metal-organic compounds
Bis[μ2-bis(diphenylphosphanyl)methane-κ2P:P′]bis(μ4-diphenylphosphinato-κ4O:O:O′:O′)bis[μ2-trifluoromethanesulfonato(0.546/0.454)]-κ2O:O′;κ2O:O-tetrasilver(I) acetonitrile disolvate
aCollege of Chemistry, Sichuan University, Chengdu 610064, People's Republic of China, bSichuan College of Chemical Technology, Luzhou 646005, People's Republic of China, and cSchool of Chemistry and Chemical Engineering, Guangxi Normal University, Guilin 541004, People's Republic of China
*Correspondence e-mail: xjl_2003@yahoo.com.cn
In the centrosymmetric tetranuclear title compound, [Ag4(C12H10O2P)2(CF3O3S)2(C25H22P2)2]·2CH3CN, the AgI atom is coordinated by one P atom from a bis(diphenylphosphanyl)methane (dppm) ligand, two O atoms from two diphenylphosphinate (dpp) ligands and one O atom from a trifluoromethanesulfonate (OTf) anion in a highly distorted tetrahedral geometry. Four AgI atoms are bridged by two dppm ligands, two dpp ligands and two OTf anions, forming a tetranuclear complex. An weak intramolecular Ag⋯Ag [3.2692 (14) Å] interaction is observed. The OTf anion and one of the phenyl groups in the dppm ligand are disordered over two sets of positions in a 0.546 (4):0.454 (4) ratio. The 0.546-occupied OTf is bonded to two Ag atoms in a μ-(κ2O:O′) mode, while the 0.454-occupied OTf is bonded in a μ-(κ2O:O) mode. The methyl group of the acetonitrile solvent molecule is also disordered over two positions with equal occupancy factors.
Related literature
For related structures, see: Fournier et al. (2004); Matsumoto et al. (2001); Sun et al. (2011); Wei et al. (2004).
Experimental
Crystal data
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Refinement
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Data collection: CrystalClear (Rigaku, 2005); cell CrystalClear; data reduction: CrystalClear; 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
10.1107/S160053681102931X/hy2447sup1.cif
contains datablocks I, global. DOI:Structure factors: contains datablock I. DOI: 10.1107/S160053681102931X/hy2447Isup2.hkl
Silver trifluoromethanesulfonate (0.052 g, 0.2 mmol) was added with stirring to a solution of diphenylphosphinic acid (0.022 g, 0.1 mmol) and bis(diphenylphosphine)methane (0.038 g, 0.1 mmol) in CH3CN (5 ml). The resulting colorless solution was allowed to stir for 1 h. By slow diffusion of diethyl ether into the solution, prismatic colorless crystals were formed suitable for X-ray
(yield: 20%).H atoms were positioned geometrically and refined as riding atoms, with C—H = 0.93 (CH), 0.97 (CH2) and 0.96 (CH3) Å and with Uiso(H) = 1.2(1.5 for methyl)Ueq(C).
Data collection: CrystalClear (Rigaku, 2005); cell
CrystalClear (Rigaku, 2005); data reduction: CrystalClear (Rigaku, 2005); 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(C12H10O2P)2(CF3O3S)2(C25H22P2)2]·2C2H3N | F(000) = 2016 |
Mr = 2014.80 | Dx = 1.599 Mg m−3 |
Monoclinic, P21/n | Mo Kα radiation, λ = 0.71073 Å |
Hall symbol: -P 2yn | Cell parameters from 9952 reflections |
a = 11.730 (7) Å | θ = 1.6–27.5° |
b = 15.169 (9) Å | µ = 1.16 mm−1 |
c = 23.688 (12) Å | T = 296 K |
β = 96.967 (7)° | Prism, colorless |
V = 4184 (4) Å3 | 0.23 × 0.19 × 0.16 mm |
Z = 2 |
Rigaku Mercury CCD diffractometer | 9645 independent reflections |
Radiation source: fine-focus sealed tube | 7705 reflections with I > 2σ(I) |
Graphite monochromator | Rint = 0.055 |
Detector resolution: 13.6612 pixels mm-1 | θmax = 27.6°, θmin = 2.5° |
ω scans | h = −15→15 |
Absorption correction: multi-scan (CrystalClear; Rigaku, 2005) | k = −19→19 |
Tmin = 0.777, Tmax = 0.837 | l = −30→30 |
41763 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)] = 0.055 | Hydrogen site location: inferred from neighbouring sites |
wR(F2) = 0.144 | H-atom parameters constrained |
S = 1.01 | w = 1/[σ2(Fo2) + (0.0595P)2 + 6.765P] where P = (Fo2 + 2Fc2)/3 |
9645 reflections | (Δ/σ)max = 0.001 |
610 parameters | Δρmax = 0.64 e Å−3 |
1173 restraints | Δρmin = −0.61 e Å−3 |
[Ag4(C12H10O2P)2(CF3O3S)2(C25H22P2)2]·2C2H3N | V = 4184 (4) Å3 |
Mr = 2014.80 | Z = 2 |
Monoclinic, P21/n | Mo Kα radiation |
a = 11.730 (7) Å | µ = 1.16 mm−1 |
b = 15.169 (9) Å | T = 296 K |
c = 23.688 (12) Å | 0.23 × 0.19 × 0.16 mm |
β = 96.967 (7)° |
