Supporting information
Crystallographic Information File (CIF) https://doi.org/10.1107/S1600536802001356/na6133sup1.cif | |
Structure factor file (CIF format) https://doi.org/10.1107/S1600536802001356/na6133Isup2.hkl |
CCDC reference: 180766
Key indicators
- Single-crystal X-ray study
- T = 293 K
- Mean (C-C) = 0.005 Å
- R factor = 0.035
- wR factor = 0.087
- Data-to-parameter ratio = 12.7
checkCIF results
No syntax errors found ADDSYM reports no extra symmetry
Data collection: XSCANS (Bruker, 1996); cell refinement: XSCANS (Bruker, 1996); data reduction: XSCANS (Bruker, 1996); program(s) used to solve structure: SHELXS86 (Sheldrick, 1990a); program(s) used to refine structure: SHELXL93 (Sheldrick, 1993); molecular graphics: SHELXTL/PC (Sheldrick, 1990b); software used to prepare material for publication: SHELXTL/PC (Sheldrick, 1990b) and SHELXL93.
[Cr(C14H10F5P)2(CO)4] | Z = 1 |
Mr = 772.44 | F(000) = 388 |
Triclinic, P1 | Dx = 1.566 Mg m−3 |
a = 8.1720 (3) Å | Mo Kα radiation, λ = 0.71073 Å |
b = 9.3069 (4) Å | Cell parameters from 100 reflections |
c = 11.8450 (5) Å | θ = 10.5–18.2° |
α = 110.015 (4)° | µ = 0.54 mm−1 |
β = 93.301 (4)° | T = 293 K |
γ = 102.208 (3)° | Trapezoidal plate, pale yellow |
V = 819.00 (6) Å3 | 0.31 × 0.25 × 0.19 mm |
Siemens Bruker P4 diffractometer | 2366 reflections with I > 2σ(I) |
Radiation source: normal-focus sealed tube | Rint = 0.017 |
Graphite monochromator | θmax = 25.0°, θmin = 1.9° |
θ/2θ scans | h = −9→1 |
Absorption correction: integration (XSCANS; Bruker, 1996) | k = −10→10 |
Tmin = 0.873, Tmax = 0.924 | l = −14→14 |
3507 measured reflections | 3 standard reflections every 100 reflections |
2847 independent reflections | intensity decay: ave. in σ(I)'s of 1.4% |
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)] = 0.035 | Hydrogen site location: inferred from neighbouring sites |
wR(F2) = 0.087 | H-atom parameters constrained |
S = 1.05 | w = 1/[σ2(Fo2) + (0.0408P)2 + 0.4223P] where P = (Fo2 + 2Fc2)/3 |
2842 reflections | (Δ/σ)max < 0.001 |
223 parameters | Δρmax = 0.30 e Å−3 |
0 restraints | Δρmin = −0.32 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 on F2 for ALL reflections except for 5 with very negative F2 or flagged by the user for potential systematic errors. Weighted R-factors wR and all goodnesses of fit S are based on F2, conventional R-factors R are based on F, with F set to zero for negative F2. The observed criterion of F2 > σ(F2) is used only for calculating R factor obs 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 | ||
Cr1 | 0.0000 | 0.0000 | 0.0000 | 0.0287 (2) | |
P1 | −0.06311 (7) | −0.21199 (7) | −0.18557 (5) | 0.0315 (2) | |
O1 | 0.3516 (2) | −0.0368 (3) | 0.0590 (2) | 0.0610 (5) | |
O2 | 0.1564 (3) | 0.2300 (2) | −0.1172 (2) | 0.0579 (5) | |
F1 | 0.0624 (2) | −0.4372 (2) | −0.3458 (2) | 0.0658 (5) | |
F2 | 0.2208 (2) | −0.3108 (2) | −0.1710 (2) | 0.0583 (4) | |
F3 | 0.1595 (3) | −0.1908 (4) | −0.4115 (3) | 0.1266 (11) | |
