Supporting information
Crystallographic Information File (CIF) https://doi.org/10.1107/S1600536807029042/br2047sup1.cif | |
Structure factor file (CIF format) https://doi.org/10.1107/S1600536807029042/br2047Isup2.hkl |
CCDC reference: 654787
Synthesis of [Ag(PCyPh2)2I]2: 1 equivalent of AgI and 2.1 equivalents of diphenylcyclohexylphosphine were added in a vial containing anhydrous methylenechloride.The mixture was allowed to stir for 3 h at room temperature in darkness. Colorless crystals were grown by slow cooling of a saturated methylenechloride solution from ambient to 273 K in the dark. (yield 54%).
H atoms were assigned calculated positions with Uiso restrained to be 0.2Ueq of the bonded C atom and a C—H distance of 0.95–0.99 Å.
The 1:2 AgI:PCyPh2 dimeric complex is similar to the reported triphenyphosphine complexes with chlorine or bromine (Cassel, 1979; Bowmaker et al.,1993; Teo & Calabrese, 1976) and the 5-phenyldibenzophosphine complex with chloride (Attar et al., 1991). The 1:2 AgI:PCyPh2 dimeric complex is the first reported complex of this type with bridging iodine and monodentate phosphine. The molecule is located on a twofold axis.
Background information on monodentate phosphine–AgX (X=Br, Cl) adducts can be found in Attar et al. (1991), Bowmaker et al. (1993), Cassel (1979) and Teo & Calabrese (1976).
Data collection: SMART (Bruker, 2002); cell refinement: SAINT (Bruker, 2002); data reduction: SAINT; program(s) used to solve structure: SHELXS97 (Sheldrick, 1997); program(s) used to refine structure: SHELXL97 (Sheldrick, 1997); molecular graphics: SHELXTL (Bruker, 2002); software used to prepare material for publication: SHELXTL.
Fig. 1. Molecular diagram of the 1:2 AgI:PCyPh2 dimeric complex with ellipsoids at 30% probability. Hydrogen atoms are omitted for clarity. |
[Ag2I2(C18H21P)4] | F(000) = 3104 |
Mr = 1542.81 | Dx = 1.574 Mg m−3 |
Monoclinic, C2/c | Mo Kα radiation, λ = 0.71073 Å |
Hall symbol: -C 2yc | Cell parameters from 934 reflections |
a = 27.805 (4) Å | θ = 2.7–22.1° |
b = 13.3327 (17) Å | µ = 1.69 mm−1 |
c = 17.598 (4) Å | T = 120 K |
β = 93.474 (13)° | Tabular, colourless |
V = 6511.8 (19) Å3 | 0.38 × 0.24 × 0.16 mm |
Z = 4 |
Bruker APEX diffractometer | 5724 independent reflections |
Radiation source: fine-focus sealed tube | 4448 reflections with I > 2σ(I) |
Graphite monochromator | Rint = 0.099 |
Detector resolution: 836.6 pixels mm-1 | θmax = 25.0°, θmin = 2.0° |
ω scans | h = −32→32 |
Absorption correction: multi-scan (SADABS; Bruker, 2002) | k = −15→15 |
Tmin = 0.556, Tmax = 0.763 | l = −20→20 |