Rigaku Mercury CCD diffractometer | 9645 independent reflections |
Absorption correction: multi-scan (CrystalClear; Rigaku, 2005) | 7705 reflections with I > 2σ(I) |
Tmin = 0.777, Tmax = 0.837 | Rint = 0.055 |
41763 measured reflections |
R[F2 > 2σ(F2)] = 0.055 | 1173 restraints |
wR(F2) = 0.144 | H-atom parameters constrained |
S = 1.01 | Δρmax = 0.64 e Å−3 |
9645 reflections | Δρmin = −0.61 e Å−3 |
610 parameters |
x | y | z | Uiso*/Ueq | Occ. (<1) | |
Ag1 | 0.47428 (3) | 0.41739 (2) | 0.415893 (15) | 0.05183 (11) | |
Ag2 | 0.33273 (3) | 0.42158 (2) | 0.526552 (16) | 0.05416 (12) | |
P1 | 0.37541 (9) | 0.60694 (7) | 0.45735 (5) | 0.0427 (2) | |
P2 | 0.37149 (10) | 0.28791 (7) | 0.38828 (5) | 0.0456 (2) | |
P3 | 0.24066 (9) | 0.28840 (7) | 0.49519 (5) | 0.0461 (2) | |
O1 | 0.4690 (2) | 0.5658 (2) | 0.42767 (13) | 0.0487 (7) | |
O2 | 0.3558 (3) | 0.56941 (19) | 0.51457 (13) | 0.0501 (7) | |
C1 | 0.4054 (4) | 0.7227 (3) | 0.46521 (19) | 0.0502 (10) | |
C2 | 0.3628 (5) | 0.7712 (4) | 0.5078 (3) | 0.0739 (16) | |
H2A | 0.3261 | 0.7437 | 0.5357 | 0.089* | |
C3 | 0.3774 (6) | 0.8633 (5) | 0.5072 (4) | 0.102 (3) | |
H3A | 0.3496 | 0.8973 | 0.5352 | 0.122* | |
C4 | 0.4314 (8) | 0.9038 (5) | 0.4663 (5) | 0.115 (3) | |
H4A | 0.4380 | 0.9648 | 0.4659 | 0.138* | |
C5 | 0.4748 (7) | 0.8553 (5) | 0.4268 (4) | 0.105 (3) | |
H5A | 0.5139 | 0.8835 | 0.4000 | 0.126* | |
C6 | 0.4632 (5) | 0.7655 (4) | 0.4246 (2) | 0.0687 (14) | |
H6A | 0.4934 | 0.7332 | 0.3965 | 0.082* | |
C7 | 0.2421 (4) | 0.6076 (3) | 0.41141 (19) | 0.0499 (10) | |
C8 | 0.2426 (6) | 0.6155 (5) | 0.3537 (2) | 0.093 (2) | |
H8A | 0.3109 | 0.6132 | 0.3375 | 0.111* | |
C9 | 0.1359 (7) | 0.6272 (7) | 0.3197 (3) | 0.127 (3) | |
H9A | 0.1348 | 0.6358 | 0.2807 | 0.153* | |
C10 | 0.0358 (6) | 0.6261 (6) | 0.3424 (4) | 0.109 (3) | |
H10A | −0.0337 | 0.6299 | 0.3190 | 0.131* | |
C11 | 0.0372 (5) | 0.6195 (5) | 0.3986 (3) | 0.091 (2) | |
H11A | −0.0316 | 0.6204 | 0.4143 | 0.109* | |
C12 | 0.1395 (4) | 0.6114 (4) | 0.4336 (3) | 0.0700 (14) | |
H12A | 0.1389 | 0.6085 | 0.4728 | 0.084* | |
C13 | 0.4580 (4) | 0.2064 (3) | 0.35683 (19) | 0.0542 (11) | |
C14 | 0.5547 (5) | 0.2354 (5) | 0.3329 (3) | 0.0808 (17) | |
H14A | 0.5737 | 0.2949 | 0.3343 | 0.097* | |
C15 | 0.6219 (6) | 0.1770 (7) | 0.3075 (3) | 0.103 (2) | |
H15A | 0.6856 | 0.1973 | 0.2916 | 0.124* | |
C16 | 0.5964 (8) | 0.0908 (6) | 0.3056 (3) | 0.106 (3) | |
H16A | 0.6424 | 0.0519 | 0.2882 | 0.127* | |
C17 | 0.5038 (8) | 0.0600 (4) | 0.3288 (3) | 0.100 (3) | |
H17A | 0.4877 | −0.0001 | 0.3277 | 0.121* | |
C18 | 0.4324 (6) | 0.1178 (4) | 0.3544 (2) | 0.0771 (16) | |
H18A | 0.3683 | 0.0965 | 0.3696 | 0.093* | |
C19 | 0.3169 (4) | 0.2252 (3) | 0.44563 (18) | 0.0484 (9) | |
H19A | 0.2655 | 0.1799 | 0.4285 | 0.058* | |
H19B | 0.3813 | 0.1956 | 0.4673 | 0.058* | |
C20 | 0.2295 (4) | 0.2085 (3) | 0.5520 (2) | 0.0575 (11) | |
C21 | 0.2167 (6) | 0.1196 (4) | 0.5430 (3) | 0.0844 (18) | |
H21A | 0.2140 | 0.0969 | 0.5064 | 0.101* | |
C22 | 0.2077 (7) | 0.0631 (5) | 0.5885 (4) | 0.111 (3) | |
H22A | 0.1982 | 0.0029 | 0.5820 | 0.134* | |
C23 | 0.2127 (8) | 0.0948 (6) | 0.6421 (4) | 0.125 (4) | |
H23A | 0.2080 | 0.0566 | 0.6725 | 0.150* | |
C24 | 0.2245 (7) | 0.1826 (7) | 0.6513 (3) | 0.109 (3) | |
H24A | 0.2267 | 0.2043 | 0.6881 | 0.130* | |
C25 | 0.2334 (5) | 0.2407 (5) | 0.6069 (2) | 0.0773 (16) | |
H25A | 0.2418 | 0.3009 | 0.6139 | 0.093* | |
C26 | 0.0955 (4) | 0.2986 (3) | 0.4593 (2) | 0.0548 (11) | |
C27 | 0.0297 (6) | 0.2276 (5) | 0.4417 (4) | 0.122 (3) | |
H27A | 0.0580 | 0.1710 | 0.4492 | 0.146* | |
C28 | −0.0801 (6) | 0.2391 (6) | 0.4125 (5) | 0.135 (4) | |
H28A | −0.1246 | 0.1900 | 0.4013 | 0.162* | |
C29 | −0.1217 (5) | 0.3196 (6) | 0.4006 (3) | 0.094 (2) | |
H29A | −0.1938 | 0.3267 | 0.3800 | 0.112* | |
C30 | −0.0595 (6) | 0.3893 (5) | 0.4184 (4) | 0.107 (3) | |
H30A | −0.0897 | 0.4453 | 0.4110 | 0.128* | |
C31 | 0.0496 (5) | 0.3807 (4) | 0.4478 (3) | 0.0821 (18) | |
H31A | 0.0917 | 0.4307 | 0.4597 | 0.099* | |
C32 | 0.2483 (6) | 0.3084 (5) | 0.3333 (3) | 0.062 (2) | 0.546 (4) |
C33 | 0.1831 (7) | 0.3845 (5) | 0.3358 (3) | 0.083 (3) | 0.546 (4) |
H33A | 0.2057 | 0.4275 | 0.3628 | 0.100* | 0.546 (4) |
C34 | 0.0843 (7) | 0.3964 (5) | 0.2978 (4) | 0.092 (3) | 0.546 (4) |
