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Acta Crystallogr Sect E Struct Rep Online. 2009 April 1; 65(Pt 4): m441.
Published online 2009 March 25. doi:  10.1107/S1600536809010241
PMCID: PMC2968815

Di-μ-bromido-tris­(triphenyl­phosphine)-1κP,2κ2 P-disilver(I) tetra­hydro­furan 0.85-solvate

Abstract

In the title binuclear silver(I) complex, [Ag2Br2(C18H15P)3]·0.85C4H8O, the two independent silver(I) ions are briged by two bromide ions. One AgI ion is coordinated by two triphenyl­phosphine groups with a square-planar geometry, while the second is coordinated by one triphenyl­phine group with a trigonal-planar geometry. The structure is very similar to that of the dichloro­methane solvate reported by Zhu, Huang & Zheng [Chin. J. Struct. Chem. (1994), 13, 325–327]. The tetrahydrofuran solvent molecule is disordered and was refined with a fixed occupancy of 0.85.

Related literature

For the structure of the dichloro­methane solvate, see: Zhu et al. (1994 [triangle]). For general background on triphenyl­phosphine–silver(I) complexes, see: Whitcomb & Rajeswaram (2006 [triangle]); Whitcomb & Roger (1996 [triangle]); Mann et al. (1937 [triangle]); Teo & Calabrese (1976 [triangle]); Bowmaker et al. (1993 [triangle]); Olmstead et al. (2004 [triangle]); Zhang et al. (2003 [triangle]); Lobana et al. (2008 [triangle]); Cingolani et al. (2003 [triangle]). For the sensitization of photothermographic materials by coordination polymers formed by the reaction of triphenyl­phosphine with silver(I) salts, see: Freedman (1994 [triangle]).

An external file that holds a picture, illustration, etc.
Object name is e-65-0m441-scheme1.jpg

Experimental

Crystal data

  • [Ag2Br2(C18H15P)3]·0.85C4H8O
  • M r = 1223.66
  • Monoclinic, An external file that holds a picture, illustration, etc.
Object name is e-65-0m441-efi1.jpg
  • a = 16.2386 (19) Å
  • b = 19.4575 (17) Å
  • c = 18.3069 (18) Å
  • β = 111.896 (1)°
  • V = 5367.0 (9) Å3
  • Z = 4
  • Mo Kα radiation
  • μ = 2.35 mm−1
  • T = 293 K
  • 0.40 × 0.12 × 0.08 mm

Data collection

  • Rigaku Mercury CCD diffractometer
  • Absorption correction: multi-scan (SPHERE in CrystalClear; Rigaku, 2002 [triangle]) T min = 0.721, T max = 0.829
  • 36137 measured reflections
  • 9804 independent reflections
  • 4750 reflections with I > 2σ(I)
  • R int = 0.095

Refinement

  • R[F 2 > 2σ(F 2)] = 0.076
  • wR(F 2) = 0.115
  • S = 1.00
  • 9804 reflections
  • 596 parameters
  • H-atom parameters constrained
  • Δρmax = 0.37 e Å−3
  • Δρmin = −0.41 e Å−3

Data collection: CrystalClear (Rigaku, 2002 [triangle]); cell refinement: CrystalClear; data reduction: CrystalClear; 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.

Supplementary Material

Crystal structure: contains datablocks I, global. DOI: 10.1107/S1600536809010241/su2091sup1.cif

Structure factors: contains datablocks I. DOI: 10.1107/S1600536809010241/su2091Isup2.hkl

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

Acknowledgments

We gratefully acknowledge financial spupport by the NSF of China (20771023), the 863 Program (2007 A A03z218) and the Analysis and Testing Foundation of Northeast Normal University.

supplementary crystallographic information

Comment

As triphenylphosphine is an electrically neutral molecule, it can react with silver (I) salts to form coordination polymers, some of which can prompt the sensitization of photothermographic (PTG) materials (Freedman, 1994). Since the first tertiary phosphine silver (I) complexes of the type [AgXLn] (L is tertiary phosphine; n is 1-4; X is a coordinating or non-coordinating anion) were prepared in 1937 by Mann et al. (1937), many complexes have been obtained by the reaction of triphenylphosphine with an appropriate silver (I) salt (Whitcomb & Rajeswaram, 2006; Whitcomb & Roger, 1996; Teo et al., 1976; Bowmaker et al., 1993; Olmstead et al., 2004; Zhang et al., 2003; Lobana et al., 2008; Cingolani et al., 2003). In this paper, we report on the tetrahydrofuran (THF) solvate of the binuclear triphenylphosphine silver(I) complex, (I), synthesized using AgBr.

The molecular structure of (I) is shown in Fig. 1. The structure is a solvo-polymorph of the dichloromethane analogue, (II), described by Zhu et al. (1994). The bond distances and angles in the complex are similar to those reported for compound (II). Complex (I) contains a rhomboid cyclic [Ag2Br2] moiety, with three coordinated triphenylphosphine molecules and a THF solvent molecule. One of the two silver(I) atoms, Ag1, is four-coordinated by two bridging bromine atoms and two P-atoms from two triphenylphosphines ligands, forming a distorted tetrahedral geometry. The other silver(I) atom, Ag2, is three-coordinated by two bridging bromine atoms and one P-atom from a triphenylphosphine ligand, to form an irregular trigonal plane.

Experimental

In a glove box, AgBr (0.15 mmol, 0.028 g) and PPh3 (0.45 mmol, 0.118 g) were dissolved in 10 mL of distilled THF. The mixture was stirred for 2h to get a clear solution, then a little (3 ml) 1,2-bis(trimethylsilyl)ethyne was added to the above solution, and stirring was continued for three hours. The solution was then concentrated and the recipient sealed and placed in the refrigerator. After a few days colorless prismatic crystals of (I) were obtained.