30202 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)] = 0.039 | Hydrogen site location: inferred from neighbouring sites |
wR(F2) = 0.090 | H-atom parameters constrained |
S = 1.05 | w = 1/[σ2(Fo2) + (0.0207P)2] where P = (Fo2 + 2Fc2)/3 |
5724 reflections | (Δ/σ)max = 0.005 |
361 parameters | Δρmax = 0.94 e Å−3 |
0 restraints | Δρmin = −0.50 e Å−3 |
[Ag2I2(C18H21P)4] | V = 6511.8 (19) Å3 |
Mr = 1542.81 | Z = 4 |
Monoclinic, C2/c | Mo Kα radiation |
a = 27.805 (4) Å | µ = 1.69 mm−1 |
b = 13.3327 (17) Å | T = 120 K |
c = 17.598 (4) Å | 0.38 × 0.24 × 0.16 mm |
β = 93.474 (13)° |
Bruker APEX diffractometer | 5724 independent reflections |
Absorption correction: multi-scan (SADABS; Bruker, 2002) | 4448 reflections with I > 2σ(I) |
Tmin = 0.556, Tmax = 0.763 | Rint = 0.099 |
30202 measured reflections |
R[F2 > 2σ(F2)] = 0.039 | 0 restraints |
wR(F2) = 0.090 | H-atom parameters constrained |
S = 1.05 | Δρmax = 0.94 e Å−3 |
5724 reflections | Δρmin = −0.50 e Å−3 |
361 parameters |
Experimental. Data collection is performed with four batch runs at φ = 0.00 ° (600 frames), at φ = 90.00 ° (600 frames), at φ = 180 ° (600 frames) and at φ = 270 ° (600 frames). Frame width = 0.30 ° in ω. Data is merged, corrected for decay, and treated with multi-scan absorption corrections. |
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 | 0.936332 (13) | 0.23521 (3) | 0.22857 (2) | 0.02529 (11) | |
I1 | 1.011583 (11) | 0.21772 (2) | 0.122587 (17) | 0.02443 (10) | |
P1 | 0.87855 (4) | 0.08676 (9) | 0.22706 (7) | 0.0218 (3) | |
P2 | 0.89485 (4) | 0.40206 (9) | 0.21388 (7) | 0.0238 (3) | |
C1 | 0.86182 (16) | −0.0960 (3) | 0.3073 (3) | 0.0258 (11) | |
H1A | 0.8616 | −0.1352 | 0.2595 | 0.031* | |
H1B | 0.8286 | −0.0719 | 0.3137 | 0.031* | |
C2 | 0.87775 (17) | −0.1632 (4) | 0.3743 (3) | 0.0345 (13) | |
H2A | 0.8736 | −0.1265 | 0.4223 | 0.041* | |
H2B | 0.8567 | −0.2231 | 0.3739 | 0.041* | |
C3 | 0.92953 (17) | −0.1967 (3) | 0.3723 (3) | 0.0347 (13) | |
H3A | 0.9325 | −0.2442 | 0.3296 | 0.042* | |
H3B | 0.9391 | −0.2324 | 0.4202 | 0.042* | |
C4 | 0.96339 (17) | −0.1084 (3) | 0.3626 (3) | 0.0314 (12) | |
H4A | 0.9652 | −0.0679 | 0.4099 | 0.038* | |
H4B | 0.9961 | −0.1340 | 0.3547 | 0.038* | |
C5 | 0.94707 (15) | −0.0418 (3) | 0.2958 (3) | 0.0241 (11) | |
H5A | 0.9496 | −0.0793 | 0.2477 | 0.029* | |
H5B | 0.9685 | 0.0175 | 0.2945 | 0.029* | |
C6 | 0.89525 (15) | −0.0071 (3) | 0.3020 (3) | 0.0236 (11) | |
H6A | 0.8945 | 0.0291 | 0.3517 | 0.028* | |
C7 | 0.82980 (17) | −0.0480 (4) | 0.1225 (3) | 0.0313 (12) | |
H7A | 0.8026 | −0.0438 | 0.1526 | 0.038* | |
C8 | 0.82872 (19) | −0.1112 (4) | 0.0600 (3) | 0.0399 (14) | |
