metal-organic compounds
Di-μ-bromido-tris(triphenylphosphine)-1κP,2κ2P-disilver(I) tetrahydrofuran 0.85-solvate
aJilin Institute of Chemical Technology, Jilin 132000, People's Republic of China, and bFaculty of Chemistry, Northeast Normal University, Changchun 130024, People's Republic of China
*Correspondence e-mail: zhangh@nenu.edu.cn
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). For general background on triphenylphosphine–silver(I) complexes, see: Whitcomb & Rajeswaram (2006); Whitcomb & Roger (1996); Mann et al. (1937); Teo & Calabrese (1976); Bowmaker et al. (1993); Olmstead et al. (2004); Zhang et al. (2003); Lobana et al. (2008); Cingolani et al. (2003). For the sensitization of photothermographic materials by coordination polymers formed by the reaction of triphenylphosphine with silver(I) salts, see: Freedman (1994).
Experimental
Crystal data
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Data collection: CrystalClear (Rigaku, 2002); 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/S1600536809010241/su2091sup1.cif
contains datablocks I, global. DOI:Structure factors: contains datablock I. DOI: 10.1107/S1600536809010241/su2091Isup2.hkl
In a
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.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 occupancy fixed at 0.85.
Data collection: CrystalClear (Rigaku, 2002); cell
CrystalClear (Rigaku, 2002); data reduction: CrystalClear (Rigaku, 2002); 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).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). |
[Ag2Br2(C18H15P)3]·0.85C4H8O | F(000) = 2448 |
Mr = 1223.66 | Dx = 1.514 Mg m−3 |
Monoclinic, P21/c | Mo Kα radiation, λ = 0.71073 Å |
Hall symbol: -P 2ybc | Cell parameters from 6309 reflections |
a = 16.2386 (19) Å | θ = 3.1–27.5° |
b = 19.4575 (17) Å | µ = 2.35 mm−1 |
c = 18.3069 (18) Å | T = 293 K |
β = 111.896 (1)° | Prism, colorless |
V = 5367.0 (9) Å3 | 0.40 × 0.12 × 0.08 mm |
Z = 4 |
Rigaku Mercury CCD diffractometer | 9804 independent reflections |
Radiation source: rotating-anode generator | 4750 reflections with I > 2σ(I) |
Graphite monochromator | Rint = 0.095 |
ω scans | θmax = 25.4°, θmin = 3.1° |
Absorption correction: multi-scan (SPHERE in CrystalClear; Rigaku, 2002) | h = −18→19 |
Tmin = 0.721, Tmax = 0.829 | k = −23→22 |
36137 measured reflections | l = −22→21 |
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)] = 0.076 | Hydrogen site location: inferred from neighbouring sites |
wR(F2) = 0.115 | H-atom parameters constrained |
S = 1.00 | w = 1/[σ2(Fo2) + (0.016P)2] where P = (Fo2 + 2Fc2)/3 |
9804 reflections | (Δ/σ)max = 0.018 |
596 parameters | Δρmax = 0.37 e Å−3 |
0 restraints | Δρmin = −0.41 e Å−3 |
[Ag2Br2(C18H15P)3]·0.85C4H8O | V = 5367.0 (9) Å3 |
Mr = 1223.66 | Z = 4 |
Monoclinic, P21/c | Mo Kα radiation |
a = 16.2386 (19) Å | µ = 2.35 mm−1 |
b = 19.4575 (17) Å | T = 293 K |
c = 18.3069 (18) Å | 0.40 × 0.12 × 0.08 mm |
β = 111.896 (1)° |
Rigaku Mercury CCD diffractometer | 9804 independent reflections |
Absorption correction: multi-scan (SPHERE in CrystalClear; Rigaku, 2002) | 4750 reflections with I > 2σ(I) |
Tmin = 0.721, Tmax = 0.829 | Rint = 0.095 |
36137 measured reflections |
R[F2 > 2σ(F2)] = 0.076 | 0 restraints |
wR(F2) = 0.115 | H-atom parameters constrained |
S = 1.00 | Δρmax = 0.37 e Å−3 |
9804 reflections | Δρmin = −0.41 e Å−3 |
596 parameters |
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. |
x | y | z | Uiso*/Ueq | Occ. (<1) | |
Ag1 | 0.172104 (16) | 0.430186 (13) | 0.311968 (13) | 0.05624 (9) | |
Ag2 | 0.309939 (18) | 0.449839 (16) | 0.211990 (14) | 0.08013 (12) | |
Br1 | 0.23309 (2) | 0.549632 (18) | 0.258758 (19) | 0.06869 (13) | |
Br2 | 0.26760 (2) | 0.335663 (19) | 0.264353 (19) | 0.07471 (14) | |