F4 | 0.3654 (3) | −0.2539 (3) | −0.3463 (2) | 0.0949 (7) | |
F5 | 0.2970 (3) | −0.0491 (3) | −0.2373 (2) | 0.1052 (9) | |
C1 | 0.2191 (3) | −0.0257 (3) | 0.0346 (2) | 0.0385 (5) | |
C2 | 0.0968 (3) | 0.1424 (3) | −0.0742 (2) | 0.0379 (5) | |
C3 | −0.1935 (3) | −0.3929 (3) | −0.1764 (2) | 0.0354 (5) | |
C4 | −0.3663 (3) | −0.4055 (3) | −0.1797 (2) | 0.0419 (6) | |
H4 | −0.4132 (3) | −0.3224 (3) | −0.1872 (2) | 0.080* | |
C5 | −0.4714 (4) | −0.5284 (3) | −0.1588 (3) | 0.0516 (7) | |
H5 | −0.5912 (4) | −0.5397 (3) | −0.1710 (3) | 0.080* | |
C6 | −0.4049 (4) | −0.6406 (3) | −0.1344 (3) | 0.0581 (8) | |
H6 | −0.4853 (4) | −0.7335 (3) | −0.1365 (3) | 0.080* | |
C7 | −0.2341 (4) | −0.6282 (4) | −0.1296 (3) | 0.0643 (9) | |
H7 | −0.1898 (4) | −0.6923 (4) | −0.0933 (3) | 0.080* | |
C8 | −0.1280 (4) | −0.5052 (3) | −0.1497 (3) | 0.0525 (7) | |
H8 | −0.0091 (4) | −0.4989 (3) | −0.1483 (3) | 0.080* | |
C9 | −0.1737 (3) | −0.2000 (3) | −0.3201 (2) | 0.0381 (5) | |
C10 | −0.1805 (4) | −0.0555 (3) | −0.3248 (3) | 0.0536 (7) | |
H10 | −0.1331 (4) | 0.0395 (3) | −0.2563 (3) | 0.080* | |
C11 | −0.2628 (5) | −0.0459 (4) | −0.4268 (3) | 0.0731 (10) | |
H11 | −0.2605 (5) | 0.0530 (4) | −0.4360 (3) | 0.080* | |
C12 | −0.3330 (5) | −0.1791 (4) | −0.5250 (3) | 0.0738 (10) | |
H12 | −0.3988 (5) | −0.1743 (4) | −0.5926 (3) | 0.080* | |
C13 | −0.3281 (4) | −0.3242 (4) | −0.5219 (3) | 0.0641 (8) | |
H13 | −0.3734 (4) | −0.4172 (4) | −0.5924 (3) | 0.080* | |
C14 | −0.2497 (4) | −0.3361 (3) | −0.4201 (2) | 0.0499 (7) | |
H14 | −0.2520 (4) | −0.4377 (3) | −0.4160 (2) | 0.080* | |
C15 | 0.1193 (3) | −0.2920 (3) | −0.2571 (2) | 0.0451 (6) | |
C16 | 0.2370 (4) | −0.1936 (4) | −0.3133 (3) | 0.0611 (8) |
U11 | U22 | U33 | U12 | U13 | U23 | |
Cr1 | 0.0285 (3) | 0.0273 (3) | 0.0294 (3) | 0.0033 (2) | 0.0024 (2) | 0.0116 (2) |
P1 | 0.0323 (3) | 0.0301 (3) | 0.0313 (3) | 0.0065 (2) | 0.0029 (2) | 0.0110 (2) |
O1 | 0.0382 (11) | 0.0767 (15) | 0.0747 (14) | 0.0185 (10) | 0.0032 (10) | 0.0340 (12) |
O2 | 0.0667 (13) | 0.0506 (11) | 0.0565 (12) | −0.0041 (10) | 0.0098 (10) | 0.0305 (10) |
F1 | 0.0646 (11) | 0.0530 (10) | 0.0636 (11) | 0.0170 (8) | 0.0185 (9) | −0.0015 (8) |
F2 | 0.0494 (9) | 0.0695 (11) | 0.0668 (11) | 0.0296 (8) | 0.0089 (8) | 0.0293 (9) |
F3 | 0.085 (2) | 0.228 (3) | 0.120 (2) | 0.032 (2) | 0.0348 (15) | 0.129 (2) |
F4 | 0.0724 (13) | 0.109 (2) | 0.120 (2) | 0.0391 (13) | 0.0603 (13) | 0.0453 (15) |
F5 | 0.106 (2) | 0.0634 (13) | 0.136 (2) | 0.0025 (12) | 0.072 (2) | 0.0248 (14) |
C1 | 0.0388 (14) | 0.0381 (13) | 0.0389 (13) | 0.0060 (11) | 0.0036 (11) | 0.0169 (11) |
C2 | 0.0378 (13) | 0.0362 (13) | 0.0358 (12) | 0.0041 (11) | 0.0022 (10) | 0.0116 (11) |
C3 | 0.0403 (13) | 0.0288 (12) | 0.0321 (12) | 0.0043 (10) | 0.0007 (10) | 0.0080 (9) |
C4 | 0.0412 (14) | 0.0418 (14) | 0.0411 (13) | 0.0063 (11) | 0.0014 (11) | 0.0162 (11) |
C5 | 0.0418 (15) | 0.054 (2) | 0.053 (2) | −0.0020 (13) | 0.0009 (12) | 0.0206 (13) |
