metal-organic compounds
Bis[μ2-bis(diphenylphosphanyl)methane-κ2P:P′]bis(μ4-diphenylphosphinato-κ4O:O:O′:O′)bis(μ2-trifluoroacetato-κ2O:O′)tetrasilver(I) acetonitrile disolvate
aSichuan College of Chemical Technology, Luzhou 646005, People's Republic of China, and bSchool of Chemistry and Chemical Engineering, Guangxi Normal University, Guilin 541004, People's Republic of China
*Correspondence e-mail: dengqihua_1@163.com
In the cation of the title compound, [Ag4(C2F3O2)2(C12H10O2P)2(C25H22P2)2]·2CH3CN, the two independent Ag+ cations are four-coordinated in a distorted tetrahedral geometry by one P atom from a bis(diphenylphosphanyl)methane (dppm) ligand, one O atom from a trifluoroacetate anion and two O atoms from two diphenylphosphinate (dpp) ligands. Two dppm ligands, two dpp ligands and two trifluoroacetate anions bridge four metal atoms, forming a centrosymmetric tetranuclear complex. Intramolecular C—H⋯O hydrogen bonds and a weak π–π interaction [centroid–centroid distance = 3.9804 (13) Å] are also observed.
Related literature
For applications of metals complexes with diphosphine ligands, see: Catalano & Malwitz (2004); Chiu & Lee (2005). For related structures, see: Kuang et al. (2002); Rudler et al. (1997); Zank et al. (1999).
Experimental
Crystal data
|
Refinement
|
Data collection: CrystalClear-SM Expert (Rigaku, 2009); cell CrystalClear-SM Expert; data reduction: CrystalClear-SM Expert; program(s) used to solve structure: SHELXS97 (Sheldrick, 2008); program(s) used to refine structure: SHELXL97 (Sheldrick, 2008); molecular graphics: SHELXTL (Sheldrick, 2008); software used to prepare material for publication: SHELXTL.
Supporting information
https://doi.org/10.1107/S1600536811045466/rz2658sup1.cif
contains datablocks I, global. DOI:Structure factors: contains datablock I. DOI: https://doi.org/10.1107/S1600536811045466/rz2658Isup2.hkl
The synthesis of the title compound was carried out by reacting silver trifluoroacetato (0.044 g, 0.2 mmol), diphenylphosphinic acid (0.022 g, 0.1 mmol) and bis(diphenylphosphine)methane (0.038 g, 0.1 mmol). The resulting mixture was allowed to stir for 1 h at room temperature. Colourless crystals of the title compound were obtained in 6 days by slow diffusion of diethyl ether into the solution (yield 15%).
All hydrogen atoms were generated geometrically and refined using a riding model, with C—H = 0.93–0.96Å and with Uiso(H) = 1.2 Ueq(C) or 1.5 Ueq(C) for methyl H atoms. The restraints SIMU and DELU were used to ensure similar geometries and displacement parameters of the Ag1, O3, C38, C39 and F1–F3 atoms. The displacement parameters of the oxygen atoms were restrained to be approximately isotropic by means of the instruction ISOR (tolerance 0.02). Five low-theta reflections were omitted from the data set.
Over the past three decades, metals complexes containing diphosphine ligands attract great interest for their importance in their potential applications in dye-sensitized solar cells and photochemical catalysts (Catalano & Malwitz, 2004; Chiu & Lee, 2005). A series of silver(I) complexes containing diphosphine ligands have been synthesized (Kuang et al., 2002). Synthetic tetranuclear silver(I) compounds have been widely reported (Rudler et al., 1997; Zank et al., 1999).
In the title compound (Fig. 1), the silver(I) atom adopts a distorted tetrahedral geometry through one P atom from a bis(diphenylphosphanyl)methane (dppm)ligand, one O atom from a trifluoroacetato anion and two O atoms from two diphenylphosphinate (dpp) ligands. Two dppm ligands, two dpp ligands and two trifluoroacetato anions bridge four metal atoms forming a centrosymmetric tetranuclear complex where the shortest Ag···Ag separation is 3.3655 (12) Å. The Ag—P and Ag—O bond distances are in the range 2.3685 (14)–2.3734 (14) and 2.278 (3)–2.505 (3) (14) Å, respectively. The O—Ag—P angles and O—Ag—O bond angles range from 80.56 (11) to 92.43 (14)° and from 106.90 (11) to 150.88 (8)°, respectively. In the crystal, intramolecular C—H···O hydrogen bonds are present (Table 1). In addition, a weak intramolecular π–π interaction of 3.9804 (13) Å between the centroids of the C8—C13 and C20—C25 phenyl rings is observed.
For applications of metals complexes of diphosphine ligands, see: Catalano & Malwitz (2004); Chiu & Lee (2005). For related structures, see: Kuang et al. (2002); Rudler et al. (1997); Zank et al. (1999).
