metal-organic compounds
Di-μ-iodido-bis[(biphenyl-2-yl)(triphenylphosphane-κP)palladium(II)]
aDepartment of Chemistry, Central Connecticut State University, New Britain, CT 06053, USA
*Correspondence e-mail: crundwellg@mail.ccsu.edu
In the title compound, [Pd2(C12H9)2I2(C18H15P)2], the dimeric complex molecule lies about an inversion center. The Pd⋯I⋯Pd bridges are slightly asymmetric, with Pd—I distances of 2.6709 (6) and 2.7486 (7) Å. The metal atom has a slightly puckered square-planar CI2P environment, the largest deviation from the least-squares plane being 0.143 (8) Å.
Related literature
For crystal structures containing Pt2I2 units, see: Grushin & Alper (1993); Marshall et al. (2001); Lang et al. (2006).
Experimental
Crystal data
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Data collection: CrysAlis CCD (Oxford Diffraction, 2009); cell CrysAlis PRO (Oxford Diffraction, 2009); data reduction: CrysAlis RED (Oxford Diffraction, 2009); program(s) used to solve structure: SHELXS97 (Sheldrick, 2008); program(s) used to refine structure: SHELXL97 (Sheldrick, 2008); molecular graphics: PLATON (Spek, 2009); software used to prepare material for publication: SHELXTL (Sheldrick, 2008).
Supporting information
10.1107/S1600536812047733/yk2076sup1.cif
contains datablocks global, I. DOI:Structure factors: contains datablock I. DOI: 10.1107/S1600536812047733/yk2076Isup2.hkl
To a 100 mL three-neck round bottom flask, 0.500 grams of tetrakis(triphenylphosphane)palladium(0) (C72H60P4Pd, 4.33 x 10 -4 mol) was dissolved in 20 ml anhydrous toluene under a stream of Ar gas. With stirring, 1.82 ml of 2-iodobiphenyl (C12H9I, 6.49 x 10 -4 mol) was added. The entire reaction was stirred under Ar gas at room temperature for six days. Small yellow crystals formed on the side of the round bottom flask after four days of slow evaporation of the toluene. The crystals slowly decomposed upon heating, being completely destroyed before reaching 150°C.
Hydrogen atoms were included in calculated positions with a C—H distance of 0.93 Å and were included in the
in riding motion approximation with Uiso = 1.2Ueq of the carrier atom.Data collection: CrysAlis CCD (Oxford Diffraction, 2009); cell
CrysAlis PRO (Oxford Diffraction, 2009); data reduction: CrysAlis RED (Oxford Diffraction, 2009); program(s) used to solve structure: SHELXS97 (Sheldrick, 2008); program(s) used to refine structure: SHELXL97 (Sheldrick, 2008); molecular graphics: PLATON (Spek, 2009); software used to prepare material for publication: SHELXTL (Sheldrick, 2008).Fig. 1. A view of the title compound. Displacement ellipsoids are drawn at the 50% probability level. |