H8A | 0.8002 | −0.1479 | 0.0462 | 0.048* | |
C9 | 0.86880 (19) | −0.1215 (4) | 0.0171 (3) | 0.0345 (13) | |
H9A | 0.8681 | −0.1672 | −0.0244 | 0.041* | |
C10 | 0.90939 (19) | −0.0653 (4) | 0.0349 (3) | 0.0331 (12) | |
H10A | 0.9367 | −0.0712 | 0.0052 | 0.040* | |
C11 | 0.91036 (17) | 0.0005 (3) | 0.0967 (3) | 0.0264 (11) | |
H11A | 0.9384 | 0.0395 | 0.1086 | 0.032* | |
C12 | 0.87082 (17) | 0.0097 (3) | 0.1414 (3) | 0.0257 (11) | |
C13 | 0.80198 (16) | 0.1262 (3) | 0.3217 (3) | 0.0258 (11) | |
H13A | 0.8223 | 0.1006 | 0.3625 | 0.031* | |
C14 | 0.75725 (17) | 0.1661 (3) | 0.3368 (3) | 0.0322 (12) | |
H14A | 0.7472 | 0.1675 | 0.3875 | 0.039* | |
C15 | 0.72758 (18) | 0.2036 (4) | 0.2778 (3) | 0.0385 (14) | |
H15A | 0.6973 | 0.2323 | 0.2879 | 0.046* | |
C16 | 0.74172 (18) | 0.1995 (4) | 0.2052 (3) | 0.0398 (14) | |
H16A | 0.7207 | 0.2232 | 0.1646 | 0.048* | |
C17 | 0.78624 (16) | 0.1612 (4) | 0.1898 (3) | 0.0325 (12) | |
H17A | 0.7958 | 0.1607 | 0.1388 | 0.039* | |
C18 | 0.81737 (15) | 0.1233 (3) | 0.2479 (3) | 0.0248 (11) | |
C19 | 0.83838 (17) | 0.3677 (3) | 0.3350 (3) | 0.0268 (11) | |
H19A | 0.8584 | 0.3071 | 0.3447 | 0.032* | |
H19B | 0.8114 | 0.3496 | 0.2982 | 0.032* | |
C20 | 0.81820 (17) | 0.4027 (4) | 0.4094 (3) | 0.0324 (12) | |
H20A | 0.7939 | 0.4558 | 0.3982 | 0.039* | |
H20B | 0.8019 | 0.3457 | 0.4331 | 0.039* | |
C21 | 0.85711 (19) | 0.4429 (4) | 0.4649 (3) | 0.0354 (13) | |
H21A | 0.8420 | 0.4715 | 0.5096 | 0.042* | |
H21B | 0.8783 | 0.3870 | 0.4830 | 0.042* | |
C22 | 0.88707 (18) | 0.5224 (4) | 0.4294 (3) | 0.0355 (13) | |
H22A | 0.8668 | 0.5822 | 0.4180 | 0.043* | |
H22B | 0.9136 | 0.5425 | 0.4662 | 0.043* | |
C23 | 0.90791 (16) | 0.4870 (3) | 0.3574 (3) | 0.0274 (11) | |
H23A | 0.9313 | 0.4325 | 0.3695 | 0.033* | |
H23B | 0.9254 | 0.5430 | 0.3344 | 0.033* | |
C24 | 0.86880 (16) | 0.4490 (3) | 0.3005 (3) | 0.0270 (11) | |
H24A | 0.8472 | 0.5066 | 0.2858 | 0.032* | |
C25 | 0.85027 (17) | 0.3252 (3) | 0.0829 (3) | 0.0277 (11) | |
H25A | 0.8797 | 0.2895 | 0.0800 | 0.033* | |
C26 | 0.81439 (19) | 0.3152 (4) | 0.0253 (3) | 0.0346 (13) | |
H26A | 0.8192 | 0.2722 | −0.0166 | 0.042* | |
C27 | 0.77145 (18) | 0.3678 (4) | 0.0283 (3) | 0.0341 (13) | |
H27A | 0.7471 | 0.3621 | −0.0117 | 0.041* | |
C28 | 0.76458 (17) | 0.4282 (4) | 0.0900 (3) | 0.0302 (12) | |
H28A | 0.7351 | 0.4637 | 0.0930 | 0.036* | |
C29 | 0.80011 (17) | 0.4378 (3) | 0.1477 (3) | 0.0281 (12) | |
H29A | 0.7948 | 0.4798 | 0.1900 | 0.034* | |
C30 | 0.84357 (16) | 0.3867 (3) | 0.1447 (3) | 0.0241 (11) | |
C31 | 0.95789 (16) | 0.5014 (3) | 0.1230 (3) | 0.0276 (11) | |
H31A | 0.9705 | 0.4364 | 0.1145 | 0.033* | |
