Supporting information
Crystallographic Information File (CIF) https://doi.org/10.1107/S160053680704620X/bt2515sup1.cif | |
Structure factor file (CIF format) https://doi.org/10.1107/S160053680704620X/bt2515Isup2.hkl |
CCDC reference: 672580
Key indicators
- Single-crystal X-ray study
- T = 150 K
- Mean (C-C) = 0.014 Å
- Disorder in solvent or counterion
- R factor = 0.056
- wR factor = 0.112
- Data-to-parameter ratio = 16.2
checkCIF/PLATON results
No syntax errors found
Alert level B PLAT366_ALERT_2_B Short? C(sp?)-C(sp?) Bond C1 - C2 ... 1.20 Ang.
Alert level C PLAT241_ALERT_2_C Check High Ueq as Compared to Neighbors for C15 PLAT244_ALERT_4_C Low 'Solvent' Ueq as Compared to Neighbors for C1S PLAT302_ALERT_4_C Anion/Solvent Disorder ......................... 11.00 Perc. PLAT320_ALERT_2_C Check Hybridisation of C1 in Main Residue . ? PLAT342_ALERT_3_C Low Bond Precision on C-C Bonds (x 1000) Ang ... 14 PLAT371_ALERT_2_C Long C(sp2)-C(sp1) Bond C2 - C3 ... 1.43 Ang. PLAT371_ALERT_2_C Long C(sp2)-C(sp1) Bond C6 - C9 ... 1.43 Ang. PLAT720_ALERT_4_C Number of Unusual/Non-Standard Label(s) ........ 2 PLAT731_ALERT_1_C Bond Calc 1.727(12), Rep 1.728(5) ...... 2.40 su-Ra CL3 -C1S 1.555 1.555 PLAT779_ALERT_2_C Suspect or Irrelevant (Bond) Angle in CIF ...... 33.70 Deg. C2S -CL5 -C2S 2.756 1.555 1.555 PLAT779_ALERT_2_C Suspect or Irrelevant (Bond) Angle in CIF ...... 33.60 Deg. C2S -CL4 -C2S 1.555 1.555 2.756 PLAT790_ALERT_4_C Centre of Gravity not Within Unit Cell: Resd. # 2 C H Cl3
Alert level G PLAT860_ALERT_3_G Note: Number of Least-Squares Restraints ....... 4
0 ALERT level A = In general: serious problem 1 ALERT level B = Potentially serious problem 12 ALERT level C = Check and explain 1 ALERT level G = General alerts; check 1 ALERT type 1 CIF construction/syntax error, inconsistent or missing data 7 ALERT type 2 Indicator that the structure model may be wrong or deficient 2 ALERT type 3 Indicator that the structure quality may be low 4 ALERT type 4 Improvement, methodology, query or suggestion 0 ALERT type 5 Informative message, check
PdI2 (11 mg, 0.031 mmol) and 1,4-bis-[(diphenylphosphanyl)-ethynyl]-benzene (15 mg, 0.030 mmol) was added to CDCl3 (0.6 ml). Crystals of the title compound was obtained after 2 days.
All hydrogen atoms were placed in calculated positions with C—H = 0.95 or 1.00 Å and were included in the refinement in the riding-motion approximation with Uiso(H) = 1.2Ueq(C). One of the CHCl3 solvent molecules is disordered over a twofold rotation axis. For each CHCl3 the three C—Cl distances were constrained to be equal with a standard uncertainty of 0.002Å [see: SADI command in SHELXTL (Sheldrick, 2001)]
Data collection: COLLECT (Nonius, 2002); cell refinement: DENZO-SMN (Otwinowski & Minor, 1997); data reduction: DENZO-SMN (Otwinowski & Minor, 1997); program(s) used to solve structure: SIR92 (Altomare et al., 1994); program(s) used to refine structure: SHELXTL (Sheldrick, 2001); molecular graphics: SHELXTL (Sheldrick, 2001); software used to prepare material for publication: SHELXTL (Sheldrick, 2001).
