Supporting information
Crystallographic Information File (CIF) https://doi.org/10.1107/S1600536803024292/cv6248sup1.cif | |
Structure factor file (CIF format) https://doi.org/10.1107/S1600536803024292/cv6248Isup2.hkl |
CCDC reference: 226686
Data collection: SMART (Bruker, 1997-2000); cell refinement: SAINT-Plus (Bruker, 1997-1999); data reduction: SAINT-Plus; program(s) used to solve structure: SHELXS97 (Sheldrick, 1997); program(s) used to refine structure: SHELXL97 (Sheldrick, 1997); molecular graphics: SHELXL97; software used to prepare material for publication: SHELXL97.
[Cr(C9H12O3)(CO)3] | Dx = 1.625 Mg m−3 |
Mr = 304.22 | Mo Kα radiation, λ = 0.71073 Å |
Trigonal, R3c | Cell parameters from 5768 reflections |
a = 12.6892 (9) Å | θ = 2.4–28.4° |
c = 13.3798 (19) Å | µ = 0.94 mm−1 |
V = 1865.7 (3) Å3 | T = 100 K |
Z = 6 | Block, colourless |
F(000) = 936 | 0.56 × 0.20 × 0.16 mm |
Bruker AXS SMART APEX CCD diffractometer | 1040 independent reflections |
Radiation source: fine-focus sealed tube | 1038 reflections with I > 2σ(I) |
Graphite monochromator | Rint = 0.032 |
ω scans | θmax = 28.4°, θmin = 3.2° |
Absorption correction: multi-scan (SADABS in SAINT-Plus; Bruker, 1997-1999) | h = −16→16 |
Tmin = 0.568, Tmax = 0.86 | k = −16→16 |
5069 measured reflections | l = −17→17 |
Refinement on F2 | Secondary atom site location: difference Fourier map |
Least-squares matrix: full | Hydrogen site location: inferred from neighbouring sites |
R[F2 > 2σ(F2)] = 0.026 | H atoms treated by a mixture of independent and constrained refinement |
wR(F2) = 0.069 | w = 1/[σ2(Fo2) + (0.0478P)2 + 0.4118P] where P = (Fo2 + 2Fc2)/3 |
S = 1.07 | (Δ/σ)max < 0.001 |
1040 reflections | Δρmax = 0.54 e Å−3 |
64 parameters | Δρmin = −0.68 e Å−3 |
1 restraint | Absolute structure: Flack (1983), 510 Friedel pairs [please check] |
Primary atom site location: structure-invariant direct methods | Absolute structure parameter: 0.12 (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 | ||
Cr1 | 0.0000 | 0.0000 | −0.03180 (7) | 0.00963 (13) | |
C1 | 0.07085 (12) | 0.12933 (16) | 0.09836 (15) | 0.0116 (3) | |
C2 | 0.12818 (17) | 0.05848 (12) | 0.10119 (14) | 0.0120 (3) | |
