Supporting information
Crystallographic Information File (CIF) https://doi.org/10.1107/S1600536803016155/tk6126sup1.cif | |
Structure factor file (CIF format) https://doi.org/10.1107/S1600536803016155/tk6126Isup2.hkl |
CCDC reference: 221652
Key indicators
- Single-crystal X-ray study
- T = 293 K
- Mean (C-C) = 0.007 Å
- R factor = 0.043
- wR factor = 0.117
- Data-to-parameter ratio = 15.7
checkCIF results
No syntax errors found ADDSYM reports no extra symmetry
Data collection: IPDS (Stoe & Cie, 2000); cell refinement: IPDS; data reduction: X-RED (Stoe & Cie, 1996); program(s) used to solve structure: SIR92 (Altomare et al., 1993); program(s) used to refine structure: SHELXL97 (Sheldrick, 1997); molecular graphics: ORTEP-3 for Windows (Farrugia, 1997); software used to prepare material for publication: WinGX (Farrugia, 1999).
[Rh(C8H12)(C9H16N2O2)(H2O)](BF4) | F(000) = 1024 |
Mr = 500.15 | Dx = 1.575 Mg m−3 |
Monoclinic, P21/c | Mo Kα radiation, λ = 0.71073 Å |
Hall symbol: -P 2ybc | Cell parameters from 8000 reflections |
a = 10.0023 (10) Å | θ = 2.1–26.1° |
b = 23.2203 (17) Å | µ = 0.86 mm−1 |
c = 9.2977 (10) Å | T = 293 K |
β = 102.368 (12)° | Block, yellow |
V = 2109.3 (4) Å3 | 0.30 × 0.25 × 0.20 mm |
Z = 4 |
Stoe IPDS diffractometer | 3630 reflections with I > 2σ(I) |
Graphite monochromator | Rint = 0.027 |
φ scans | θmax = 26.1°, θmin = 2.1° |
Absorption correction: part of the refinement model (ΔF) (Parkin, S. et al. 1995) | h = −12→12 |
Tmin = 0.776, Tmax = 0.837 | k = −28→27 |
16245 measured reflections | l = −11→11 |
4070 independent 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)] = 0.043 | Hydrogen site location: inferred from neighbouring sites |
wR(F2) = 0.117 | H atoms treated by a mixture of independent and constrained refinement |
S = 0.99 | w = 1/[σ2(Fo2) + (0.0689P)2 + 4.0982P] where P = (Fo2 + 2Fc2)/3 |
4070 reflections | (Δ/σ)max < 0.001 |
260 parameters | Δρmax = 0.90 e Å−3 |
3 restraints | Δρmin = −0.68 e Å−3 |
Experimental. The data were collected on a Stoe Imaging Plate Diffraction System (IPDS). The crystal-to-detector distance was 70 mm. 152 frames (2 min per frame) were obtained with 0 < φ < 198.9° and with the crystals rotated through 1.3° in φ. Coverage of the unique set was over 97% complete to at least 26.09°. |
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 | ||
C3 | −0.0431 (4) | 0.1707 (2) | −0.1141 (6) | 0.0594 (12) | |
C4 | −0.0172 (4) | 0.1408 (2) | −0.2292 (5) | 0.0616 (12) | |
