25—C26−179.1 (5)
P3—Ag1—P2—C2521.9 (2)C31—P2—C25—C26−69.4 (5)
P1—Ag1—P2—C25170.9 (2)Ag1—P2—C25—C2662.4 (5)
O1—Ag1—P2—C25−66.3 (5)C30—C25—C26—C27−0.6 (10)
P2—Ag1—P3—C4380.6 (3)P2—C25—C26—C27178.4 (5)
P1—Ag1—P3—C43−67.0 (3)C25—C26—C27—C281.3 (11)
O1—Ag1—P3—C43172.3 (5)C26—C27—C28—C290.0 (11)
P2—Ag1—P3—C49−162.1 (2)C27—C28—C29—C30−2.0 (11)
P1—Ag1—P3—C4950.3 (3)C26—C25—C30—C29−1.4 (9)
O1—Ag1—P3—C49−70.4 (5)P2—C25—C30—C29179.8 (5)
P2—Ag1—P3—C37−35.3 (2)C28—C29—C30—C252.7 (11)
P1—Ag1—P3—C37177.0 (2)C19—P2—C31—C36−114.7 (5)
O1—Ag1—P3—C3756.4 (5)C25—P2—C31—C36138.3 (5)
O2—Cl1—O1—Ag1129.0 (9)Ag1—P2—C31—C365.8 (6)
O4'—Cl1—O1—Ag1−139.7 (17)C19—P2—C31—C3268.7 (6)
O3'—Cl1—O1—Ag1142 (3)C25—P2—C31—C32−38.3 (6)
O2'—Cl1—O1—Ag164.0 (16)Ag1—P2—C31—C32−170.8 (4)
O3—Cl1—O1—Ag17.6 (14)C36—C31—C32—C33−0.4 (10)
O1'—Cl1—O1—Ag1−23.2 (10)P2—C31—C32—C33176.2 (5)
O4—Cl1—O1—Ag1−110.2 (12)C31—C32—C33—C34−0.7 (11)
P2—Ag1—O1—Cl1−106.1 (11)C32—C33—C34—C351.6 (12)
P3—Ag1—O1—Cl1135.6 (12)C33—C34—C35—C36−1.4 (12)
P1—Ag1—O1—Cl113.9 (13)C32—C31—C36—C350.6 (10)
C7—P1—C1—C2146.1 (6)P2—C31—C36—C35−176.2 (5)
C13—P1—C1—C2−107.6 (6)C34—C35—C36—C310.3 (11)
Ag1—P1—C1—C220.7 (7)C43—P3—C37—C38−79.7 (6)
C7—P1—C1—C6−33.1 (7)C49—P3—C37—C38169.7 (5)
C13—P1—C1—C673.2 (7)Ag1—P3—C37—C3837.1 (6)
Ag1—P1—C1—C6−158.5 (5)C43—P3—C37—C4299.3 (5)
C6—C1—C2—C3−1.8 (11)C49—P3—C37—C42−11.3 (6)
P1—C1—C2—C3179.0 (6)Ag1—P3—C37—C42−143.8 (4)
C1—C2—C3—C4−0.5 (13)C42—C37—C38—C39−0.6 (9)
C2—C3—C4—C52.4 (14)P3—C37—C38—C39178.5 (5)
C3—C4—C5—C6−1.9 (13)C37—C38—C39—C400.1 (10)
C4—C5—C6—C1−0.4 (12)C38—C39—C40—C411.1 (10)
C2—C1—C6—C52.3 (11)C39—C40—C41—C42−1.9 (11)
P1—C1—C6—C5−178.6 (6)C40—C41—C42—C371.5 (11)
C1—P1—C7—C8−59.7 (7)C38—C37—C42—C41−0.2 (9)
C13—P1—C7—C8−167.6 (6)P3—C37—C42—C41−179.3 (5)
Ag1—P1—C7—C866.4 (6)C49—P3—C43—C4497.5 (7)
C1—P1—C7—C12118.7 (7)C37—P3—C43—C44−9.2 (8)
C13—P1—C7—C1210.9 (7)Ag1—P3—C43—C44−139.3 (6)
Ag1—P1—C7—C12−115.1 (6)C49—P3—C43—C48−87.6 (6)
C12—C7—C8—C90.3 (13)C37—P3—C43—C48165.8 (6)
P1—C7—C8—C9178.8 (7)Ag1—P3—C43—C4835.7 (7)
C7—C8—C9—C105.1 (15)C48—C43—C44—C450.4 (12)
C8—C9—C10—C11−8.9 (16)P3—C43—C44—C45175.5 (7)
C9—C10—C11—C127.4 (16)C43—C44—C45—C46−0.6 (15)
C8—C7—C12—C11−1.8 (12)C44—C45—C46—C471.3 (16)
P1—C7—C12—C11179.7 (7)C45—C46—C47—C48−1.8 (16)
C10—C11—C12—C7−1.9 (14)C44—C43—C48—C47−0.9 (13)
C7—P1—C13—C18−83.5 (6)P3—C43—C48—C47−176.5 (7)
C1—P1—C13—C18170.5 (5)C46—C47—C48—C431.7 (15)
Ag1—P1—C13—C1842.0 (6)C43—P3—C49—C50168.3 (5)
C7—P1—C13—C1496.3 (6)C37—P3—C49—C50−84.6 (6)
C1—P1—C13—C14−9.7 (7)Ag1—P3—C49—C5052.5 (6)
Ag1—P1—C13—C14−138.2 (6)C43—P3—C49—C54−15.9 (7)
C18—C13—C14—C151.4 (11)C37—P3—C49—C5491.1 (6)
P1—C13—C14—C15−178.4 (6)Ag1—P3—C49—C54−131.8 (5)
C13—C14—C15—C160.9 (12)C54—C49—C50—C51−0.5 (10)
C14—C15—C16—C17−2.2 (12)P3—C49—C50—C51175.5 (6)
C15—C16—C17—C181.4 (12)C49—C50—C51—C520.9 (12)
C14—C13—C18—C17−2.3 (10)C50—C51—C52—C53−0.8 (13)
P1—C13—C18—C17177.5 (5)C51—C52—C53—C540.3 (13)
C16—C17—C18—C131.0 (11)C52—C53—C54—C490.1 (11)
C31—P2—C19—C247.9 (6)C50—C49—C54—C530.0 (10)
C25—P2—C19—C24113.5 (6)P3—C49—C54—C53−175.8 (5)
Ag1—P2—C19—C24−119.6 (5)

Footnotes

Supplementary data and figures for this paper are available from the IUCr electronic archives (Reference: SU2189).

References

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  • Di Nicola, C., Effendy, Marchetti, F., Pettinari, C., Skelton, B. W. & White, A. H. (2007). Inorg. Chim. Acta, 360, 1433–1450.
  • Effendy, Marchetti, F., Pettinari, C., Pettinari, R., Skelton, B.W &, White, A. H. (2007a). Inorg. Chim. Acta, 360, 1388–1413.
  • Effendy, Marchetti, F., Pettinari, C., Pettinari, R., Skelton, B. W. & White, A. H. (2007c). Inorg. Chim. Acta, 360, 1451–1465.
  • Effendy, Marchetti, F., Pettinari, C., Skelton, B. W. & White, A. H. (2007b). Inorg. Chim. Acta, 360, 1424–1432.
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