Data collection: CrystalClear-SM Expert (Rigaku, 2009); cell
CrystalClear-SM Expert (Rigaku, 2009); data reduction: CrystalClear-SM Expert (Rigaku, 2009); program(s) used to solve structure: SHELXS97 (Sheldrick, 2008); program(s) used to refine structure: SHELXL97 (Sheldrick, 2008); molecular graphics: SHELXTL (Sheldrick, 2008); software used to prepare material for publication: SHELXTL (Sheldrick, 2008).[Ag4(C2F3O2)2(C12H10O2P)2(C25H22P2)2]·2C2H3N | F(000) = 1944 |
Mr = 1942.70 | Dx = 1.576 Mg m−3 |
Monoclinic, P21/n | Mo Kα radiation, λ = 0.71073 Å |
Hall symbol: -P 2yn | Cell parameters from 9421 reflections |
a = 11.724 (5) Å | θ = 2.1–27.5° |
b = 14.777 (6) Å | µ = 1.13 mm−1 |
c = 24.183 (10) Å | T = 296 K |
β = 102.254 (5)° | Prism, colourless |
V = 4094 (3) Å3 | 0.20 × 0.20 × 0.20 mm |
Z = 2 |
Rigaku Mercury CCD diffractometer | 7192 independent reflections |
Radiation source: fine-focus sealed tube | 6033 reflections with I > 2σ(I) |
Graphite monochromator | Rint = 0.057 |
Detector resolution: 13.6612 pixels mm-1 | θmax = 25.0°, θmin = 2.5° |
ω scans | h = −13→13 |
Absorption correction: multi-scan (CrystalClear-SM Expert; Rigaku, 2009) | k = −17→17 |
Tmin = 0.806, Tmax = 0.806 | l = −28→28 |
34844 measured reflections |
Refinement on F2 | Primary atom site location: structure-invariant direct methods |
Least-squares matrix: full | Secondary atom site location: difference Fourier map |
R[F2 > 2σ(F2)] = 0.046 | Hydrogen site location: inferred from neighbouring sites |
wR(F2) = 0.117 | H-atom parameters constrained |
S = 1.01 | w = 1/[σ2(Fo2) + (0.0503P)2 + 7.4307P] where P = (Fo2 + 2Fc2)/3 |
7192 reflections | (Δ/σ)max = 0.001 |
480 parameters | Δρmax = 1.08 e Å−3 |
60 restraints | Δρmin = −0.59 e Å−3 |
[Ag4(C2F3O2)2(C12H10O2P)2(C25H22P2)2]·2C2H3N | V = 4094 (3) Å3 |
Mr = 1942.70 | Z = 2 |
Monoclinic, P21/n | Mo Kα radiation |
a = 11.724 (5) Å | µ = 1.13 mm−1 |
b = 14.777 (6) Å | T = 296 K |
c = 24.183 (10) Å | 0.20 × 0.20 × 0.20 mm |
β = 102.254 (5)° |
Rigaku Mercury CCD diffractometer | 7192 independent reflections |
Absorption correction: multi-scan (CrystalClear-SM Expert; Rigaku, 2009) | 6033 reflections with I > 2σ(I) |
Tmin = 0.806, Tmax = 0.806 | Rint = 0.057 |
34844 measured reflections |
R[F2 > 2σ(F2)] = 0.046 | 60 restraints |
wR(F2) = 0.117 | H-atom parameters constrained |
S = 1.01 | Δρmax = 1.08 e Å−3 |
7192 reflections | Δρmin = −0.59 e Å−3 |
480 parameters |
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. |
x | y | z | Uiso*/Ueq | ||
Ag1 | 0.54210 (3) | 0.92166 (3) | 0.087708 (16) | 0.04807 (13) | |
Ag2 | 0.66296 (3) | 0.91321 (2) | −0.026597 (15) | 0.04551 (13) | |
C1 | 0.6904 (4) | 0.7175 (3) | 0.06180 (18) | 0.0384 (10) | |
H1A | 0.7435 | 0.6710 | 0.0803 | 0.046* | |
H1B | 0.6232 | 0.6873 | 0.0389 | 0.046* | |
C2 | 0.7857 (4) | 0.6966 (3) | −0.0368 (2) | 0.0457 (11) | |
C3 | 0.8256 (6) | 0.6101 (4) | −0.0213 (3) | 0.0708 (17) | |
H3 | 0.8354 | 0.5916 | 0.0162 | 0.085* | |
C4 | 0.8511 (7) | 0.5508 (5) | −0.0616 (3) | 0.087 (2) | |
H4 | 0.8787 | 0.4930 | −0.0508 | 0.104* | |
C5 | 0.8363 (6) | 0.5760 (5) | −0.1163 (3) | 0.083 (2) | |
H5 | 0.8561 | 0.5364 | −0.1427 | 0.099* | |
C6 | 0.7922 (6) | 0.6594 (5) | −0.1331 (3) | 0.0785 (19) | |
H6 | 0.7787 | 0.6756 | −0.1711 | 0.094* | |
C7 | 0.7674 (5) | 0.7208 (4) | −0.0931 (2) | 0.0618 (14) | |
H7 | 0.7384 | 0.7779 | −0.1046 | 0.074* | |
C8 | 0.9111 (4) | 0.8015 (3) | 0.0557 (2) | 0.0438 (11) | |
C9 | 0.9731 (5) | 0.7357 (4) | 0.0905 (3) | 0.081 (2) | |
H9 | 0.9382 | 0.6805 | 0.0951 | 0.098* | |
C10 | 1.0871 (6) | 0.7523 (5) | 0.1185 (4) | 0.106 (3) | |
H10 | 1.1290 | 0.7078 | 0.1414 | 0.128* | |
C11 | 1.1380 (5) | 0.8335 (5) | 0.1127 (3) | 0.086 (2) | |
H11 | 1.2150 | 0.8435 | 0.1312 | 0.103* | |
C12 | 1.0781 (6) | 0.8999 (5) | 0.0803 (3) | 0.0767 (18) | |
H12 | 1.1129 | 0.9557 | 0.0772 | 0.092* | |