H4 | −0.0692 | 0.1410 | −0.3249 | 0.074* | |
C5 | 0.1032 (4) | 0.1091 (2) | −0.1772 (4) | 0.0499 (10) | |
C6 | −0.1589 (6) | 0.2102 (3) | −0.1058 (9) | 0.094 (2) | |
H6A | −0.1474 | 0.2250 | −0.0075 | 0.113* | |
H6B | −0.2436 | 0.1894 | −0.1311 | 0.113* | |
H6C | −0.1602 | 0.2415 | −0.1734 | 0.113* | |
C7 | 0.1757 (6) | 0.0699 (2) | −0.2573 (5) | 0.0679 (14) | |
H7A | 0.2557 | 0.0552 | −0.1915 | 0.082* | |
H7B | 0.2023 | 0.0902 | −0.3366 | 0.082* | |
H7C | 0.1165 | 0.0384 | −0.2963 | 0.082* | |
C8 | 0.0912 (5) | 0.1849 (2) | 0.1467 (5) | 0.0594 (11) | |
H8A | 0.0146 | 0.2083 | 0.1602 | 0.071* | |
H8B | 0.1068 | 0.1556 | 0.2228 | 0.071* | |
C11 | 0.1891 (6) | 0.2665 (2) | 0.0585 (7) | 0.0746 (15) | |
H11A | 0.1212 | 0.2932 | 0.0792 | 0.090* | |
H11B | 0.1585 | 0.2522 | −0.0412 | 0.090* | |
C12 | 0.3220 (7) | 0.2952 (3) | 0.0745 (10) | 0.097 (2) | |
H12A | 0.3134 | 0.3288 | 0.0112 | 0.117* | |
H12B | 0.3546 | 0.3076 | 0.1756 | 0.117* | |
C14 | 0.5276 (8) | 0.2804 (4) | −0.0027 (13) | 0.144 (4) | |
H14A | 0.4981 | 0.3087 | −0.0780 | 0.172* | |
H14B | 0.5802 | 0.2513 | −0.0386 | 0.172* | |
H14C | 0.5829 | 0.2985 | 0.0824 | 0.172* | |
C21 | 0.3261 (4) | 0.0217 (3) | 0.4232 (5) | 0.0667 (14) | |
H21A | 0.3549 | −0.0180 | 0.4419 | 0.080* | |
H21B | 0.3412 | 0.0414 | 0.5174 | 0.080* | |
C22 | 0.4144 (4) | 0.04942 (18) | 0.3301 (4) | 0.0439 (8) | |
H22 | 0.4774 | 0.0787 | 0.3818 | 0.053* | |
C23 | 0.4621 (4) | 0.02082 (16) | 0.2209 (4) | 0.0425 (8) | |
H23 | 0.5525 | 0.0337 | 0.2094 | 0.051* | |
C24 | 0.4301 (5) | −0.0406 (2) | 0.1751 (6) | 0.0628 (12) | |
H24A | 0.4732 | −0.0495 | 0.0937 | 0.075* | |
H24B | 0.4703 | −0.0657 | 0.2565 | 0.075* | |
C25 | 0.2823 (5) | −0.0536 (2) | 0.1302 (7) | 0.0743 (16) | |
H25A | 0.2543 | −0.0738 | 0.2102 | 0.089* | |
H25B | 0.2682 | −0.0795 | 0.0463 | 0.089* | |
C26 | 0.1906 (4) | −0.00171 (19) | 0.0897 (5) | 0.0499 (9) | |
H26 | 0.1264 | −0.0049 | −0.0057 | 0.060* | |
C27 | 0.1430 (4) | 0.03170 (18) | 0.1930 (4) | 0.0449 (8) | |
H27 | 0.0516 | 0.0479 | 0.1559 | 0.054* | |
C28 | 0.1763 (5) | 0.0226 (3) | 0.3556 (5) | 0.0625 (12) | |
H28A | 0.1365 | −0.0136 | 0.3772 | 0.075* | |
H28B | 0.1338 | 0.0531 | 0.4016 | 0.075* | |
B1 | 0.7996 (5) | 0.1222 (2) | 0.3265 (6) | 0.0491 (10) | |
F1 | 0.9197 (3) | 0.14890 (16) | 0.3789 (4) | 0.0886 (10) | |
F2 | 0.8175 (6) | 0.0704 (2) | 0.2741 (9) | 0.184 (3) | |
F3 | 0.7379 (5) | 0.1170 (3) | 0.4425 (6) | 0.147 (2) | |