Refinement

The H-atoms were included in calculated positions and treated as riding atoms: C-H = 0.93 - 0.97 Å with Uiso(H) = 1.2Ueq(parent C-atom). The intensity data were measured at room temperature and the crystal did not diffract very strongly; less than 50% of the data can be considered to be observed [I>2σ(I)]. Hence, the bond distances and angles are not very precise and some C-atoms suffer from thermal disorder. A disordered THF molecule is present in the asymmetric unit: occupancy fixed at 0.85.

Figures

Fig. 1.
The molecular structure of compound (I) showing the thermal ellipsoids drawn at the 30% probabilty level (the H-atoms and the THF molecule of crystallization have been omitted for clarity).

Crystal data

[Ag2Br2(C18H15P)3]·0.85C4H8OF(000) = 2448
Mr = 1223.66Dx = 1.514 Mg m3
Monoclinic, P21/cMo Kα radiation, λ = 0.71073 Å
Hall symbol: -P 2ybcCell parameters from 6309 reflections
a = 16.2386 (19) Åθ = 3.1–27.5°
b = 19.4575 (17) ŵ = 2.35 mm1
c = 18.3069 (18) ÅT = 293 K
β = 111.896 (1)°Prism, colorless
V = 5367.0 (9) Å30.40 × 0.12 × 0.08 mm
Z = 4

Data collection

Rigaku Mercury CCD diffractometer9804 independent reflections
Radiation source: rotating-anode generator4750 reflections with I > 2σ(I)
graphiteRint = 0.095
ω scansθmax = 25.4°, θmin = 3.1°
Absorption correction: multi-scan (SPHERE in CrystalClear; Rigaku, 2002)h = −18→19
Tmin = 0.721, Tmax = 0.829k = −23→22
36137 measured reflectionsl = −22→21

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)] = 0.076Hydrogen site location: inferred from neighbouring sites
wR(F2) = 0.115H-atom parameters constrained
S = 1.00w = 1/[σ2(Fo2) + (0.016P)2] where P = (Fo2 + 2Fc2)/3
9804 reflections(Δ/σ)max = 0.018
596 parametersΔρmax = 0.37 e Å3
0 restraintsΔρmin = −0.41 e Å3

Special details

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.

Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2)