C6 | 0.064 (2) | 0.0403 (15) | 0.064 (2) | −0.0040 (14) | 0.009 (2) | 0.0211 (14) |
C7 | 0.073 (2) | 0.044 (2) | 0.089 (2) | 0.016 (2) | 0.014 (2) | 0.038 (2) |
C8 | 0.051 (2) | 0.0424 (15) | 0.072 (2) | 0.0155 (13) | 0.0111 (14) | 0.0281 (14) |
C9 | 0.0390 (13) | 0.0426 (14) | 0.0325 (12) | 0.0082 (11) | 0.0029 (10) | 0.0148 (11) |
C10 | 0.070 (2) | 0.045 (2) | 0.0437 (15) | 0.0067 (14) | −0.0061 (14) | 0.0198 (12) |
C11 | 0.101 (3) | 0.064 (2) | 0.060 (2) | 0.016 (2) | −0.010 (2) | 0.036 (2) |
C12 | 0.094 (3) | 0.086 (3) | 0.044 (2) | 0.022 (2) | −0.015 (2) | 0.030 (2) |
C13 | 0.075 (2) | 0.068 (2) | 0.0360 (15) | 0.009 (2) | −0.0082 (14) | 0.0108 (14) |
C14 | 0.058 (2) | 0.048 (2) | 0.0366 (14) | 0.0091 (13) | −0.0010 (12) | 0.0110 (12) |
C15 | 0.0429 (14) | 0.0466 (15) | 0.0441 (14) | 0.0147 (12) | 0.0101 (12) | 0.0118 (12) |
C16 | 0.052 (2) | 0.075 (2) | 0.064 (2) | 0.020 (2) | 0.024 (2) | 0.029 (2) |
Cr1—C2i | 1.894 (2) | F5—C16 | 1.305 (4) |
Cr1—C2 | 1.894 (2) | C3—C8 | 1.387 (4) |
Cr1—C1 | 1.896 (3) | C3—C4 | 1.389 (4) |
Cr1—C1i | 1.896 (3) | C4—C5 | 1.382 (4) |
Cr1—P1i | 2.3368 (6) | C5—C6 | 1.378 (4) |
Cr1—P1 | 2.3368 (6) | C6—C7 | 1.372 (5) |
P1—C3 | 1.833 (2) | C7—C8 | 1.382 (4) |
P1—C9 | 1.835 (2) | C9—C10 | 1.377 (4) |
P1—C15 | 1.918 (3) | C9—C14 | 1.396 (4) |
O1—C1 | 1.139 (3) | C10—C11 | 1.387 (4) |
O2—C2 | 1.143 (3) | C11—C12 | 1.362 (5) |
F1—C15 | 1.361 (3) | C12—C13 | 1.372 (5) |
F2—C15 | 1.358 (3) | C13—C14 | 1.381 (4) |
F3—C16 | 1.302 (4) | C15—C16 | 1.525 (4) |
F4—C16 | 1.310 (4) | ||
C1—Cr1—P1 | 93.83 (8) | C5—C4—C3 | 120.9 (3) |
C1—Cr1—C2 | 88.55 (10) | C6—C5—C4 | 119.9 (3) |
C2—Cr1—P1 | 91.80 (7) | C7—C6—C5 | 119.6 (3) |
C3—P1—Cr1 | 113.08 (8) | C6—C7—C8 | 120.9 (3) |
C9—P1—Cr1 | 121.34 (8) | C7—C8—C3 | 120.2 (3) |
C15—P1—Cr1 | 118.45 (8) | C10—C9—C14 | 118.8 (2) |
C3—P1—C9 | 102.16 (11) | C10—C9—P1 | 120.3 (2) |
C3—P1—C15 | 99.58 (11) | C14—C9—P1 | 120.9 (2) |
C9—P1—C15 | 98.81 (11) | C9—C10—C11 | 120.5 (3) |
O1—C1—Cr1 | 177.7 (2) | C12—C11—C10 | 120.3 (3) |
O2—C2—Cr1 | 178.9 (2) | C11—C12—C13 | 120.1 (3) |
C2i—Cr1—C2 | 180.0 | C12—C13—C14 | 120.3 (3) |
C2i—Cr1—C1 | 91.45 (10) | C13—C14—C9 | 120.0 (3) |
C2i—Cr1—C1i | 88.55 (10) | F2—C15—F1 | 106.2 (2) |
C2—Cr1—C1i | 91.45 (10) | F2—C15—C16 | 105.4 (2) |
C1—Cr1—C1i | 180.0 | F1—C15—C16 | 105.6 (2) |
C2i—Cr1—P1i | 91.80 (7) | F2—C15—P1 | 109.0 (2) |
C2—Cr1—P1i | 88.20 (7) | F1—C15—P1 | 111.7 (2) |
C1—Cr1—P1i | 86.17 (8) | C16—C15—P1 | 118.1 (2) |
C1i—Cr1—P1i | 93.83 (8) | F3—C16—F5 | 108.9 (3) |
C2i—Cr1—P1 | 88.20 (7) | F3—C16—F4 | 106.0 (3) |
C1i—Cr1—P1 | 86.17 (8) | F5—C16—F4 | 107.8 (3) |
P1i—Cr1—P1 | 180.0 | F3—C16—C15 | 111.2 (3) |
C8—C3—C4 | 118.5 (2) | F5—C16—C15 | 111.5 (3) |
C8—C3—P1 | 123.9 (2) | F4—C16—C15 | 111.2 (3) |
C4—C3—P1 | 117.0 (2) | ||
C3—P1—Cr1—C1 | 99.5 (1) | C15—P1—Cr1—C1 | −16.4 (1) |
C9—P1—Cr1—C1 | −138.7 (1) |
Symmetry code: (i) −x, −y, −z. |