F4 | 0.7116 (4) | 0.15416 (18) | 0.2259 (5) | 0.1083 (13) | |
N1 | 0.0571 (3) | 0.15740 (15) | 0.0043 (4) | 0.0493 (8) | |
N2 | 0.1488 (3) | 0.11937 (15) | −0.0341 (3) | 0.0427 (7) | |
O10 | 0.2070 (4) | 0.21926 (15) | 0.1620 (4) | 0.0634 (8) | |
O13 | 0.4149 (4) | 0.25550 (17) | 0.0350 (6) | 0.0979 (15) | |
O1 | 0.4428 (3) | 0.14028 (12) | 0.0913 (4) | 0.0526 (7) | |
Rh1 | 0.29942 (3) | 0.076409 (12) | 0.12152 (3) | 0.03547 (13) | |
H1b | 0.524 (2) | 0.1385 (16) | 0.142 (4) | 0.043* | |
H1a | 0.423 (4) | 0.1759 (9) | 0.081 (4) | 0.043* |
U11 | U22 | U33 | U12 | U13 | U23 | |
C3 | 0.043 (2) | 0.064 (3) | 0.071 (3) | 0.0082 (19) | 0.011 (2) | 0.031 (2) |
C4 | 0.048 (2) | 0.081 (3) | 0.050 (2) | −0.009 (2) | −0.0034 (18) | 0.030 (2) |
C5 | 0.047 (2) | 0.069 (3) | 0.0341 (18) | −0.0075 (19) | 0.0080 (15) | 0.0081 (17) |
C6 | 0.056 (3) | 0.080 (4) | 0.144 (6) | 0.022 (3) | 0.017 (3) | 0.042 (4) |
C7 | 0.074 (3) | 0.096 (4) | 0.038 (2) | −0.014 (3) | 0.020 (2) | −0.016 (2) |
C8 | 0.072 (3) | 0.060 (3) | 0.055 (2) | 0.020 (2) | 0.033 (2) | 0.001 (2) |
C11 | 0.077 (3) | 0.046 (3) | 0.105 (4) | 0.018 (2) | 0.030 (3) | 0.005 (3) |
C12 | 0.086 (4) | 0.055 (3) | 0.150 (6) | 0.013 (3) | 0.023 (4) | 0.001 (4) |
C14 | 0.082 (5) | 0.104 (6) | 0.261 (12) | 0.013 (4) | 0.072 (6) | 0.075 (7) |
C21 | 0.049 (2) | 0.113 (4) | 0.036 (2) | 0.007 (2) | 0.0037 (17) | 0.005 (2) |
C22 | 0.0390 (18) | 0.047 (2) | 0.0397 (18) | 0.0049 (15) | −0.0039 (15) | −0.0018 (16) |
C23 | 0.0363 (17) | 0.041 (2) | 0.047 (2) | 0.0071 (15) | 0.0035 (15) | 0.0015 (15) |
C24 | 0.070 (3) | 0.044 (2) | 0.070 (3) | 0.011 (2) | 0.004 (2) | −0.009 (2) |
C25 | 0.061 (3) | 0.045 (3) | 0.117 (5) | −0.007 (2) | 0.019 (3) | −0.018 (3) |
C26 | 0.0410 (19) | 0.054 (2) | 0.053 (2) | −0.0102 (17) | 0.0059 (16) | −0.0100 (18) |
C27 | 0.0359 (17) | 0.057 (2) | 0.0408 (19) | −0.0022 (16) | 0.0052 (14) | 0.0031 (17) |
C28 | 0.053 (2) | 0.090 (4) | 0.044 (2) | −0.004 (2) | 0.0077 (18) | 0.016 (2) |
B1 | 0.039 (2) | 0.042 (2) | 0.065 (3) | −0.0039 (18) | 0.009 (2) | −0.007 (2) |
F1 | 0.0619 (18) | 0.093 (2) | 0.104 (2) | −0.0247 (16) | 0.0036 (16) | 0.0014 (19) |
F2 | 0.131 (4) | 0.119 (4) | 0.274 (8) | 0.040 (3) | −0.017 (4) | −0.121 (5) |
F3 | 0.097 (3) | 0.220 (6) | 0.136 (4) | −0.002 (3) | 0.050 (3) | 0.063 (4) |
F4 | 0.096 (3) | 0.103 (3) | 0.104 (3) | −0.004 (2) | −0.027 (2) | 0.019 (2) |
N1 | 0.0473 (17) | 0.055 (2) | 0.0494 (18) | 0.0155 (15) | 0.0181 (15) | 0.0114 (15) |