P1 | 0.01808 (6) | 0.41825 (4) | 0.21950 (4) | 0.0519 (3) | |
P2 | 0.22977 (5) | 0.44191 (4) | 0.45510 (4) | 0.0485 (3) | |
P3 | 0.38713 (6) | 0.46569 (5) | 0.12429 (5) | 0.0626 (3) | |
C101 | 0.00382 (19) | 0.40749 (14) | 0.11612 (15) | 0.0508 (11) | |
C102 | −0.0673 (2) | 0.37370 (17) | 0.06109 (16) | 0.0826 (15) | |
H10A | −0.1113 | 0.3545 | 0.0758 | 0.099* | |
C103 | −0.0727 (2) | 0.36858 (18) | −0.01647 (17) | 0.0834 (15) | |
H10B | −0.1214 | 0.3472 | −0.0540 | 0.100* | |
C104 | −0.0071 (2) | 0.39468 (16) | −0.03775 (16) | 0.0739 (14) | |
H10G | −0.0113 | 0.3909 | −0.0896 | 0.089* | |
C105 | 0.0644 (2) | 0.42627 (16) | 0.01636 (16) | 0.0736 (13) | |
H10F | 0.1095 | 0.4434 | 0.0018 | 0.088* | |
C106 | 0.06945 (18) | 0.43261 (15) | 0.09268 (14) | 0.0571 (12) | |
H10C | 0.1184 | 0.4544 | 0.1294 | 0.068* | |
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 | −0.1318 | 0.4967 | 0.1094 | 0.085* | |
C109 | −0.1594 (2) | 0.57895 (17) | 0.16262 (17) | 0.0831 (15) | |
H10E | −0.2060 | 0.5953 | 0.1188 | 0.100* | |
C110 | −0.1347 (2) | 0.61364 (16) | 0.23307 (17) | 0.0751 (13) | |
H11A | −0.1646 | 0.6535 | 0.2367 | 0.090* | |
C111 | −0.0673 (2) | 0.58987 (16) | 0.29710 (18) | 0.0751 (14) | |
H11B | −0.0515 | 0.6129 | 0.3449 | 0.090* | |
C112 | −0.0221 (2) | 0.53159 (15) | 0.29149 (15) | 0.0649 (13) | |
H11C | 0.0252 | 0.5163 | 0.3355 | 0.078* | |
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) | |
H11D | 0.0355 | 0.2731 | 0.2318 | 0.105* | |
C115 | −0.0632 (2) | 0.22693 (17) | 0.25242 (19) | 0.1044 (17) | |
H11E | −0.0414 | 0.1825 | 0.2538 | 0.125* | |
C116 | −0.1392 (2) | 0.23703 (16) | 0.26362 (18) | 0.0853 (15) | |
H11F | −0.1704 | 0.2000 | 0.2725 | 0.102* | |
C117 | −0.1703 (2) | 0.30293 (16) | 0.26176 (17) | 0.0840 (14) | |
H11G | −0.2227 | 0.3108 | 0.2699 | 0.101* | |
C118 | −0.1237 (2) | 0.35738 (15) | 0.24780 (16) | 0.0652 (12) | |
H11H | −0.1455 | 0.4018 | 0.2465 | 0.078* | |
C201 | 0.34954 (19) | 0.44201 (15) | 0.50661 (15) | 0.0538 (11) | |
C202 | 0.39821 (18) | 0.40313 (15) | 0.47389 (17) | 0.0627 (13) | |
H20E | 0.3698 | 0.3802 | 0.4265 | 0.075* | |
C203 | 0.4888 (2) | 0.39844 (17) | 0.51154 (18) | 0.0853 (16) | |
H20F | 0.5208 | 0.3711 | 0.4898 | 0.102* | |
C204 | 0.5329 (2) | 0.43282 (19) | 0.57997 (18) | 0.0964 (17) | |
H20G | 0.5942 | 0.4295 | 0.6048 | 0.116* | |
C205 | 0.4844 (2) | 0.47214 (19) | 0.61093 (19) | 0.0981 (17) | |
H20D | 0.5135 | 0.4960 | 0.6575 | 0.118* | |
C206 | 0.3944 (2) | 0.47745 (18) | 0.57535 (16) | 0.0790 (15) | |
H20A | 0.3631 | 0.5051 | 0.5975 | 0.095* | |
C207 | 0.1921 (2) | 0.52024 (15) | 0.48663 (15) | 0.0567 (12) | |
C208 | 0.2164 (2) | 0.58233 (16) | 0.46320 (19) | 0.0945 (15) | |
H20B | 0.2534 | 0.5819 | 0.4347 | 0.113* | |
C209 | 0.1880 (3) | 0.6440 (2) | 0.4805 (2) | 0.1249 (19) | |
H20C | 0.2043 | 0.6847 | 0.4629 | 0.150* | |
C210 | 0.1354 (3) | 0.64572 (18) | 0.5238 (2) | 0.1132 (19) | |
H21A | 0.1167 | 0.6875 | 0.5371 | 0.136* | |
C211 | 0.1107 (2) | 0.58514 (17) | 0.54747 (19) | 0.0973 (15) | |
H21B | 0.0736 | 0.5859 | 0.5758 | 0.117* | |
C212 | 0.1398 (2) | 0.52266 (17) | 0.53001 (16) | 0.0704 (13) | |
H21C | 0.1235 | 0.4821 | 0.5480 | 0.084* | |
C213 | 0.19096 (18) | 0.37368 (14) | 0.50264 (15) | 0.0509 (11) | |
C214 | 0.11738 (19) | 0.33772 (15) | 0.45777 (17) | 0.0655 (13) | |
H21D | 0.0894 | 0.3487 | 0.4048 | 0.079* | |
C215 | 0.0833 (2) | 0.28525 (16) | 0.48909 (18) | 0.0841 (15) | |
H21E | 0.0315 | 0.2626 | 0.4584 | 0.101* | |
C216 | 0.1273 (2) | 0.26735 (16) | 0.56627 (18) | 0.0838 (14) | |
H21F | 0.1068 | 0.2314 | 0.5884 | 0.101* | |
C217 | 0.2027 (2) | 0.30337 (16) | 0.61092 (17) | 0.0752 (14) | |
H21G | 0.2324 | 0.2912 | 0.6634 | 0.090* | |
C218 | 0.23466 (19) | 0.35619 (15) | 0.58029 (15) | 0.0607 (12) | |