[Pd2I4(C34H24P2)2]·3CHCl3 | F(000) = 3976 |
Mr = 2067.45 | Dx = 1.790 Mg m−3 |
Monoclinic, C2/c | Mo Kα radiation, λ = 0.71073 Å |
Hall symbol: -C 2yc | Cell parameters from 19576 reflections |
a = 20.8960 (9) Å | θ = 2.6–25.0° |
b = 9.5920 (5) Å | µ = 2.52 mm−1 |
c = 38.832 (2) Å | T = 150 K |
β = 99.804 (3)° | Needle, colourless |
V = 7669.6 (7) Å3 | 0.14 × 0.06 × 0.02 mm |
Z = 4 |
Nonius KappaCCD diffractometer | 6672 independent reflections |
Radiation source: fine-focus sealed tube | 3732 reflections with I > 2σ(I) |
Graphite monochromator | Rint = 0.086 |
Detector resolution: 9 pixels mm-1 | θmax = 25.0°, θmin = 2.6° |
ϕ scans and ω scans with κ offsets | h = −24→24 |
Absorption correction: multi-scan (SORTAV; Blessing, 1995) | k = −11→11 |
Tmin = 0.827, Tmax = 0.958 | l = −45→46 |
19576 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)] = 0.056 | Hydrogen site location: inferred from neighbouring sites |
wR(F2) = 0.112 | H-atom parameters constrained |
S = 1.01 | w = 1/[σ2(Fo2) + (0.024P)2 + 42.7375P] where P = (Fo2 + 2Fc2)/3 |
6672 reflections | (Δ/σ)max = 0.002 |
411 parameters | Δρmax = 1.06 e Å−3 |
4 restraints | Δρmin = −0.91 e Å−3 |
[Pd2I4(C34H24P2)2]·3CHCl3 | V = 7669.6 (7) Å3 |
Mr = 2067.45 | Z = 4 |
Monoclinic, C2/c | Mo Kα radiation |
a = 20.8960 (9) Å | µ = 2.52 mm−1 |
b = 9.5920 (5) Å | T = 150 K |
c = 38.832 (2) Å | 0.14 × 0.06 × 0.02 mm |
β = 99.804 (3)° |
Nonius KappaCCD diffractometer | 6672 independent reflections |
Absorption correction: multi-scan (SORTAV; Blessing, 1995) | 3732 reflections with I > 2σ(I) |
Tmin = 0.827, Tmax = 0.958 | Rint = 0.086 |
19576 measured reflections |
R[F2 > 2σ(F2)] = 0.056 | 4 restraints |
wR(F2) = 0.112 | H-atom parameters constrained |
S = 1.01 | w = 1/[σ2(Fo2) + (0.024P)2 + 42.7375P] where P = (Fo2 + 2Fc2)/3 |
6672 reflections | Δρmax = 1.06 e Å−3 |
411 parameters | Δρmin = −0.91 e Å−3 |
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 | Occ. (<1) | |
Pd1 | 0.67135 (3) | 0.12571 (7) | 0.633756 (18) | 0.0337 (2) | |
I1 | 0.72848 (3) | −0.04250 (7) | 0.595490 (18) | 0.0489 (2) | |
I2 | 0.61881 (3) | 0.24764 (6) | 0.681462 (16) | 0.04193 (19) | |
P1 | 0.57291 (10) | 0.0364 (2) | 0.60639 (6) | 0.0338 (6) | |
P2 | 0.77171 (11) | 0.2254 (2) | 0.65447 (6) | 0.0363 (6) | |