C3 | 0.32426 (11) | 0.23496 (10) | 0.10977 (10) | 0.0166 (2) | |
H3A | 0.2990 | 0.2653 | 0.1670 | 0.025* | |
H3B | 0.3153 | 0.2715 | 0.0481 | 0.025* | |
H3C | 0.4096 | 0.2568 | 0.1180 | 0.025* | |
C4 | −0.08832 (15) | −0.13608 (15) | −0.11035 (11) | 0.0147 (2) | |
O2 | −0.14375 (11) | −0.22219 (10) | −0.15796 (8) | 0.0218 (2) | |
O1 | 0.24923 (10) | 0.10457 (10) | 0.10416 (8) | 0.0145 (2) | |
H1 | 0.1199 (19) | 0.217 (3) | 0.091 (2) | 0.015 (6)* |
U11 | U22 | U33 | U12 | U13 | U23 | |
Cr1 | 0.00922 (15) | 0.00922 (15) | 0.01047 (19) | 0.00461 (7) | 0.000 | 0.000 |
C1 | 0.0117 (6) | 0.0101 (7) | 0.0129 (7) | 0.0053 (4) | −0.0013 (4) | −0.0024 (6) |
C2 | 0.0104 (7) | 0.0122 (6) | 0.0123 (7) | 0.0049 (4) | −0.0008 (5) | −0.0001 (4) |
C3 | 0.0116 (5) | 0.0118 (5) | 0.0224 (5) | 0.0028 (5) | −0.0003 (4) | −0.0014 (4) |
C4 | 0.0137 (6) | 0.0153 (6) | 0.0152 (5) | 0.0074 (6) | 0.0008 (5) | −0.0006 (4) |
O2 | 0.0191 (5) | 0.0193 (5) | 0.0226 (5) | 0.0062 (5) | −0.0038 (4) | −0.0079 (4) |
O1 | 0.0086 (4) | 0.0127 (4) | 0.0202 (5) | 0.0038 (4) | −0.0020 (3) | −0.0010 (4) |
Cr1—C4 | 1.8459 (17) | C1—C2i | 1.4231 (18) |
Cr1—C4i | 1.8459 (17) | C1—H1 | 0.97 (3) |
Cr1—C4ii | 1.8459 (17) | C2—O1 | 1.343 (2) |
Cr1—C1 | 2.2491 (18) | C2—C1ii | 1.4231 (18) |
Cr1—C1ii | 2.2491 (18) | C3—O1 | 1.4402 (15) |
Cr1—C1i | 2.2491 (18) | C3—H3A | 0.9800 |
Cr1—C2 | 2.2705 (18) | C3—H3B | 0.9800 |
Cr1—C2i | 2.2705 (18) | C3—H3C | 0.9800 |
Cr1—C2ii | 2.2705 (18) | C4—O2 | 1.1515 (19) |
C1—C2 | 1.4118 (18) | ||
C4—Cr1—C4i | 90.78 (8) | C4—Cr1—C2ii | 86.51 (7) |
C4—Cr1—C4ii | 90.78 (8) | C4i—Cr1—C2ii | 130.30 (6) |
C4i—Cr1—C4ii | 90.78 (8) | C4ii—Cr1—C2ii | 138.82 (6) |
C4—Cr1—C1 | 163.27 (7) | C1—Cr1—C2ii | 77.66 (7) |
C4i—Cr1—C1 | 103.55 (7) | C1ii—Cr1—C2ii | 36.40 (4) |
C4ii—Cr1—C1 | 97.51 (7) | C1i—Cr1—C2ii | 36.70 (4) |
C4—Cr1—C1ii | 103.55 (7) | C2—Cr1—C2ii | 65.09 (8) |
C4i—Cr1—C1ii | 97.51 (7) | C2i—Cr1—C2ii | 65.09 (8) |
C4ii—Cr1—C1ii | 163.27 (7) | C2—C1—C2i | 119.03 (17) |
C1—Cr1—C1ii | 66.47 (8) | C2—C1—Cr1 | 72.63 (10) |
C4—Cr1—C1i | 97.51 (7) | C2i—C1—Cr1 | 72.47 (10) |
C4i—Cr1—C1i | 163.27 (7) | C2—C1—H1 | 119.4 (12) |