C32 | 0.97607 (17) | 0.5842 (4) | 0.0841 (3) | 0.0335 (12) | |
H32A | 1.0020 | 0.5757 | 0.0519 | 0.040* | |
C33 | 0.95618 (17) | 0.6771 (4) | 0.0929 (3) | 0.0306 (12) | |
H33A | 0.9666 | 0.7320 | 0.0636 | 0.037* | |
C34 | 0.92163 (19) | 0.6915 (4) | 0.1434 (3) | 0.0402 (14) | |
H34A | 0.9100 | 0.7573 | 0.1521 | 0.048* | |
C35 | 0.90309 (17) | 0.6105 (3) | 0.1825 (3) | 0.0327 (12) | |
H35A | 0.8777 | 0.6207 | 0.2153 | 0.039* | |
C36 | 0.92213 (16) | 0.5132 (3) | 0.1732 (3) | 0.0263 (11) |
U11 | U22 | U33 | U12 | U13 | U23 | |
Ag1 | 0.0247 (2) | 0.0233 (2) | 0.0284 (2) | −0.00002 (15) | 0.00537 (16) | 0.00078 (16) |
I1 | 0.02476 (19) | 0.02417 (18) | 0.02487 (19) | 0.00026 (13) | 0.00564 (14) | −0.00068 (13) |
P1 | 0.0205 (6) | 0.0209 (7) | 0.0238 (7) | −0.0006 (5) | 0.0011 (5) | 0.0009 (5) |
P2 | 0.0269 (7) | 0.0186 (6) | 0.0265 (7) | 0.0007 (5) | 0.0061 (6) | −0.0029 (5) |
C1 | 0.020 (3) | 0.025 (3) | 0.032 (3) | 0.000 (2) | −0.002 (2) | 0.005 (2) |
C2 | 0.030 (3) | 0.029 (3) | 0.044 (3) | −0.003 (2) | 0.004 (2) | 0.011 (2) |
C3 | 0.030 (3) | 0.026 (3) | 0.048 (3) | 0.002 (2) | 0.002 (3) | 0.011 (2) |
C4 | 0.029 (3) | 0.022 (3) | 0.044 (3) | 0.001 (2) | 0.002 (2) | 0.004 (2) |
C5 | 0.023 (3) | 0.018 (2) | 0.031 (3) | −0.002 (2) | 0.004 (2) | 0.000 (2) |
C6 | 0.019 (2) | 0.023 (3) | 0.029 (3) | −0.001 (2) | 0.002 (2) | 0.003 (2) |
C7 | 0.030 (3) | 0.034 (3) | 0.030 (3) | −0.001 (2) | 0.002 (2) | −0.001 (2) |
C8 | 0.037 (3) | 0.044 (3) | 0.038 (3) | −0.013 (3) | −0.010 (3) | −0.002 (3) |
C9 | 0.054 (4) | 0.028 (3) | 0.019 (3) | 0.002 (3) | −0.007 (3) | −0.005 (2) |
C10 | 0.043 (3) | 0.030 (3) | 0.027 (3) | 0.008 (2) | 0.009 (2) | 0.004 (2) |
C11 | 0.027 (3) | 0.027 (3) | 0.026 (3) | −0.005 (2) | −0.001 (2) | −0.005 (2) |
C12 | 0.031 (3) | 0.021 (3) | 0.025 (3) | −0.002 (2) | −0.002 (2) | 0.000 (2) |
C13 | 0.023 (3) | 0.025 (3) | 0.029 (3) | −0.001 (2) | 0.002 (2) | −0.002 (2) |
C14 | 0.031 (3) | 0.024 (3) | 0.043 (3) | −0.004 (2) | 0.013 (3) | −0.004 (2) |
C15 | 0.019 (3) | 0.027 (3) | 0.069 (4) | 0.005 (2) | 0.006 (3) | 0.005 (3) |
C16 | 0.024 (3) | 0.036 (3) | 0.058 (4) | −0.001 (2) | −0.007 (3) | 0.018 (3) |
C17 | 0.024 (3) | 0.033 (3) | 0.040 (3) | −0.006 (2) | −0.002 (2) | 0.009 (2) |
C18 | 0.017 (2) | 0.019 (2) | 0.038 (3) | −0.0030 (19) | −0.002 (2) | 0.003 (2) |
C19 | 0.030 (3) | 0.024 (3) | 0.026 (3) | 0.000 (2) | 0.005 (2) | 0.001 (2) |
C20 | 0.029 (3) | 0.037 (3) | 0.032 (3) | 0.002 (2) | 0.008 (2) | −0.002 (2) |
C21 | 0.048 (3) | 0.036 (3) | 0.023 (3) | 0.010 (3) | 0.005 (2) | −0.002 (2) |
C22 | 0.034 (3) | 0.042 (3) | 0.030 (3) | 0.003 (3) | 0.000 (2) | −0.011 (2) |