xyzUiso*/UeqOcc. (<1)
Ag10.172104 (16)0.430186 (13)0.311968 (13)0.05624 (9)
Ag20.309939 (18)0.449839 (16)0.211990 (14)0.08013 (12)
Br10.23309 (2)0.549632 (18)0.258758 (19)0.06869 (13)
Br20.26760 (2)0.335663 (19)0.264353 (19)0.07471 (14)
P10.01808 (6)0.41825 (4)0.21950 (4)0.0519 (3)
P20.22977 (5)0.44191 (4)0.45510 (4)0.0485 (3)
P30.38713 (6)0.46569 (5)0.12429 (5)0.0626 (3)
C1010.00382 (19)0.40749 (14)0.11612 (15)0.0508 (11)
C102−0.0673 (2)0.37370 (17)0.06109 (16)0.0826 (15)
H10A−0.11130.35450.07580.099*
C103−0.0727 (2)0.36858 (18)−0.01647 (17)0.0834 (15)
H10B−0.12140.3472−0.05400.100*
C104−0.0071 (2)0.39468 (16)−0.03775 (16)0.0739 (14)
H10G−0.01130.3909−0.08960.089*
C1050.0644 (2)0.42627 (16)0.01636 (16)0.0736 (13)
H10F0.10950.44340.00180.088*
C1060.06945 (18)0.43261 (15)0.09268 (14)0.0571 (12)
H10C0.11840.45440.12940.068*
C107−0.04536 (17)0.49553 (14)0.22217 (14)0.0456 (10)
C108−0.1150 (2)0.52007 (16)0.15705 (16)0.0712 (13)
H10D−0.13180.49670.10940.085*
C109−0.1594 (2)0.57895 (17)0.16262 (17)0.0831 (15)
H10E−0.20600.59530.11880.100*
C110−0.1347 (2)0.61364 (16)0.23307 (17)0.0751 (13)
H11A−0.16460.65350.23670.090*
C111−0.0673 (2)0.58987 (16)0.29710 (18)0.0751 (14)
H11B−0.05150.61290.34490.090*
C112−0.0221 (2)0.53159 (15)0.29149 (15)0.0649 (13)
H11C0.02520.51630.33550.078*
C113−0.04710 (18)0.34765 (15)0.23595 (15)0.0516 (11)
C114−0.0173 (2)0.28130 (16)0.23901 (18)0.0875 (14)
H11D0.03550.27310.23180.105*
C115−0.0632 (2)0.22693 (17)0.25242 (19)0.1044 (17)
H11E−0.04140.18250.25380.125*
C116−0.1392 (2)0.23703 (16)0.26362 (18)0.0853 (15)
H11F−0.17040.20000.27250.102*
C117−0.1703 (2)0.30293 (16)0.26176 (17)0.0840 (14)
H11G−0.22270.31080.26990.101*
C118−0.1237 (2)0.35738 (15)0.24780 (16)0.0652 (12)
H11H−0.14550.40180.24650.078*
C2010.34954 (19)0.44201 (15)0.50661 (15)0.0538 (11)
C2020.39821 (18)0.40313 (15)0.47389 (17)0.0627 (13)
H20E0.36980.38020.42650.075*
C2030.4888 (2)0.39844 (17)0.51154 (18)0.0853 (16)
H20F0.52080.37110.48980.102*
C2040.5329 (2)0.43282 (19)0.57997 (18)0.0964 (17)
H20G0.59420.42950.60480.116*
C2050.4844 (2)0.47214 (19)0.61093 (19)0.0981 (17)
H20D0.51350.49600.65750.118*
C2060.3944 (2)0.47745 (18)0.57535 (16)0.0790 (15)
H20A0.36310.50510.59750.095*
C2070.1921 (2)0.52024 (15)0.48663 (15)0.0567 (12)
C2080.2164 (2)0.58233 (16)0.46320 (19)0.0945 (15)
H20B0.25340.58190.43470.113*
C2090.1880 (3)0.6440 (2)0.4805 (2)0.1249 (19)
H20C0.20430.68470.46290.150*
C2100.1354 (3)0.64572 (18)0.5238 (2)0.1132 (19)
H21A0.11670.68750.53710.136*
C2110.1107 (2)0.58514 (17)0.54747 (19)0.0973 (15)
H21B0.07360.58590.57580.117*
C2120.1398 (2)0.52266 (17)0.53001 (16)0.0704 (13)
H21C0.12350.48210.54800.084*
C2130.19096 (18)0.37368 (14)0.50264 (15)0.0509 (11)
C2140.11738 (19)0.33772 (15)0.45777 (17)0.0655 (13)
H21D0.08940.34870.40480.079*
C2150.0833 (2)0.28525 (16)0.48909 (18)0.0841 (15)
H21E0.03150.26260.45840.101*
C2160.1273 (2)0.26735 (16)0.56627 (18)0.0838 (14)
H21F0.10680.23140.58840.101*
C2170.2027 (2)0.30337 (16)0.61092 (17)0.0752 (14)
H21G0.23240.29120.66340.090*
C2180.23466 (19)0.35619 (15)0.58029 (15)0.0607 (12)
H21H0.28520.38000.61140.073*
C3010.3497 (2)0.53937 (15)0.05832 (16)0.0585 (12)
C3020.3280 (2)0.59806 (16)0.08938 (19)0.0826 (15)
H30A0.32890.59800.14050.099*
C3030.3048 (2)0.65782 (18)0.0436 (2)0.0967 (17)
H30B0.29230.69800.06500.116*
C3040.3003 (2)0.65737 (18)−0.03249 (18)0.0871 (16)
H30C0.28430.6970−0.06300.105*
C3050.3194 (2)0.59866 (17)−0.06341 (18)0.0798 (15)
H30D0.31550.5980−0.11540.096*
C3060.3448 (2)0.53976 (16)−0.01771 (16)0.0646 (13)
H30E0.35850.5001−0.03920.077*
C3070.38065 (19)0.39381 (15)0.05913 (16)0.0542 (12)
C3080.3072 (2)0.35043 (15)0.03950 (16)0.0695 (13)
H30F0.26490.35700.06190.083*
C3090.2978 (2)0.29778 (17)−0.01327 (18)0.0878 (16)
H30G0.24790.2698−0.02730.105*
C3100.3590 (2)0.28579 (15)−0.04500 (18)0.0881 (16)
H31A0.35170.2501−0.08070.106*
C3110.4333 (2)0.32783 (16)−0.02323 (17)0.0813 (14)
H31B0.47680.3195−0.04390.098*
C3120.4440 (2)0.38156 (16)0.02830 (17)0.0825 (14)
H31C0.49400.40940.04210.099*
C3130.50559 (19)0.48006 (15)0.17267 (15)0.0552 (11)
C3140.5493 (2)0.53755 (16)0.16275 (16)0.0694 (14)
H31D0.51750.57160.12800.083*
C3150.6389 (2)0.54602 (18)0.20288 (17)0.0817 (15)
H31E0.66630.58560.19460.098*
C3160.6876 (2)0.49874 (16)0.25364 (17)0.0793 (15)
H31F0.74810.50560.28100.095*
C3170.6473 (2)0.44027 (17)0.26461 (17)0.0835 (15)
H31G0.68090.40600.29780.100*
C3180.5564 (2)0.43179 (17)0.22653 (17)0.0737 (14)
H31H0.52910.39320.23720.088*
O110.6007 (2)0.26438 (16)0.28899 (18)0.1287 (16)0.85
C110.5807 (3)0.2330 (2)0.2174 (3)0.132 (2)0.85
H11I0.61790.19280.22280.158*0.85
H11J0.59080.26430.18040.158*0.85
C120.4917 (3)0.2138 (3)0.1907 (3)0.157 (3)0.85
H12A0.45710.24130.14540.188*0.85
H12B0.48510.16580.17540.188*0.85
C130.4646 (3)0.2242 (3)0.2490 (3)0.155 (3)0.85
H13A0.45180.18050.26810.186*0.85
H13B0.41060.25130.23090.186*0.85
C140.5310 (3)0.2589 (2)0.3100 (2)0.126 (2)0.85
H14C0.51040.30400.31770.151*0.85
H14A0.54680.23330.35880.151*0.85

Atomic displacement parameters (Å2)