C1 | 0.5693 (4) | 0.0548 (9) | 0.5615 (3) | 0.044 (3) | |
C2 | 0.5810 (4) | 0.0764 (9) | 0.5327 (2) | 0.040 (2) | |
C3 | 0.6019 (4) | 0.1060 (10) | 0.5002 (2) | 0.040 (2) | |
C4 | 0.6216 (5) | 0.2398 (11) | 0.4932 (3) | 0.061 (3) | |
H4A | 0.6192 | 0.3123 | 0.5096 | 0.073* | |
C5 | 0.6448 (5) | 0.2686 (11) | 0.4626 (3) | 0.059 (3) | |
H5A | 0.6577 | 0.3608 | 0.4580 | 0.071* | |
C6 | 0.6491 (4) | 0.1649 (10) | 0.4388 (2) | 0.043 (2) | |
C7 | 0.6299 (4) | 0.0311 (9) | 0.4456 (2) | 0.043 (2) | |
H7A | 0.6329 | −0.0411 | 0.4291 | 0.051* | |
C8 | 0.6064 (4) | 0.0008 (10) | 0.4760 (2) | 0.043 (2) | |
H8A | 0.5933 | −0.0915 | 0.4803 | 0.052* | |
C9 | 0.6710 (4) | 0.1963 (9) | 0.4067 (3) | 0.045 (3) | |
C10 | 0.6902 (4) | 0.2313 (9) | 0.3808 (2) | 0.039 (2) | |
C11 | 0.5605 (4) | −0.1473 (9) | 0.6139 (2) | 0.034 (2) | |
C12 | 0.5926 (4) | −0.2073 (10) | 0.6446 (2) | 0.045 (3) | |
H12A | 0.6227 | −0.1541 | 0.6604 | 0.054* | |
C13 | 0.5805 (4) | −0.3451 (10) | 0.6522 (3) | 0.047 (3) | |
H13A | 0.6024 | −0.3867 | 0.6731 | 0.056* | |
C14 | 0.5369 (5) | −0.4205 (10) | 0.6294 (3) | 0.053 (3) | |
H14A | 0.5283 | −0.5145 | 0.6348 | 0.063* | |
C15 | 0.5047 (5) | −0.3619 (11) | 0.5983 (3) | 0.064 (3) | |
H15A | 0.4745 | −0.4155 | 0.5826 | 0.077* | |
C16 | 0.5172 (4) | −0.2262 (9) | 0.5908 (3) | 0.044 (3) | |
H16A | 0.4960 | −0.1858 | 0.5695 | 0.053* | |
C21 | 0.4980 (4) | 0.1166 (9) | 0.6141 (2) | 0.034 (2) | |
C22 | 0.4672 (4) | 0.0657 (10) | 0.6404 (2) | 0.045 (3) | |
H22A | 0.4846 | −0.0130 | 0.6536 | 0.054* | |
C23 | 0.4114 (4) | 0.1278 (11) | 0.6476 (3) | 0.051 (3) | |
H23A | 0.3904 | 0.0911 | 0.6655 | 0.061* | |
C24 | 0.3862 (5) | 0.2435 (11) | 0.6288 (3) | 0.061 (3) | |
H24A | 0.3479 | 0.2864 | 0.6339 | 0.073* | |
C25 | 0.4161 (4) | 0.2965 (9) | 0.6030 (3) | 0.057 (3) | |
H25A | 0.3988 | 0.3763 | 0.5903 | 0.069* | |
C26 | 0.4718 (4) | 0.2337 (9) | 0.5956 (2) | 0.045 (2) | |
H26A | 0.4924 | 0.2708 | 0.5776 | 0.053* | |
C31 | 0.7750 (4) | 0.3889 (10) | 0.6778 (3) | 0.041 (2) | |
C32 | 0.8069 (5) | 0.4039 (11) | 0.7117 (3) | 0.055 (3) | |
H32A | 0.8268 | 0.3249 | 0.7238 | 0.066* | |
C33 | 0.8103 (5) | 0.5302 (14) | 0.7282 (3) | 0.076 (4) | |
H33A | 0.8324 | 0.5386 | 0.7517 | 0.092* | |
C34 | 0.7823 (5) | 0.6428 (14) | 0.7111 (4) | 0.080 (4) | |
H34A | 0.7843 | 0.7297 | 0.7230 | 0.096* | |