H34A | 0.0407 | 0.4473 | 0.2994 | 0.111* | 0.546 (4) |
C35 | 0.0506 (7) | 0.3321 (6) | 0.2574 (4) | 0.109 (3) | 0.546 (4) |
H35A | −0.0155 | 0.3400 | 0.2320 | 0.131* | 0.546 (4) |
C36 | 0.1158 (8) | 0.2560 (6) | 0.2549 (4) | 0.107 (3) | 0.546 (4) |
H36A | 0.0932 | 0.2130 | 0.2278 | 0.129* | 0.546 (4) |
C37 | 0.2146 (8) | 0.2441 (5) | 0.2928 (4) | 0.102 (3) | 0.546 (4) |
H37A | 0.2582 | 0.1932 | 0.2912 | 0.122* | 0.546 (4) |
C32A | 0.2485 (8) | 0.3032 (7) | 0.3374 (4) | 0.069 (3) | 0.454 (4) |
C33A | 0.2426 (9) | 0.3856 (7) | 0.3116 (5) | 0.106 (3) | 0.454 (4) |
H33B | 0.3025 | 0.4256 | 0.3196 | 0.127* | 0.454 (4) |
C34A | 0.1473 (11) | 0.4083 (6) | 0.2737 (5) | 0.109 (3) | 0.454 (4) |
H34B | 0.1433 | 0.4634 | 0.2564 | 0.131* | 0.454 (4) |
C35A | 0.0578 (9) | 0.3486 (7) | 0.2616 (5) | 0.109 (3) | 0.454 (4) |
H35B | −0.0061 | 0.3637 | 0.2363 | 0.131* | 0.454 (4) |
C36A | 0.0636 (8) | 0.2661 (7) | 0.2875 (5) | 0.095 (3) | 0.454 (4) |
H36B | 0.0037 | 0.2262 | 0.2794 | 0.114* | 0.454 (4) |
C37A | 0.1590 (9) | 0.2435 (6) | 0.3254 (4) | 0.087 (3) | 0.454 (4) |
H37B | 0.1629 | 0.1883 | 0.3426 | 0.104* | 0.454 (4) |
S3 | 0.6892 (4) | 0.4984 (3) | 0.3233 (2) | 0.0534 (9) | 0.546 (4) |
F1 | 0.5949 (11) | 0.5743 (8) | 0.2281 (4) | 0.129 (3) | 0.546 (4) |
F2 | 0.4775 (11) | 0.5059 (10) | 0.2761 (5) | 0.171 (4) | 0.546 (4) |
F3 | 0.5531 (10) | 0.6323 (7) | 0.3112 (4) | 0.116 (3) | 0.546 (4) |
O3 | 0.6061 (8) | 0.4384 (7) | 0.3385 (4) | 0.105 (2) | 0.546 (4) |
O4 | 0.7736 (8) | 0.4696 (7) | 0.2896 (4) | 0.089 (2) | 0.546 (4) |
O5 | 0.7325 (7) | 0.5485 (6) | 0.3733 (3) | 0.090 (2) | 0.546 (4) |
C38 | 0.5805 (10) | 0.5538 (7) | 0.2844 (4) | 0.112 (3) | 0.546 (4) |
S3B | 0.6771 (9) | 0.5015 (6) | 0.3148 (4) | 0.101 (3) | 0.454 (4) |
F1B | 0.5476 (12) | 0.5333 (11) | 0.2273 (6) | 0.128 (4) | 0.454 (4) |
F2B | 0.6761 (10) | 0.6489 (7) | 0.2723 (5) | 0.131 (3) | 0.454 (4) |
F3B | 0.4952 (11) | 0.5877 (11) | 0.2957 (6) | 0.128 (4) | 0.454 (4) |
O3B | 0.6535 (9) | 0.4851 (8) | 0.3711 (4) | 0.085 (3) | 0.454 (4) |
O4B | 0.7099 (14) | 0.4260 (9) | 0.2841 (5) | 0.113 (3) | 0.454 (4) |
O5B | 0.7712 (12) | 0.5619 (10) | 0.3130 (6) | 0.139 (4) | 0.454 (4) |
C38B | 0.6009 (10) | 0.5791 (9) | 0.2748 (6) | 0.112 (4) | 0.454 (4) |
N1 | 0.1746 (8) | 1.0190 (5) | 0.4011 (4) | 0.148 (3) | |
C39 | 0.1507 (8) | 0.9478 (8) | 0.3896 (6) | 0.163 (5) | |
C40A | 0.150 (2) | 0.8812 (15) | 0.3496 (14) | 0.212 (9) | 0.50 |
H40A | 0.2094 | 0.8395 | 0.3615 | 0.318* | 0.50 |
H40B | 0.1624 | 0.9060 | 0.3135 | 0.318* | 0.50 |
H40C | 0.0767 | 0.8518 | 0.3459 | 0.318* | 0.50 |
C40B | 0.1071 (16) | 0.8694 (11) | 0.4110 (12) | 0.162 (7) | 0.50 |
H40D | 0.0406 | 0.8506 | 0.3863 | 0.243* | 0.50 |
H40E | 0.0863 | 0.8799 | 0.4484 | 0.243* | 0.50 |
H40F | 0.1649 | 0.8243 | 0.4129 | 0.243* | 0.50 |
U11 | U22 | U33 | U12 | U13 | U23 | |
Ag1 | 0.0551 (2) | 0.0487 (2) | 0.0512 (2) | −0.00963 (15) | 0.00500 (15) | −0.00754 (14) |
Ag2 | 0.0505 (2) | 0.0516 (2) | 0.0602 (2) | −0.00592 (15) | 0.00608 (15) | −0.00487 (15) |
P1 | 0.0388 (5) | 0.0407 (5) | 0.0469 (6) | 0.0029 (4) | −0.0016 (4) | −0.0006 (4) |
P2 | 0.0493 (6) | 0.0425 (6) | 0.0446 (6) | −0.0038 (5) | 0.0038 (4) | −0.0052 (4) |
P3 | 0.0407 (5) | 0.0460 (6) | 0.0517 (6) | −0.0020 (4) | 0.0063 (4) | 0.0041 (5) |
O1 | 0.0421 (15) | 0.0478 (16) | 0.0559 (17) | 0.0036 (12) | 0.0049 (12) | −0.0051 (13) |
O2 | 0.0537 (17) | 0.0481 (17) | 0.0466 (16) | 0.0017 (13) | −0.0021 (13) | 0.0021 (12) |
C1 | 0.045 (2) | 0.041 (2) | 0.061 (3) | 0.0041 (18) | −0.0083 (19) | −0.0002 (18) |
C2 | 0.067 (3) | 0.056 (3) | 0.094 (4) | 0.012 (3) | −0.009 (3) | −0.024 (3) |
C3 | 0.086 (5) | 0.067 (4) | 0.142 (7) | 0.027 (4) | −0.027 (4) | −0.042 (4) |
C4 | 0.109 (6) | 0.043 (3) | 0.176 (9) | −0.007 (4) | −0.055 (6) | 0.008 (4) |
C5 | 0.115 (6) | 0.059 (4) | 0.130 (6) | −0.018 (4) | −0.031 (5) | 0.036 (4) |
C6 | 0.073 (3) | 0.057 (3) | 0.072 (3) | −0.009 (3) | −0.008 (3) | 0.020 (2) |
C7 | 0.045 (2) | 0.049 (2) | 0.053 (2) | 0.0040 (19) | −0.0026 (18) | −0.0054 (19) |
C8 | 0.076 (4) | 0.146 (6) | 0.053 (3) | 0.007 (4) | −0.006 (3) | −0.010 (4) |
C9 | 0.097 (6) | 0.210 (10) | 0.064 (4) | 0.013 (6) | −0.031 (4) | −0.004 (5) |