[Pd2(C12H9)2I2(C18H15P)2] | F(000) = 1272 |
Mr = 1297.52 | Dx = 1.672 Mg m−3 |
Monoclinic, P21/c | Melting point: 423 K |
Hall symbol: -P 2ybc | Mo Kα radiation, λ = 0.71073 Å |
a = 9.6957 (4) Å | Cell parameters from 4701 reflections |
b = 20.0969 (10) Å | θ = 4.1–29.6° |
c = 18.3718 (7) Å | µ = 2.00 mm−1 |
β = 133.962 (4)° | T = 293 K |
V = 2576.8 (2) Å3 | Block, yellow |
Z = 2 | 0.25 × 0.18 × 0.12 mm |
Oxford Diffraction Xcalibur Sapphire3 diffractometer | 6087 independent reflections |
Radiation source: fine-focus sealed tube | 3783 reflections with I > 2σ(I) |
Graphite monochromator | Rint = 0.035 |
Detector resolution: 16.1790 pixels mm-1 | θmax = 28.3°, θmin = 4.3° |
ω scans | h = −12→10 |
Absorption correction: multi-scan (CrysAlis RED; Oxford Diffraction, 2009) | k = −25→19 |
Tmin = 0.845, Tmax = 1.000 | l = −24→23 |
12030 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)] = 0.057 | Hydrogen site location: inferred from neighbouring sites |
wR(F2) = 0.134 | H-atom parameters constrained |
S = 1.02 | w = 1/[σ2(Fo2) + (0.0678P)2 + 0.4388P] where P = (Fo2 + 2Fc2)/3 |
6087 reflections | (Δ/σ)max = 0.001 |
298 parameters | Δρmax = 1.92 e Å−3 |
0 restraints | Δρmin = −0.77 e Å−3 |
[Pd2(C12H9)2I2(C18H15P)2] | V = 2576.8 (2) Å3 |
Mr = 1297.52 | Z = 2 |
Monoclinic, P21/c | Mo Kα radiation |
a = 9.6957 (4) Å | µ = 2.00 mm−1 |
b = 20.0969 (10) Å | T = 293 K |
c = 18.3718 (7) Å | 0.25 × 0.18 × 0.12 mm |
β = 133.962 (4)° |
Oxford Diffraction Xcalibur Sapphire3 diffractometer | 6087 independent reflections |
Absorption correction: multi-scan (CrysAlis RED; Oxford Diffraction, 2009) | 3783 reflections with I > 2σ(I) |
Tmin = 0.845, Tmax = 1.000 | Rint = 0.035 |
12030 measured reflections |
R[F2 > 2σ(F2)] = 0.057 | 0 restraints |
wR(F2) = 0.134 | H-atom parameters constrained |
S = 1.02 | Δρmax = 1.92 e Å−3 |
6087 reflections | Δρmin = −0.77 e Å−3 |
298 parameters |
Experimental. Empirical absorption correction using spherical harmonics implemented in SCALE3 ABSPACK scaling algorithm (CrysAlis RED; Oxford Diffraction, 2009) Hydrogen atoms were placed in calculated positions with C—H distances of 0.93 Å and were included in the refinement in riding motion approximation with Uiso = 1.2Ueq of the carrier atom. |