N2 | 0.0411 (16) | 0.056 (2) | 0.0326 (14) | 0.0106 (14) | 0.0120 (12) | 0.0043 (13) |
O10 | 0.076 (2) | 0.0573 (19) | 0.0597 (19) | 0.0116 (16) | 0.0209 (16) | −0.0103 (15) |
O13 | 0.081 (3) | 0.056 (2) | 0.171 (5) | 0.0175 (19) | 0.058 (3) | 0.035 (3) |
O1 | 0.0449 (15) | 0.0381 (15) | 0.074 (2) | 0.0022 (12) | 0.0114 (14) | 0.0076 (13) |
Rh1 | 0.03480 (18) | 0.03818 (19) | 0.03272 (18) | 0.00378 (10) | 0.00567 (12) | −0.00176 (10) |
Rh1—O1 | 2.123 (3) | C14—H14A | 0.9600 |
Rh1—N2 | 2.103 (3) | C14—H14B | 0.9600 |
Rh1—C22 | 2.126 (4) | C14—H14C | 0.9600 |
Rh1—C23 | 2.127 (3) | C21—C28 | 1.496 (6) |
Rh1—C26 | 2.104 (4) | C21—C22 | 1.507 (6) |
Rh1—C27 | 2.101 (4) | C21—H21A | 0.9700 |
C3—C4 | 1.347 (7) | C21—H21B | 0.9700 |
C3—N1 | 1.356 (5) | C22—C23 | 1.381 (5) |
C3—C6 | 1.491 (7) | C22—H22 | 0.9800 |
C4—C5 | 1.405 (6) | C23—C24 | 1.504 (6) |
C4—H4 | 0.9300 | C23—H23 | 0.9800 |
C5—N2 | 1.332 (5) | C24—C25 | 1.479 (7) |
C5—C7 | 1.464 (7) | C24—H24A | 0.9700 |
C6—H6A | 0.9600 | C24—H24B | 0.9700 |
C6—H6B | 0.9600 | C25—C26 | 1.512 (7) |
C6—H6C | 0.9600 | C25—H25A | 0.9700 |
C7—H7A | 0.9600 | C25—H25B | 0.9700 |
C7—H7B | 0.9600 | C26—C27 | 1.396 (6) |
C7—H7C | 0.9600 | C26—H26 | 0.9800 |
C8—O10 | 1.388 (6) | C27—C28 | 1.492 (5) |
C8—N1 | 1.443 (6) | C27—H27 | 0.9800 |
C8—H8A | 0.9700 | C28—H28A | 0.9700 |
C8—H8B | 0.9700 | C28—H28B | 0.9700 |
C11—O10 | 1.444 (7) | B1—F2 | 1.324 (6) |
C11—C12 | 1.467 (8) | B1—F1 | 1.347 (5) |
C11—H11A | 0.9700 | B1—F3 | 1.358 (6) |
C11—H11B | 0.9700 | B1—F4 | 1.359 (6) |
C12—O13 | 1.412 (7) | N1—N2 | 1.374 (4) |
C12—H12A | 0.9700 | O1—H1b | 0.845 (18) |
C12—H12B | 0.9700 | O1—H1a | 0.852 (18) |
C14—O13 | 1.377 (7) | ||
O1—Rh1—N2 | 88.99 (12) | H12A—C12—H12B | 108.4 |
O1—Rh1—C22 | 94.45 (14) | O13—C14—H14A | 109.5 |
O1—Rh1—C23 | 90.33 (13) | O13—C14—H14B | 109.5 |
O1—Rh1—C26 | 158.08 (15) | O13—C14—H14C | 109.5 |
O1—Rh1—C27 | 163.13 (14) | H14A—C14—H14B | 109.5 |
N2—Rh1—C22 | 159.22 (13) | H14A—C14—H14C | 109.5 |
N2—Rh1—C23 | 162.80 (13) | H14B—C14—H14C | 109.5 |
N2—Rh1—C26 | 92.26 (15) | C28—C21—C22 | 114.2 (4) |
N2—Rh1—C27 | 88.83 (14) | C28—C21—H21A | 108.7 |
C22—Rh1—C23 | 37.89 (15) | C22—C21—H21A | 108.7 |
C22—Rh1—C26 | 92.09 (16) | C28—C21—H21B | 108.7 |
C22—Rh1—C27 | 81.95 (15) | C22—C21—H21B | 108.7 |
C23—Rh1—C26 | 82.09 (16) | H21A—C21—H21B | 107.6 |
C23—Rh1—C27 | 96.61 (15) | C23—C22—C21 | 123.7 (4) |
C26—Rh1—C27 | 38.77 (16) | C23—C22—H22 | 114.1 |