C35 | 0.7511 (5) | 0.6362 (12) | 0.6771 (4) | 0.068 (4) | |
H35A | 0.7321 | 0.7168 | 0.6654 | 0.082* | |
C36 | 0.7483 (4) | 0.5061 (11) | 0.6601 (3) | 0.053 (3) | |
H36A | 0.7279 | 0.4988 | 0.6364 | 0.063* | |
C41 | 0.8270 (4) | 0.1125 (9) | 0.6827 (2) | 0.038 (2) | |
C42 | 0.8062 (5) | 0.0596 (10) | 0.7121 (3) | 0.056 (3) | |
H42A | 0.7633 | 0.0772 | 0.7160 | 0.067* | |
C43 | 0.8482 (6) | −0.0186 (11) | 0.7354 (3) | 0.067 (3) | |
H43A | 0.8343 | −0.0508 | 0.7561 | 0.080* | |
C44 | 0.9086 (6) | −0.0514 (11) | 0.7300 (3) | 0.071 (3) | |
H44A | 0.9364 | −0.1086 | 0.7461 | 0.085* | |
C45 | 0.9286 (5) | 0.0010 (11) | 0.7005 (3) | 0.066 (3) | |
H45A | 0.9710 | −0.0205 | 0.6963 | 0.080* | |
C46 | 0.8881 (5) | 0.0846 (10) | 0.6767 (3) | 0.053 (3) | |
H46A | 0.9029 | 0.1214 | 0.6567 | 0.064* | |
Cl1 | 0.56608 (16) | 0.6246 (3) | 0.51296 (10) | 0.0983 (11) | |
Cl2 | 0.7013 (2) | 0.6345 (6) | 0.5168 (2) | 0.255 (4) | |
Cl3 | 0.6484 (3) | 0.4900 (7) | 0.56931 (13) | 0.206 (3) | |
C1S | 0.63949 (19) | 0.6309 (12) | 0.5412 (2) | 0.150 (8) | |
H1SA | 0.6412 | 0.7185 | 0.5553 | 0.180* | |
Cl5 | 1.03790 (18) | −0.6728 (4) | 0.72255 (9) | 0.1068 (12) | |
Cl4 | 1.0000 | −0.4169 (5) | 0.7500 | 0.125 (2) | |
C2S | 0.9795 (9) | −0.5888 (12) | 0.7413 (6) | 0.110 (13) | 0.50 |
H2SA | 0.9404 | −0.5888 | 0.7242 | 0.132* | 0.50 |
U11 | U22 | U33 | U12 | U13 | U23 | |
Pd1 | 0.0336 (4) | 0.0372 (4) | 0.0304 (4) | −0.0009 (3) | 0.0059 (3) | −0.0015 (4) |
I1 | 0.0401 (4) | 0.0537 (4) | 0.0545 (5) | 0.0011 (3) | 0.0122 (3) | −0.0148 (4) |
I2 | 0.0428 (4) | 0.0494 (4) | 0.0349 (4) | −0.0031 (3) | 0.0102 (3) | −0.0075 (3) |
P1 | 0.0339 (13) | 0.0402 (15) | 0.0282 (15) | −0.0027 (11) | 0.0075 (11) | −0.0005 (12) |
P2 | 0.0398 (14) | 0.0423 (16) | 0.0275 (14) | −0.0021 (12) | 0.0076 (12) | 0.0013 (12) |
C1 | 0.045 (6) | 0.042 (6) | 0.048 (7) | −0.003 (5) | 0.015 (5) | −0.009 (5) |
C2 | 0.043 (6) | 0.041 (6) | 0.037 (6) | −0.012 (5) | 0.009 (5) | 0.003 (5) |
C3 | 0.051 (6) | 0.044 (6) | 0.027 (6) | −0.006 (5) | 0.012 (5) | 0.001 (5) |
C4 | 0.101 (9) | 0.050 (7) | 0.036 (7) | −0.014 (6) | 0.024 (6) | −0.004 (5) |
C5 | 0.081 (8) | 0.058 (7) | 0.044 (7) | −0.025 (6) | 0.023 (6) | −0.002 (6) |
C6 | 0.050 (6) | 0.044 (6) | 0.036 (6) | −0.009 (5) | 0.009 (5) | −0.001 (5) |