H21H | 0.2852 | 0.3800 | 0.6114 | 0.073* | |
C301 | 0.3497 (2) | 0.53937 (15) | 0.05832 (16) | 0.0585 (12) | |
C302 | 0.3280 (2) | 0.59806 (16) | 0.08938 (19) | 0.0826 (15) | |
H30A | 0.3289 | 0.5980 | 0.1405 | 0.099* | |
C303 | 0.3048 (2) | 0.65782 (18) | 0.0436 (2) | 0.0967 (17) | |
H30B | 0.2923 | 0.6980 | 0.0650 | 0.116* | |
C304 | 0.3003 (2) | 0.65737 (18) | −0.03249 (18) | 0.0871 (16) | |
H30C | 0.2843 | 0.6970 | −0.0630 | 0.105* | |
C305 | 0.3194 (2) | 0.59866 (17) | −0.06341 (18) | 0.0798 (15) | |
H30D | 0.3155 | 0.5980 | −0.1154 | 0.096* | |
C306 | 0.3448 (2) | 0.53976 (16) | −0.01771 (16) | 0.0646 (13) | |
H30E | 0.3585 | 0.5001 | −0.0392 | 0.077* | |
C307 | 0.38065 (19) | 0.39381 (15) | 0.05913 (16) | 0.0542 (12) | |
C308 | 0.3072 (2) | 0.35043 (15) | 0.03950 (16) | 0.0695 (13) | |
H30F | 0.2649 | 0.3570 | 0.0619 | 0.083* | |
C309 | 0.2978 (2) | 0.29778 (17) | −0.01327 (18) | 0.0878 (16) | |
H30G | 0.2479 | 0.2698 | −0.0273 | 0.105* | |
C310 | 0.3590 (2) | 0.28579 (15) | −0.04500 (18) | 0.0881 (16) | |
H31A | 0.3517 | 0.2501 | −0.0807 | 0.106* | |
C311 | 0.4333 (2) | 0.32783 (16) | −0.02323 (17) | 0.0813 (14) | |
H31B | 0.4768 | 0.3195 | −0.0439 | 0.098* | |
C312 | 0.4440 (2) | 0.38156 (16) | 0.02830 (17) | 0.0825 (14) | |
H31C | 0.4940 | 0.4094 | 0.0421 | 0.099* | |
C313 | 0.50559 (19) | 0.48006 (15) | 0.17267 (15) | 0.0552 (11) | |
C314 | 0.5493 (2) | 0.53755 (16) | 0.16275 (16) | 0.0694 (14) | |
H31D | 0.5175 | 0.5716 | 0.1280 | 0.083* | |
C315 | 0.6389 (2) | 0.54602 (18) | 0.20288 (17) | 0.0817 (15) | |
H31E | 0.6663 | 0.5856 | 0.1946 | 0.098* | |
C316 | 0.6876 (2) | 0.49874 (16) | 0.25364 (17) | 0.0793 (15) | |
H31F | 0.7481 | 0.5056 | 0.2810 | 0.095* | |
C317 | 0.6473 (2) | 0.44027 (17) | 0.26461 (17) | 0.0835 (15) | |
H31G | 0.6809 | 0.4060 | 0.2978 | 0.100* | |
C318 | 0.5564 (2) | 0.43179 (17) | 0.22653 (17) | 0.0737 (14) | |
H31H | 0.5291 | 0.3932 | 0.2372 | 0.088* | |
O11 | 0.6007 (2) | 0.26438 (16) | 0.28899 (18) | 0.1287 (16) | 0.85 |
C11 | 0.5807 (3) | 0.2330 (2) | 0.2174 (3) | 0.132 (2) | 0.85 |
H11I | 0.6179 | 0.1928 | 0.2228 | 0.158* | 0.85 |
H11J | 0.5908 | 0.2643 | 0.1804 | 0.158* | 0.85 |
C12 | 0.4917 (3) | 0.2138 (3) | 0.1907 (3) | 0.157 (3) | 0.85 |
H12A | 0.4571 | 0.2413 | 0.1454 | 0.188* | 0.85 |
H12B | 0.4851 | 0.1658 | 0.1754 | 0.188* | 0.85 |
C13 | 0.4646 (3) | 0.2242 (3) | 0.2490 (3) | 0.155 (3) | 0.85 |
H13A | 0.4518 | 0.1805 | 0.2681 | 0.186* | 0.85 |
H13B | 0.4106 | 0.2513 | 0.2309 | 0.186* | 0.85 |
C14 | 0.5310 (3) | 0.2589 (2) | 0.3100 (2) | 0.126 (2) | 0.85 |
H14C | 0.5104 | 0.3040 | 0.3177 | 0.151* | 0.85 |
H14A | 0.5468 | 0.2333 | 0.3588 | 0.151* | 0.85 |
U11 | U22 | U33 | U12 | U13 | U23 | |
Ag1 | 0.04831 (14) | 0.07159 (17) | 0.04870 (12) | 0.00071 (14) | 0.01794 (10) | −0.00254 (13) |
Ag2 | 0.05967 (17) | 0.1225 (3) | 0.06481 (15) | −0.00171 (18) | 0.03082 (12) | −0.00557 (16) |
Br1 | 0.0779 (2) | 0.0623 (2) | 0.07304 (19) | −0.0086 (2) | 0.03638 (16) | −0.00307 (18) |
Br2 | 0.0881 (3) | 0.0738 (2) | 0.0647 (2) | 0.0226 (2) | 0.03131 (17) | −0.00624 (19) |
P1 | 0.0470 (5) | 0.0608 (6) | 0.0481 (4) | −0.0007 (5) | 0.0180 (4) | −0.0051 (4) |
P2 | 0.0496 (5) | 0.0526 (5) | 0.0450 (4) | −0.0035 (4) | 0.0196 (3) | −0.0037 (4) |
P3 | 0.0593 (5) | 0.0730 (6) | 0.0632 (5) | −0.0054 (5) | 0.0318 (4) | −0.0106 (5) |
C101 | 0.0480 (19) | 0.057 (2) | 0.0455 (16) | 0.0037 (16) | 0.0154 (14) | −0.0045 (15) |
C102 | 0.084 (3) | 0.109 (3) | 0.0589 (19) | −0.021 (2) | 0.0313 (17) | −0.0320 (19) |
C103 | 0.074 (3) | 0.112 (3) | 0.058 (2) | −0.015 (2) | 0.0182 (18) | −0.026 (2) |
C104 | 0.085 (2) | 0.095 (3) | 0.0521 (17) | 0.014 (2) | 0.0371 (15) | −0.0034 (18) |
C105 | 0.070 (2) | 0.096 (3) | 0.0567 (18) | 0.025 (2) | 0.0261 (15) | 0.0230 (19) |