C13 | 0.9638 (5) | 0.8835 (4) | 0.0518 (2) | 0.0608 (14) | |
H13 | 0.9223 | 0.9290 | 0.0296 | 0.073* | |
C14 | 0.5474 (4) | 0.7051 (3) | 0.14380 (18) | 0.0438 (11) | |
C15 | 0.5558 (6) | 0.6126 (4) | 0.1397 (2) | 0.0673 (16) | |
H15 | 0.6127 | 0.5872 | 0.1230 | 0.081* | |
C16 | 0.4787 (7) | 0.5568 (5) | 0.1607 (3) | 0.087 (2) | |
H16 | 0.4850 | 0.4942 | 0.1584 | 0.105* | |
C17 | 0.3939 (6) | 0.5940 (6) | 0.1848 (3) | 0.085 (2) | |
H17 | 0.3410 | 0.5567 | 0.1976 | 0.102* | |
C18 | 0.3867 (5) | 0.6852 (6) | 0.1902 (3) | 0.075 (2) | |
H18 | 0.3307 | 0.7098 | 0.2079 | 0.090* | |
C19 | 0.4623 (4) | 0.7420 (4) | 0.1696 (2) | 0.0590 (14) | |
H19 | 0.4563 | 0.8044 | 0.1729 | 0.071* | |
C20 | 0.7694 (4) | 0.7932 (3) | 0.17396 (19) | 0.0448 (11) | |
C21 | 0.8085 (5) | 0.7232 (4) | 0.2106 (3) | 0.0722 (17) | |
H21 | 0.7679 | 0.6687 | 0.2071 | 0.087* | |
C22 | 0.9087 (6) | 0.7338 (6) | 0.2529 (3) | 0.091 (2) | |
H22 | 0.9336 | 0.6863 | 0.2778 | 0.109* | |
C23 | 0.9698 (7) | 0.8112 (6) | 0.2584 (3) | 0.100 (3) | |
H23 | 1.0357 | 0.8174 | 0.2873 | 0.120* | |
C24 | 0.9360 (7) | 0.8798 (6) | 0.2221 (4) | 0.106 (3) | |
H24 | 0.9804 | 0.9324 | 0.2252 | 0.128* | |
C25 | 0.8344 (6) | 0.8724 (4) | 0.1798 (3) | 0.0770 (18) | |
H25 | 0.8103 | 0.9208 | 0.1556 | 0.092* | |
C26 | 0.6109 (4) | 1.2297 (3) | 0.0284 (2) | 0.0469 (12) | |
C27 | 0.5551 (6) | 1.2773 (4) | 0.0637 (3) | 0.0758 (19) | |
H27 | 0.5217 | 1.2470 | 0.0900 | 0.091* | |
C28 | 0.5490 (8) | 1.3714 (6) | 0.0598 (4) | 0.113 (3) | |
H28 | 0.5077 | 1.4036 | 0.0821 | 0.135* | |
C29 | 0.6024 (9) | 1.4159 (5) | 0.0238 (5) | 0.126 (5) | |
H29 | 0.6035 | 1.4788 | 0.0242 | 0.152* | |
C30 | 0.6548 (8) | 1.3706 (5) | −0.0131 (4) | 0.109 (3) | |
H30 | 0.6870 | 1.4023 | −0.0393 | 0.131* | |
C31 | 0.6599 (5) | 1.2760 (4) | −0.0113 (3) | 0.0732 (18) | |
H31 | 0.6955 | 1.2443 | −0.0362 | 0.088* | |
C32 | 0.7743 (4) | 1.1088 (3) | 0.08724 (19) | 0.0411 (10) | |
C33 | 0.8771 (4) | 1.1165 (4) | 0.0682 (3) | 0.0623 (15) | |
H33 | 0.8753 | 1.1158 | 0.0295 | 0.075* | |
C34 | 0.9828 (5) | 1.1255 (5) | 0.1063 (3) | 0.083 (2) | |
H34 | 1.0516 | 1.1303 | 0.0932 | 0.100* | |
C35 | 0.9864 (6) | 1.1272 (5) | 0.1625 (3) | 0.083 (2) | |
H35 | 1.0577 | 1.1337 | 0.1878 | 0.099* | |
C36 | 0.8866 (6) | 1.1196 (5) | 0.1822 (3) | 0.081 (2) | |
H36 | 0.8901 | 1.1208 | 0.2210 | 0.097* | |
C38 | 0.3389 (7) | 1.0357 (6) | 0.2187 (3) | 0.0934 (15) | |
C39 | 0.3725 (6) | 1.0221 (5) | 0.1619 (3) | 0.0804 (12) | |
C40 | 0.8585 (15) | 0.3690 (11) | 0.1793 (11) | 0.393 (18) | |
H40A | 0.9376 | 0.3619 | 0.1999 | 0.590* | |
H40B | 0.8366 | 0.3177 | 0.1551 | 0.590* | |
H40C | 0.8076 | 0.3734 | 0.2055 | 0.590* | |
C41 | 0.8488 (9) | 0.4537 (7) | 0.1442 (6) | 0.150 (5) | |
C37O | 0.7795 (3) | 1.1099 (2) | 0.14489 (10) | 0.0608 (14) | |
H37O | 0.7116 | 1.1042 | 0.1587 | 0.073* | |
F1 | 0.2990 (3) | 1.1197 (2) | 0.22513 (10) | 0.1335 (18) | |
F2 | 0.4197 (3) | 1.0317 (2) | 0.26317 (10) | 0.155 (2) | |
F3 | 0.2555 (3) | 0.9843 (2) | 0.22562 (10) | 0.160 (2) | |
N1 | 0.8428 (7) | 0.5182 (5) | 0.1215 (4) | 0.124 (3) | |
O1 | 0.5435 (3) | 1.0716 (2) | 0.06592 (14) | 0.0466 (8) | |
O2 | 0.6484 (3) | 1.0685 (2) | −0.01761 (13) | 0.0440 (7) | |
O3 | 0.4545 (4) | 0.9706 (3) | 0.16520 (18) | 0.0879 (12) | |
O4 | 0.3134 (4) | 1.0629 (3) | 0.12293 (16) | 0.0762 (12) | |
P1 | 0.76367 (10) | 0.78230 (8) | 0.01470 (5) | 0.0374 (3) | |
P2 | 0.64141 (10) | 0.78438 (8) | 0.11642 (5) | 0.0375 (3) | |
P3 | 0.63580 (10) | 1.10991 (8) | 0.03764 (5) | 0.0385 (3) |
U11 | U22 | U33 | U12 | U13 | U23 | |
Ag1 | 0.0513 (2) | 0.0492 (2) | 0.0450 (2) | 0.01425 (17) | 0.01323 (17) | 0.00685 (16) |
Ag2 | 0.0429 (2) | 0.0487 (2) | 0.0454 (2) | 0.01025 (16) | 0.01052 (16) | 0.00678 (15) |
C1 | 0.039 (2) | 0.041 (2) | 0.036 (2) | 0.0013 (19) | 0.0084 (18) | 0.0010 (18) |