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 | ||
Pd1 | 0.79025 (6) | 0.05054 (2) | 0.37739 (3) | 0.04167 (15) | |
I1 | 1.16659 (5) | 0.06784 (2) | 0.53368 (3) | 0.05752 (17) | |
C1 | 0.7754 (8) | 0.1416 (4) | 0.3248 (4) | 0.0551 (17) | |
C2 | 0.8449 (9) | 0.1495 (4) | 0.2822 (5) | 0.067 (2) | |
H2 | 0.9040 | 0.1142 | 0.2801 | 0.081* | |
C3 | 0.8265 (13) | 0.2129 (6) | 0.2404 (6) | 0.088 (3) | |
H3 | 0.8758 | 0.2197 | 0.2121 | 0.106* | |
C4 | 0.7348 (15) | 0.2634 (5) | 0.2430 (7) | 0.100 (3) | |
H4 | 0.7177 | 0.3040 | 0.2135 | 0.120* | |
C5 | 0.6681 (12) | 0.2555 (4) | 0.2877 (6) | 0.083 (3) | |
H5 | 0.6088 | 0.2910 | 0.2895 | 0.099* | |
C6 | 0.6881 (9) | 0.1952 (3) | 0.3305 (5) | 0.0588 (18) | |
C7 | 0.6180 (11) | 0.1889 (4) | 0.3831 (6) | 0.068 (2) | |
C8 | 0.7372 (13) | 0.1662 (4) | 0.4818 (6) | 0.079 (2) | |
H8 | 0.8631 | 0.1549 | 0.5171 | 0.095* | |
C9 | 0.6734 (18) | 0.1603 (5) | 0.5279 (8) | 0.106 (3) | |
H9 | 0.7567 | 0.1455 | 0.5944 | 0.127* | |
C10 | 0.489 (2) | 0.1758 (6) | 0.4780 (12) | 0.119 (4) | |
H10 | 0.4438 | 0.1685 | 0.5086 | 0.143* | |
C11 | 0.3707 (18) | 0.2021 (6) | 0.3832 (11) | 0.112 (4) | |
H11 | 0.2478 | 0.2155 | 0.3512 | 0.134* | |
C12 | 0.4308 (12) | 0.2092 (5) | 0.3339 (8) | 0.092 (3) | |
H12 | 0.3492 | 0.2272 | 0.2691 | 0.110* | |
P3 | 0.4805 (2) | 0.03204 (8) | 0.23017 (10) | 0.0410 (4) | |
C13 | 0.4662 (8) | −0.0292 (3) | 0.1506 (4) | 0.0480 (15) | |
C14 | 0.6076 (11) | −0.0734 (4) | 0.1914 (6) | 0.071 (2) | |
H14 | 0.7146 | −0.0723 | 0.2607 | 0.085* | |
C15 | 0.5987 (12) | −0.1206 (4) | 0.1328 (7) | 0.086 (3) | |
H15 | 0.6977 | −0.1510 | 0.1627 | 0.103* | |
C16 | 0.4449 (14) | −0.1217 (5) | 0.0326 (7) | 0.086 (3) | |
H16 | 0.4369 | −0.1535 | −0.0071 | 0.104* | |
C17 | 0.3022 (14) | −0.0773 (5) | −0.0111 (6) | 0.093 (3) | |
H17 | 0.1976 | −0.0781 | −0.0808 | 0.112* | |
C18 | 0.3103 (11) | −0.0303 (4) | 0.0472 (5) | 0.080 (2) | |
H18 | 0.2114 | 0.0002 | 0.0168 | 0.097* | |
C19 | 0.3357 (8) | −0.0016 (3) | 0.2508 (4) | 0.0459 (14) | |
C20 | 0.1854 (10) | −0.0459 (4) | 0.1846 (5) | 0.0637 (19) | |
H20 | 0.1653 | −0.0646 | 0.1315 | 0.076* | |
C21 | 0.0680 (11) | −0.0617 (4) | 0.1982 (7) | 0.080 (2) | |
H21 | −0.0323 | −0.0914 | 0.1542 | 0.096* | |
C22 | 0.0958 (12) | −0.0342 (5) | 0.2767 (7) | 0.087 (3) | |
H22 | 0.0118 | −0.0442 | 0.2836 | 0.105* | |
C23 | 0.2466 (12) | 0.0077 (5) | 0.3437 (7) | 0.079 (2) | |
H23 | 0.2669 | 0.0255 | 0.3973 | 0.095* | |