C106 | 0.0438 (18) | 0.079 (2) | 0.0479 (16) | 0.0015 (18) | 0.0166 (14) | 0.0018 (17) |
C107 | 0.0373 (16) | 0.060 (2) | 0.0452 (15) | −0.0012 (15) | 0.0218 (12) | 0.0043 (15) |
C108 | 0.072 (2) | 0.083 (3) | 0.0632 (19) | −0.004 (2) | 0.0303 (16) | 0.0070 (19) |
C109 | 0.081 (2) | 0.096 (3) | 0.078 (2) | 0.031 (2) | 0.0355 (17) | 0.022 (2) |
C110 | 0.070 (2) | 0.062 (2) | 0.110 (2) | 0.0080 (19) | 0.0527 (16) | −0.0022 (19) |
C111 | 0.065 (2) | 0.068 (2) | 0.088 (2) | −0.0039 (19) | 0.0236 (18) | −0.0306 (19) |
C112 | 0.060 (2) | 0.075 (2) | 0.0500 (18) | 0.003 (2) | 0.0098 (16) | −0.0131 (18) |
C113 | 0.0396 (18) | 0.061 (2) | 0.0521 (17) | −0.0003 (16) | 0.0147 (13) | −0.0077 (16) |
C114 | 0.082 (2) | 0.066 (2) | 0.139 (2) | 0.017 (2) | 0.0688 (17) | 0.005 (2) |
C115 | 0.128 (3) | 0.047 (2) | 0.167 (3) | 0.006 (2) | 0.089 (2) | 0.008 (2) |
C116 | 0.099 (3) | 0.061 (2) | 0.104 (2) | −0.023 (2) | 0.0473 (19) | −0.010 (2) |
C117 | 0.083 (2) | 0.079 (3) | 0.111 (2) | −0.005 (2) | 0.0613 (16) | 0.010 (2) |
C118 | 0.075 (2) | 0.047 (2) | 0.084 (2) | 0.0006 (18) | 0.0425 (15) | 0.0128 (17) |
C201 | 0.0556 (18) | 0.054 (2) | 0.0568 (16) | −0.0097 (16) | 0.0271 (13) | 0.0001 (16) |
C202 | 0.0341 (19) | 0.075 (2) | 0.073 (2) | −0.0039 (17) | 0.0140 (15) | −0.0096 (18) |
C203 | 0.059 (2) | 0.108 (3) | 0.086 (2) | 0.006 (2) | 0.0237 (19) | 0.007 (2) |
C204 | 0.054 (3) | 0.150 (4) | 0.067 (2) | 0.006 (3) | 0.0009 (19) | 0.023 (2) |
C205 | 0.070 (3) | 0.140 (3) | 0.075 (2) | −0.037 (3) | 0.018 (2) | −0.026 (2) |
C206 | 0.061 (2) | 0.121 (3) | 0.0543 (19) | −0.024 (2) | 0.0203 (16) | −0.026 (2) |
C207 | 0.064 (2) | 0.055 (2) | 0.0489 (17) | −0.0067 (17) | 0.0195 (15) | −0.0026 (16) |
C208 | 0.120 (3) | 0.062 (2) | 0.131 (2) | −0.012 (2) | 0.0817 (18) | −0.022 (2) |
C209 | 0.175 (4) | 0.076 (3) | 0.154 (3) | −0.017 (3) | 0.098 (2) | −0.021 (2) |
C210 | 0.134 (3) | 0.067 (3) | 0.146 (3) | 0.012 (2) | 0.060 (2) | −0.033 (2) |
C211 | 0.102 (3) | 0.088 (3) | 0.121 (2) | 0.022 (2) | 0.0646 (18) | −0.022 (2) |
C212 | 0.079 (2) | 0.069 (2) | 0.0730 (19) | 0.011 (2) | 0.0386 (16) | 0.0043 (18) |
C213 | 0.0508 (18) | 0.051 (2) | 0.0545 (17) | 0.0040 (16) | 0.0242 (13) | 0.0006 (15) |
C214 | 0.055 (2) | 0.070 (2) | 0.0660 (19) | −0.0041 (19) | 0.0163 (16) | 0.0121 (18) |
C215 | 0.071 (2) | 0.056 (2) | 0.130 (3) | −0.010 (2) | 0.0440 (19) | 0.009 (2) |
C216 | 0.095 (2) | 0.067 (2) | 0.120 (2) | 0.0102 (19) | 0.0753 (16) | 0.0272 (19) |
C217 | 0.083 (2) | 0.070 (2) | 0.074 (2) | 0.018 (2) | 0.0315 (17) | 0.0097 (19) |
C218 | 0.054 (2) | 0.062 (2) | 0.0650 (19) | −0.0105 (18) | 0.0212 (15) | 0.0061 (17) |
C301 | 0.0513 (19) | 0.065 (2) | 0.0597 (17) | −0.0014 (17) | 0.0214 (14) | −0.0147 (17) |
C302 | 0.074 (3) | 0.091 (3) | 0.080 (2) | 0.009 (2) | 0.0258 (18) | −0.005 (2) |
C303 | 0.085 (3) | 0.079 (3) | 0.118 (3) | 0.011 (2) | 0.027 (2) | −0.033 (2) |
C304 | 0.087 (3) | 0.080 (3) | 0.089 (2) | 0.010 (2) | 0.026 (2) | 0.003 (2) |
C305 | 0.066 (2) | 0.094 (3) | 0.079 (2) | −0.001 (2) | 0.0267 (18) | 0.005 (2) |
C306 | 0.064 (2) | 0.068 (2) | 0.0592 (18) | −0.0032 (19) | 0.0195 (16) | −0.0171 (17) |
C307 | 0.0476 (19) | 0.053 (2) | 0.0595 (18) | −0.0010 (17) | 0.0171 (15) | −0.0005 (16) |
C308 | 0.079 (2) | 0.065 (2) | 0.0651 (19) | −0.012 (2) | 0.0278 (17) | −0.0027 (18) |
C309 | 0.097 (3) | 0.074 (3) | 0.080 (2) | −0.023 (2) | 0.018 (2) | −0.003 (2) |
C310 | 0.152 (3) | 0.037 (2) | 0.079 (2) | −0.016 (2) | 0.047 (2) | −0.0093 (18) |
C311 | 0.123 (3) | 0.064 (2) | 0.0759 (19) | 0.002 (2) | 0.0590 (17) | −0.0107 (18) |
C312 | 0.095 (2) | 0.077 (2) | 0.095 (2) | −0.021 (2) | 0.0578 (17) | −0.0362 (19) |
C313 | 0.0551 (19) | 0.064 (2) | 0.0494 (16) | 0.0007 (17) | 0.0229 (14) | −0.0165 (16) |