C7 | 0.051 (6) | 0.044 (6) | 0.033 (6) | −0.014 (5) | 0.009 (5) | −0.001 (5) |
C8 | 0.047 (6) | 0.045 (6) | 0.038 (6) | −0.008 (5) | 0.010 (5) | 0.007 (5) |
C9 | 0.039 (6) | 0.051 (6) | 0.045 (7) | −0.012 (5) | 0.009 (5) | 0.006 (5) |
C10 | 0.037 (5) | 0.040 (6) | 0.042 (6) | −0.016 (5) | 0.010 (5) | −0.001 (5) |
C11 | 0.032 (5) | 0.041 (6) | 0.033 (6) | −0.002 (5) | 0.012 (5) | −0.003 (5) |
C12 | 0.054 (6) | 0.048 (7) | 0.036 (7) | −0.011 (5) | 0.012 (5) | 0.000 (5) |
C13 | 0.038 (6) | 0.047 (7) | 0.052 (7) | 0.000 (5) | 0.002 (5) | 0.004 (6) |
C14 | 0.062 (7) | 0.033 (6) | 0.065 (8) | −0.005 (5) | 0.018 (6) | 0.012 (6) |
C15 | 0.068 (7) | 0.043 (7) | 0.079 (10) | −0.021 (6) | 0.007 (7) | −0.009 (7) |
C16 | 0.043 (6) | 0.033 (6) | 0.054 (7) | −0.009 (5) | 0.000 (5) | 0.001 (5) |
C21 | 0.034 (5) | 0.034 (6) | 0.035 (6) | 0.000 (4) | 0.006 (5) | 0.001 (5) |
C22 | 0.045 (6) | 0.055 (6) | 0.040 (6) | −0.002 (5) | 0.023 (5) | −0.004 (5) |
C23 | 0.050 (6) | 0.060 (7) | 0.043 (7) | −0.003 (6) | 0.009 (5) | −0.005 (6) |
C24 | 0.038 (6) | 0.056 (7) | 0.089 (9) | −0.005 (6) | 0.012 (6) | −0.018 (7) |
C25 | 0.035 (6) | 0.034 (6) | 0.102 (10) | 0.006 (5) | 0.006 (6) | 0.006 (6) |
C26 | 0.044 (6) | 0.039 (6) | 0.051 (7) | −0.009 (5) | 0.010 (5) | −0.001 (5) |
C31 | 0.040 (6) | 0.054 (7) | 0.029 (6) | −0.014 (5) | 0.003 (5) | 0.001 (5) |
C32 | 0.059 (7) | 0.048 (7) | 0.061 (8) | 0.000 (5) | 0.017 (6) | −0.014 (6) |
C33 | 0.067 (8) | 0.091 (10) | 0.071 (10) | 0.005 (8) | 0.012 (7) | −0.029 (9) |
C34 | 0.047 (8) | 0.072 (10) | 0.126 (14) | −0.017 (7) | 0.026 (8) | −0.049 (10) |
C35 | 0.047 (7) | 0.052 (8) | 0.111 (12) | −0.007 (6) | 0.025 (8) | 0.002 (8) |
C36 | 0.046 (6) | 0.053 (7) | 0.059 (8) | −0.011 (6) | 0.006 (6) | 0.001 (6) |
C41 | 0.036 (5) | 0.039 (6) | 0.037 (6) | −0.001 (5) | −0.001 (5) | 0.001 (5) |
C42 | 0.052 (6) | 0.064 (7) | 0.049 (7) | −0.005 (6) | 0.004 (6) | 0.024 (6) |
C43 | 0.071 (8) | 0.064 (8) | 0.056 (8) | −0.009 (7) | −0.017 (7) | 0.032 (6) |
C44 | 0.064 (8) | 0.058 (8) | 0.080 (10) | 0.004 (7) | −0.021 (7) | 0.023 (7) |
C45 | 0.050 (7) | 0.074 (9) | 0.073 (9) | 0.026 (6) | 0.005 (7) | 0.000 (7) |
C46 | 0.049 (6) | 0.062 (7) | 0.048 (7) | 0.008 (6) | 0.005 (6) | −0.002 (6) |
Cl1 | 0.106 (3) | 0.084 (2) | 0.103 (3) | −0.009 (2) | 0.012 (2) | −0.011 (2) |