C24 | 0.3684 (9) | 0.0237 (4) | 0.3323 (5) | 0.0603 (18) | |
H24 | 0.4727 | 0.0514 | 0.3789 | 0.072* | |
C25 | 0.3342 (8) | 0.1009 (3) | 0.1431 (4) | 0.0488 (15) | |
C26 | 0.1787 (10) | 0.1252 (4) | 0.1242 (6) | 0.075 (2) | |
H26 | 0.1425 | 0.1057 | 0.1548 | 0.090* | |
C27 | 0.0765 (12) | 0.1788 (5) | 0.0592 (7) | 0.097 (3) | |
H27 | −0.0303 | 0.1947 | 0.0449 | 0.116* | |
C28 | 0.1319 (12) | 0.2082 (5) | 0.0165 (7) | 0.089 (3) | |
H28 | 0.0675 | 0.2458 | −0.0234 | 0.107* | |
C29 | 0.2765 (12) | 0.1840 (4) | 0.0309 (6) | 0.080 (2) | |
H29 | 0.3082 | 0.2032 | −0.0019 | 0.097* | |
C30 | 0.3794 (10) | 0.1307 (4) | 0.0942 (5) | 0.068 (2) | |
H30 | 0.4813 | 0.1143 | 0.1042 | 0.082* |
U11 | U22 | U33 | U12 | U13 | U23 | |
Pd1 | 0.0298 (2) | 0.0497 (3) | 0.0306 (2) | 0.00165 (18) | 0.01537 (18) | 0.00405 (19) |
I1 | 0.0344 (2) | 0.0661 (3) | 0.0443 (2) | −0.00152 (18) | 0.01692 (19) | 0.0123 (2) |
C1 | 0.035 (3) | 0.065 (5) | 0.035 (3) | −0.013 (3) | 0.013 (3) | 0.002 (3) |
C2 | 0.053 (4) | 0.087 (6) | 0.041 (4) | −0.005 (4) | 0.025 (3) | 0.011 (4) |
C3 | 0.081 (6) | 0.118 (9) | 0.057 (5) | −0.021 (5) | 0.045 (5) | 0.010 (5) |
C4 | 0.102 (7) | 0.092 (8) | 0.064 (5) | −0.038 (6) | 0.043 (6) | 0.008 (5) |
C5 | 0.088 (6) | 0.052 (5) | 0.061 (5) | −0.008 (4) | 0.034 (5) | 0.006 (4) |
C6 | 0.053 (4) | 0.042 (4) | 0.049 (4) | −0.007 (3) | 0.023 (3) | 0.003 (3) |
C7 | 0.071 (5) | 0.050 (5) | 0.074 (5) | −0.003 (4) | 0.047 (5) | −0.012 (4) |
C8 | 0.098 (6) | 0.075 (6) | 0.073 (5) | 0.003 (5) | 0.062 (5) | −0.008 (4) |
C9 | 0.161 (11) | 0.092 (8) | 0.106 (8) | 0.002 (7) | 0.108 (9) | −0.007 (6) |
C10 | 0.149 (12) | 0.107 (10) | 0.156 (12) | −0.014 (8) | 0.125 (11) | −0.031 (8) |
C11 | 0.110 (9) | 0.109 (9) | 0.152 (11) | −0.009 (7) | 0.104 (9) | −0.040 (8) |
C12 | 0.076 (6) | 0.078 (7) | 0.099 (7) | −0.003 (4) | 0.053 (6) | −0.020 (5) |
P3 | 0.0330 (7) | 0.0439 (10) | 0.0318 (7) | 0.0029 (6) | 0.0172 (6) | 0.0024 (6) |
C13 | 0.044 (3) | 0.047 (4) | 0.045 (3) | 0.000 (3) | 0.028 (3) | −0.008 (3) |
C14 | 0.069 (5) | 0.075 (6) | 0.064 (5) | 0.007 (4) | 0.045 (4) | −0.008 (4) |
C15 | 0.080 (6) | 0.091 (7) | 0.084 (6) | 0.010 (5) | 0.056 (5) | −0.015 (5) |
C16 | 0.101 (7) | 0.092 (7) | 0.085 (6) | −0.006 (5) | 0.071 (6) | −0.027 (5) |
C17 | 0.093 (7) | 0.112 (8) | 0.054 (5) | −0.004 (5) | 0.043 (5) | −0.023 (5) |
C18 | 0.067 (5) | 0.088 (6) | 0.043 (4) | 0.012 (4) | 0.022 (4) | −0.015 (4) |
C19 | 0.041 (3) | 0.044 (4) | 0.043 (3) | 0.002 (3) | 0.026 (3) | 0.004 (3) |