C314 | 0.061 (2) | 0.069 (2) | 0.074 (2) | −0.0044 (19) | 0.0199 (17) | 0.0019 (19) |
C315 | 0.058 (2) | 0.103 (3) | 0.083 (2) | −0.013 (2) | 0.0250 (18) | −0.007 (2) |
C316 | 0.055 (2) | 0.097 (3) | 0.078 (2) | 0.002 (2) | 0.0154 (18) | −0.031 (2) |
C317 | 0.081 (3) | 0.084 (3) | 0.071 (2) | 0.028 (2) | 0.0124 (19) | −0.003 (2) |
C318 | 0.073 (2) | 0.072 (2) | 0.078 (2) | −0.001 (2) | 0.0311 (17) | −0.011 (2) |
O11 | 0.118 (3) | 0.128 (3) | 0.129 (2) | −0.019 (2) | 0.033 (2) | 0.021 (2) |
C11 | 0.116 (3) | 0.134 (5) | 0.177 (4) | 0.002 (3) | 0.093 (3) | 0.020 (3) |
C12 | 0.130 (5) | 0.173 (5) | 0.150 (4) | 0.014 (4) | 0.031 (4) | −0.054 (4) |
C13 | 0.072 (4) | 0.142 (5) | 0.247 (6) | 0.009 (4) | 0.056 (4) | 0.011 (5) |
C14 | 0.167 (5) | 0.124 (4) | 0.090 (3) | 0.049 (4) | 0.051 (3) | 0.051 (3) |
Ag1—P2 | 2.4423 (8) | C209—C210 | 1.365 (6) |
Ag1—P1 | 2.4530 (8) | C209—H20C | 0.9300 |
Ag1—Br2 | 2.7487 (5) | C210—C211 | 1.367 (5) |
Ag1—Br1 | 2.8374 (5) | C210—H21A | 0.9300 |
Ag2—P3 | 2.3968 (11) | C211—C212 | 1.384 (5) |
Ag2—Br2 | 2.6112 (5) | C211—H21B | 0.9300 |
Ag2—Br1 | 2.6186 (5) | C212—H21C | 0.9300 |
P1—C113 | 1.826 (3) | C213—C214 | 1.364 (4) |
P1—C101 | 1.831 (3) | C213—C218 | 1.374 (3) |
P1—C107 | 1.833 (3) | C214—C215 | 1.383 (5) |
P2—C207 | 1.815 (3) | C214—H21D | 0.9300 |
P2—C201 | 1.818 (3) | C215—C216 | 1.369 (4) |
P2—C213 | 1.824 (3) | C215—H21E | 0.9300 |
P3—C313 | 1.814 (3) | C216—C217 | 1.382 (4) |
P3—C307 | 1.816 (3) | C216—H21F | 0.9300 |
P3—C301 | 1.826 (3) | C217—C218 | 1.363 (4) |
C101—C106 | 1.378 (4) | C217—H21G | 0.9300 |
C101—C102 | 1.383 (4) | C218—H21H | 0.9300 |
C102—C103 | 1.393 (4) | C301—C306 | 1.364 (4) |
C102—H10A | 0.9300 | C301—C302 | 1.378 (4) |
C103—C104 | 1.361 (5) | C302—C303 | 1.400 (5) |
C103—H10B | 0.9300 | C302—H30A | 0.9300 |
C104—C105 | 1.360 (4) | C303—C304 | 1.368 (5) |
C104—H10G | 0.9300 | C303—H30B | 0.9300 |
C105—C106 | 1.374 (4) | C304—C305 | 1.361 (5) |
C105—H10F | 0.9300 | C304—H30C | 0.9300 |
C106—H10C | 0.9300 | C305—C306 | 1.388 (4) |
C107—C112 | 1.374 (4) | C305—H30D | 0.9300 |
C107—C108 | 1.387 (3) | C306—H30E | 0.9300 |
C108—C109 | 1.377 (5) | C307—C312 | 1.366 (5) |
C108—H10D | 0.9300 | C307—C308 | 1.394 (4) |
C109—C110 | 1.376 (4) | C308—C309 | 1.377 (4) |
C109—H10E | 0.9300 | C308—H30F | 0.9300 |
C110—C111 | 1.353 (4) | C309—C310 | 1.346 (6) |
C110—H11A | 0.9300 | C309—H30G | 0.9300 |
C111—C112 | 1.375 (4) | C310—C311 | 1.387 (5) |
C111—H11B | 0.9300 | C310—H31A | 0.9300 |
C112—H11C | 0.9300 | C311—C312 | 1.375 (4) |
C113—C118 | 1.354 (5) | C311—H31B | 0.9300 |
C113—C114 | 1.372 (4) | C312—H31C | 0.9300 |
C114—C115 | 1.368 (5) | C313—C314 | 1.373 (4) |
C114—H11D | 0.9300 | C313—C318 | 1.389 (4) |
C115—C116 | 1.338 (5) | C314—C315 | 1.373 (4) |
C115—H11E | 0.9300 | C314—H31D | 0.9300 |
C116—C117 | 1.374 (4) | C315—C316 | 1.337 (4) |
C116—H11F | 0.9300 | C315—H31E | 0.9300 |
C117—C118 | 1.380 (5) | C316—C317 | 1.365 (5) |
C117—H11G | 0.9300 | C316—H31F | 0.9300 |
C118—H11H | 0.9300 | C317—C318 | 1.387 (4) |
C201—C206 | 1.381 (4) | C317—H31G | 0.9300 |
C201—C202 | 1.382 (4) | C318—H31H | 0.9300 |
C202—C203 | 1.375 (4) | O11—C14 | 1.328 (6) |
C202—H20E | 0.9300 | O11—C11 | 1.371 (5) |
C203—C204 | 1.364 (4) | C11—C12 | 1.392 (7) |
C203—H20F | 0.9300 | C11—H11I | 0.9700 |
C204—C205 | 1.363 (5) | C11—H11J | 0.9700 |
C204—H20G | 0.9300 | C12—C13 | 1.314 (8) |
C205—C206 | 1.365 (5) | C12—H12A | 0.9700 |
C205—H20D | 0.9300 | C12—H12B | 0.9700 |
C206—H20A | 0.9300 | C13—C14 | 1.402 (6) |
C207—C212 | 1.364 (5) | C13—H13A | 0.9700 |
C207—C208 | 1.388 (4) | C13—H13B | 0.9700 |
C208—C209 | 1.366 (5) | C14—H14C | 0.9700 |
C208—H20B | 0.9300 | C14—H14A | 0.9700 |
P2—Ag1—P1 | 129.31 (3) | C210—C209—H20C | 120.2 |