C2 | 0.040 (2) | 0.051 (3) | 0.050 (3) | −0.003 (2) | 0.016 (2) | −0.005 (2) |
C3 | 0.100 (5) | 0.055 (3) | 0.065 (4) | 0.013 (3) | 0.033 (3) | −0.006 (3) |
C4 | 0.111 (6) | 0.063 (4) | 0.094 (5) | 0.008 (4) | 0.041 (4) | −0.023 (4) |
C5 | 0.084 (5) | 0.090 (5) | 0.080 (5) | −0.007 (4) | 0.029 (4) | −0.042 (4) |
C6 | 0.086 (5) | 0.103 (5) | 0.049 (3) | −0.006 (4) | 0.022 (3) | −0.024 (3) |
C7 | 0.060 (3) | 0.076 (4) | 0.052 (3) | 0.003 (3) | 0.016 (3) | −0.010 (3) |
C8 | 0.033 (2) | 0.050 (3) | 0.048 (3) | 0.004 (2) | 0.009 (2) | −0.005 (2) |
C9 | 0.046 (3) | 0.058 (4) | 0.127 (6) | 0.003 (3) | −0.012 (3) | 0.002 (4) |
C10 | 0.052 (4) | 0.079 (5) | 0.162 (8) | 0.008 (4) | −0.035 (4) | 0.005 (5) |
C11 | 0.043 (3) | 0.095 (5) | 0.109 (6) | −0.002 (4) | −0.006 (3) | −0.021 (4) |
C12 | 0.065 (4) | 0.079 (4) | 0.083 (5) | −0.028 (4) | 0.009 (3) | −0.009 (4) |
C13 | 0.059 (3) | 0.062 (3) | 0.059 (3) | −0.009 (3) | 0.008 (3) | 0.007 (3) |
C14 | 0.042 (2) | 0.056 (3) | 0.033 (2) | −0.004 (2) | 0.0079 (19) | 0.003 (2) |
C15 | 0.094 (5) | 0.064 (4) | 0.050 (3) | −0.018 (3) | 0.030 (3) | −0.001 (3) |
C16 | 0.134 (7) | 0.074 (4) | 0.062 (4) | −0.047 (4) | 0.036 (4) | −0.004 (3) |
C17 | 0.081 (5) | 0.122 (6) | 0.054 (4) | −0.048 (5) | 0.019 (3) | 0.013 (4) |
C18 | 0.043 (3) | 0.122 (6) | 0.063 (4) | 0.004 (4) | 0.017 (3) | 0.036 (4) |
C19 | 0.048 (3) | 0.079 (4) | 0.052 (3) | 0.009 (3) | 0.014 (2) | 0.022 (3) |
C20 | 0.043 (3) | 0.054 (3) | 0.035 (2) | −0.001 (2) | 0.0044 (19) | −0.002 (2) |
C21 | 0.063 (4) | 0.074 (4) | 0.071 (4) | 0.002 (3) | −0.005 (3) | 0.010 (3) |
C22 | 0.072 (4) | 0.116 (6) | 0.070 (4) | 0.013 (4) | −0.017 (3) | 0.020 (4) |
C23 | 0.084 (5) | 0.113 (6) | 0.083 (5) | −0.004 (5) | −0.028 (4) | −0.005 (5) |
C24 | 0.093 (6) | 0.102 (6) | 0.105 (6) | −0.029 (5) | −0.024 (5) | −0.024 (5) |
C25 | 0.076 (4) | 0.062 (4) | 0.082 (4) | −0.001 (3) | −0.007 (3) | −0.007 (3) |
C26 | 0.044 (3) | 0.042 (3) | 0.046 (3) | 0.003 (2) | −0.009 (2) | −0.003 (2) |
C27 | 0.074 (4) | 0.064 (4) | 0.080 (4) | 0.024 (3) | −0.006 (3) | −0.022 (3) |
C28 | 0.115 (7) | 0.074 (5) | 0.125 (8) | 0.035 (5) | −0.030 (6) | −0.045 (5) |
C29 | 0.131 (9) | 0.043 (4) | 0.162 (11) | 0.012 (5) | −0.065 (8) | −0.015 (5) |
C30 | 0.119 (7) | 0.060 (5) | 0.126 (7) | −0.023 (5) | −0.027 (6) | 0.037 (5) |
C31 | 0.072 (4) | 0.053 (3) | 0.083 (4) | −0.014 (3) | −0.010 (3) | 0.017 (3) |
C32 | 0.038 (2) | 0.041 (2) | 0.043 (3) | −0.001 (2) | 0.0029 (19) | −0.0015 (19) |
C33 | 0.041 (3) | 0.086 (4) | 0.061 (3) | −0.007 (3) | 0.011 (2) | −0.008 (3) |
C34 | 0.035 (3) | 0.117 (6) | 0.094 (5) | −0.010 (3) | 0.008 (3) | −0.013 (4) |
C35 | 0.051 (4) | 0.101 (5) | 0.080 (5) | 0.001 (4) | −0.020 (3) | −0.009 (4) |
C36 | 0.075 (4) | 0.107 (5) | 0.049 (3) | 0.004 (4) | −0.015 (3) | −0.002 (3) |
C38 | 0.108 (3) | 0.123 (3) | 0.062 (3) | 0.014 (3) | 0.047 (2) | 0.003 (3) |
C39 | 0.099 (3) | 0.096 (3) | 0.060 (2) | 0.034 (2) | 0.048 (2) | 0.013 (2) |
C40 | 0.195 (16) | 0.238 (18) | 0.68 (4) | −0.046 (14) | −0.05 (2) | 0.32 (2) |
C41 | 0.095 (7) | 0.094 (7) | 0.238 (14) | −0.001 (6) | −0.019 (8) | 0.025 (8) |
C37O | 0.055 (3) | 0.075 (4) | 0.050 (3) | 0.002 (3) | 0.004 (2) | 0.001 (3) |
F1 | 0.157 (4) | 0.148 (4) | 0.111 (3) | 0.031 (3) | 0.061 (3) | −0.034 (3) |
F2 | 0.164 (5) | 0.242 (6) | 0.056 (3) | 0.039 (5) | 0.018 (3) | 0.006 (3) |
F3 | 0.210 (5) | 0.187 (5) | 0.121 (4) | −0.077 (4) | 0.121 (4) | −0.039 (3) |
N1 | 0.138 (7) | 0.076 (5) | 0.142 (7) | 0.013 (5) | −0.005 (5) | 0.022 (4) |
O1 | 0.0314 (16) | 0.0489 (19) | 0.059 (2) | −0.0002 (14) | 0.0086 (14) | 0.0036 (15) |
O2 | 0.0459 (18) | 0.0400 (17) | 0.0433 (18) | 0.0018 (14) | 0.0030 (14) | −0.0048 (13) |
O3 | 0.108 (3) | 0.101 (3) | 0.067 (2) | 0.042 (2) | 0.0471 (19) | 0.013 (2) |
O4 | 0.085 (3) | 0.103 (3) | 0.047 (2) | 0.024 (3) | 0.027 (2) | 0.019 (2) |