C20 | 0.053 (4) | 0.066 (5) | 0.057 (4) | −0.011 (3) | 0.033 (4) | −0.004 (4) |
C21 | 0.060 (5) | 0.085 (6) | 0.072 (5) | −0.022 (4) | 0.037 (4) | 0.006 (4) |
C22 | 0.063 (5) | 0.116 (8) | 0.091 (6) | −0.013 (5) | 0.056 (5) | 0.008 (6) |
C23 | 0.077 (5) | 0.101 (7) | 0.082 (5) | −0.001 (5) | 0.064 (5) | 0.001 (5) |
C24 | 0.053 (4) | 0.068 (5) | 0.059 (4) | −0.010 (3) | 0.038 (4) | −0.014 (4) |
C25 | 0.032 (3) | 0.051 (4) | 0.037 (3) | 0.001 (3) | 0.014 (3) | 0.003 (3) |
C26 | 0.056 (4) | 0.075 (6) | 0.076 (5) | 0.019 (4) | 0.039 (4) | 0.020 (4) |
C27 | 0.074 (6) | 0.104 (8) | 0.097 (7) | 0.047 (5) | 0.054 (6) | 0.040 (6) |
C28 | 0.067 (5) | 0.076 (6) | 0.076 (6) | 0.023 (4) | 0.031 (5) | 0.030 (5) |
C29 | 0.072 (5) | 0.075 (6) | 0.056 (4) | −0.001 (4) | 0.031 (4) | 0.023 (4) |
C30 | 0.053 (4) | 0.077 (6) | 0.053 (4) | 0.007 (4) | 0.028 (4) | 0.020 (4) |
Pd1—C1 | 2.028 (7) | C14—C15 | 1.392 (10) |
Pd1—P3 | 2.2792 (14) | C14—H14 | 0.9300 |
Pd1—I1 | 2.6709 (6) | C15—C16 | 1.343 (11) |
Pd1—I1i | 2.7486 (7) | C15—H15 | 0.9300 |
I1—Pd1i | 2.7486 (7) | C16—C17 | 1.347 (12) |
C1—C2 | 1.349 (9) | C16—H16 | 0.9300 |
C1—C6 | 1.417 (10) | C17—C18 | 1.389 (11) |
C2—C3 | 1.434 (12) | C17—H17 | 0.9300 |
C2—H2 | 0.9300 | C18—H18 | 0.9300 |
C3—C4 | 1.372 (13) | C19—C20 | 1.391 (9) |
C3—H3 | 0.9300 | C19—C24 | 1.392 (8) |
C4—C5 | 1.361 (12) | C20—C21 | 1.362 (10) |
C4—H4 | 0.9300 | C20—H20 | 0.9300 |
C5—C6 | 1.385 (10) | C21—C22 | 1.384 (12) |
C5—H5 | 0.9300 | C21—H21 | 0.9300 |
C6—C7 | 1.525 (10) | C22—C23 | 1.366 (12) |
C7—C8 | 1.386 (11) | C22—H22 | 0.9300 |
C7—C12 | 1.414 (10) | C23—C24 | 1.374 (9) |
C8—C9 | 1.356 (11) | C23—H23 | 0.9300 |
C8—H8 | 0.9300 | C24—H24 | 0.9300 |
C9—C10 | 1.366 (14) | C25—C26 | 1.380 (9) |
C9—H9 | 0.9300 | C25—C30 | 1.380 (9) |
C10—C11 | 1.362 (15) | C26—C27 | 1.389 (11) |
C10—H10 | 0.9300 | C26—H26 | 0.9300 |
C11—C12 | 1.385 (13) | C27—C28 | 1.354 (11) |
C11—H11 | 0.9300 | C27—H27 | 0.9300 |
C12—H12 | 0.9300 | C28—C29 | 1.326 (11) |
P3—C19 | 1.821 (6) | C28—H28 | 0.9300 |
P3—C25 | 1.827 (6) | C29—C30 | 1.373 (10) |
P3—C13 | 1.842 (6) | C29—H29 | 0.9300 |
C13—C14 | 1.342 (9) | C30—H30 | 0.9300 |
C13—C18 | 1.381 (9) | ||
C1—Pd1—P3 | 89.00 (16) | C13—C14—C15 | 121.9 (8) |
C1—Pd1—I1 | 89.25 (16) | C13—C14—H14 | 119.1 |
P3—Pd1—I1 | 171.22 (4) | C15—C14—H14 | 119.1 |
C1—Pd1—I1i | 174.70 (18) | C16—C15—C14 | 119.1 (8) |
P3—Pd1—I1i | 95.49 (4) | C16—C15—H15 | 120.5 |