P2—Ag1—Br2 | 111.52 (2) | C208—C209—H20C | 120.2 |
P1—Ag1—Br2 | 105.57 (2) | C209—C210—C211 | 119.0 (4) |
P2—Ag1—Br1 | 104.39 (2) | C209—C210—H21A | 120.5 |
P1—Ag1—Br1 | 103.72 (2) | C211—C210—H21A | 120.5 |
Br2—Ag1—Br1 | 97.398 (16) | C210—C211—C212 | 121.3 (4) |
P3—Ag2—Br2 | 129.08 (3) | C210—C211—H21B | 119.4 |
P3—Ag2—Br1 | 123.75 (3) | C212—C211—H21B | 119.4 |
Br2—Ag2—Br1 | 106.740 (18) | C207—C212—C211 | 120.3 (3) |
Ag2—Br1—Ag1 | 76.985 (14) | C207—C212—H21C | 119.8 |
Ag2—Br2—Ag1 | 78.701 (15) | C211—C212—H21C | 119.8 |
C113—P1—C101 | 103.10 (13) | C214—C213—C218 | 119.6 (3) |
C113—P1—C107 | 104.27 (14) | C214—C213—P2 | 117.8 (2) |
C101—P1—C107 | 105.40 (12) | C218—C213—P2 | 122.5 (2) |
C113—P1—Ag1 | 117.50 (8) | C213—C214—C215 | 121.7 (3) |
C101—P1—Ag1 | 115.31 (10) | C213—C214—H21D | 119.2 |
C107—P1—Ag1 | 110.02 (8) | C215—C214—H21D | 119.2 |
C207—P2—C201 | 104.85 (13) | C216—C215—C214 | 118.7 (3) |
C207—P2—C213 | 104.01 (15) | C216—C215—H21E | 120.7 |
C201—P2—C213 | 104.27 (13) | C214—C215—H21E | 120.7 |
C207—P2—Ag1 | 112.33 (9) | C215—C216—C217 | 119.2 (3) |
C201—P2—Ag1 | 117.70 (10) | C215—C216—H21F | 120.4 |
C213—P2—Ag1 | 112.43 (9) | C217—C216—H21F | 120.4 |
C313—P3—C307 | 103.33 (14) | C218—C217—C216 | 121.9 (3) |
C313—P3—C301 | 103.47 (14) | C218—C217—H21G | 119.1 |
C307—P3—C301 | 104.29 (13) | C216—C217—H21G | 119.1 |
C313—P3—Ag2 | 114.64 (10) | C217—C218—C213 | 118.9 (3) |
C307—P3—Ag2 | 115.10 (11) | C217—C218—H21H | 120.6 |
C301—P3—Ag2 | 114.55 (12) | C213—C218—H21H | 120.6 |
C106—C101—C102 | 118.3 (3) | C306—C301—C302 | 119.3 (3) |
C106—C101—P1 | 117.83 (19) | C306—C301—P3 | 123.9 (2) |
C102—C101—P1 | 123.8 (3) | C302—C301—P3 | 116.8 (2) |
C101—C102—C103 | 119.6 (3) | C301—C302—C303 | 119.7 (3) |
C101—C102—H10A | 120.2 | C301—C302—H30A | 120.2 |
C103—C102—H10A | 120.2 | C303—C302—H30A | 120.2 |
C104—C103—C102 | 120.5 (3) | C304—C303—C302 | 120.3 (3) |
C104—C103—H10B | 119.8 | C304—C303—H30B | 119.9 |
C102—C103—H10B | 119.8 | C302—C303—H30B | 119.9 |
C105—C104—C103 | 120.5 (3) | C305—C304—C303 | 119.7 (3) |
C105—C104—H10G | 119.8 | C305—C304—H30C | 120.2 |
C103—C104—H10G | 119.8 | C303—C304—H30C | 120.2 |
C104—C105—C106 | 119.5 (3) | C304—C305—C306 | 120.3 (3) |
C104—C105—H10F | 120.3 | C304—C305—H30D | 119.8 |
C106—C105—H10F | 120.3 | C306—C305—H30D | 119.8 |
C105—C106—C101 | 121.7 (3) | C301—C306—C305 | 120.7 (3) |
C105—C106—H10C | 119.2 | C301—C306—H30E | 119.6 |
C101—C106—H10C | 119.2 | C305—C306—H30E | 119.6 |
C112—C107—C108 | 118.3 (3) | C312—C307—C308 | 119.4 (3) |
C112—C107—P1 | 118.66 (19) | C312—C307—P3 | 122.5 (2) |
C108—C107—P1 | 123.1 (2) | C308—C307—P3 | 118.0 (3) |
C109—C108—C107 | 120.3 (3) | C309—C308—C307 | 119.4 (3) |
C109—C108—H10D | 119.9 | C309—C308—H30F | 120.3 |
C107—C108—H10D | 119.9 | C307—C308—H30F | 120.3 |
C110—C109—C108 | 120.0 (3) | C310—C309—C308 | 121.7 (3) |
C110—C109—H10E | 120.0 | C310—C309—H30G | 119.2 |
C108—C109—H10E | 120.0 | C308—C309—H30G | 119.2 |
C111—C110—C109 | 120.2 (3) | C309—C310—C311 | 118.5 (3) |
C111—C110—H11A | 119.9 | C309—C310—H31A | 120.8 |
C109—C110—H11A | 119.9 | C311—C310—H31A | 120.8 |
C110—C111—C112 | 120.0 (3) | C312—C311—C310 | 121.2 (4) |
C110—C111—H11B | 120.0 | C312—C311—H31B | 119.4 |
C112—C111—H11B | 120.0 | C310—C311—H31B | 119.4 |
C107—C112—C111 | 121.3 (2) | C307—C312—C311 | 119.7 (3) |
C107—C112—H11C | 119.4 | C307—C312—H31C | 120.2 |
C111—C112—H11C | 119.4 | C311—C312—H31C | 120.2 |
C118—C113—C114 | 117.1 (3) | C314—C313—C318 | 116.4 (3) |
C118—C113—P1 | 123.0 (2) | C314—C313—P3 | 124.6 (2) |
C114—C113—P1 | 119.8 (3) | C318—C313—P3 | 118.9 (2) |
C115—C114—C113 | 121.8 (3) | C315—C314—C313 | 121.6 (3) |
C115—C114—H11D | 119.1 | C315—C314—H31D | 119.2 |
C113—C114—H11D | 119.1 | C313—C314—H31D | 119.2 |