C10 | 0.067 (4) | 0.147 (7) | 0.103 (6) | 0.017 (4) | −0.036 (4) | −0.010 (5) |
C11 | 0.045 (3) | 0.107 (5) | 0.115 (6) | 0.011 (3) | −0.011 (3) | −0.010 (4) |
C12 | 0.052 (3) | 0.076 (4) | 0.078 (4) | 0.011 (3) | −0.006 (2) | −0.009 (3) |
C13 | 0.062 (3) | 0.054 (3) | 0.047 (2) | 0.006 (2) | 0.0042 (19) | −0.0079 (19) |
C14 | 0.070 (4) | 0.091 (4) | 0.086 (4) | 0.001 (3) | 0.025 (3) | −0.023 (3) |
C15 | 0.085 (5) | 0.140 (7) | 0.089 (5) | 0.027 (5) | 0.031 (4) | −0.015 (5) |
C16 | 0.130 (7) | 0.121 (7) | 0.066 (4) | 0.071 (6) | 0.015 (4) | −0.004 (4) |
C17 | 0.176 (8) | 0.062 (4) | 0.063 (4) | 0.039 (4) | 0.014 (4) | −0.003 (3) |
C18 | 0.117 (5) | 0.053 (3) | 0.065 (3) | 0.009 (3) | 0.025 (3) | −0.005 (2) |
C19 | 0.044 (2) | 0.044 (2) | 0.057 (2) | −0.0055 (18) | 0.0060 (18) | 0.0000 (18) |
C20 | 0.052 (3) | 0.062 (3) | 0.060 (3) | 0.007 (2) | 0.015 (2) | 0.016 (2) |
C21 | 0.099 (5) | 0.069 (4) | 0.091 (4) | 0.006 (3) | 0.039 (4) | 0.024 (3) |
C22 | 0.121 (6) | 0.079 (5) | 0.145 (7) | 0.018 (4) | 0.060 (5) | 0.054 (5) |
C23 | 0.133 (7) | 0.130 (7) | 0.125 (7) | 0.052 (6) | 0.066 (6) | 0.081 (6) |
C24 | 0.103 (5) | 0.159 (8) | 0.069 (4) | 0.048 (5) | 0.029 (4) | 0.042 (5) |
C25 | 0.074 (4) | 0.101 (5) | 0.058 (3) | 0.014 (3) | 0.016 (3) | 0.022 (3) |
C26 | 0.038 (2) | 0.061 (3) | 0.066 (3) | −0.006 (2) | 0.0057 (19) | 0.005 (2) |
C27 | 0.061 (4) | 0.062 (4) | 0.227 (10) | −0.007 (3) | −0.045 (5) | 0.003 (5) |
C28 | 0.064 (4) | 0.104 (6) | 0.222 (10) | −0.020 (4) | −0.045 (5) | 0.005 (6) |
C29 | 0.050 (3) | 0.119 (6) | 0.107 (5) | −0.005 (4) | −0.011 (3) | 0.027 (4) |
C30 | 0.072 (4) | 0.088 (5) | 0.149 (7) | 0.013 (4) | −0.034 (4) | 0.025 (5) |
C31 | 0.065 (3) | 0.066 (4) | 0.108 (5) | 0.005 (3) | −0.019 (3) | 0.013 (3) |
C32 | 0.069 (5) | 0.052 (4) | 0.060 (4) | −0.010 (4) | −0.012 (4) | 0.001 (4) |
C33 | 0.089 (5) | 0.072 (5) | 0.079 (5) | 0.002 (5) | −0.026 (4) | 0.003 (4) |
C34 | 0.092 (5) | 0.085 (5) | 0.091 (5) | 0.004 (5) | −0.023 (5) | 0.012 (5) |
C35 | 0.106 (6) | 0.094 (5) | 0.112 (6) | −0.017 (5) | −0.046 (5) | 0.010 (5) |
C36 | 0.107 (6) | 0.101 (5) | 0.102 (6) | −0.009 (5) | −0.039 (5) | −0.014 (5) |
C37 | 0.102 (6) | 0.087 (5) | 0.104 (6) | −0.007 (5) | −0.039 (5) | −0.008 (5) |
C32A | 0.075 (5) | 0.060 (5) | 0.067 (5) | −0.013 (5) | −0.014 (5) | 0.007 (5) |
C33A | 0.109 (6) | 0.089 (6) | 0.106 (6) | −0.014 (5) | −0.040 (5) | 0.023 (5) |
C34A | 0.108 (6) | 0.096 (6) | 0.111 (6) | −0.015 (5) | −0.036 (5) | 0.019 (5) |
C35A | 0.107 (6) | 0.096 (6) | 0.111 (6) | −0.014 (5) | −0.044 (5) | 0.017 (5) |
C36A | 0.091 (6) | 0.090 (5) | 0.095 (6) | −0.019 (5) | −0.029 (5) | −0.003 (5) |
C37A | 0.088 (6) | 0.079 (5) | 0.084 (6) | −0.019 (5) | −0.030 (5) | 0.007 (5) |
S3 | 0.0522 (16) | 0.0584 (18) | 0.0537 (18) | 0.0065 (14) | 0.0231 (14) | 0.0032 (14) |
F1 | 0.153 (8) | 0.160 (8) | 0.076 (5) | 0.043 (6) | 0.025 (5) | 0.049 (5) |
F2 | 0.154 (7) | 0.197 (8) | 0.151 (7) | −0.012 (7) | −0.027 (6) | 0.005 (7) |
F3 | 0.136 (7) | 0.114 (6) | 0.099 (5) | 0.042 (5) | 0.014 (5) | −0.004 (4) |
O3 | 0.113 (5) | 0.118 (6) | 0.093 (5) | −0.016 (5) | 0.049 (4) | 0.005 (4) |
O4 | 0.090 (5) | 0.114 (6) | 0.072 (4) | 0.023 (5) | 0.049 (4) | 0.009 (4) |
O5 | 0.100 (5) | 0.099 (5) | 0.073 (5) | 0.000 (5) | 0.022 (4) | −0.007 (4) |
C38 | 0.105 (6) | 0.138 (7) | 0.094 (6) | 0.051 (5) | 0.015 (5) | 0.040 (6) |
S3B | 0.114 (5) | 0.113 (5) | 0.078 (4) | −0.020 (4) | 0.025 (3) | 0.001 (3) |
F1B | 0.116 (8) | 0.157 (9) | 0.110 (7) | 0.004 (7) | 0.008 (6) | 0.003 (7) |
F2B | 0.151 (7) | 0.123 (7) | 0.125 (6) | 0.012 (6) | 0.043 (6) | 0.038 (5) |
F3B | 0.109 (7) | 0.162 (9) | 0.122 (7) | 0.061 (6) | 0.045 (6) | 0.020 (7) |
O3B | 0.086 (6) | 0.115 (7) | 0.060 (5) | 0.006 (5) | 0.029 (4) | 0.005 (5) |
O4B | 0.140 (8) | 0.126 (8) | 0.078 (6) | 0.040 (7) | 0.033 (6) | −0.011 (6) |
O5B | 0.134 (8) | 0.156 (8) | 0.133 (8) | −0.034 (7) | 0.047 (7) | 0.001 (7) |
C38B | 0.119 (7) | 0.133 (7) | 0.091 (7) | 0.019 (7) | 0.049 (6) | 0.028 (7) |
N1 | 0.151 (7) | 0.080 (5) | 0.205 (8) | −0.016 (5) | −0.011 (6) | −0.017 (5) |
C39 | 0.092 (6) | 0.102 (7) | 0.276 (13) | 0.005 (5) | −0.052 (7) | −0.025 (8) |
C40A | 0.176 (17) | 0.173 (17) | 0.27 (2) | 0.027 (15) | −0.042 (17) | −0.088 (16) |