Cl2 | 0.114 (4) | 0.210 (6) | 0.467 (11) | −0.044 (4) | 0.127 (5) | −0.152 (7) |
Cl3 | 0.205 (5) | 0.282 (7) | 0.101 (4) | 0.136 (5) | −0.064 (4) | −0.085 (4) |
C1S | 0.059 (9) | 0.165 (16) | 0.21 (2) | −0.002 (10) | −0.009 (11) | −0.137 (15) |
Cl5 | 0.127 (3) | 0.115 (3) | 0.084 (3) | 0.009 (2) | 0.033 (2) | −0.017 (2) |
Cl4 | 0.150 (5) | 0.084 (4) | 0.159 (6) | 0.000 | 0.081 (4) | 0.000 |
C2S | 0.042 (18) | 0.12 (2) | 0.18 (4) | 0.011 (13) | 0.05 (2) | 0.10 (2) |
Pd1—P1 | 2.313 (2) | C23—C24 | 1.383 (13) |
Pd1—P2 | 2.321 (2) | C23—H23A | 0.9500 |
Pd1—I2 | 2.5880 (9) | C24—C25 | 1.365 (13) |
Pd1—I1 | 2.6155 (9) | C24—H24A | 0.9500 |
P1—C1 | 1.743 (10) | C25—C26 | 1.384 (11) |
P1—C11 | 1.812 (9) | C25—H25A | 0.9500 |
P1—C21 | 1.813 (8) | C26—H26A | 0.9500 |
P2—C10i | 1.749 (9) | C31—C32 | 1.379 (12) |
P2—C31 | 1.806 (10) | C31—C36 | 1.384 (12) |
P2—C41 | 1.809 (9) | C32—C33 | 1.367 (13) |
C1—C2 | 1.202 (11) | C32—H32A | 0.9500 |
C2—C3 | 1.434 (12) | C33—C34 | 1.349 (16) |
C3—C4 | 1.388 (12) | C33—H33A | 0.9500 |
C3—C8 | 1.393 (11) | C34—C35 | 1.370 (15) |
C4—C5 | 1.388 (12) | C34—H34A | 0.9500 |
C4—H4A | 0.9500 | C35—C36 | 1.408 (13) |
C5—C6 | 1.371 (12) | C35—H35A | 0.9500 |
C5—H5A | 0.9500 | C36—H36A | 0.9500 |
C6—C7 | 1.384 (11) | C41—C46 | 1.364 (11) |
C6—C9 | 1.430 (12) | C41—C42 | 1.386 (12) |
C7—C8 | 1.384 (11) | C42—C43 | 1.373 (12) |
C7—H7A | 0.9500 | C42—H42A | 0.9500 |
C8—H8A | 0.9500 | C43—C44 | 1.351 (13) |
C9—C10 | 1.191 (11) | C43—H43A | 0.9500 |
C10—P2i | 1.749 (9) | C44—C45 | 1.381 (14) |
C11—C16 | 1.386 (11) | C44—H44A | 0.9500 |
C11—C12 | 1.390 (11) | C45—C46 | 1.396 (13) |
C12—C13 | 1.386 (12) | C45—H45A | 0.9500 |
C12—H12A | 0.9500 | C46—H46A | 0.9500 |
C13—C14 | 1.363 (12) | Cl1—C1S | 1.728 (5) |
C13—H13A | 0.9500 | Cl2—C1S | 1.728 (5) |
C14—C15 | 1.396 (13) | Cl3—C1S | 1.728 (5) |
C14—H14A | 0.9500 | C1S—H1SA | 1.0000 |
C15—C16 | 1.370 (12) | Cl5—C2Sii | 1.71 (2) |
C15—H15A | 0.9500 | Cl5—C2S | 1.723 (11) |
C16—H16A | 0.9500 | Cl4—C2S | 1.723 (11) |
C21—C22 | 1.384 (11) | Cl4—C2Sii | 1.723 (11) |
C21—C26 | 1.395 (11) | C2S—C2Sii | 1.00 (4) |
C22—C23 | 1.379 (11) | C2S—Cl5ii | 1.71 (2) |
C22—H22A | 0.9500 | C2S—H2SA | 0.9600 |
P1—Pd1—P2 | 172.93 (9) | C22—C23—H23A | 120.1 |
P1—Pd1—I2 | 92.51 (6) | C24—C23—H23A | 120.1 |