P1 | 0.0333 (6) | 0.0411 (6) | 0.0386 (6) | 0.0049 (5) | 0.0098 (5) | 0.0001 (5) |
P2 | 0.0355 (6) | 0.0428 (6) | 0.0348 (6) | 0.0044 (5) | 0.0086 (5) | 0.0029 (5) |
P3 | 0.0337 (6) | 0.0376 (6) | 0.0416 (6) | −0.0001 (5) | 0.0021 (5) | −0.0008 (5) |
Ag1—O1 | 2.278 (3) | C20—P2 | 1.822 (5) |
Ag1—P2 | 2.3685 (14) | C21—C22 | 1.393 (8) |
Ag1—O3 | 2.430 (4) | C21—H21 | 0.9300 |
Ag1—O2i | 2.505 (3) | C22—C23 | 1.342 (10) |
Ag1—Ag2 | 3.3655 (12) | C22—H22 | 0.9300 |
Ag2—O2 | 2.314 (3) | C23—C24 | 1.343 (11) |
Ag2—P1 | 2.3734 (14) | C23—H23 | 0.9300 |
Ag2—O1i | 2.416 (3) | C24—C25 | 1.400 (9) |
Ag2—O4i | 2.429 (4) | C24—H24 | 0.9300 |
C1—P1 | 1.835 (4) | C25—H25 | 0.9300 |
C1—P2 | 1.837 (4) | C26—C27 | 1.375 (8) |
C1—H1A | 0.9700 | C26—C31 | 1.396 (8) |
C1—H1B | 0.9700 | C26—P3 | 1.800 (5) |
C2—C7 | 1.380 (7) | C27—C28 | 1.394 (10) |
C2—C3 | 1.386 (8) | C27—H27 | 0.9300 |
C2—P1 | 1.832 (5) | C28—C29 | 1.346 (14) |
C3—C4 | 1.390 (8) | C28—H28 | 0.9300 |
C3—H3 | 0.9300 | C29—C30 | 1.362 (14) |
C4—C5 | 1.350 (10) | C29—H29 | 0.9300 |
C4—H4 | 0.9300 | C30—C31 | 1.399 (9) |
C5—C6 | 1.365 (10) | C30—H30 | 0.9300 |
C5—H5 | 0.9300 | C31—H31 | 0.9300 |
C6—C7 | 1.399 (8) | C32—C37O | 1.383 (5) |
C6—H6 | 0.9300 | C32—C33 | 1.384 (7) |
C7—H7 | 0.9300 | C32—P3 | 1.802 (5) |
C8—C13 | 1.373 (7) | C33—C34 | 1.385 (8) |
C8—C9 | 1.386 (8) | C33—H33 | 0.9300 |
C8—P1 | 1.823 (5) | C34—C35 | 1.350 (9) |
C9—C10 | 1.386 (8) | C34—H34 | 0.9300 |
C9—H9 | 0.9300 | C35—C36 | 1.359 (10) |
C10—C11 | 1.360 (10) | C35—H35 | 0.9300 |
C10—H10 | 0.9300 | C36—C37O | 1.390 (7) |
C11—C12 | 1.355 (9) | C36—H36 | 0.9300 |
C11—H11 | 0.9300 | C38—F2 | 1.275 (8) |
C12—C13 | 1.393 (8) | C38—F3 | 1.277 (9) |
C12—H12 | 0.9300 | C38—F1 | 1.347 (9) |
C13—H13 | 0.9300 | C38—C39 | 1.521 (8) |
C14—C15 | 1.376 (7) | C39—O4 | 1.206 (7) |
C14—C19 | 1.394 (7) | C39—O3 | 1.215 (7) |
C14—P2 | 1.826 (5) | C40—C41 | 1.503 (16) |
C15—C16 | 1.396 (8) | C40—H40A | 0.9600 |
C15—H15 | 0.9300 | C40—H40B | 0.9600 |
C16—C17 | 1.370 (10) | C40—H40C | 0.9600 |
C16—H16 | 0.9300 | C41—N1 | 1.096 (11) |
C17—C18 | 1.358 (10) | C37O—H37O | 0.9300 |
C17—H17 | 0.9300 | O1—P3 | 1.508 (3) |
C18—C19 | 1.388 (8) | O1—Ag2i | 2.416 (3) |
C18—H18 | 0.9300 | O2—P3 | 1.505 (3) |
C19—H19 | 0.9300 | O2—Ag1i | 2.505 (3) |
C20—C21 | 1.376 (7) | O4—Ag2i | 2.429 (4) |
C20—C25 | 1.387 (8) | ||
O1—Ag1—P2 | 150.88 (8) | C21—C22—H22 | 119.4 |
O1—Ag1—O3 | 85.06 (14) | C22—C23—C24 | 120.1 (7) |
P2—Ag1—O3 | 106.90 (11) | C22—C23—H23 | 120.0 |
O1—Ag1—O2i | 80.56 (11) | C24—C23—H23 | 120.0 |
P2—Ag1—O2i | 124.08 (8) | C23—C24—C25 | 120.4 (7) |
O3—Ag1—O2i | 92.43 (14) | C23—C24—H24 | 119.8 |
O1—Ag1—Ag2 | 79.70 (9) | C25—C24—H24 | 119.8 |
P2—Ag1—Ag2 | 86.71 (3) | C20—C25—C24 | 120.2 (7) |
O3—Ag1—Ag2 | 164.76 (12) | C20—C25—H25 | 119.9 |
O2i—Ag1—Ag2 | 85.22 (8) | C24—C25—H25 | 119.9 |
O2—Ag2—P1 | 143.96 (8) | C27—C26—C31 | 119.6 (6) |
O2—Ag2—O1i | 81.77 (11) | C27—C26—P3 | 120.7 (5) |
P1—Ag2—O1i | 127.51 (8) | C31—C26—P3 | 119.3 (4) |
O2—Ag2—O4i | 88.39 (14) | C26—C27—C28 | 119.5 (8) |
P1—Ag2—O4i | 111.96 (11) | C26—C27—H27 | 120.2 |
O1i—Ag2—O4i | 85.26 (13) | C28—C27—H27 | 120.2 |
O2—Ag2—Ag1 | 80.43 (8) | C29—C28—C27 | 120.5 (9) |
P1—Ag2—Ag1 | 86.74 (3) | C29—C28—H28 | 119.8 |
O1i—Ag2—Ag1 | 76.03 (8) | C27—C28—H28 | 119.8 |
O4i—Ag2—Ag1 | 159.35 (10) | C28—C29—C30 | 121.3 (8) |
P1—C1—P2 | 115.1 (2) | C28—C29—H29 | 119.4 |
P1—C1—H1A | 108.5 | C30—C29—H29 | 119.4 |
P2—C1—H1A | 108.5 | C29—C30—C31 | 119.5 (9) |
P1—C1—H1B | 108.5 | C29—C30—H30 | 120.2 |
P2—C1—H1B | 108.5 | C31—C30—H30 | 120.2 |
H1A—C1—H1B | 107.5 | C26—C31—C30 | 119.4 (8) |
C7—C2—C3 | 118.6 (5) | C26—C31—H31 | 120.3 |
C7—C2—P1 | 118.5 (4) | C30—C31—H31 | 120.3 |
C3—C2—P1 | 122.8 (4) | C37O—C32—C33 | 118.6 (4) |
C2—C3—C4 | 120.2 (6) | C37O—C32—P3 | 120.8 (3) |
C2—C3—H3 | 119.9 | C33—C32—P3 | 120.2 (4) |
C4—C3—H3 | 119.9 | C32—C33—C34 | 120.3 (6) |