C40B | 0.092 (11) | 0.120 (13) | 0.261 (19) | −0.028 (10) | −0.032 (13) | 0.057 (14) |
Ag1—O1 | 2.270 (3) | C22—H22A | 0.9300 |
Ag1—O2i | 2.435 (3) | C23—C24 | 1.353 (13) |
Ag1—O3 | 2.557 (8) | C23—H23A | 0.9300 |
Ag1—O3B | 2.672 (11) | C24—C25 | 1.386 (9) |
Ag1—P2 | 2.3554 (15) | C24—H24A | 0.9300 |
Ag2—O1i | 2.451 (3) | C25—H25A | 0.9300 |
Ag2—O2 | 2.280 (3) | C26—C27 | 1.360 (8) |
Ag2—O5i | 2.619 (8) | C26—C31 | 1.371 (5) |
Ag2—O3Bi | 2.795 (10) | C27—C28 | 1.396 (9) |
Ag2—P3 | 2.3676 (16) | C27—H27A | 0.9300 |
Ag1—Ag2 | 3.2692 (14) | C28—C29 | 1.333 (11) |
P1—O1 | 1.509 (3) | C28—H28A | 0.9300 |
P1—O2 | 1.513 (3) | C29—C30 | 1.324 (10) |
P1—C7 | 1.794 (4) | C29—H29A | 0.9300 |
P1—C1 | 1.796 (5) | C30—C31 | 1.387 (8) |
P2—C32A | 1.779 (7) | C30—H30A | 0.9300 |
P2—C13 | 1.816 (5) | C31—H31A | 0.9300 |
P2—C19 | 1.836 (4) | C32—C33 | 1.3900 |
P2—C32 | 1.851 (6) | C32—C37 | 1.3900 |
P3—C26 | 1.815 (5) | C33—C34 | 1.3900 |
P3—C20 | 1.827 (5) | C33—H33A | 0.9300 |
P3—C19 | 1.831 (5) | C34—C35 | 1.3900 |
C1—C2 | 1.389 (7) | C34—H34A | 0.9300 |
C1—C6 | 1.402 (7) | C35—C36 | 1.3900 |
C2—C3 | 1.409 (9) | C35—H35A | 0.9300 |
C2—H2A | 0.9300 | C36—C37 | 1.3900 |
C3—C4 | 1.366 (12) | C36—H36A | 0.9300 |
C3—H3A | 0.9300 | C37—H37A | 0.9300 |
C4—C5 | 1.337 (12) | C32A—C33A | 1.3900 |
C4—H4A | 0.9300 | C32A—C37A | 1.3900 |
C5—C6 | 1.370 (9) | C33A—C34A | 1.3900 |
C5—H5A | 0.9300 | C33A—H33B | 0.9300 |
C6—H6A | 0.9300 | C34A—C35A | 1.3900 |
C7—C12 | 1.371 (7) | C34A—H34B | 0.9300 |
C7—C8 | 1.373 (7) | C35A—C36A | 1.3900 |
C8—C9 | 1.415 (9) | C35A—H35B | 0.9300 |
C8—H8A | 0.9300 | C36A—C37A | 1.3900 |
C9—C10 | 1.350 (11) | C36A—H36B | 0.9300 |
C9—H9A | 0.9300 | C37A—H37B | 0.9300 |
C10—C11 | 1.332 (10) | S3—O3 | 1.412 (8) |
C10—H10A | 0.9300 | S3—O4 | 1.415 (6) |
C11—C12 | 1.379 (7) | S3—O5 | 1.446 (7) |
C11—H11A | 0.9300 | S3—C38 | 1.702 (10) |
C12—H12A | 0.9300 | F1—C38 | 1.399 (8) |
C13—C18 | 1.376 (7) | F2—C38 | 1.402 (8) |
C13—C14 | 1.399 (8) | F3—C38 | 1.405 (8) |
C14—C15 | 1.372 (9) | S3B—O3B | 1.416 (9) |
C14—H14A | 0.9300 | S3B—O4B | 1.434 (8) |
C15—C16 | 1.340 (12) | S3B—O5B | 1.439 (8) |
C15—H15A | 0.9300 | S3B—C38B | 1.696 (12) |
C16—C17 | 1.359 (12) | F1B—C38B | 1.403 (8) |
C16—H16A | 0.9300 | F2B—C38B | 1.384 (8) |
C17—C18 | 1.401 (9) | F3B—C38B | 1.396 (8) |
C17—H17A | 0.9300 | N1—C39 | 1.141 (11) |
C18—H18A | 0.9300 | C39—C40A | 1.39 (2) |
C19—H19A | 0.9700 | C39—C40B | 1.413 (19) |
C19—H19B | 0.9700 | C40A—H40A | 0.9600 |
C20—C21 | 1.372 (8) | C40A—H40B | 0.9600 |
C20—C25 | 1.385 (8) | C40A—H40C | 0.9600 |
C21—C22 | 1.390 (9) | C40B—H40D | 0.9600 |
C21—H21A | 0.9300 | C40B—H40E | 0.9600 |
C22—C23 | 1.353 (13) | C40B—H40F | 0.9600 |
O1—Ag1—P2 | 147.19 (8) | C20—C21—C22 | 120.2 (7) |
O1—Ag1—O2i | 82.38 (10) | C20—C21—H21A | 119.9 |
P2—Ag1—O2i | 127.29 (8) | C22—C21—H21A | 119.9 |
O1—Ag1—O3 | 89.6 (2) | C23—C22—C21 | 120.6 (8) |
P2—Ag1—O3 | 103.8 (2) | C23—C22—H22A | 119.7 |
O2i—Ag1—O3 | 87.6 (3) | C21—C22—H22A | 119.7 |
O1—Ag1—Ag2 | 81.85 (8) | C24—C23—C22 | 119.5 (7) |
P2—Ag1—Ag2 | 86.92 (4) | C24—C23—H23A | 120.2 |
O2i—Ag1—Ag2 | 84.82 (9) | C22—C23—H23A | 120.2 |
O3—Ag1—Ag2 | 169.2 (2) | C23—C24—C25 | 121.3 (8) |
O2—Ag2—P3 | 148.93 (8) | C23—C24—H24A | 119.3 |
O2—Ag2—O1i | 81.83 (10) | C25—C24—H24A | 119.3 |
P3—Ag2—O1i | 125.28 (8) | C20—C25—C24 | 119.4 (7) |
O2—Ag2—Ag1 | 80.79 (8) | C20—C25—H25A | 120.3 |
P3—Ag2—Ag1 | 89.34 (4) | C24—C25—H25A | 120.3 |
O1i—Ag2—Ag1 | 79.01 (8) | C27—C26—C31 | 117.6 (5) |
O1—P1—O2 | 117.39 (19) | C27—C26—P3 | 122.8 (4) |
O1—P1—C7 | 110.5 (2) | C31—C26—P3 | 119.6 (4) |
O2—P1—C7 | 109.2 (2) | C26—C27—C28 | 120.5 (7) |
O1—P1—C1 | 107.9 (2) | C26—C27—H27A | 119.7 |
O2—P1—C1 | 108.9 (2) | C28—C27—H27A | 119.7 |
C7—P1—C1 | 101.7 (2) | C29—C28—C27 | 120.8 (7) |
C32A—P2—C13 | 105.0 (4) | C29—C28—H28A | 119.6 |
C32A—P2—C19 | 104.0 (4) | C27—C28—H28A | 119.6 |
C13—P2—C19 | 102.3 (2) | C30—C29—C28 | 119.3 (6) |
C13—P2—C32 | 104.6 (3) | C30—C29—H29A | 120.3 |
C19—P2—C32 | 107.2 (3) | C28—C29—H29A | 120.3 |
C32A—P2—Ag1 | 115.2 (3) | C29—C30—C31 | 121.7 (7) |
C13—P2—Ag1 | 112.91 (17) | C29—C30—H30A | 119.2 |
C19—P2—Ag1 | 116.07 (15) | C31—C30—H30A | 119.2 |
C32—P2—Ag1 | 112.7 (3) | C26—C31—C30 | 120.1 (6) |
C26—P3—C20 | 104.8 (2) | C26—C31—H31A | 120.0 |
