Supporting information
Crystallographic Information File (CIF) https://doi.org/10.1107/S1600536803015691/cf6271sup1.cif | |
Structure factor file (CIF format) https://doi.org/10.1107/S1600536803015691/cf6271Isup2.hkl |
CCDC reference: 221644
Key indicators
- Single-crystal X-ray study
- T = 293 K
- Mean (C-C) = 0.006 Å
- R factor = 0.022
- wR factor = 0.049
- Data-to-parameter ratio = 14.7
checkCIF results
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Alert Level A:
PUBL_003 Alert A The contact author's name is missing, _publ_contact_author_name. ADDSYM reports no extra symmetry General Notes
REFLT_03 From the CIF: _diffrn_reflns_theta_max 24.98 From the CIF: _reflns_number_total 2795 Count of symmetry unique reflns 1889 Completeness (_total/calc) 147.96% TEST3: Check Friedels for noncentro structure Estimate of Friedel pairs measured 906 Fraction of Friedel pairs measured 0.480 Are heavy atom types Z>Si present yes WARNING: Large fraction of Friedel related reflns may be needed to determine absolute structure
1 Alert Level A = Potentially serious problem
0 Alert Level B = Potential problem
0 Alert Level C = Please check
Data collection: MSC/AFC Diffractometer Control Software (Molecular Structure Corporation, 1991); cell refinement: MSC/AFC Diffractometer Control Software; data reduction: TEXSAN (Molecular Structure Corporation, 1999); program(s) used to solve structure: SHELXTL-NT (Bruker, 1998); program(s) used to refine structure: SHELXTL-NT; molecular graphics: SHELXTL-NT; software used to prepare material for publication: SHELXTL-NT.
[Rh(C5H7O2)(C10H19P)(CO)] | Dx = 1.419 Mg m−3 |
Mr = 400.25 | Mo Kα radiation, λ = 0.71073 Å |
Orthorhombic, P212121 | Cell parameters from 25 reflections |
a = 11.970 (2) Å | θ = 26.4–31.7° |
b = 12.270 (3) Å | µ = 1.00 mm−1 |
c = 12.758 (3) Å | T = 293 K |
V = 1873.7 (7) Å3 | Prism, yellow |
Z = 4 | 0.36 × 0.30 × 0.15 mm |
F(000) = 824 |
Rigaku AFC-7S diffractometer | 2580 reflections with I > 2σ(I) |
Radiation source: Normal-focus sealed tube | Rint = 0.013 |
Graphite monochromator | θmax = 25.0°, θmin = 2.3° |
ω–2θ scans | h = −10→14 |
Absorption correction: ψ scan (North et al., 1968) | k = 0→14 |
Tmin = 0.766, Tmax = 0.860 | l = −1→15 |
3098 measured reflections | 3 standard reflections every 150 reflections |
2795 independent reflections | intensity decay: none |
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)] = 0.022 | H-atom parameters constrained |