Rh1—N2—N1 | 123.1 (2) | C21—C22—H22 | 114.1 |
Rh1—N2—C5 | 130.1 (3) | Rh1—C22—H22 | 114.1 |
Rh1—C22—C21 | 112.4 (3) | C22—C23—C24 | 125.3 (4) |
Rh1—C22—C23 | 71.1 (2) | C22—C23—H23 | 113.9 |
Rh1—C23—C22 | 71.0 (2) | C24—C23—H23 | 113.9 |
Rh1—C23—C24 | 110.9 (3) | Rh1—C23—H23 | 113.9 |
Rh1—C26—C25 | 112.6 (3) | C25—C24—C23 | 114.3 (4) |
Rh1—C26—C27 | 70.5 (2) | C25—C24—H24A | 108.7 |
Rh1—C27—C26 | 70.7 (2) | C23—C24—H24A | 108.7 |
Rh1—C27—C28 | 111.7 (3) | C25—C24—H24B | 108.7 |
C4—C3—N1 | 107.0 (4) | C23—C24—H24B | 108.7 |
C4—C3—C6 | 129.9 (5) | H24A—C24—H24B | 107.6 |
N1—C3—C6 | 123.0 (5) | C24—C25—C26 | 115.1 (4) |
C3—C4—C5 | 107.1 (4) | C24—C25—H25A | 108.5 |
C3—C4—H4 | 126.5 | C26—C25—H25A | 108.5 |
C5—C4—H4 | 126.5 | C24—C25—H25B | 108.5 |
N2—C5—C4 | 109.6 (4) | C26—C25—H25B | 108.5 |
N2—C5—C7 | 121.2 (4) | H25A—C25—H25B | 107.5 |
C4—C5—C7 | 129.2 (4) | C27—C26—C25 | 123.4 (4) |
C3—C6—H6A | 109.5 | C27—C26—H26 | 114.2 |
C3—C6—H6B | 109.5 | C25—C26—H26 | 114.2 |
H6A—C6—H6B | 109.5 | Rh1—C26—H26 | 114.2 |
C3—C6—H6C | 109.5 | C26—C27—C28 | 125.7 (4) |
H6A—C6—H6C | 109.5 | C26—C27—H27 | 113.6 |
H6B—C6—H6C | 109.5 | C28—C27—H27 | 113.6 |
C5—C7—H7A | 109.5 | Rh1—C27—H27 | 113.6 |
C5—C7—H7B | 109.5 | C27—C28—C21 | 114.5 (4) |
H7A—C7—H7B | 109.5 | C27—C28—H28A | 108.6 |
C5—C7—H7C | 109.5 | C21—C28—H28A | 108.6 |
H7A—C7—H7C | 109.5 | C27—C28—H28B | 108.6 |
H7B—C7—H7C | 109.5 | C21—C28—H28B | 108.6 |
O10—C8—N1 | 112.1 (3) | H28A—C28—H28B | 107.6 |
O10—C8—H8A | 109.2 | F2—B1—F1 | 111.8 (4) |
N1—C8—H8A | 109.2 | F2—B1—F3 | 109.4 (6) |
O10—C8—H8B | 109.2 | F1—B1—F3 | 105.9 (5) |
N1—C8—H8B | 109.2 | F2—B1—F4 | 111.2 (5) |
H8A—C8—H8B | 107.9 | F1—B1—F4 | 113.2 (4) |
O10—C11—C12 | 107.3 (5) | F3—B1—F4 | 104.9 (4) |
O10—C11—H11A | 110.3 | C3—N1—N2 | 110.7 (4) |
C12—C11—H11A | 110.3 | C3—N1—C8 | 129.2 (4) |
O10—C11—H11B | 110.3 | N2—N1—C8 | 118.8 (3) |
C12—C11—H11B | 110.3 | C5—N2—N1 | 105.6 (3) |
H11A—C11—H11B | 108.5 | C8—O10—C11 | 112.7 (4) |
O13—C12—C11 | 108.0 (5) | C14—O13—C12 | 114.4 (6) |
O13—C12—H12A | 110.1 | Rh1—O1—H1b | 119 (3) |
C11—C12—H12A | 110.1 | Rh1—O1—H1a | 123 (3) |
O13—C12—H12B | 110.1 | H1b—O1—H1a | 106 (3) |
C11—C12—H12B | 110.1 |
D—H···A | D—H | H···A | D···A | D—H···A |
O1—H1a···O10 | 0.85 (2) | 2.64 (3) | 3.166 (4) | 121 (3) |
O1—H1a···O13 | 0.85 (2) | 1.89 (2) | 2.729 (5) | 167 (4) |
O1—H1b···F4 | 0.85 (2) | 1.91 (2) | 2.731 (5) | 164 (4) |
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