C26—P3—C19 | 104.3 (2) | C30—C31—H31A | 120.0 |
C20—P3—C19 | 102.1 (2) | C33—C32—C37 | 120.0 |
C26—P3—Ag2 | 116.15 (16) | C33—C32—P2 | 119.7 (4) |
C20—P3—Ag2 | 113.91 (18) | C37—C32—P2 | 120.0 (4) |
C19—P3—Ag2 | 114.10 (14) | C32—C33—C34 | 120.0 |
P1—O1—Ag1 | 119.96 (17) | C32—C33—H33A | 120.0 |
P1—O1—Ag2i | 117.81 (16) | C34—C33—H33A | 120.0 |
Ag1—O1—Ag2i | 95.36 (10) | C33—C34—C35 | 120.0 |
P1—O2—Ag2 | 120.97 (17) | C33—C34—H34A | 120.0 |
P1—O2—Ag1i | 111.96 (17) | C35—C34—H34A | 120.0 |
Ag2—O2—Ag1i | 95.53 (10) | C36—C35—C34 | 120.0 |
C2—C1—C6 | 120.0 (5) | C36—C35—H35A | 120.0 |
C2—C1—P1 | 120.6 (4) | C34—C35—H35A | 120.0 |
C6—C1—P1 | 119.1 (4) | C35—C36—C37 | 120.0 |
C1—C2—C3 | 117.6 (7) | C35—C36—H36A | 120.0 |
C1—C2—H2A | 121.2 | C37—C36—H36A | 120.0 |
C3—C2—H2A | 121.2 | C36—C37—C32 | 120.0 |
C4—C3—C2 | 121.3 (7) | C36—C37—H37A | 120.0 |
C4—C3—H3A | 119.3 | C32—C37—H37A | 120.0 |
C2—C3—H3A | 119.3 | C33A—C32A—C37A | 120.0 |
C5—C4—C3 | 119.9 (7) | C33A—C32A—P2 | 114.1 (6) |
C5—C4—H4A | 120.1 | C37A—C32A—P2 | 125.8 (6) |
C3—C4—H4A | 120.1 | C34A—C33A—C32A | 120.0 |
C4—C5—C6 | 121.9 (8) | C34A—C33A—H33B | 120.0 |
C4—C5—H5A | 119.1 | C32A—C33A—H33B | 120.0 |
C6—C5—H5A | 119.1 | C33A—C34A—C35A | 120.0 |
C5—C6—C1 | 119.2 (7) | C33A—C34A—H34B | 120.0 |
C5—C6—H6A | 120.4 | C35A—C34A—H34B | 120.0 |
C1—C6—H6A | 120.4 | C36A—C35A—C34A | 120.0 |
C12—C7—C8 | 119.2 (5) | C36A—C35A—H35B | 120.0 |
C12—C7—P1 | 120.6 (4) | C34A—C35A—H35B | 120.0 |
C8—C7—P1 | 119.7 (4) | C37A—C36A—C35A | 120.0 |
C7—C8—C9 | 117.9 (7) | C37A—C36A—H36B | 120.0 |
C7—C8—H8A | 121.1 | C35A—C36A—H36B | 120.0 |
C9—C8—H8A | 121.1 | C36A—C37A—C32A | 120.0 |
C10—C9—C8 | 121.6 (7) | C36A—C37A—H37B | 120.0 |
C10—C9—H9A | 119.2 | C32A—C37A—H37B | 120.0 |
C8—C9—H9A | 119.2 | O3—S3—O4 | 119.8 (7) |
C11—C10—C9 | 119.5 (6) | O3—S3—O5 | 108.4 (7) |
C11—C10—H10A | 120.2 | O4—S3—O5 | 115.1 (7) |
C9—C10—H10A | 120.2 | O3—S3—C38 | 87.8 (7) |
C10—C11—C12 | 120.8 (7) | O4—S3—C38 | 112.1 (6) |
C10—C11—H11A | 119.6 | O5—S3—C38 | 110.4 (6) |
C12—C11—H11A | 119.6 | S3—O3—Ag1 | 139.4 (7) |
C7—C12—C11 | 120.9 (6) | F1—C38—F2 | 100.5 (10) |
C7—C12—H12A | 119.6 | F1—C38—F3 | 107.5 (10) |
C11—C12—H12A | 119.6 | F2—C38—F3 | 105.2 (10) |
C18—C13—C14 | 118.3 (5) | F1—C38—S3 | 117.2 (8) |
C18—C13—P2 | 123.5 (4) | F2—C38—S3 | 113.3 (9) |
C14—C13—P2 | 118.2 (4) | F3—C38—S3 | 111.8 (8) |
C15—C14—C13 | 120.8 (7) | O3B—S3B—O4B | 115.6 (10) |
C15—C14—H14A | 119.6 | O3B—S3B—O5B | 112.3 (10) |
C13—C14—H14A | 119.6 | O4B—S3B—O5B | 103.8 (11) |
C16—C15—C14 | 120.4 (8) | O3B—S3B—C38B | 119.9 (8) |
C16—C15—H15A | 119.8 | O4B—S3B—C38B | 115.2 (9) |
C14—C15—H15A | 119.8 | O5B—S3B—C38B | 84.0 (9) |
C15—C16—C17 | 120.5 (7) | F2B—C38B—F3B | 122.8 (14) |
C15—C16—H16A | 119.7 | F2B—C38B—F1B | 124.6 (13) |
C17—C16—H16A | 119.7 | F3B—C38B—F1B | 90.2 (12) |
C16—C17—C18 | 120.6 (7) | F2B—C38B—S3B | 105.0 (9) |
C16—C17—H17A | 119.7 | F3B—C38B—S3B | 107.3 (10) |
C18—C17—H17A | 119.7 | F1B—C38B—S3B | 104.9 (11) |
C13—C18—C17 | 119.4 (7) | N1—C39—C40A | 147 (2) |
C13—C18—H18A | 120.3 | N1—C39—C40B | 143 (2) |
C17—C18—H18A | 120.3 | C40A—C39—C40B | 70.0 (17) |
P3—C19—P2 | 116.4 (2) | C39—C40A—H40A | 109.5 |
P3—C19—H19A | 108.2 | C39—C40A—H40B | 109.5 |
P2—C19—H19A | 108.2 | C39—C40A—H40C | 109.5 |
P3—C19—H19B | 108.2 | C39—C40B—H40D | 109.5 |
P2—C19—H19B | 108.2 | C39—C40B—H40E | 109.5 |
H19A—C19—H19B | 107.3 | H40D—C40B—H40E | 109.5 |
C21—C20—C25 | 118.9 (5) | C39—C40B—H40F | 109.5 |
C21—C20—P3 | 123.7 (4) | H40D—C40B—H40F | 109.5 |
C25—C20—P3 | 117.4 (4) | H40E—C40B—H40F | 109.5 |
O1—Ag1—Ag2—O2 | 0.50 (10) | P2—C13—C14—C15 | −178.7 (5) |
P2—Ag1—Ag2—O2 | −148.59 (8) | C13—C14—C15—C16 | −0.5 (11) |
O2i—Ag1—Ag2—O2 | 83.53 (11) | C14—C15—C16—C17 | −0.2 (12) |
O3—Ag1—Ag2—O2 | 38.0 (13) | C15—C16—C17—C18 | 1.0 (12) |
O1—Ag1—Ag2—P3 | 150.92 (8) | C14—C13—C18—C17 | 0.6 (9) |
P2—Ag1—Ag2—P3 | 1.83 (4) | P2—C13—C18—C17 | 179.4 (5) |
O2i—Ag1—Ag2—P3 | −126.06 (8) | C16—C17—C18—C13 | −1.2 (10) |
O3—Ag1—Ag2—P3 | −171.6 (13) | C26—P3—C19—P2 | 82.8 (3) |
O1—Ag1—Ag2—O1i | −82.88 (11) | C20—P3—C19—P2 | −168.3 (2) |
P2—Ag1—Ag2—O1i | 128.03 (8) | Ag2—P3—C19—P2 | −45.0 (3) |
O2i—Ag1—Ag2—O1i | 0.14 (10) | C32A—P2—C19—P3 | −79.4 (5) |