U11U22U33U12U13U23
Ag10.04831 (14)0.07159 (17)0.04870 (12)0.00071 (14)0.01794 (10)−0.00254 (13)
Ag20.05967 (17)0.1225 (3)0.06481 (15)−0.00171 (18)0.03082 (12)−0.00557 (16)
Br10.0779 (2)0.0623 (2)0.07304 (19)−0.0086 (2)0.03638 (16)−0.00307 (18)
Br20.0881 (3)0.0738 (2)0.0647 (2)0.0226 (2)0.03131 (17)−0.00624 (19)
P10.0470 (5)0.0608 (6)0.0481 (4)−0.0007 (5)0.0180 (4)−0.0051 (4)
P20.0496 (5)0.0526 (5)0.0450 (4)−0.0035 (4)0.0196 (3)−0.0037 (4)
P30.0593 (5)0.0730 (6)0.0632 (5)−0.0054 (5)0.0318 (4)−0.0106 (5)
C1010.0480 (19)0.057 (2)0.0455 (16)0.0037 (16)0.0154 (14)−0.0045 (15)
C1020.084 (3)0.109 (3)0.0589 (19)−0.021 (2)0.0313 (17)−0.0320 (19)
C1030.074 (3)0.112 (3)0.058 (2)−0.015 (2)0.0182 (18)−0.026 (2)
C1040.085 (2)0.095 (3)0.0521 (17)0.014 (2)0.0371 (15)−0.0034 (18)
C1050.070 (2)0.096 (3)0.0567 (18)0.025 (2)0.0261 (15)0.0230 (19)
C1060.0438 (18)0.079 (2)0.0479 (16)0.0015 (18)0.0166 (14)0.0018 (17)
C1070.0373 (16)0.060 (2)0.0452 (15)−0.0012 (15)0.0218 (12)0.0043 (15)
C1080.072 (2)0.083 (3)0.0632 (19)−0.004 (2)0.0303 (16)0.0070 (19)
C1090.081 (2)0.096 (3)0.078 (2)0.031 (2)0.0355 (17)0.022 (2)
C1100.070 (2)0.062 (2)0.110 (2)0.0080 (19)0.0527 (16)−0.0022 (19)
C1110.065 (2)0.068 (2)0.088 (2)−0.0039 (19)0.0236 (18)−0.0306 (19)
C1120.060 (2)0.075 (2)0.0500 (18)0.003 (2)0.0098 (16)−0.0131 (18)
C1130.0396 (18)0.061 (2)0.0521 (17)−0.0003 (16)0.0147 (13)−0.0077 (16)
C1140.082 (2)0.066 (2)0.139 (2)0.017 (2)0.0688 (17)0.005 (2)
C1150.128 (3)0.047 (2)0.167 (3)0.006 (2)0.089 (2)0.008 (2)
C1160.099 (3)0.061 (2)0.104 (2)−0.023 (2)0.0473 (19)−0.010 (2)
C1170.083 (2)0.079 (3)0.111 (2)−0.005 (2)0.0613 (16)0.010 (2)
C1180.075 (2)0.047 (2)0.084 (2)0.0006 (18)0.0425 (15)0.0128 (17)
C2010.0556 (18)0.054 (2)0.0568 (16)−0.0097 (16)0.0271 (13)0.0001 (16)
C2020.0341 (19)0.075 (2)0.073 (2)−0.0039 (17)0.0140 (15)−0.0096 (18)
C2030.059 (2)0.108 (3)0.086 (2)0.006 (2)0.0237 (19)0.007 (2)
C2040.054 (3)0.150 (4)0.067 (2)0.006 (3)0.0009 (19)0.023 (2)
C2050.070 (3)0.140 (3)0.075 (2)−0.037 (3)0.018 (2)−0.026 (2)
C2060.061 (2)0.121 (3)0.0543 (19)−0.024 (2)0.0203 (16)−0.026 (2)
C2070.064 (2)0.055 (2)0.0489 (17)−0.0067 (17)0.0195 (15)−0.0026 (16)
C2080.120 (3)0.062 (2)0.131 (2)−0.012 (2)0.0817 (18)−0.022 (2)
C2090.175 (4)0.076 (3)0.154 (3)−0.017 (3)0.098 (2)−0.021 (2)
C2100.134 (3)0.067 (3)0.146 (3)0.012 (2)0.060 (2)−0.033 (2)
C2110.102 (3)0.088 (3)0.121 (2)0.022 (2)0.0646 (18)−0.022 (2)
C2120.079 (2)0.069 (2)0.0730 (19)0.011 (2)0.0386 (16)0.0043 (18)
C2130.0508 (18)0.051 (2)0.0545 (17)0.0040 (16)0.0242 (13)0.0006 (15)
C2140.055 (2)0.070 (2)0.0660 (19)−0.0041 (19)0.0163 (16)0.0121 (18)
C2150.071 (2)0.056 (2)0.130 (3)−0.010 (2)0.0440 (19)0.009 (2)
C2160.095 (2)0.067 (2)0.120 (2)0.0102 (19)0.0753 (16)0.0272 (19)
C2170.083 (2)0.070 (2)0.074 (2)0.018 (2)0.0315 (17)0.0097 (19)
C2180.054 (2)0.062 (2)0.0650 (19)−0.0105 (18)0.0212 (15)0.0061 (17)
C3010.0513 (19)0.065 (2)0.0597 (17)−0.0014 (17)0.0214 (14)−0.0147 (17)
C3020.074 (3)0.091 (3)0.080 (2)0.009 (2)0.0258 (18)−0.005 (2)
C3030.085 (3)0.079 (3)0.118 (3)0.011 (2)0.027 (2)−0.033 (2)
C3040.087 (3)0.080 (3)0.089 (2)0.010 (2)0.026 (2)0.003 (2)
C3050.066 (2)0.094 (3)0.079 (2)−0.001 (2)0.0267 (18)0.005 (2)
C3060.064 (2)0.068 (2)0.0592 (18)−0.0032 (19)0.0195 (16)−0.0171 (17)
C3070.0476 (19)0.053 (2)0.0595 (18)−0.0010 (17)0.0171 (15)−0.0005 (16)
C3080.079 (2)0.065 (2)0.0651 (19)−0.012 (2)0.0278 (17)−0.0027 (18)
C3090.097 (3)0.074 (3)0.080 (2)−0.023 (2)0.018 (2)−0.003 (2)
C3100.152 (3)0.037 (2)0.079 (2)−0.016 (2)0.047 (2)−0.0093 (18)
C3110.123 (3)0.064 (2)0.0759 (19)0.002 (2)0.0590 (17)−0.0107 (18)
C3120.095 (2)0.077 (2)0.095 (2)−0.021 (2)0.0578 (17)−0.0362 (19)
C3130.0551 (19)0.064 (2)0.0494 (16)0.0007 (17)0.0229 (14)−0.0165 (16)
C3140.061 (2)0.069 (2)0.074 (2)−0.0044 (19)0.0199 (17)0.0019 (19)
C3150.058 (2)0.103 (3)0.083 (2)−0.013 (2)0.0250 (18)−0.007 (2)
C3160.055 (2)0.097 (3)0.078 (2)0.002 (2)0.0154 (18)−0.031 (2)
C3170.081 (3)0.084 (3)0.071 (2)0.028 (2)0.0124 (19)−0.003 (2)
C3180.073 (2)0.072 (2)0.078 (2)−0.001 (2)0.0311 (17)−0.011 (2)
O110.118 (3)0.128 (3)0.129 (2)−0.019 (2)0.033 (2)0.021 (2)
C110.116 (3)0.134 (5)0.177 (4)0.002 (3)0.093 (3)0.020 (3)
C120.130 (5)0.173 (5)0.150 (4)0.014 (4)0.031 (4)−0.054 (4)
C130.072 (4)0.142 (5)0.247 (6)0.009 (4)0.056 (4)0.011 (5)
C140.167 (5)0.124 (4)0.090 (3)0.049 (4)0.051 (3)0.051 (3)