I1—Pd1—I1i | 86.730 (18) | C14—C15—H15 | 120.5 |
Pd1—I1—Pd1i | 93.270 (18) | C15—C16—C17 | 120.6 (8) |
C2—C1—C6 | 121.2 (7) | C15—C16—H16 | 119.7 |
C2—C1—Pd1 | 118.9 (6) | C17—C16—H16 | 119.7 |
C6—C1—Pd1 | 119.9 (5) | C16—C17—C18 | 120.4 (8) |
C1—C2—C3 | 119.2 (8) | C16—C17—H17 | 119.8 |
C1—C2—H2 | 120.4 | C18—C17—H17 | 119.8 |
C3—C2—H2 | 120.4 | C13—C18—C17 | 119.6 (7) |
C4—C3—C2 | 118.7 (8) | C13—C18—H18 | 120.2 |
C4—C3—H3 | 120.6 | C17—C18—H18 | 120.2 |
C2—C3—H3 | 120.6 | C20—C19—C24 | 119.5 (6) |
C5—C4—C3 | 121.8 (9) | C20—C19—P3 | 123.1 (5) |
C5—C4—H4 | 119.1 | C24—C19—P3 | 117.1 (5) |
C3—C4—H4 | 119.1 | C21—C20—C19 | 119.3 (7) |
C4—C5—C6 | 120.4 (9) | C21—C20—H20 | 120.3 |
C4—C5—H5 | 119.8 | C19—C20—H20 | 120.3 |
C6—C5—H5 | 119.8 | C20—C21—C22 | 121.0 (7) |
C5—C6—C1 | 118.6 (7) | C20—C21—H21 | 119.5 |
C5—C6—C7 | 119.0 (7) | C22—C21—H21 | 119.5 |
C1—C6—C7 | 122.4 (6) | C23—C22—C21 | 119.9 (8) |
C8—C7—C12 | 117.8 (8) | C23—C22—H22 | 120.1 |
C8—C7—C6 | 121.5 (7) | C21—C22—H22 | 120.1 |
C12—C7—C6 | 120.6 (8) | C22—C23—C24 | 120.1 (8) |
C9—C8—C7 | 121.2 (9) | C22—C23—H23 | 120.0 |
C9—C8—H8 | 119.4 | C24—C23—H23 | 120.0 |
C7—C8—H8 | 119.4 | C23—C24—C19 | 120.1 (7) |
C8—C9—C10 | 121.0 (11) | C23—C24—H24 | 120.0 |
C8—C9—H9 | 119.5 | C19—C24—H24 | 120.0 |
C10—C9—H9 | 119.5 | C26—C25—C30 | 118.0 (6) |
C11—C10—C9 | 119.5 (12) | C26—C25—P3 | 122.5 (5) |
C11—C10—H10 | 120.3 | C30—C25—P3 | 119.6 (5) |
C9—C10—H10 | 120.3 | C25—C26—C27 | 119.5 (8) |
C10—C11—C12 | 121.1 (11) | C25—C26—H26 | 120.2 |
C10—C11—H11 | 119.5 | C27—C26—H26 | 120.2 |
C12—C11—H11 | 119.5 | C28—C27—C26 | 120.2 (8) |
C11—C12—C7 | 119.2 (10) | C28—C27—H27 | 119.9 |
C11—C12—H12 | 120.4 | C26—C27—H27 | 119.9 |
C7—C12—H12 | 120.4 | C29—C28—C27 | 121.0 (8) |
C19—P3—C25 | 102.8 (3) | C29—C28—H28 | 119.5 |
C19—P3—C13 | 105.9 (3) | C27—C28—H28 | 119.5 |
C25—P3—C13 | 103.1 (3) | C28—C29—C30 | 120.1 (8) |
C19—P3—Pd1 | 112.63 (19) | C28—C29—H29 | 119.9 |
C25—P3—Pd1 | 119.9 (2) | C30—C29—H29 | 119.9 |
C13—P3—Pd1 | 111.23 (19) | C29—C30—C25 | 121.1 (7) |
C14—C13—C18 | 118.5 (7) | C29—C30—H30 | 119.5 |
C14—C13—P3 | 120.9 (5) | C25—C30—H30 | 119.5 |
C18—C13—P3 | 120.6 (5) |
Symmetry code: (i) −x+2, −y, −z+1. |
Experimental details
Crystal data | |
Chemical formula | [Pd2(C12H9)2I2(C18H15P)2] |
Mr | 1297.52 |
Crystal system, space group | Monoclinic, P21/c |
Temperature (K) | 293 |
a, b, c (Å) | 9.6957 (4), 20.0969 (10), 18.3718 (7) |
β (°) | 133.962 (4) |
V (Å3) | 2576.8 (2) |