wR(F2) = 0.049 | w = 1/[σ2(Fo2) + (0.0248P)2 + 0.2043P] where P = (Fo2 + 2Fc2)/3 |
S = 1.05 | (Δ/σ)max = 0.001 |
2795 reflections | Δρmax = 0.25 e Å−3 |
190 parameters | Δρmin = −0.21 e Å−3 |
0 restraints | Absolute structure: Flack (1983), 956 Friedel pairs |
Primary atom site location: structure-invariant direct methods | Absolute structure parameter: −0.05 (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 | ||
Rh1 | 0.91546 (2) | 0.964193 (18) | 0.12852 (2) | 0.04217 (8) | |
P1 | 1.05392 (6) | 0.84271 (6) | 0.14477 (7) | 0.04182 (19) | |
O1 | 0.8260 (2) | 0.87419 (19) | 0.2330 (2) | 0.0571 (6) | |
O2 | 0.78003 (18) | 1.07020 (15) | 0.1194 (2) | 0.0537 (6) | |
O3 | 1.0552 (3) | 1.0884 (3) | −0.0182 (3) | 0.0970 (11) | |
C1 | 0.7300 (3) | 0.8948 (3) | 0.2710 (3) | 0.0526 (8) | |
C2 | 0.6643 (3) | 0.9823 (3) | 0.2434 (3) | 0.0577 (9) | |
H2A | 0.5955 | 0.9880 | 0.2767 | 0.069* | |
C3 | 0.6899 (3) | 1.0634 (3) | 0.1706 (3) | 0.0515 (9) | |
C4 | 0.6065 (3) | 1.1523 (3) | 0.1506 (4) | 0.0850 (15) | |
H4A | 0.6360 | 1.2021 | 0.0996 | 0.127* | |
H4B | 0.5917 | 1.1906 | 0.2147 | 0.127* | |
H4C | 0.5384 | 1.1210 | 0.1246 | 0.127* | |
C5 | 0.6914 (4) | 0.8173 (3) | 0.3532 (4) | 0.0806 (13) | |
H5A | 0.7468 | 0.7617 | 0.3632 | 0.121* | |
H5B | 0.6224 | 0.7843 | 0.3316 | 0.121* | |
H5C | 0.6801 | 0.8558 | 0.4178 | 0.121* | |
C6 | 1.0000 (3) | 1.0407 (3) | 0.0384 (3) | 0.0594 (9) | |
C7 | 1.1974 (3) | 0.8907 (3) | 0.1247 (4) | 0.0574 (8) | |
H7A | 1.2482 | 0.8316 | 0.1415 | 0.069* | |
H7B | 1.2071 | 0.9076 | 0.0509 | 0.069* | |
C8 | 1.2304 (4) | 0.9883 (3) | 0.1872 (4) | 0.0720 (11) | |
H8A | 1.1843 | 1.0492 | 0.1834 | 0.086* | |
C9 | 1.3161 (5) | 0.9950 (5) | 0.2452 (5) | 0.113 (2) | |
H9A | 1.3643 | 0.9360 | 0.2512 | 0.136* | |
H9B | 1.3307 | 1.0591 | 0.2817 | 0.136* | |
C10 | 1.0552 (3) | 0.7796 (3) | 0.2744 (3) | 0.0580 (10) | |
H10A | 0.9891 | 0.7345 | 0.2813 | 0.070* | |
H10B | 1.1197 | 0.7321 | 0.2791 | 0.070* | |
C11 | 1.0584 (3) | 0.8571 (3) | 0.3640 (3) | 0.0640 (10) | |
H11A | 1.0016 | 0.9086 | 0.3676 | 0.077* | |
C12 | 1.1315 (4) | 0.8593 (4) | 0.4361 (4) | 0.0859 (14) | |
H12A | 1.1899 | 0.8093 | 0.4357 | 0.103* | |
H12B | 1.1267 | 0.9110 | 0.4893 | 0.103* | |
C13 | 1.0429 (3) | 0.7248 (3) | 0.0526 (3) | 0.0538 (9) | |
C14 | 1.0500 (5) | 0.7693 (4) | −0.0597 (3) | 0.0863 (16) | |
H14A | 1.0442 | 0.7101 | −0.1086 | 0.129* | |
H14B | 1.1201 | 0.8059 | −0.0693 | 0.129* | |
H14C | 0.9899 | 0.8198 | −0.0714 | 0.129* | |
C15 | 1.1343 (4) | 0.6397 (3) | 0.0703 (4) | 0.0775 (13) | |