C5—C4—C3 | 120.8 (7) | C32—C33—H33 | 119.8 |
C5—C4—H4 | 119.6 | C34—C33—H33 | 119.8 |
C3—C4—H4 | 119.6 | C35—C34—C33 | 120.3 (6) |
C4—C5—C6 | 120.1 (6) | C35—C34—H34 | 119.8 |
C4—C5—H5 | 119.9 | C33—C34—H34 | 119.8 |
C6—C5—H5 | 119.9 | C34—C35—C36 | 120.4 (6) |
C5—C6—C7 | 120.1 (6) | C34—C35—H35 | 119.8 |
C5—C6—H6 | 119.9 | C36—C35—H35 | 119.8 |
C7—C6—H6 | 119.9 | C35—C36—C37O | 120.5 (6) |
C2—C7—C6 | 120.1 (6) | C35—C36—H36 | 119.8 |
C2—C7—H7 | 119.9 | C37O—C36—H36 | 119.8 |
C6—C7—H7 | 119.9 | F2—C38—F3 | 108.4 (6) |
C13—C8—C9 | 118.4 (5) | F2—C38—F1 | 99.1 (6) |
C13—C8—P1 | 119.2 (4) | F3—C38—F1 | 103.8 (5) |
C9—C8—P1 | 122.4 (4) | F2—C38—C39 | 117.9 (6) |
C10—C9—C8 | 120.0 (6) | F3—C38—C39 | 113.1 (7) |
C10—C9—H9 | 120.0 | F1—C38—C39 | 112.9 (6) |
C8—C9—H9 | 120.0 | O4—C39—O3 | 132.8 (6) |
C11—C10—C9 | 120.3 (7) | O4—C39—C38 | 115.1 (6) |
C11—C10—H10 | 119.9 | O3—C39—C38 | 112.1 (6) |
C9—C10—H10 | 119.9 | C41—C40—H40A | 109.5 |
C12—C11—C10 | 120.9 (6) | C41—C40—H40B | 109.5 |
C12—C11—H11 | 119.5 | H40A—C40—H40B | 109.5 |
C10—C11—H11 | 119.5 | C41—C40—H40C | 109.5 |
C11—C12—C13 | 119.1 (6) | H40A—C40—H40C | 109.5 |
C11—C12—H12 | 120.4 | H40B—C40—H40C | 109.5 |
C13—C12—H12 | 120.4 | N1—C41—C40 | 175.8 (18) |
C8—C13—C12 | 121.3 (6) | C32—C37O—C36 | 119.8 (4) |
C8—C13—H13 | 119.4 | C32—C37O—H37O | 120.1 |
C12—C13—H13 | 119.4 | C36—C37O—H37O | 120.1 |
C15—C14—C19 | 119.3 (5) | P3—O1—Ag1 | 120.75 (18) |
C15—C14—P2 | 123.7 (4) | P3—O1—Ag2i | 122.82 (19) |
C19—C14—P2 | 117.1 (4) | Ag1—O1—Ag2i | 97.24 (11) |
C14—C15—C16 | 120.0 (6) | P3—O2—Ag2 | 120.65 (18) |
C14—C15—H15 | 120.0 | P3—O2—Ag1i | 109.62 (17) |
C16—C15—H15 | 120.0 | Ag2—O2—Ag1i | 93.85 (11) |
C17—C16—C15 | 120.1 (7) | C39—O3—Ag1 | 126.4 (4) |
C17—C16—H16 | 119.9 | C39—O4—Ag2i | 131.2 (4) |
C15—C16—H16 | 119.9 | C8—P1—C2 | 102.9 (2) |
C18—C17—C16 | 120.3 (6) | C8—P1—C1 | 105.0 (2) |
C18—C17—H17 | 119.8 | C2—P1—C1 | 102.3 (2) |
C16—C17—H17 | 119.8 | C8—P1—Ag2 | 115.56 (16) |
C17—C18—C19 | 120.5 (6) | C2—P1—Ag2 | 113.99 (17) |
C17—C18—H18 | 119.7 | C1—P1—Ag2 | 115.47 (15) |
C19—C18—H18 | 119.7 | C20—P2—C14 | 103.4 (2) |
C18—C19—C14 | 119.8 (6) | C20—P2—C1 | 104.8 (2) |
C18—C19—H19 | 120.1 | C14—P2—C1 | 102.7 (2) |
C14—C19—H19 | 120.1 | C20—P2—Ag1 | 115.88 (17) |
C21—C20—C25 | 118.0 (5) | C14—P2—Ag1 | 111.04 (16) |
C21—C20—P2 | 123.0 (4) | C1—P2—Ag1 | 117.35 (15) |
C25—C20—P2 | 118.9 (4) | O2—P3—O1 | 117.7 (2) |
C20—C21—C22 | 120.1 (6) | O2—P3—C26 | 109.4 (2) |
C20—C21—H21 | 120.0 | O1—P3—C26 | 108.3 (2) |
C22—C21—H21 | 120.0 | O2—P3—C32 | 110.1 (2) |
C23—C22—C21 | 121.2 (7) | O1—P3—C32 | 109.1 (2) |
C23—C22—H22 | 119.4 | C26—P3—C32 | 101.0 (2) |
O1—Ag1—Ag2—O2 | 4.02 (11) | O4—C39—O3—Ag1 | −0.8 (14) |
P2—Ag1—Ag2—O2 | −150.12 (8) | C38—C39—O3—Ag1 | 178.5 (5) |
O3—Ag1—Ag2—O2 | 3.6 (5) | O1—Ag1—O3—C39 | 48.8 (6) |
O2i—Ag1—Ag2—O2 | 85.27 (11) | P2—Ag1—O3—C39 | −158.3 (6) |
O1—Ag1—Ag2—P1 | 150.22 (9) | O2i—Ag1—O3—C39 | −31.5 (7) |
P2—Ag1—Ag2—P1 | −3.92 (4) | Ag2—Ag1—O3—C39 | 49.2 (10) |
O3—Ag1—Ag2—P1 | 149.8 (5) | O3—C39—O4—Ag2i | −10.2 (14) |
O2i—Ag1—Ag2—P1 | −128.54 (8) | C38—C39—O4—Ag2i | 170.4 (5) |
O1—Ag1—Ag2—O1i | −79.80 (12) | C13—C8—P1—C2 | 112.4 (4) |
P2—Ag1—Ag2—O1i | 126.07 (8) | C9—C8—P1—C2 | −66.9 (5) |
O3—Ag1—Ag2—O1i | −80.2 (5) | C13—C8—P1—C1 | −140.9 (4) |
O2i—Ag1—Ag2—O1i | 1.45 (10) | C9—C8—P1—C1 | 39.8 (5) |
O1—Ag1—Ag2—O4i | −54.1 (3) | C13—C8—P1—Ag2 | −12.5 (5) |
P2—Ag1—Ag2—O4i | 151.8 (3) | C9—C8—P1—Ag2 | 168.2 (4) |
O3—Ag1—Ag2—O4i | −54.5 (6) | C7—C2—P1—C8 | −112.0 (4) |
O2i—Ag1—Ag2—O4i | 27.1 (3) | C3—C2—P1—C8 | 64.6 (5) |
C7—C2—C3—C4 | 2.7 (9) | C7—C2—P1—C1 | 139.2 (4) |
P1—C2—C3—C4 | −173.9 (5) | C3—C2—P1—C1 | −44.1 (5) |
C2—C3—C4—C5 | −0.7 (11) | C7—C2—P1—Ag2 | 13.9 (4) |
C3—C4—C5—C6 | −2.1 (11) | C3—C2—P1—Ag2 | −169.5 (4) |
C4—C5—C6—C7 | 2.9 (11) | P2—C1—P1—C8 | 78.2 (3) |