Geometric parameters (Å, °)

Ag1—P22.4423 (8)C209—C2101.365 (6)
Ag1—P12.4530 (8)C209—H20C0.9300
Ag1—Br22.7487 (5)C210—C2111.367 (5)
Ag1—Br12.8374 (5)C210—H21A0.9300
Ag2—P32.3968 (11)C211—C2121.384 (5)
Ag2—Br22.6112 (5)C211—H21B0.9300
Ag2—Br12.6186 (5)C212—H21C0.9300
P1—C1131.826 (3)C213—C2141.364 (4)
P1—C1011.831 (3)C213—C2181.374 (3)
P1—C1071.833 (3)C214—C2151.383 (5)
P2—C2071.815 (3)C214—H21D0.9300
P2—C2011.818 (3)C215—C2161.369 (4)
P2—C2131.824 (3)C215—H21E0.9300
P3—C3131.814 (3)C216—C2171.382 (4)
P3—C3071.816 (3)C216—H21F0.9300
P3—C3011.826 (3)C217—C2181.363 (4)
C101—C1061.378 (4)C217—H21G0.9300
C101—C1021.383 (4)C218—H21H0.9300
C102—C1031.393 (4)C301—C3061.364 (4)
C102—H10A0.9300C301—C3021.378 (4)
C103—C1041.361 (5)C302—C3031.400 (5)
C103—H10B0.9300C302—H30A0.9300
C104—C1051.360 (4)C303—C3041.368 (5)
C104—H10G0.9300C303—H30B0.9300
C105—C1061.374 (4)C304—C3051.361 (5)
C105—H10F0.9300C304—H30C0.9300
C106—H10C0.9300C305—C3061.388 (4)
C107—C1121.374 (4)C305—H30D0.9300
C107—C1081.387 (3)C306—H30E0.9300
C108—C1091.377 (5)C307—C3121.366 (5)
C108—H10D0.9300C307—C3081.394 (4)
C109—C1101.376 (4)C308—C3091.377 (4)
C109—H10E0.9300C308—H30F0.9300
C110—C1111.353 (4)C309—C3101.346 (6)
C110—H11A0.9300C309—H30G0.9300
C111—C1121.375 (4)C310—C3111.387 (5)
C111—H11B0.9300C310—H31A0.9300
C112—H11C0.9300C311—C3121.375 (4)
C113—C1181.354 (5)C311—H31B0.9300
C113—C1141.372 (4)C312—H31C0.9300
C114—C1151.368 (5)C313—C3141.373 (4)
C114—H11D0.9300C313—C3181.389 (4)
C115—C1161.338 (5)C314—C3151.373 (4)
C115—H11E0.9300C314—H31D0.9300
C116—C1171.374 (4)C315—C3161.337 (4)
C116—H11F0.9300C315—H31E0.9300
C117—C1181.380 (5)C316—C3171.365 (5)
C117—H11G0.9300C316—H31F0.9300
C118—H11H0.9300C317—C3181.387 (4)
C201—C2061.381 (4)C317—H31G0.9300
C201—C2021.382 (4)C318—H31H0.9300
C202—C2031.375 (4)O11—C141.328 (6)
C202—H20E0.9300O11—C111.371 (5)
C203—C2041.364 (4)C11—C121.392 (7)
C203—H20F0.9300C11—H11I0.9700
C204—C2051.363 (5)C11—H11J0.9700
C204—H20G0.9300C12—C131.314 (8)
C205—C2061.365 (5)C12—H12A0.9700
C205—H20D0.9300C12—H12B0.9700
C206—H20A0.9300C13—C141.402 (6)
C207—C2121.364 (5)C13—H13A0.9700
C207—C2081.388 (4)C13—H13B0.9700
C208—C2091.366 (5)C14—H14C0.9700
C208—H20B0.9300C14—H14A0.9700
P2—Ag1—P1129.31 (3)C210—C209—H20C120.2
P2—Ag1—Br2111.52 (2)C208—C209—H20C120.2
P1—Ag1—Br2105.57 (2)C209—C210—C211119.0 (4)
P2—Ag1—Br1104.39 (2)C209—C210—H21A120.5
P1—Ag1—Br1103.72 (2)C211—C210—H21A120.5
Br2—Ag1—Br197.398 (16)C210—C211—C212121.3 (4)
P3—Ag2—Br2129.08 (3)C210—C211—H21B119.4
P3—Ag2—Br1123.75 (3)C212—C211—H21B119.4
Br2—Ag2—Br1106.740 (18)C207—C212—C211120.3 (3)
Ag2—Br1—Ag176.985 (14)C207—C212—H21C119.8
Ag2—Br2—Ag178.701 (15)C211—C212—H21C119.8
C113—P1—C101103.10 (13)C214—C213—C218119.6 (3)
C113—P1—C107104.27 (14)C214—C213—P2117.8 (2)
C101—P1—C107105.40 (12)C218—C213—P2122.5 (2)
C113—P1—Ag1117.50 (8)C213—C214—C215121.7 (3)
C101—P1—Ag1115.31 (10)C213—C214—H21D119.2
C107—P1—Ag1110.02 (8)C215—C214—H21D119.2
C207—P2—C201104.85 (13)C216—C215—C214118.7 (3)
C207—P2—C213104.01 (15)C216—C215—H21E120.7
C201—P2—C213104.27 (13)C214—C215—H21E120.7
C207—P2—Ag1112.33 (9)C215—C216—C217119.2 (3)
C201—P2—Ag1117.70 (10)C215—C216—H21F120.4
C213—P2—Ag1112.43 (9)C217—C216—H21F120.4
C313—P3—C307103.33 (14)C218—C217—C216121.9 (3)
C313—P3—C301103.47 (14)C218—C217—H21G119.1
C307—P3—C301104.29 (13)C216—C217—H21G119.1
C313—P3—Ag2114.64 (10)C217—C218—C213118.9 (3)
C307—P3—Ag2115.10 (11)C217—C218—H21H120.6
C301—P3—Ag2114.55 (12)C213—C218—H21H120.6
C106—C101—C102118.3 (3)C306—C301—C302119.3 (3)
C106—C101—P1117.83 (19)C306—C301—P3123.9 (2)
C102—C101—P1123.8 (3)C302—C301—P3116.8 (2)
C101—C102—C103119.6 (3)C301—C302—C303119.7 (3)
C101—C102—H10A120.2C301—C302—H30A120.2
C103—C102—H10A120.2C303—C302—H30A120.2