H15A | 1.1249 | 0.5809 | 0.0215 | 0.116* | |
H15B | 1.1291 | 0.6120 | 0.1406 | 0.116* | |
H15C | 1.2062 | 0.6727 | 0.0602 | 0.116* | |
C16 | 0.9286 (4) | 0.6723 (3) | 0.0698 (4) | 0.0812 (13) | |
H16A | 0.9203 | 0.6112 | 0.0234 | 0.122* | |
H16B | 0.8710 | 0.7247 | 0.0557 | 0.122* | |
H16C | 0.9227 | 0.6479 | 0.1411 | 0.122* |
U11 | U22 | U33 | U12 | U13 | U23 | |
Rh1 | 0.03689 (12) | 0.04215 (11) | 0.04748 (13) | 0.00288 (10) | 0.00297 (13) | 0.00589 (12) |
P1 | 0.0390 (4) | 0.0429 (4) | 0.0436 (5) | 0.0036 (3) | 0.0003 (4) | 0.0010 (4) |
O1 | 0.0482 (14) | 0.0538 (13) | 0.0693 (17) | 0.0027 (11) | 0.0147 (13) | 0.0123 (12) |
O2 | 0.0435 (12) | 0.0475 (11) | 0.0701 (16) | 0.0065 (9) | 0.0002 (14) | 0.0074 (12) |
O3 | 0.070 (2) | 0.107 (2) | 0.114 (3) | 0.0069 (17) | 0.0280 (19) | 0.060 (2) |
C1 | 0.046 (2) | 0.0538 (18) | 0.058 (2) | −0.0078 (16) | 0.0092 (17) | −0.0044 (16) |
C2 | 0.0366 (18) | 0.067 (2) | 0.069 (2) | 0.0003 (16) | 0.0099 (18) | −0.009 (2) |
C3 | 0.0394 (19) | 0.0510 (19) | 0.064 (2) | 0.0011 (14) | −0.0060 (17) | −0.0088 (15) |
C4 | 0.053 (2) | 0.080 (2) | 0.122 (4) | 0.023 (2) | 0.006 (3) | 0.008 (3) |
C5 | 0.079 (3) | 0.076 (2) | 0.087 (4) | −0.004 (2) | 0.027 (3) | 0.012 (2) |
C6 | 0.048 (2) | 0.058 (2) | 0.072 (2) | 0.0092 (19) | 0.0060 (19) | 0.021 (2) |
C7 | 0.0419 (18) | 0.0599 (18) | 0.070 (2) | 0.0023 (14) | −0.001 (2) | −0.004 (2) |
C8 | 0.058 (3) | 0.074 (2) | 0.084 (3) | −0.017 (2) | 0.000 (2) | 0.000 (2) |
C9 | 0.103 (4) | 0.127 (4) | 0.109 (4) | −0.046 (3) | −0.021 (4) | −0.001 (3) |
C10 | 0.071 (3) | 0.0524 (19) | 0.050 (2) | 0.0138 (17) | 0.0017 (19) | 0.0093 (16) |
C11 | 0.077 (3) | 0.068 (2) | 0.047 (2) | 0.0158 (17) | 0.002 (2) | 0.0063 (19) |
C12 | 0.104 (4) | 0.099 (3) | 0.054 (3) | 0.015 (3) | −0.009 (3) | 0.008 (2) |
C13 | 0.059 (2) | 0.0484 (18) | 0.054 (2) | 0.0023 (15) | −0.0041 (17) | −0.0062 (16) |
C14 | 0.135 (5) | 0.079 (3) | 0.045 (2) | 0.005 (3) | −0.002 (3) | −0.012 (2) |
C15 | 0.082 (3) | 0.059 (2) | 0.092 (3) | 0.021 (2) | −0.004 (3) | −0.018 (2) |
C16 | 0.068 (3) | 0.070 (2) | 0.106 (3) | −0.011 (2) | −0.017 (3) | −0.023 (2) |
Rh1—C6 | 1.797 (4) | C8—C9 | 1.267 (7) |
Rh1—O1 | 2.036 (2) | C8—H8A | 0.930 |
Rh1—O2 | 2.082 (2) | C9—H9A | 0.930 |
Rh1—P1 | 2.2387 (8) | C9—H9B | 0.930 |
P1—C10 | 1.826 (3) | C10—C11 | 1.487 (5) |
P1—C7 | 1.834 (3) | C10—H10A | 0.970 |
P1—C13 | 1.869 (3) | C10—H10B | 0.970 |
O1—C1 | 1.272 (4) | C11—C12 | 1.270 (6) |
O2—C3 | 1.264 (4) | C11—H11A | 0.930 |