Z | 2 |
Radiation type | Mo Kα |
µ (mm−1) | 2.00 |
Crystal size (mm) | 0.25 × 0.18 × 0.12 |
Data collection | |
Diffractometer | Oxford Diffraction Xcalibur Sapphire3 diffractometer |
Absorption correction | Multi-scan (CrysAlis RED; Oxford Diffraction, 2009) |
Tmin, Tmax | 0.845, 1.000 |
No. of measured, independent and observed [I > 2σ(I)] reflections | 12030, 6087, 3783 |
Rint | 0.035 |
(sin θ/λ)max (Å−1) | 0.667 |
Refinement | |
R[F2 > 2σ(F2)], wR(F2), S | 0.057, 0.134, 1.02 |
No. of reflections | 6087 |
No. of parameters | 298 |
H-atom treatment | H-atom parameters constrained |
Δρmax, Δρmin (e Å−3) | 1.92, −0.77 |
Computer programs: CrysAlis CCD (Oxford Diffraction, 2009), CrysAlis PRO (Oxford Diffraction, 2009), CrysAlis RED (Oxford Diffraction, 2009), SHELXS97 (Sheldrick, 2008), SHELXL97 (Sheldrick, 2008), PLATON (Spek, 2009), SHELXTL (Sheldrick, 2008).
Acknowledgements
This research was funded by a CCSU–AAUP research grant.
References
Grushin, V. V. & Alper, H. (1993). Organometallics, 12, 1890–1901. CSD CrossRef CAS Web of Science Google Scholar
Lang, H., Taher, D., Walfort, B. & Pritzkow, H. (2006). J. Organomet. Chem. 691, 3834–3845. Web of Science CSD CrossRef CAS Google Scholar
Marshall, W. J., Young, R. J. & Grushin, V. V. (2001). Organometallics, 20, 523–533. Web of Science CSD CrossRef CAS Google Scholar
Oxford Diffraction (2009). CrysAlis CCD, CrysAlis PRO and CrysAlis RED. Oxford Diffraction Ltd, Yarnton, England. Google Scholar
Sheldrick, G. M. (2008). Acta Cryst. A64, 112–122. Web of Science CrossRef CAS IUCr Journals Google Scholar
Spek, A. L. (2009). Acta Cryst. D65, 148–155. Web of Science CrossRef CAS IUCr Journals Google Scholar
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The molecule of the title compound sits on a crystallographic inversion center; thereby requiring only half the molecule to be defined in the asymmetric unit and resulting in a trans- configuration. The metal centers are a slightly puckered square planar geometry. Like similar compounds containing bridging iodines, the iodines are not centered directly between the two metals; instead they have distances of 2.6709 (6) Å and 2.7486 (7) Å from the metal centers [Grushin & Alper, 1993; Marshall et al., 2001; & Lang et al., 2006]. The biphenyl ring is not planar; within the molecule one ring has an angle of 51.89 (39)° relative to the other. All other bond lengths and angles fall within normal values.