P2—Pd1—I2 | 91.96 (6) | C25—C24—C23 | 120.3 (9) |
P1—Pd1—I1 | 88.09 (6) | C25—C24—H24A | 119.8 |
P2—Pd1—I1 | 88.75 (6) | C23—C24—H24A | 119.8 |
I2—Pd1—I1 | 167.36 (4) | C24—C25—C26 | 119.9 (10) |
C1—P1—C11 | 106.1 (4) | C24—C25—H25A | 120.1 |
C1—P1—C21 | 103.4 (4) | C26—C25—H25A | 120.1 |
C11—P1—C21 | 103.6 (4) | C25—C26—C21 | 120.8 (9) |
C1—P1—Pd1 | 107.8 (3) | C25—C26—H26A | 119.6 |
C11—P1—Pd1 | 115.3 (3) | C21—C26—H26A | 119.6 |
C21—P1—Pd1 | 119.5 (3) | C32—C31—C36 | 118.5 (10) |
C10i—P2—C31 | 101.7 (4) | C32—C31—P2 | 122.7 (8) |
C10i—P2—C41 | 106.7 (4) | C36—C31—P2 | 118.6 (8) |
C31—P2—C41 | 104.5 (4) | C33—C32—C31 | 121.3 (11) |
C10i—P2—Pd1 | 109.3 (3) | C33—C32—H32A | 119.4 |
C31—P2—Pd1 | 119.1 (3) | C31—C32—H32A | 119.4 |
C41—P2—Pd1 | 114.2 (3) | C34—C33—C32 | 119.6 (12) |
C2—C1—P1 | 165.4 (9) | C34—C33—H33A | 120.2 |
C1—C2—C3 | 173.7 (10) | C32—C33—H33A | 120.2 |
C4—C3—C8 | 118.9 (8) | C33—C34—C35 | 122.2 (13) |
C4—C3—C2 | 120.0 (8) | C33—C34—H34A | 118.9 |
C8—C3—C2 | 121.1 (8) | C35—C34—H34A | 118.9 |
C3—C4—C5 | 120.6 (9) | C34—C35—C36 | 117.9 (12) |
C3—C4—H4A | 119.7 | C34—C35—H35A | 121.0 |
C5—C4—H4A | 119.7 | C36—C35—H35A | 121.0 |
C6—C5—C4 | 120.4 (9) | C31—C36—C35 | 120.4 (10) |
C6—C5—H5A | 119.8 | C31—C36—H36A | 119.8 |
C4—C5—H5A | 119.8 | C35—C36—H36A | 119.8 |
C5—C6—C7 | 119.3 (9) | C46—C41—C42 | 120.2 (9) |
C5—C6—C9 | 120.1 (9) | C46—C41—P2 | 122.3 (7) |
C7—C6—C9 | 120.5 (9) | C42—C41—P2 | 117.4 (7) |
C6—C7—C8 | 120.9 (9) | C43—C42—C41 | 119.3 (10) |
C6—C7—H7A | 119.5 | C43—C42—H42A | 120.3 |
C8—C7—H7A | 119.5 | C41—C42—H42A | 120.3 |
C7—C8—C3 | 119.8 (8) | C44—C43—C42 | 122.2 (11) |
C7—C8—H8A | 120.1 | C44—C43—H43A | 118.9 |
C3—C8—H8A | 120.1 | C42—C43—H43A | 118.9 |
C10—C9—C6 | 175.6 (10) | C43—C44—C45 | 117.9 (10) |
C9—C10—P2i | 172.5 (9) | C43—C44—H44A | 121.0 |
C16—C11—C12 | 119.8 (8) | C45—C44—H44A | 121.0 |
C16—C11—P1 | 121.5 (7) | C44—C45—C46 | 121.6 (10) |
C12—C11—P1 | 118.7 (7) | C44—C45—H45A | 119.2 |
C13—C12—C11 | 119.9 (9) | C46—C45—H45A | 119.2 |
C13—C12—H12A | 120.1 | C41—C46—C45 | 118.7 (10) |
C11—C12—H12A | 120.1 | C41—C46—H46A | 120.6 |
C14—C13—C12 | 119.6 (10) | C45—C46—H46A | 120.6 |
C14—C13—H13A | 120.2 | Cl2—C1S—Cl1 | 108.6 (5) |
C12—C13—H13A | 120.2 | Cl2—C1S—Cl3 | 110.6 (6) |
C13—C14—C15 | 121.1 (9) | Cl1—C1S—Cl3 | 111.2 (5) |