C116—C115—C114 | 120.6 (3) | C316—C315—C314 | 121.6 (3) |
C116—C115—H11E | 119.7 | C316—C315—H31E | 119.2 |
C114—C115—H11E | 119.7 | C314—C315—H31E | 119.2 |
C115—C116—C117 | 119.0 (3) | C315—C316—C317 | 118.9 (3) |
C115—C116—H11F | 120.5 | C315—C316—H31F | 120.5 |
C117—C116—H11F | 120.5 | C317—C316—H31F | 120.5 |
C116—C117—C118 | 120.0 (3) | C316—C317—C318 | 120.3 (3) |
C116—C117—H11G | 120.0 | C316—C317—H31G | 119.9 |
C118—C117—H11G | 120.0 | C318—C317—H31G | 119.9 |
C113—C118—C117 | 121.5 (3) | C317—C318—C313 | 121.1 (3) |
C113—C118—H11H | 119.3 | C317—C318—H31H | 119.5 |
C117—C118—H11H | 119.3 | C313—C318—H31H | 119.5 |
C206—C201—C202 | 118.4 (3) | C14—O11—C11 | 108.5 (3) |
C206—C201—P2 | 124.9 (3) | O11—C11—C12 | 107.4 (4) |
C202—C201—P2 | 116.67 (19) | O11—C11—H11I | 110.2 |
C203—C202—C201 | 119.8 (3) | C12—C11—H11I | 110.2 |
C203—C202—H20E | 120.1 | O11—C11—H11J | 110.2 |
C201—C202—H20E | 120.1 | C12—C11—H11J | 110.2 |
C204—C203—C202 | 121.6 (3) | H11I—C11—H11J | 108.5 |
C204—C203—H20F | 119.2 | C13—C12—C11 | 107.0 (4) |
C202—C203—H20F | 119.2 | C13—C12—H12A | 110.3 |
C205—C204—C203 | 118.1 (3) | C11—C12—H12A | 110.3 |
C205—C204—H20G | 121.0 | C13—C12—H12B | 110.3 |
C203—C204—H20G | 121.0 | C11—C12—H12B | 110.3 |
C204—C205—C206 | 121.7 (3) | H12A—C12—H12B | 108.6 |
C204—C205—H20D | 119.1 | C12—C13—C14 | 109.2 (5) |
C206—C205—H20D | 119.1 | C12—C13—H13A | 109.8 |
C205—C206—C201 | 120.3 (3) | C14—C13—H13A | 109.8 |
C205—C206—H20A | 119.9 | C12—C13—H13B | 109.8 |
C201—C206—H20A | 119.9 | C14—C13—H13B | 109.8 |
C212—C207—C208 | 117.5 (3) | H13A—C13—H13B | 108.3 |
C212—C207—P2 | 124.9 (2) | O11—C14—C13 | 107.1 (4) |
C208—C207—P2 | 117.7 (3) | O11—C14—H14C | 110.3 |
C209—C208—C207 | 122.2 (4) | C13—C14—H14C | 110.3 |
C209—C208—H20B | 118.9 | O11—C14—H14A | 110.3 |
C207—C208—H20B | 118.9 | C13—C14—H14A | 110.3 |
C210—C209—C208 | 119.7 (4) | H14C—C14—H14A | 108.6 |
P3—Ag2—Br1—Ag1 | 169.76 (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—Ag2 | 117.60 (2) | C202—C203—C204—C205 | 0.4 (6) |
P1—Ag1—Br1—Ag2 | −105.01 (3) | C203—C204—C205—C206 | 0.1 (6) |
Br2—Ag1—Br1—Ag2 | 3.069 (11) | C204—C205—C206—C201 | 0.7 (6) |
P3—Ag2—Br2—Ag1 | −169.18 (3) | C202—C201—C206—C205 | −2.0 (5) |
Br1—Ag2—Br2—Ag1 | 3.432 (12) | P2—C201—C206—C205 | 177.7 (3) |
P2—Ag1—Br2—Ag2 | −111.76 (3) | C201—P2—C207—C212 | −114.6 (2) |
P1—Ag1—Br2—Ag2 | 103.47 (3) | C213—P2—C207—C212 | −5.4 (3) |
Br1—Ag1—Br2—Ag2 | −3.058 (11) | Ag1—P2—C207—C212 | 116.4 (2) |
P2—Ag1—P1—C113 | −55.84 (13) | C201—P2—C207—C208 | 67.2 (2) |
Br2—Ag1—P1—C113 | 80.24 (12) | C213—P2—C207—C208 | 176.4 (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—C209 | 176.7 (2) |
Br1—Ag1—P1—C101 | 60.17 (11) | C207—C208—C209—C210 | 1.5 (5) |
P2—Ag1—P1—C107 | 63.21 (11) | C208—C209—C210—C211 | −1.5 (5) |
Br2—Ag1—P1—C107 | −160.71 (10) | C209—C210—C211—C212 | 1.7 (5) |
Br1—Ag1—P1—C107 | −58.84 (10) | C208—C207—C212—C211 | 1.7 (4) |
P1—Ag1—P2—C207 | −63.49 (13) | P2—C207—C212—C211 | −176.5 (2) |
Br2—Ag1—P2—C207 | 162.41 (12) | C210—C211—C212—C207 | −1.8 (4) |
Br1—Ag1—P2—C207 | 58.29 (12) | C207—P2—C213—C214 | 102.5 (3) |
P1—Ag1—P2—C201 | 174.61 (11) | C201—P2—C213—C214 | −147.8 (3) |
Br2—Ag1—P2—C201 | 40.51 (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—C213 | 53.42 (12) | C201—P2—C213—C218 | 29.9 (3) |
Br2—Ag1—P2—C213 | −80.67 (11) | Ag1—P2—C213—C218 | 158.5 (2) |
Br1—Ag1—P2—C213 | 175.20 (11) | C218—C213—C214—C215 | 2.3 (5) |
Br2—Ag2—P3—C313 | −95.32 (11) | P2—C213—C214—C215 | −179.9 (3) |
Br1—Ag2—P3—C313 | 93.20 (11) | C213—C214—C215—C216 | −3.0 (5) |
Br2—Ag2—P3—C307 | 24.36 (10) | C214—C215—C216—C217 | 1.8 (5) |
Br1—Ag2—P3—C307 | −147.13 (10) | C215—C216—C217—C218 | −0.2 (5) |