C104—C103—C102120.5 (3)C304—C303—C302120.3 (3)
C104—C103—H10B119.8C304—C303—H30B119.9
C102—C103—H10B119.8C302—C303—H30B119.9
C105—C104—C103120.5 (3)C305—C304—C303119.7 (3)
C105—C104—H10G119.8C305—C304—H30C120.2
C103—C104—H10G119.8C303—C304—H30C120.2
C104—C105—C106119.5 (3)C304—C305—C306120.3 (3)
C104—C105—H10F120.3C304—C305—H30D119.8
C106—C105—H10F120.3C306—C305—H30D119.8
C105—C106—C101121.7 (3)C301—C306—C305120.7 (3)
C105—C106—H10C119.2C301—C306—H30E119.6
C101—C106—H10C119.2C305—C306—H30E119.6
C112—C107—C108118.3 (3)C312—C307—C308119.4 (3)
C112—C107—P1118.66 (19)C312—C307—P3122.5 (2)
C108—C107—P1123.1 (2)C308—C307—P3118.0 (3)
C109—C108—C107120.3 (3)C309—C308—C307119.4 (3)
C109—C108—H10D119.9C309—C308—H30F120.3
C107—C108—H10D119.9C307—C308—H30F120.3
C110—C109—C108120.0 (3)C310—C309—C308121.7 (3)
C110—C109—H10E120.0C310—C309—H30G119.2
C108—C109—H10E120.0C308—C309—H30G119.2
C111—C110—C109120.2 (3)C309—C310—C311118.5 (3)
C111—C110—H11A119.9C309—C310—H31A120.8
C109—C110—H11A119.9C311—C310—H31A120.8
C110—C111—C112120.0 (3)C312—C311—C310121.2 (4)
C110—C111—H11B120.0C312—C311—H31B119.4
C112—C111—H11B120.0C310—C311—H31B119.4
C107—C112—C111121.3 (2)C307—C312—C311119.7 (3)
C107—C112—H11C119.4C307—C312—H31C120.2
C111—C112—H11C119.4C311—C312—H31C120.2
C118—C113—C114117.1 (3)C314—C313—C318116.4 (3)
C118—C113—P1123.0 (2)C314—C313—P3124.6 (2)
C114—C113—P1119.8 (3)C318—C313—P3118.9 (2)
C115—C114—C113121.8 (3)C315—C314—C313121.6 (3)
C115—C114—H11D119.1C315—C314—H31D119.2
C113—C114—H11D119.1C313—C314—H31D119.2
C116—C115—C114120.6 (3)C316—C315—C314121.6 (3)
C116—C115—H11E119.7C316—C315—H31E119.2
C114—C115—H11E119.7C314—C315—H31E119.2
C115—C116—C117119.0 (3)C315—C316—C317118.9 (3)
C115—C116—H11F120.5C315—C316—H31F120.5
C117—C116—H11F120.5C317—C316—H31F120.5
C116—C117—C118120.0 (3)C316—C317—C318120.3 (3)
C116—C117—H11G120.0C316—C317—H31G119.9
C118—C117—H11G120.0C318—C317—H31G119.9
C113—C118—C117121.5 (3)C317—C318—C313121.1 (3)
C113—C118—H11H119.3C317—C318—H31H119.5
C117—C118—H11H119.3C313—C318—H31H119.5
C206—C201—C202118.4 (3)C14—O11—C11108.5 (3)
C206—C201—P2124.9 (3)O11—C11—C12107.4 (4)
C202—C201—P2116.67 (19)O11—C11—H11I110.2
C203—C202—C201119.8 (3)C12—C11—H11I110.2
C203—C202—H20E120.1O11—C11—H11J110.2
C201—C202—H20E120.1C12—C11—H11J110.2
C204—C203—C202121.6 (3)H11I—C11—H11J108.5
C204—C203—H20F119.2C13—C12—C11107.0 (4)
C202—C203—H20F119.2C13—C12—H12A110.3
C205—C204—C203118.1 (3)C11—C12—H12A110.3
C205—C204—H20G121.0C13—C12—H12B110.3
C203—C204—H20G121.0C11—C12—H12B110.3
C204—C205—C206121.7 (3)H12A—C12—H12B108.6
C204—C205—H20D119.1C12—C13—C14109.2 (5)
C206—C205—H20D119.1C12—C13—H13A109.8
C205—C206—C201120.3 (3)C14—C13—H13A109.8
C205—C206—H20A119.9C12—C13—H13B109.8
C201—C206—H20A119.9C14—C13—H13B109.8
C212—C207—C208117.5 (3)H13A—C13—H13B108.3
C212—C207—P2124.9 (2)O11—C14—C13107.1 (4)
C208—C207—P2117.7 (3)O11—C14—H14C110.3
C209—C208—C207122.2 (4)C13—C14—H14C110.3
C209—C208—H20B118.9O11—C14—H14A110.3
C207—C208—H20B118.9C13—C14—H14A110.3
C210—C209—C208119.7 (4)H14C—C14—H14A108.6
P3—Ag2—Br1—Ag1169.76 (3)P2—C201—C202—C203−177.2 (3)
Br2—Ag2—Br1—Ag1−3.346 (12)C201—C202—C203—C204−1.7 (5)
P2—Ag1—Br1—Ag2117.60 (2)C202—C203—C204—C2050.4 (6)
P1—Ag1—Br1—Ag2−105.01 (3)C203—C204—C205—C2060.1 (6)
Br2—Ag1—Br1—Ag23.069 (11)C204—C205—C206—C2010.7 (6)
P3—Ag2—Br2—Ag1−169.18 (3)C202—C201—C206—C205−2.0 (5)
Br1—Ag2—Br2—Ag13.432 (12)P2—C201—C206—C205177.7 (3)
P2—Ag1—Br2—Ag2−111.76 (3)C201—P2—C207—C212−114.6 (2)
P1—Ag1—Br2—Ag2103.47 (3)C213—P2—C207—C212−5.4 (3)
Br1—Ag1—Br2—Ag2−3.058 (11)Ag1—P2—C207—C212116.4 (2)
P2—Ag1—P1—C113−55.84 (13)C201—P2—C207—C20867.2 (2)
Br2—Ag1—P1—C11380.24 (12)C213—P2—C207—C208176.4 (2)
Br1—Ag1—P1—C113−177.89 (12)Ag1—P2—C207—C208−61.8 (2)