C13—C14—H14A | 119.4 | Cl2—C1S—H1SA | 108.8 |
C15—C14—H14A | 119.4 | Cl1—C1S—H1SA | 108.8 |
C16—C15—C14 | 119.1 (10) | Cl3—C1S—H1SA | 108.8 |
C16—C15—H15A | 120.5 | C2Sii—Cl5—C2S | 33.7 (14) |
C14—C15—H15A | 120.5 | C2S—Cl4—C2Sii | 33.6 (15) |
C15—C16—C11 | 120.5 (10) | C2Sii—C2S—Cl5ii | 74 (2) |
C15—C16—H16A | 119.8 | C2Sii—C2S—Cl4 | 73.2 (7) |
C11—C16—H16A | 119.8 | Cl5ii—C2S—Cl4 | 111.7 (10) |
C22—C21—C26 | 118.2 (8) | C2Sii—C2S—Cl5 | 72.5 (17) |
C22—C21—P1 | 119.7 (7) | Cl5ii—C2S—Cl5 | 113.0 (10) |
C26—C21—P1 | 122.0 (7) | Cl4—C2S—Cl5 | 111.2 (10) |
C23—C22—C21 | 121.0 (9) | C2Sii—C2S—H2SA | 179.2 |
C23—C22—H22A | 119.5 | Cl5ii—C2S—H2SA | 106.9 |
C21—C22—H22A | 119.5 | Cl4—C2S—H2SA | 106.8 |
C22—C23—C24 | 119.8 (9) | Cl5—C2S—H2SA | 106.8 |
Symmetry codes: (i) −x+3/2, −y+1/2, −z+1; (ii) −x+2, y, −z+3/2. |
Experimental details
Crystal data | |
Chemical formula | [Pd2I4(C34H24P2)2]·3CHCl3 |
Mr | 2067.45 |
Crystal system, space group | Monoclinic, C2/c |
Temperature (K) | 150 |
a, b, c (Å) | 20.8960 (9), 9.5920 (5), 38.832 (2) |
β (°) | 99.804 (3) |
V (Å3) | 7669.6 (7) |
Z | 4 |
Radiation type | Mo Kα |
µ (mm−1) | 2.52 |
Crystal size (mm) | 0.14 × 0.06 × 0.02 |
Data collection | |
Diffractometer | Nonius KappaCCD diffractometer |
Absorption correction | Multi-scan (SORTAV; Blessing, 1995) |
Tmin, Tmax | 0.827, 0.958 |
No. of measured, independent and observed [I > 2σ(I)] reflections | 19576, 6672, 3732 |
Rint | 0.086 |
(sin θ/λ)max (Å−1) | 0.595 |
Refinement | |
R[F2 > 2σ(F2)], wR(F2), S | 0.056, 0.112, 1.01 |
No. of reflections | 6672 |
No. of parameters | 411 |
No. of restraints | 4 |
H-atom treatment | H-atom parameters constrained |
w = 1/[σ2(Fo2) + (0.024P)2 + 42.7375P] where P = (Fo2 + 2Fc2)/3 | |
Δρmax, Δρmin (e Å−3) | 1.06, −0.91 |
Computer programs: COLLECT (Nonius, 2002), DENZO-SMN (Otwinowski & Minor, 1997), SIR92 (Altomare et al., 1994), SHELXTL (Sheldrick, 2001).
The bidentate phosphane ligand used in this work has been previously found to form a triangle when reacted with PtCl2 (Baumgartner et al., 2002). In this work, we report the formation of a rectangle using PdI2 as the metal source. The Pd centres in the title compound exhibit a slightly distorted square planar geometry, where the P—Pd—I angles deviate from 90° by less than 3°.