Br2—Ag2—P3—C301 | 145.26 (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—C106 | 96.8 (2) | C313—P3—C301—C306 | 91.1 (3) |
Ag1—P1—C101—C106 | −24.7 (3) | C307—P3—C301—C306 | −16.7 (3) |
C113—P1—C101—C102 | 23.6 (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—C102 | 153.0 (2) | C307—P3—C301—C302 | 165.3 (3) |
C106—C101—C102—C103 | −2.7 (5) | Ag2—P3—C301—C302 | 38.6 (3) |
P1—C101—C102—C103 | 179.5 (2) | C306—C301—C302—C303 | −2.5 (5) |
C101—C102—C103—C104 | 2.0 (5) | P3—C301—C302—C303 | 175.6 (3) |
C102—C103—C104—C105 | −0.2 (5) | C301—C302—C303—C304 | 2.4 (5) |
C103—C104—C105—C106 | −1.0 (5) | C302—C303—C304—C305 | −0.6 (5) |
C104—C105—C106—C101 | 0.2 (5) | C303—C304—C305—C306 | −1.1 (5) |
C102—C101—C106—C105 | 1.6 (4) | C302—C301—C306—C305 | 0.8 (5) |
P1—C101—C106—C105 | 179.5 (2) | P3—C301—C306—C305 | −177.1 (2) |
C113—P1—C107—C112 | 96.1 (3) | C304—C305—C306—C301 | 1.0 (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—C312 | 79.2 (3) |
C113—P1—C107—C108 | −85.0 (3) | Ag2—P3—C307—C312 | −154.4 (2) |
C101—P1—C107—C108 | 23.2 (3) | C313—P3—C307—C308 | 152.2 (2) |
Ag1—P1—C107—C108 | 148.1 (2) | C301—P3—C307—C308 | −99.9 (2) |
C112—C107—C108—C109 | −0.3 (5) | Ag2—P3—C307—C308 | 26.5 (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—C309 | 176.3 (2) |
C108—C109—C110—C111 | −0.3 (5) | C307—C308—C309—C310 | 1.8 (5) |
C109—C110—C111—C112 | 1.2 (5) | C308—C309—C310—C311 | 0.2 (5) |
C108—C107—C112—C111 | 1.1 (5) | C309—C310—C311—C312 | −1.3 (4) |
P1—C107—C112—C111 | −179.9 (3) | C308—C307—C312—C311 | 1.7 (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—C307 | 0.3 (4) |
C107—P1—C113—C118 | −0.8 (2) | C307—P3—C313—C314 | 113.2 (3) |
Ag1—P1—C113—C118 | 121.3 (2) | C301—P3—C313—C314 | 4.7 (3) |
C101—P1—C113—C114 | 71.3 (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—C115 | 0.8 (4) | Ag2—P3—C313—C318 | 56.1 (3) |
P1—C113—C114—C115 | 179.0 (2) | C318—C313—C314—C315 | 1.2 (5) |
C113—C114—C115—C116 | −0.5 (5) | P3—C313—C314—C315 | 178.2 (3) |
C114—C115—C116—C117 | −0.3 (5) | C313—C314—C315—C316 | −0.2 (5) |
C115—C116—C117—C118 | 0.6 (4) | C314—C315—C316—C317 | 1.1 (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—C313 | 4.3 (5) |
C116—C117—C118—C113 | −0.2 (4) | C314—C313—C318—C317 | −3.3 (5) |
C207—P2—C201—C206 | 22.9 (3) | P3—C313—C318—C317 | 179.6 (3) |
C213—P2—C201—C206 | −86.1 (3) | C14—O11—C11—C12 | 6.2 (5) |
Ag1—P2—C201—C206 | 148.6 (2) | O11—C11—C12—C13 | −8.9 (6) |
C207—P2—C201—C202 | −157.5 (2) | C11—C12—C13—C14 | 8.2 (6) |
C213—P2—C201—C202 | 93.5 (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—C203 | 2.5 (5) |
Experimental details
Crystal data | |
Chemical formula | [Ag2Br2(C18H15P)3]·0.85C4H8O |
Mr | 1223.66 |
Crystal system, space group | Monoclinic, P21/c |
Temperature (K) | 293 |
a, b, c (Å) | 16.2386 (19), 19.4575 (17), 18.3069 (18) |
β (°) | 111.896 (1) |
V (Å3) | 5367.0 (9) |
Z | 4 |
Radiation type | Mo Kα |
µ (mm−1) | 2.35 |
Crystal size (mm) | 0.40 × 0.12 × 0.08 |
Data collection | |
Diffractometer | Rigaku Mercury CCD diffractometer |
Absorption correction | Multi-scan (SPHERE in CrystalClear; Rigaku, 2002) |
Tmin, Tmax | 0.721, 0.829 |
No. of measured, independent and observed [I > 2σ(I)] reflections | 36137, 9804, 4750 |
Rint | 0.095 |
(sin θ/λ)max (Å−1) | 0.602 |
Refinement | |
R[F2 > 2σ(F2)], wR(F2), S | 0.076, 0.115, 1.00 |
No. of reflections | 9804 |
No. of parameters | 596 |
H-atom treatment | H-atom parameters constrained |
Δρmax, Δρmin (e Å−3) | 0.37, −0.41 |
Computer programs: CrystalClear (Rigaku, 2002), SHELXS97 (Sheldrick, 2008), SHELXL97 (Sheldrick, 2008), SHELXTL (Sheldrick, 2008).
Acknowledgements
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.
References
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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.