O3—Ag1—Ag2—O1i | −45.4 (13) | C13—P2—C19—P3 | 171.6 (2) |
O1—Ag1—P2—C32A | 27.5 (5) | C32—P2—C19—P3 | −78.7 (4) |
O2i—Ag1—P2—C32A | 178.4 (5) | Ag1—P2—C19—P3 | 48.2 (3) |
O3—Ag1—P2—C32A | −84.0 (5) | C26—P3—C20—C21 | 74.9 (5) |
Ag2—Ag1—P2—C32A | 97.3 (5) | C19—P3—C20—C21 | −33.6 (5) |
O1—Ag1—P2—C13 | 148.0 (2) | Ag2—P3—C20—C21 | −157.1 (4) |
O2i—Ag1—P2—C13 | −61.1 (2) | C26—P3—C20—C25 | −104.5 (4) |
O3—Ag1—P2—C13 | 36.6 (3) | C19—P3—C20—C25 | 147.0 (4) |
Ag2—Ag1—P2—C13 | −142.17 (16) | Ag2—P3—C20—C25 | 23.5 (4) |
O1—Ag1—P2—C19 | −94.3 (2) | C25—C20—C21—C22 | 0.0 (9) |
O2i—Ag1—P2—C19 | 56.58 (19) | P3—C20—C21—C22 | −179.4 (5) |
O3—Ag1—P2—C19 | 154.2 (3) | C20—C21—C22—C23 | −0.7 (12) |
Ag2—Ag1—P2—C19 | −24.53 (16) | C21—C22—C23—C24 | 1.2 (13) |
O1—Ag1—P2—C32 | 29.8 (4) | C22—C23—C24—C25 | −0.9 (13) |
O2i—Ag1—P2—C32 | −179.4 (3) | C21—C20—C25—C24 | 0.2 (9) |
O3—Ag1—P2—C32 | −81.7 (4) | P3—C20—C25—C24 | 179.6 (5) |
Ag2—Ag1—P2—C32 | 99.5 (3) | C23—C24—C25—C20 | 0.3 (11) |
O2—Ag2—P3—C26 | −30.1 (3) | C20—P3—C26—C27 | −49.7 (7) |
O1i—Ag2—P3—C26 | −176.92 (19) | C19—P3—C26—C27 | 57.2 (7) |
Ag1—Ag2—P3—C26 | −100.90 (18) | Ag2—P3—C26—C27 | −176.3 (6) |
O2—Ag2—P3—C20 | −152.0 (2) | C20—P3—C26—C31 | 131.9 (5) |
O1i—Ag2—P3—C20 | 61.20 (19) | C19—P3—C26—C31 | −121.2 (5) |
Ag1—Ag2—P3—C20 | 137.22 (17) | Ag2—P3—C26—C31 | 5.3 (5) |
O2—Ag2—P3—C19 | 91.3 (2) | C31—C26—C27—C28 | 0.7 (13) |
O1i—Ag2—P3—C19 | −55.48 (19) | P3—C26—C27—C28 | −177.8 (8) |
Ag1—Ag2—P3—C19 | 20.54 (16) | C26—C27—C28—C29 | 1.0 (16) |
O2—P1—O1—Ag1 | 51.1 (2) | C27—C28—C29—C30 | −2.3 (15) |
C7—P1—O1—Ag1 | −75.0 (2) | C28—C29—C30—C31 | 2.0 (14) |
C1—P1—O1—Ag1 | 174.54 (18) | C27—C26—C31—C30 | −1.0 (11) |
O2—P1—O1—Ag2i | −64.2 (2) | P3—C26—C31—C30 | 177.5 (6) |
C7—P1—O1—Ag2i | 169.74 (19) | C29—C30—C31—C26 | −0.3 (13) |
C1—P1—O1—Ag2i | 59.3 (2) | C32A—P2—C32—C33 | 103 (10) |
P2—Ag1—O1—P1 | 46.6 (3) | C13—P2—C32—C33 | −161.2 (5) |
O2i—Ag1—O1—P1 | −110.4 (2) | C19—P2—C32—C33 | 90.7 (5) |
O3—Ag1—O1—P1 | 162.0 (3) | Ag1—P2—C32—C33 | −38.2 (6) |
Ag2—Ag1—O1—P1 | −24.58 (17) | C32A—P2—C32—C37 | −71 (10) |
P2—Ag1—O1—Ag2i | 173.13 (7) | C13—P2—C32—C37 | 24.8 (6) |
O2i—Ag1—O1—Ag2i | 16.11 (11) | C19—P2—C32—C37 | −83.3 (6) |
O3—Ag1—O1—Ag2i | −71.5 (3) | Ag1—P2—C32—C37 | 147.9 (5) |
Ag2—Ag1—O1—Ag2i | 101.93 (9) | C37—C32—C33—C34 | 0.0 |
O1—P1—O2—Ag2 | −50.8 (3) | P2—C32—C33—C34 | −174.0 (7) |
C7—P1—O2—Ag2 | 75.9 (2) | C32—C33—C34—C35 | 0.0 |
C1—P1—O2—Ag2 | −173.76 (18) | C33—C34—C35—C36 | 0.0 |
O1—P1—O2—Ag1i | 60.5 (2) | C34—C35—C36—C37 | 0.0 |
C7—P1—O2—Ag1i | −172.76 (17) | C35—C36—C37—C32 | 0.0 |
C1—P1—O2—Ag1i | −62.5 (2) | C33—C32—C37—C36 | 0.0 |
P3—Ag2—O2—P1 | −49.5 (3) | P2—C32—C37—C36 | 174.0 (7) |
O1i—Ag2—O2—P1 | 103.7 (2) | C13—P2—C32A—C33A | −111.7 (6) |
Ag1—Ag2—O2—P1 | 23.58 (18) | C19—P2—C32A—C33A | 141.2 (6) |
P3—Ag2—O2—Ag1i | −169.22 (8) | C32—P2—C32A—C33A | −27 (10) |
O1i—Ag2—O2—Ag1i | −16.06 (11) | Ag1—P2—C32A—C33A | 13.1 (7) |
Ag1—Ag2—O2—Ag1i | −96.17 (10) | C13—P2—C32A—C37A | 72.7 (8) |
O1—P1—C1—C2 | −155.7 (4) | C19—P2—C32A—C37A | −34.4 (9) |
O2—P1—C1—C2 | −27.2 (4) | C32—P2—C32A—C37A | 157 (11) |
C7—P1—C1—C2 | 88.0 (4) | Ag1—P2—C32A—C37A | −162.5 (7) |
O1—P1—C1—C6 | 30.2 (4) | C37A—C32A—C33A—C34A | 0.0 |
O2—P1—C1—C6 | 158.7 (3) | P2—C32A—C33A—C34A | −175.9 (9) |
C7—P1—C1—C6 | −86.1 (4) | C32A—C33A—C34A—C35A | 0.0 |
C6—C1—C2—C3 | 1.8 (7) | C33A—C34A—C35A—C36A | 0.0 |
P1—C1—C2—C3 | −172.3 (4) | C34A—C35A—C36A—C37A | 0.0 |
C1—C2—C3—C4 | 0.0 (9) | C35A—C36A—C37A—C32A | 0.0 |
C2—C3—C4—C5 | −2.0 (11) | C33A—C32A—C37A—C36A | 0.0 |
C3—C4—C5—C6 | 2.4 (11) | P2—C32A—C37A—C36A | 175.4 (10) |
C4—C5—C6—C1 | −0.7 (10) | O4—S3—O3—Ag1 | 155.6 (8) |
C2—C1—C6—C5 | −1.5 (7) | O5—S3—O3—Ag1 | 20.7 (12) |
P1—C1—C6—C5 | 172.7 (4) | C38—S3—O3—Ag1 | −90.1 (10) |
O1—P1—C7—C12 | 156.6 (4) | O1—Ag1—O3—S3 | 28.5 (10) |
O2—P1—C7—C12 | 26.0 (5) | P2—Ag1—O3—S3 | 178.2 (10) |
C1—P1—C7—C12 | −89.0 (5) | O2i—Ag1—O3—S3 | −53.9 (10) |
O1—P1—C7—C8 | −31.7 (5) | Ag2—Ag1—O3—S3 | −9 (2) |
O2—P1—C7—C8 | −162.2 (5) | O3—S3—C38—F1 | −130.0 (11) |
C1—P1—C7—C8 | 82.7 (5) | O4—S3—C38—F1 | −8.5 (13) |
C12—C7—C8—C9 | −0.1 (11) | O5—S3—C38—F1 | 121.2 (10) |
P1—C7—C8—C9 | −172.0 (7) | O3—S3—C38—F2 | −13.5 (10) |
C7—C8—C9—C10 | −3.4 (14) | O4—S3—C38—F2 | 107.9 (10) |