P2—Ag1—P1—C101−177.78 (10)C212—C207—C208—C209−1.6 (4)
Br2—Ag1—P1—C101−41.69 (11)P2—C207—C208—C209176.7 (2)
Br1—Ag1—P1—C10160.17 (11)C207—C208—C209—C2101.5 (5)
P2—Ag1—P1—C10763.21 (11)C208—C209—C210—C211−1.5 (5)
Br2—Ag1—P1—C107−160.71 (10)C209—C210—C211—C2121.7 (5)
Br1—Ag1—P1—C107−58.84 (10)C208—C207—C212—C2111.7 (4)
P1—Ag1—P2—C207−63.49 (13)P2—C207—C212—C211−176.5 (2)
Br2—Ag1—P2—C207162.41 (12)C210—C211—C212—C207−1.8 (4)
Br1—Ag1—P2—C20758.29 (12)C207—P2—C213—C214102.5 (3)
P1—Ag1—P2—C201174.61 (11)C201—P2—C213—C214−147.8 (3)
Br2—Ag1—P2—C20140.51 (11)Ag1—P2—C213—C214−19.2 (3)
Br1—Ag1—P2—C201−63.61 (11)C207—P2—C213—C218−79.7 (3)
P1—Ag1—P2—C21353.42 (12)C201—P2—C213—C21829.9 (3)
Br2—Ag1—P2—C213−80.67 (11)Ag1—P2—C213—C218158.5 (2)
Br1—Ag1—P2—C213175.20 (11)C218—C213—C214—C2152.3 (5)
Br2—Ag2—P3—C313−95.32 (11)P2—C213—C214—C215−179.9 (3)
Br1—Ag2—P3—C31393.20 (11)C213—C214—C215—C216−3.0 (5)
Br2—Ag2—P3—C30724.36 (10)C214—C215—C216—C2171.8 (5)
Br1—Ag2—P3—C307−147.13 (10)C215—C216—C217—C218−0.2 (5)
Br2—Ag2—P3—C301145.26 (10)C216—C217—C218—C213−0.4 (5)
Br1—Ag2—P3—C301−26.22 (11)C214—C213—C218—C217−0.6 (5)
C113—P1—C101—C106−154.1 (2)P2—C213—C218—C217−178.3 (3)
C107—P1—C101—C10696.8 (2)C313—P3—C301—C30691.1 (3)
Ag1—P1—C101—C106−24.7 (3)C307—P3—C301—C306−16.7 (3)
C113—P1—C101—C10223.6 (3)Ag2—P3—C301—C306−143.4 (2)
C107—P1—C101—C102−85.4 (3)C313—P3—C301—C302−86.9 (3)
Ag1—P1—C101—C102153.0 (2)C307—P3—C301—C302165.3 (3)
C106—C101—C102—C103−2.7 (5)Ag2—P3—C301—C30238.6 (3)
P1—C101—C102—C103179.5 (2)C306—C301—C302—C303−2.5 (5)
C101—C102—C103—C1042.0 (5)P3—C301—C302—C303175.6 (3)
C102—C103—C104—C105−0.2 (5)C301—C302—C303—C3042.4 (5)
C103—C104—C105—C106−1.0 (5)C302—C303—C304—C305−0.6 (5)
C104—C105—C106—C1010.2 (5)C303—C304—C305—C306−1.1 (5)
C102—C101—C106—C1051.6 (4)C302—C301—C306—C3050.8 (5)
P1—C101—C106—C105179.5 (2)P3—C301—C306—C305−177.1 (2)
C113—P1—C107—C11296.1 (3)C304—C305—C306—C3011.0 (5)
C101—P1—C107—C112−155.7 (3)C313—P3—C307—C312−28.7 (3)
Ag1—P1—C107—C112−30.8 (3)C301—P3—C307—C31279.2 (3)
C113—P1—C107—C108−85.0 (3)Ag2—P3—C307—C312−154.4 (2)
C101—P1—C107—C10823.2 (3)C313—P3—C307—C308152.2 (2)
Ag1—P1—C107—C108148.1 (2)C301—P3—C307—C308−99.9 (2)
C112—C107—C108—C109−0.3 (5)Ag2—P3—C307—C30826.5 (2)
P1—C107—C108—C109−179.2 (3)C312—C307—C308—C309−2.8 (4)
C107—C108—C109—C110−0.1 (5)P3—C307—C308—C309176.3 (2)
C108—C109—C110—C111−0.3 (5)C307—C308—C309—C3101.8 (5)
C109—C110—C111—C1121.2 (5)C308—C309—C310—C3110.2 (5)
C108—C107—C112—C1111.1 (5)C309—C310—C311—C312−1.3 (4)
P1—C107—C112—C111−179.9 (3)C308—C307—C312—C3111.7 (4)
C110—C111—C112—C107−1.6 (5)P3—C307—C312—C311−177.4 (2)
C101—P1—C113—C118−110.7 (2)C310—C311—C312—C3070.3 (4)
C107—P1—C113—C118−0.8 (2)C307—P3—C313—C314113.2 (3)
Ag1—P1—C113—C118121.3 (2)C301—P3—C313—C3144.7 (3)
C101—P1—C113—C11471.3 (2)Ag2—P3—C313—C314−120.7 (3)
C107—P1—C113—C114−178.8 (2)C307—P3—C313—C318−69.9 (3)
Ag1—P1—C113—C114−56.8 (3)C301—P3—C313—C318−178.4 (3)
C118—C113—C114—C1150.8 (4)Ag2—P3—C313—C31856.1 (3)
P1—C113—C114—C115179.0 (2)C318—C313—C314—C3151.2 (5)
C113—C114—C115—C116−0.5 (5)P3—C313—C314—C315178.2 (3)
C114—C115—C116—C117−0.3 (5)C313—C314—C315—C316−0.2 (5)
C115—C116—C117—C1180.6 (4)C314—C315—C316—C3171.1 (5)
C114—C113—C118—C117−0.5 (4)C315—C316—C317—C318−3.1 (5)
P1—C113—C118—C117−178.6 (2)C316—C317—C318—C3134.3 (5)
C116—C117—C118—C113−0.2 (4)C314—C313—C318—C317−3.3 (5)
C207—P2—C201—C20622.9 (3)P3—C313—C318—C317179.6 (3)
C213—P2—C201—C206−86.1 (3)C14—O11—C11—C126.2 (5)
Ag1—P2—C201—C206148.6 (2)O11—C11—C12—C13−8.9 (6)
C207—P2—C201—C202−157.5 (2)C11—C12—C13—C148.2 (6)
C213—P2—C201—C20293.5 (3)C11—O11—C14—C13−1.3 (5)
Ag1—P2—C201—C202−31.8 (3)C12—C13—C14—O11−4.5 (6)
C206—C201—C202—C2032.5 (5)