O3—C6 | 1.141 (4) | C12—H12A | 0.930 |
C1—C2 | 1.377 (5) | C12—H12B | 0.930 |
C1—C5 | 1.490 (5) | C13—C16 | 1.528 (5) |
C2—C3 | 1.395 (5) | C13—C15 | 1.529 (5) |
C2—H2A | 0.930 | C13—C14 | 1.536 (5) |
C3—C4 | 1.500 (5) | C14—H14A | 0.960 |
C4—H4A | 0.960 | C14—H14B | 0.960 |
C4—H4B | 0.960 | C14—H14C | 0.960 |
C4—H4C | 0.960 | C15—H15A | 0.960 |
C5—H5A | 0.960 | C15—H15B | 0.960 |
C5—H5B | 0.960 | C15—H15C | 0.960 |
C5—H5C | 0.960 | C16—H16A | 0.960 |
C7—C8 | 1.493 (5) | C16—H16B | 0.960 |
C7—H7A | 0.970 | C16—H16C | 0.960 |
C7—H7B | 0.970 | ||
C6—Rh1—O1 | 177.45 (14) | C9—C8—C7 | 125.3 (5) |
C6—Rh1—O2 | 94.38 (13) | C9—C8—H8A | 117.3 |
O1—Rh1—O2 | 88.03 (10) | C7—C8—H8A | 117.3 |
C6—Rh1—P1 | 89.44 (12) | C8—C9—H9A | 120.0 |
O1—Rh1—P1 | 88.15 (7) | C8—C9—H9B | 120.0 |
O2—Rh1—P1 | 176.15 (7) | H9A—C9—H9B | 120.0 |
C10—P1—C7 | 104.8 (2) | C11—C10—P1 | 115.2 (2) |
C10—P1—C13 | 104.03 (16) | C11—C10—H10A | 108.5 |
C7—P1—C13 | 103.08 (17) | P1—C10—H10A | 108.5 |
C10—P1—Rh1 | 111.84 (13) | C11—C10—H10B | 108.5 |
C7—P1—Rh1 | 117.82 (11) | P1—C10—H10B | 108.5 |
C13—P1—Rh1 | 113.89 (12) | H10A—C10—H10B | 107.5 |
C1—O1—Rh1 | 128.1 (2) | C12—C11—C10 | 126.0 (4) |
C3—O2—Rh1 | 126.5 (2) | C12—C11—H11A | 117.0 |
O1—C1—C2 | 125.0 (3) | C10—C11—H11A | 117.0 |
O1—C1—C5 | 114.9 (3) | C11—C12—H12A | 120.0 |
C2—C1—C5 | 120.1 (3) | C11—C12—H12B | 120.0 |
C1—C2—C3 | 126.9 (3) | H12A—C12—H12B | 120.0 |
C1—C2—H2A | 116.5 | C16—C13—C15 | 109.3 (3) |
C3—C2—H2A | 116.5 | C16—C13—C14 | 109.4 (4) |
O2—C3—C2 | 125.4 (3) | C15—C13—C14 | 110.0 (4) |
O2—C3—C4 | 115.6 (3) | C16—C13—P1 | 107.4 (3) |
C2—C3—C4 | 119.0 (3) | C15—C13—P1 | 112.6 (3) |
C3—C4—H4A | 109.5 | C14—C13—P1 | 107.9 (2) |
C3—C4—H4B | 109.5 | C13—C14—H14A | 109.5 |
H4A—C4—H4B | 109.5 | C13—C14—H14B | 109.5 |
C3—C4—H4C | 109.5 | H14A—C14—H14B | 109.5 |
H4A—C4—H4C | 109.5 | C13—C14—H14C | 109.5 |
H4B—C4—H4C | 109.5 | H14A—C14—H14C | 109.5 |
C1—C5—H5A | 109.5 | H14B—C14—H14C | 109.5 |
C1—C5—H5B | 109.5 | C13—C15—H15A | 109.5 |
H5A—C5—H5B | 109.5 | C13—C15—H15B | 109.5 |
C1—C5—H5C | 109.5 | H15A—C15—H15B | 109.5 |
H5A—C5—H5C | 109.5 | C13—C15—H15C | 109.5 |
H5B—C5—H5C | 109.5 | H15A—C15—H15C | 109.5 |
O3—C6—Rh1 | 178.8 (3) | H15B—C15—H15C | 109.5 |
C8—C7—P1 | 115.5 (3) | C13—C16—H16A | 109.5 |
C8—C7—H7A | 108.4 | C13—C16—H16B | 109.5 |
P1—C7—H7A | 108.4 | H16A—C16—H16B | 109.5 |
C8—C7—H7B | 108.4 | C13—C16—H16C | 109.5 |
P1—C7—H7B | 108.4 | H16A—C16—H16C | 109.5 |
H7A—C7—H7B | 107.5 | H16B—C16—H16C | 109.5 |