C8—C9—C10—C11 | 4.4 (16) | O5—S3—C38—F2 | −122.3 (9) |
C9—C10—C11—C12 | −1.8 (14) | O3—S3—C38—F3 | 105.2 (10) |
C8—C7—C12—C11 | 2.6 (9) | O4—S3—C38—F3 | −133.3 (10) |
P1—C7—C12—C11 | 174.4 (5) | O5—S3—C38—F3 | −3.6 (11) |
C10—C11—C12—C7 | −1.7 (11) | O3B—S3B—C38B—F2B | 107.0 (12) |
C32A—P2—C13—C18 | −75.7 (6) | O4B—S3B—C38B—F2B | −107.8 (12) |
C19—P2—C13—C18 | 32.6 (5) | O5B—S3B—C38B—F2B | −5.3 (11) |
C32—P2—C13—C18 | −79.1 (5) | O3B—S3B—C38B—F3B | −25.1 (16) |
Ag1—P2—C13—C18 | 158.1 (4) | O4B—S3B—C38B—F3B | 120.1 (15) |
C32A—P2—C13—C14 | 103.2 (5) | O5B—S3B—C38B—F3B | −137.5 (13) |
C19—P2—C13—C14 | −148.5 (4) | O3B—S3B—C38B—F1B | −120.1 (13) |
C32—P2—C13—C14 | 99.8 (5) | O4B—S3B—C38B—F1B | 25.1 (14) |
Ag1—P2—C13—C14 | −23.1 (5) | O5B—S3B—C38B—F1B | 127.6 (11) |
C18—C13—C14—C15 | 0.3 (9) |
Symmetry code: (i) −x+1, −y+1, −z+1. |
Experimental details
Crystal data | |
Chemical formula | [Ag4(C12H10O2P)2(CF3O3S)2(C25H22P2)2]·2C2H3N |
Mr | 2014.80 |
Crystal system, space group | Monoclinic, P21/n |
Temperature (K) | 296 |
a, b, c (Å) | 11.730 (7), 15.169 (9), 23.688 (12) |
β (°) | 96.967 (7) |
V (Å3) | 4184 (4) |
Z | 2 |
Radiation type | Mo Kα |
µ (mm−1) | 1.16 |
Crystal size (mm) | 0.23 × 0.19 × 0.16 |
Data collection | |
Diffractometer | Rigaku Mercury CCD diffractometer |
Absorption correction | Multi-scan (CrystalClear; Rigaku, 2005) |
Tmin, Tmax | 0.777, 0.837 |
No. of measured, independent and observed [I > 2σ(I)] reflections | 41763, 9645, 7705 |
Rint | 0.055 |
(sin θ/λ)max (Å−1) | 0.651 |
Refinement | |
R[F2 > 2σ(F2)], wR(F2), S | 0.055, 0.144, 1.01 |
No. of reflections | 9645 |
No. of parameters | 610 |
No. of restraints | 1173 |
H-atom treatment | H-atom parameters constrained |
Δρmax, Δρmin (e Å−3) | 0.64, −0.61 |
Computer programs: CrystalClear (Rigaku, 2005), SHELXS97 (Sheldrick, 2008), SHELXL97 (Sheldrick, 2008), SHELXTL (Sheldrick, 2008).
Ag1—O1 | 2.270 (3) | Ag2—O1i | 2.451 (3) |
Ag1—O2i | 2.435 (3) | Ag2—O2 | 2.280 (3) |
Ag1—O3 | 2.557 (8) | Ag2—O5i | 2.619 (8) |
Ag1—O3B | 2.672 (11) | Ag2—O3Bi | 2.795 (10) |
Ag1—P2 | 2.3554 (15) | Ag2—P3 | 2.3676 (16) |
Symmetry code: (i) −x+1, −y+1, −z+1. |
References
Fournier, É., Lebrun, F., Drouin, M., Decken, A. & Harvey, P. D. (2004). Inorg. Chem. 43, 3127–3135. Web of Science CSD CrossRef PubMed CAS Google Scholar
Matsumoto, K., Tanaka, R., Shimomura, R., Matsumoto, C. & Nakao, Y. (2001). Inorg. Chim. Acta, 322, 125–129. Web of Science CSD CrossRef CAS Google Scholar
Rigaku (2005). CrystalClear. Rigaku Corporation, Tokyo, Japan. Google Scholar
Sheldrick, G. M. (2008). Acta Cryst. A64, 112–122. Web of Science CrossRef CAS IUCr Journals Google Scholar
Sun, D., Luo, G.-G., Zhang, N., Huang, R.-B. & Zheng, L.-S. (2011). Chem. Commun. 47, 1461–1463. Web of Science CSD CrossRef CAS Google Scholar
Wei, Q.-H., Yin, G.-Q., Zhang, L.-Y., Shi, L.-X., Mao, Z.-W. & Chen, Z.-N. (2004). Inorg. Chem. 43, 3484–3491. Web of Science CSD CrossRef PubMed CAS 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.
Silver clusters have been intensively reported in many fields of chemistry (Fournier et al., 2004; Wei et al., 2004). Phosphine ligands, especially the type Ph2P(CH2)nPPh2 ligands, which are known to function as 'stabilizing units' on silver(I) centers, have been used in metal-rich silver chalcogenide clusters (Sun et al., 2011). Information on the structures of tetranuclear silver(I) compounds by the reactions between silver(I) salt and bis(diphenylphosphine)methane (dppm) ligand continues to be reported (Matsumoto et al., 2001).
In the title tetranuclear compound, the dppm ligand links two AgI atoms through the P atoms (Fig. 1). The AgI atom adopts a highly distorted tetrahedral geometry. The Ag—P bond distances are 2.3554 (15) and 2.3676 (16) Å and the Ag—O distances are in the range of 2.270 (3)–2.795 (10) Å (Table 1). An intramolecular Ag···Ag distance is 3.2692 (14) Å. The trifluoromethanesulfonate (OTf) anion and one of the phenyl groups in the dppm ligand are disordered over two sets of positions in an occupancy ratio of 0.546 (4):0.454 (4). The 0.546-occupied OTf is bonded to two Ag atoms in a µ-(κ2O:O') mode, while the 0.454-occupied OTf in a µ-(κ2O:O) mode (Fig. 1).