C4ii—Cr1—C1i | 103.55 (7) | C2i—C1—H1 | 121.5 (12) |
C1—Cr1—C1i | 66.47 (8) | Cr1—C1—H1 | 123.2 (17) |
C1ii—Cr1—C1i | 66.47 (8) | O1—C2—C1 | 124.38 (13) |
C4—Cr1—C2 | 138.82 (6) | O1—C2—C1ii | 114.77 (12) |
C4i—Cr1—C2 | 86.51 (7) | C1—C2—C1ii | 120.83 (17) |
C4ii—Cr1—C2 | 130.30 (6) | O1—C2—Cr1 | 129.93 (13) |
C1—Cr1—C2 | 36.40 (4) | C1—C2—Cr1 | 70.98 (10) |
C1ii—Cr1—C2 | 36.70 (4) | C1ii—C2—Cr1 | 70.83 (10) |
C1i—Cr1—C2 | 77.66 (7) | O1—C3—H3A | 109.5 |
C4—Cr1—C2i | 130.30 (6) | O1—C3—H3B | 109.5 |
C4i—Cr1—C2i | 138.82 (6) | H3A—C3—H3B | 109.5 |
C4ii—Cr1—C2i | 86.51 (7) | O1—C3—H3C | 109.5 |
C1—Cr1—C2i | 36.70 (4) | H3A—C3—H3C | 109.5 |
C1ii—Cr1—C2i | 77.66 (7) | H3B—C3—H3C | 109.5 |
C1i—Cr1—C2i | 36.40 (4) | O2—C4—Cr1 | 178.85 (15) |
C2—Cr1—C2i | 65.09 (8) | C2—O1—C3 | 117.19 (11) |
C4—Cr1—C1—C2 | 83.9 (2) | C1—Cr1—C2—O1 | −119.36 (16) |
C4i—Cr1—C1—C2 | −64.39 (11) | C1ii—Cr1—C2—O1 | 106.71 (14) |
C4ii—Cr1—C1—C2 | −157.02 (11) | C1i—Cr1—C2—O1 | 173.73 (12) |
C1ii—Cr1—C1—C2 | 28.00 (11) | C2i—Cr1—C2—O1 | −150.07 (13) |
C1i—Cr1—C1—C2 | 101.42 (9) | C2ii—Cr1—C2—O1 | 137.17 (14) |
C2i—Cr1—C1—C2 | 129.20 (19) | C4—Cr1—C2—C1 | −154.23 (11) |
C2ii—Cr1—C1—C2 | 64.54 (9) | C4i—Cr1—C2—C1 | 118.56 (11) |
C4—Cr1—C1—C2i | −45.3 (2) | C4ii—Cr1—C2—C1 | 30.49 (15) |
C4i—Cr1—C1—C2i | 166.41 (11) | C1ii—Cr1—C2—C1 | −133.94 (18) |
C4ii—Cr1—C1—C2i | 73.78 (11) | C1i—Cr1—C2—C1 | −66.92 (9) |
C1ii—Cr1—C1—C2i | −101.20 (8) | C2i—Cr1—C2—C1 | −30.71 (11) |
C1i—Cr1—C1—C2i | −27.78 (10) | C2ii—Cr1—C2—C1 | −103.47 (8) |
C2—Cr1—C1—C2i | −129.20 (19) | C4—Cr1—C2—C1ii | −20.30 (17) |
C2ii—Cr1—C1—C2i | −64.66 (10) | C4i—Cr1—C2—C1ii | −107.50 (11) |
C2i—C1—C2—O1 | −176.40 (11) | C4ii—Cr1—C2—C1ii | 164.43 (10) |
Cr1—C1—C2—O1 | 125.92 (18) | C1—Cr1—C2—C1ii | 133.94 (18) |
C2i—C1—C2—C1ii | 5.3 (4) | C1i—Cr1—C2—C1ii | 67.02 (9) |
Cr1—C1—C2—C1ii | −52.4 (2) | C2i—Cr1—C2—C1ii | 103.23 (9) |
C2i—C1—C2—Cr1 | 57.68 (19) | C2ii—Cr1—C2—C1ii | 30.47 (11) |
C4—Cr1—C2—O1 | 86.41 (16) | C1—C2—O1—C3 | 3.2 (2) |
C4i—Cr1—C2—O1 | −0.79 (12) | C1ii—C2—O1—C3 | −178.41 (14) |
C4ii—Cr1—C2—O1 | −88.86 (13) | Cr1—C2—O1—C3 | 96.49 (12) |
Symmetry codes: (i) −y, x−y, z; (ii) −x+y, −x, z. |