C23 | 0.024 (3) | 0.028 (3) | 0.029 (3) | 0.006 (2) | −0.001 (2) | −0.004 (2) |
C24 | 0.027 (3) | 0.025 (3) | 0.030 (3) | 0.003 (2) | 0.004 (2) | −0.004 (2) |
C25 | 0.036 (3) | 0.023 (3) | 0.026 (3) | −0.004 (2) | 0.010 (2) | −0.002 (2) |
C26 | 0.047 (3) | 0.027 (3) | 0.030 (3) | −0.010 (3) | 0.009 (3) | −0.008 (2) |
C27 | 0.035 (3) | 0.037 (3) | 0.030 (3) | −0.015 (3) | 0.002 (2) | −0.005 (2) |
C28 | 0.029 (3) | 0.030 (3) | 0.032 (3) | 0.001 (2) | 0.005 (2) | 0.001 (2) |
C29 | 0.036 (3) | 0.029 (3) | 0.021 (3) | −0.001 (2) | 0.009 (2) | 0.000 (2) |
C30 | 0.027 (3) | 0.021 (3) | 0.025 (3) | −0.002 (2) | 0.008 (2) | 0.003 (2) |
C31 | 0.027 (3) | 0.023 (3) | 0.034 (3) | 0.002 (2) | 0.009 (2) | −0.001 (2) |
C32 | 0.027 (3) | 0.032 (3) | 0.043 (3) | −0.001 (2) | 0.011 (2) | 0.004 (2) |
C33 | 0.036 (3) | 0.026 (3) | 0.030 (3) | −0.009 (2) | 0.000 (2) | 0.005 (2) |
C34 | 0.048 (4) | 0.018 (3) | 0.055 (4) | 0.001 (2) | 0.012 (3) | 0.000 (3) |
C35 | 0.034 (3) | 0.025 (3) | 0.041 (3) | 0.004 (2) | 0.012 (2) | 0.001 (2) |
C36 | 0.023 (3) | 0.021 (3) | 0.035 (3) | −0.001 (2) | 0.006 (2) | −0.002 (2) |
Ag1—P2 | 2.5120 (12) | C13—C14 | 1.393 (6) |
Ag1—P1 | 2.5485 (12) | C14—C15 | 1.380 (7) |
Ag1—I1 | 2.8955 (6) | C15—C16 | 1.360 (7) |
Ag1—I1i | 2.9245 (7) | C16—C17 | 1.381 (6) |
P1—C12 | 1.826 (5) | C17—C18 | 1.395 (6) |
P1—C18 | 1.828 (4) | C19—C24 | 1.523 (6) |
P1—C6 | 1.856 (4) | C19—C20 | 1.529 (6) |
P2—C36 | 1.830 (5) | C20—C21 | 1.511 (6) |
P2—C30 | 1.829 (5) | C21—C22 | 1.508 (7) |
P2—C24 | 1.837 (5) | C22—C23 | 1.501 (6) |
C1—C6 | 1.513 (6) | C23—C24 | 1.520 (6) |
C1—C2 | 1.525 (6) | C25—C30 | 1.384 (6) |
C2—C3 | 1.510 (6) | C25—C26 | 1.385 (7) |
C3—C4 | 1.524 (6) | C26—C27 | 1.388 (7) |
C4—C5 | 1.520 (6) | C27—C28 | 1.375 (6) |
C5—C6 | 1.524 (6) | C28—C29 | 1.379 (6) |
C7—C8 | 1.384 (7) | C29—C30 | 1.391 (6) |
C7—C12 | 1.399 (6) | C31—C36 | 1.379 (6) |
C8—C9 | 1.391 (7) | C31—C32 | 1.409 (6) |
C9—C10 | 1.374 (7) | C32—C33 | 1.369 (6) |
C10—C11 | 1.397 (6) | C33—C34 | 1.361 (7) |
C11—C12 | 1.396 (6) | C34—C35 | 1.396 (6) |
C13—C18 | 1.392 (6) | C35—C36 | 1.414 (6) |
P2—Ag1—P1 | 113.67 (4) | C7—C12—P1 | 124.0 (4) |
P2—Ag1—I1 | 110.50 (3) | C18—C13—C14 | 121.1 (5) |
P1—Ag1—I1 | 114.23 (3) | C15—C14—C13 | 119.7 (5) |
P2—Ag1—I1i | 111.24 (3) | C16—C15—C14 | 119.9 (5) |
P1—Ag1—I1i | 103.01 (3) | C15—C16—C17 | 120.9 (5) |
I1—Ag1—I1i | 103.45 (2) | C16—C17—C18 | 120.9 (5) |
Ag1—I1—Ag1i | 75.796 (19) | C13—C18—C17 | 117.6 (4) |
C12—P1—C18 | 104.6 (2) | C13—C18—P1 | 122.5 (3) |
C12—P1—C6 | 102.7 (2) | C17—C18—P1 | 119.5 (4) |
C18—P1—C6 | 103.4 (2) | C24—C19—C20 | 111.5 (4) |