C3—C2—C7—C6 | −1.9 (8) | P2—C1—P1—C2 | −174.7 (2) |
P1—C2—C7—C6 | 174.9 (5) | P2—C1—P1—Ag2 | −50.3 (3) |
C5—C6—C7—C2 | −0.9 (10) | O2—Ag2—P1—C8 | −26.8 (2) |
C13—C8—C9—C10 | −2.6 (10) | O1i—Ag2—P1—C8 | −165.19 (19) |
P1—C8—C9—C10 | 176.7 (6) | O4i—Ag2—P1—C8 | 93.4 (2) |
C8—C9—C10—C11 | 1.0 (13) | Ag1—Ag2—P1—C8 | −95.58 (17) |
C9—C10—C11—C12 | 1.0 (13) | O2—Ag2—P1—C2 | −145.7 (2) |
C10—C11—C12—C13 | −1.4 (12) | O1i—Ag2—P1—C2 | 75.89 (19) |
C9—C8—C13—C12 | 2.2 (9) | O4i—Ag2—P1—C2 | −25.5 (2) |
P1—C8—C13—C12 | −177.1 (5) | Ag1—Ag2—P1—C2 | 145.50 (16) |
C11—C12—C13—C8 | −0.3 (10) | O2—Ag2—P1—C1 | 96.2 (2) |
C19—C14—C15—C16 | 0.7 (9) | O1i—Ag2—P1—C1 | −42.2 (2) |
P2—C14—C15—C16 | −178.6 (5) | O4i—Ag2—P1—C1 | −143.6 (2) |
C14—C15—C16—C17 | 0.8 (10) | Ag1—Ag2—P1—C1 | 27.41 (16) |
C15—C16—C17—C18 | −2.3 (11) | C21—C20—P2—C14 | 31.1 (5) |
C16—C17—C18—C19 | 2.4 (10) | C25—C20—P2—C14 | −152.1 (5) |
C17—C18—C19—C14 | −0.9 (9) | C21—C20—P2—C1 | −76.2 (5) |
C15—C14—C19—C18 | −0.6 (8) | C25—C20—P2—C1 | 100.6 (5) |
P2—C14—C19—C18 | 178.7 (4) | C21—C20—P2—Ag1 | 152.8 (4) |
C25—C20—C21—C22 | 1.6 (9) | C25—C20—P2—Ag1 | −30.4 (5) |
P2—C20—C21—C22 | 178.5 (5) | C15—C14—P2—C20 | −85.6 (5) |
C20—C21—C22—C23 | −1.0 (12) | C19—C14—P2—C20 | 95.1 (4) |
C21—C22—C23—C24 | −1.2 (14) | C15—C14—P2—C1 | 23.2 (5) |
C22—C23—C24—C25 | 2.5 (14) | C19—C14—P2—C1 | −156.1 (4) |
C21—C20—C25—C24 | −0.3 (10) | C15—C14—P2—Ag1 | 149.5 (4) |
P2—C20—C25—C24 | −177.3 (6) | C19—C14—P2—Ag1 | −29.8 (4) |
C23—C24—C25—C20 | −1.8 (13) | P1—C1—P2—C20 | −84.1 (3) |
C31—C26—C27—C28 | −0.5 (9) | P1—C1—P2—C14 | 168.1 (2) |
P3—C26—C27—C28 | 172.6 (5) | P1—C1—P2—Ag1 | 46.0 (3) |
C26—C27—C28—C29 | −3.5 (12) | O1—Ag1—P2—C20 | 43.1 (3) |
C27—C28—C29—C30 | 5.9 (14) | O3—Ag1—P2—C20 | −68.0 (2) |
C28—C29—C30—C31 | −4.1 (13) | O2i—Ag1—P2—C20 | −173.02 (19) |
C27—C26—C31—C30 | 2.2 (8) | Ag2—Ag1—P2—C20 | 105.01 (17) |
P3—C26—C31—C30 | −171.0 (5) | O1—Ag1—P2—C14 | 160.7 (2) |
C29—C30—C31—C26 | 0.0 (11) | O3—Ag1—P2—C14 | 49.6 (2) |
C37O—C32—C33—C34 | −0.1 (9) | O2i—Ag1—P2—C14 | −55.46 (19) |
P3—C32—C33—C34 | 173.0 (5) | Ag2—Ag1—P2—C14 | −137.43 (16) |
C32—C33—C34—C35 | −0.4 (11) | O1—Ag1—P2—C1 | −81.6 (3) |
C33—C34—C35—C36 | 0.5 (12) | O3—Ag1—P2—C1 | 167.3 (2) |
C34—C35—C36—C37O | 0.0 (12) | O2i—Ag1—P2—C1 | 62.24 (19) |
F2—C38—C39—O4 | −148.7 (7) | Ag2—Ag1—P2—C1 | −19.73 (16) |
F3—C38—C39—O4 | 83.5 (9) | Ag2—O2—P3—O1 | −49.7 (3) |
F1—C38—C39—O4 | −34.0 (10) | Ag1i—O2—P3—O1 | 57.4 (2) |
F2—C38—C39—O3 | 31.8 (11) | Ag2—O2—P3—C26 | −173.8 (2) |
F3—C38—C39—O3 | −96.0 (8) | Ag1i—O2—P3—C26 | −66.7 (2) |
F1—C38—C39—O3 | 146.5 (7) | Ag2—O2—P3—C32 | 76.0 (2) |
C33—C32—C37O—C36 | 0.6 (7) | Ag1i—O2—P3—C32 | −176.91 (18) |
P3—C32—C37O—C36 | −172.6 (4) | Ag1—O1—P3—O2 | 56.4 (3) |
C35—C36—C37O—C32 | −0.5 (9) | Ag2i—O1—P3—O2 | −67.5 (3) |
P2—Ag1—O1—P3 | 33.9 (3) | Ag1—O1—P3—C26 | −178.9 (2) |
O3—Ag1—O1—P3 | 150.2 (2) | Ag2i—O1—P3—C26 | 57.2 (3) |
O2i—Ag1—O1—P3 | −116.5 (2) | Ag1—O1—P3—C32 | −69.8 (3) |
Ag2—Ag1—O1—P3 | −29.65 (19) | Ag2i—O1—P3—C32 | 166.3 (2) |
P2—Ag1—O1—Ag2i | 169.19 (9) | C27—C26—P3—O2 | 155.7 (4) |
O3—Ag1—O1—Ag2i | −74.42 (15) | C31—C26—P3—O2 | −31.1 (5) |
O2i—Ag1—O1—Ag2i | 18.88 (12) | C27—C26—P3—O1 | 26.3 (5) |
Ag2—Ag1—O1—Ag2i | 105.69 (10) | C31—C26—P3—O1 | −160.6 (4) |
P1—Ag2—O2—P3 | −50.7 (3) | C27—C26—P3—C32 | −88.2 (4) |
O1i—Ag2—O2—P3 | 97.1 (2) | C31—C26—P3—C32 | 84.9 (4) |
O4i—Ag2—O2—P3 | −177.4 (2) | C37O—C32—P3—O2 | −155.2 (3) |
Ag1—Ag2—O2—P3 | 20.03 (18) | C33—C32—P3—O2 | 31.7 (5) |
P1—Ag2—O2—Ag1i | −166.27 (7) | C37O—C32—P3—O1 | −24.8 (4) |
O1i—Ag2—O2—Ag1i | −18.40 (11) | C33—C32—P3—O1 | 162.2 (4) |
O4i—Ag2—O2—Ag1i | 67.05 (14) | C37O—C32—P3—C26 | 89.1 (4) |
Ag1—Ag2—O2—Ag1i | −95.51 (9) | C33—C32—P3—C26 | −83.9 (5) |
Symmetry code: (i) −x+1, −y+2, −z. |
D—H···A | D—H | H···A | D···A | D—H···A |
C19—H19···O3 | 0.93 | 2.46 | 3.380 (8) | 169 |