Footnotes

Supplementary data and figures for this paper are available from the IUCr electronic archives (Reference: SU2091).

References

  • Bowmaker, G. A., Effendy, Hanna, J. V., Healy, P. C., Skelton, B. W. & White, A. H. (1993). J. Chem. Soc. Dalton Trans. pp. 1387–1397.
  • Cingolani, A., Effendy, Hanna, J. V., Pellei, M., Pettinari, C., Santini, C., Skelton, B. W. & White, A. H. (2003). Inorg. Chem.42, 4938–4948. [PubMed]
  • Freedman, J. R. (1994). World Patent WO 94/03833, Polaroid.
  • Lobana, T. S., Sharma, R. & Butcher, R. J. (2008). Polyhedron, 27, 1375–1380.
  • Mann, F. G., Well, A. F. & Purdie, D. (1937). J. Chem. Soc. Dalton Trans. pp. 1830–1838.
  • Olmstead, M. M., Sheffrin, M. & Jiang, F.-L. (2004). Acta Cryst. E60, m1142–m1143.
  • Rigaku (2002). CrystalClear Rigaku Corporation, Tokyo, Japan.
  • Sheldrick, G. M. (2008). Acta Cryst. A64, 112–122. [PubMed]
  • Teo, B. K. & Calabrese, J. C. (1976). Chem. Commun.6, 185–186.
  • Whitcomb, D. R. & Rajeswaram, M. (2006). Polyhedron, 25, 2033–???
  • Whitcomb, D. R. & Roger, R. D. (1996). J. Chem. Crystallogr.26, 99–105.
  • Zhang, K., Prabhavathy, J., Yip, J. H. K., Koh, L. L., Tan, G. K. & Vittal, J. J. (2003). J. Am. Chem. Soc.125, 8452–8453. [PubMed]
  • Zhu, Y.-B., Huang, Y.-Q. & Zheng, L.-S. (1994). Chin. J. Struct. Chem.13, 325–327.

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