C12—P1—Ag1 | 119.22 (15) | C21—C20—C19 | 112.1 (4) |
C18—P1—Ag1 | 112.61 (15) | C22—C21—C20 | 111.9 (4) |
C6—P1—Ag1 | 112.67 (14) | C23—C22—C21 | 112.4 (4) |
C36—P2—C30 | 98.9 (2) | C22—C23—C24 | 111.3 (4) |
C36—P2—C24 | 104.0 (2) | C23—C24—C19 | 111.6 (4) |
C30—P2—C24 | 105.1 (2) | C23—C24—P2 | 111.0 (3) |
C36—P2—Ag1 | 123.97 (15) | C19—C24—P2 | 110.1 (3) |
C30—P2—Ag1 | 107.71 (15) | C30—C25—C26 | 120.4 (5) |
C24—P2—Ag1 | 114.71 (16) | C25—C26—C27 | 120.4 (5) |
C6—C1—C2 | 111.0 (4) | C28—C27—C26 | 119.2 (5) |
C3—C2—C1 | 112.9 (4) | C27—C28—C29 | 120.5 (5) |
C2—C3—C4 | 111.8 (4) | C28—C29—C30 | 120.8 (4) |
C5—C4—C3 | 112.3 (4) | C25—C30—C29 | 118.6 (4) |
C4—C5—C6 | 111.2 (4) | C25—C30—P2 | 116.9 (4) |
C1—C6—C5 | 110.7 (4) | C29—C30—P2 | 124.3 (4) |
C1—C6—P1 | 116.4 (3) | C36—C31—C32 | 121.1 (4) |
C5—C6—P1 | 110.5 (3) | C33—C32—C31 | 119.6 (5) |
C8—C7—C12 | 120.1 (5) | C34—C33—C32 | 120.5 (5) |
C7—C8—C9 | 120.8 (5) | C33—C34—C35 | 120.6 (5) |
C10—C9—C8 | 119.8 (5) | C34—C35—C36 | 120.1 (5) |
C9—C10—C11 | 119.8 (5) | C31—C36—C35 | 117.9 (4) |
C12—C11—C10 | 121.1 (4) | C31—C36—P2 | 119.4 (3) |
C11—C12—C7 | 118.4 (4) | C35—C36—P2 | 122.1 (4) |
C11—C12—P1 | 117.2 (3) |
Symmetry code: (i) −x+2, y, −z+1/2. |
Experimental details
Crystal data | |
Chemical formula | [Ag2I2(C18H21P)4] |
Mr | 1542.81 |
Crystal system, space group | Monoclinic, C2/c |
Temperature (K) | 120 |
a, b, c (Å) | 27.805 (4), 13.3327 (17), 17.598 (4) |
β (°) | 93.474 (13) |
V (Å3) | 6511.8 (19) |
Z | 4 |
Radiation type | Mo Kα |
µ (mm−1) | 1.69 |
Crystal size (mm) | 0.38 × 0.24 × 0.16 |
Data collection | |
Diffractometer | Bruker APEX |
Absorption correction | Multi-scan (SADABS; Bruker, 2002) |
Tmin, Tmax | 0.556, 0.763 |
No. of measured, independent and observed [I > 2σ(I)] reflections | 30202, 5724, 4448 |
Rint | 0.099 |
(sin θ/λ)max (Å−1) | 0.595 |
Refinement | |
R[F2 > 2σ(F2)], wR(F2), S | 0.039, 0.090, 1.05 |
No. of reflections | 5724 |
No. of parameters | 361 |
H-atom treatment | H-atom parameters constrained |
Δρmax, Δρmin (e Å−3) | 0.94, −0.50 |
Computer programs: SMART (Bruker, 2002), SAINT (Bruker, 2002), SAINT, SHELXS97 (Sheldrick, 1997), SHELXL97 (Sheldrick, 1997), SHELXTL (Bruker, 2002), SHELXTL.
The 1:2 AgI:PCyPh2 dimeric complex is similar to the reported triphenyphosphine complexes with chlorine or bromine (Cassel, 1979; Bowmaker et al.,1993; Teo & Calabrese, 1976) and the 5-phenyldibenzophosphine complex with chloride (Attar et al., 1991). The 1:2 AgI:PCyPh2 dimeric complex is the first reported complex of this type with bridging iodine and monodentate phosphine. The molecule is located on a twofold axis.