C7—H7···O4i | 0.93 | 2.45 | 3.368 (7) | 171 |
Symmetry code: (i) −x+1, −y+2, −z. |
Experimental details
Crystal data | |
Chemical formula | [Ag4(C2F3O2)2(C12H10O2P)2(C25H22P2)2]·2C2H3N |
Mr | 1942.70 |
Crystal system, space group | Monoclinic, P21/n |
Temperature (K) | 296 |
a, b, c (Å) | 11.724 (5), 14.777 (6), 24.183 (10) |
β (°) | 102.254 (5) |
V (Å3) | 4094 (3) |
Z | 2 |
Radiation type | Mo Kα |
µ (mm−1) | 1.13 |
Crystal size (mm) | 0.20 × 0.20 × 0.20 |
Data collection | |
Diffractometer | Rigaku Mercury CCD |
Absorption correction | Multi-scan (CrystalClear-SM Expert; Rigaku, 2009) |
Tmin, Tmax | 0.806, 0.806 |
No. of measured, independent and observed [I > 2σ(I)] reflections | 34844, 7192, 6033 |
Rint | 0.057 |
(sin θ/λ)max (Å−1) | 0.595 |
Refinement | |
R[F2 > 2σ(F2)], wR(F2), S | 0.046, 0.117, 1.01 |
No. of reflections | 7192 |
No. of parameters | 480 |
No. of restraints | 60 |
H-atom treatment | H-atom parameters constrained |
Δρmax, Δρmin (e Å−3) | 1.08, −0.59 |
Computer programs: CrystalClear-SM Expert (Rigaku, 2009), SHELXS97 (Sheldrick, 2008), SHELXL97 (Sheldrick, 2008), SHELXTL (Sheldrick, 2008).
D—H···A | D—H | H···A | D···A | D—H···A |
C19—H19···O3 | 0.93 | 2.46 | 3.380 (8) | 169 |
C7—H7···O4i | 0.93 | 2.45 | 3.368 (7) | 171 |
Symmetry code: (i) −x+1, −y+2, −z. |
References
Catalano, V. J. & Malwitz, M. A. (2004). J. Am. Chem. Soc. 126, 6560–6561. Web of Science CSD CrossRef PubMed CAS Google Scholar
Chiu, P. L. & Lee, H. M. (2005). Organometallics, 24, 1692–1702. Web of Science CSD CrossRef CAS Google Scholar
Kuang, S. M., Cuttell, D. G., McMillin, D. R., Fanwick, P. E. & Walton, R. A. (2002). Inorg. Chem. 41, 3313–3322. Web of Science CSD CrossRef PubMed CAS Google Scholar
Rigaku (2009). CrystalClear-SM Expert. Rigaku Corporation, Tokyo, Japan. Google Scholar
Rudler, H., Denise, B. & Ribeiro Gregorio, J. (1997). Chem. Commun. pp. 2299–2300. CSD CrossRef Web of Science Google Scholar
Sheldrick, G. M. (2008). Acta Cryst. A64, 112–122. Web of Science CrossRef CAS IUCr Journals Google Scholar
Zank, J., Schier, A. & Schmidbaur, H. (1999). J. Chem. Soc. Dalton Trans. pp. 415–420. Web of Science CSD CrossRef Google Scholar
This is an open-access article distributed under the terms of the Creative Commons Attribution (CC-BY) Licence, which permits unrestricted use, distribution, and reproduction in any medium, provided the original authors and source are cited.
Over the past three decades, metals complexes containing diphosphine ligands attract great interest for their importance in their potential applications in dye-sensitized solar cells and photochemical catalysts (Catalano & Malwitz, 2004; Chiu & Lee, 2005). A series of silver(I) complexes containing diphosphine ligands have been synthesized (Kuang et al., 2002). Synthetic tetranuclear silver(I) compounds have been widely reported (Rudler et al., 1997; Zank et al., 1999).
In the title compound (Fig. 1), the silver(I) atom adopts a distorted tetrahedral geometry through one P atom from a bis(diphenylphosphanyl)methane (dppm)ligand, one O atom from a trifluoroacetato anion and two O atoms from two diphenylphosphinate (dpp) ligands. Two dppm ligands, two dpp ligands and two trifluoroacetato anions bridge four metal atoms forming a centrosymmetric tetranuclear complex where the shortest Ag···Ag separation is 3.3655 (12) Å. The Ag—P and Ag—O bond distances are in the range 2.3685 (14)–2.3734 (14) and 2.278 (3)–2.505 (3) (14) Å, respectively. The O—Ag—P angles and O—Ag—O bond angles range from 80.56 (11) to 92.43 (14)° and from 106.90 (11) to 150.88 (8)°, respectively. In the crystal, intramolecular C—H···O hydrogen bonds are present (Table 1). In addition, a weak intramolecular π–π interaction of 3.9804 (13) Å between the centroids of the C8—C13 and C20—C25 phenyl rings is observed.