Supporting information
Crystallographic Information File (CIF) https://doi.org/10.1107/S1600536805013516/sj6080sup1.cif | |
Structure factor file (CIF format) https://doi.org/10.1107/S1600536805013516/sj6080Isup2.hkl |
CCDC reference: 274632
Key indicators
- Single-crystal X-ray study
- T = 153 K
- Mean (C-C) = 0.008 Å
- R factor = 0.068
- wR factor = 0.171
- Data-to-parameter ratio = 19.0
checkCIF/PLATON results
No syntax errors found
Alert level C PLAT094_ALERT_2_C Ratio of Maximum / Minimum Residual Density .... 2.75 PLAT242_ALERT_2_C Check Low Ueq as Compared to Neighbors for Fe1 PLAT244_ALERT_4_C Low 'Solvent' Ueq as Compared to Neighbors for S1 PLAT244_ALERT_4_C Low 'Solvent' Ueq as Compared to Neighbors for C12 PLAT341_ALERT_3_C Low Bond Precision on C-C bonds (x 1000) Ang ... 8
0 ALERT level A = In general: serious problem 0 ALERT level B = Potentially serious problem 5 ALERT level C = Check and explain 0 ALERT level G = General alerts; check 0 ALERT type 1 CIF construction/syntax error, inconsistent or missing data 2 ALERT type 2 Indicator that the structure model may be wrong or deficient 1 ALERT type 3 Indicator that the structure quality may be low 2 ALERT type 4 Improvement, methodology, query or suggestion
Data collection: CrystalClear (Rigaku, 2001); cell refinement: CrystalClear; data reduction: TEXSAN (Molecular Structure Corporation 2000); program(s) used to solve structure: DIRDIF94 (Beurskens et al., 1994); program(s) used to refine structure: SHELXL97 (Sheldrick, 1997); molecular graphics: ORTEPII (Johnson, 1976); software used to prepare material for publication: TEXSAN.
[Fe(C5H5)(C4H9NSi)(CO)2](CF3SO3) | F(000) = 864.00 |
Mr = 425.23 | Dx = 1.546 Mg m−3 |
Monoclinic, P21/n | Mo Kα radiation, λ = 0.7107 Å |
Hall symbol: -P 2yn | Cell parameters from 7143 reflections |
a = 17.370 (5) Å | θ = 3.1–27.5° |
b = 13.131 (4) Å | µ = 1.05 mm−1 |
c = 8.011 (2) Å | T = 153 K |
β = 91.803 (7)° | Block, yellow |
V = 1826.4 (9) Å3 | 0.30 × 0.13 × 0.10 mm |
Z = 4 |
Rigaku/MSC Mercury CCD diffractometer | 3344 reflections with I > 2σ(I) |
Detector resolution: 14.62 pixels mm-1 | Rint = 0.042 |
ω scans | θmax = 27.5° |
Absorption correction: multi-scan (Jacobson, 1998) | h = −22→22 |
Tmin = 0.758, Tmax = 0.900 | k = −14→17 |
17930 measured reflections | l = −10→10 |
4113 independent reflections |
Refinement on F2 | H-atom parameters constrained |
R[F2 > 2σ(F2)] = 0.068 | w = 1/[σ2(Fo2) + (0.0484P)2 + 7.0396P] where P = (Fo2 + 2Fc2)/3 |
wR(F2) = 0.171 | (Δ/σ)max = 0.001 |
S = 1.16 | Δρmax = 1.65 e Å−3 |
4113 reflections | Δρmin = −0.60 e Å−3 |
217 parameters |
Refinement. Refinement was carried out using all reflections. The weighted R-factor (wR) and goodness of fit (S) are based on F2. R-factor (gt) are based on F. The threshold expression of F2 > 2.0 σ(F2) is used only for calculating R-factor (gt). |
x | y | z | Uiso*/Ueq | ||
Fe1 | 0.64307 (4) | 0.44959 (5) | 0.72220 (8) | 0.0219 (2) | |
S1 | 0.70694 (9) | 0.1433 (1) | 0.2504 (2) | 0.0392 (3) | |
Si1 | 0.46863 (7) | 0.1658 (1) | 0.7336 (2) | 0.0289 (3) | |
F1 | 0.6608 (3) | 0.3320 (3) | 0.2458 (6) | 0.081 (1) | |
F2 | 0.5868 (3) | 0.2328 (6) | 0.3734 (6) | 0.106 (2) | |
F3 | 0.5872 (3) | 0.2291 (6) | 0.1065 (6) | 0.113 (2) | |
O1 | 0.5505 (3) | 0.5886 (4) | 0.9174 (9) | 0.087 (2) | |
O2 | 0.5827 (3) | 0.5220 (4) | 0.3973 (6) | 0.059 (1) | |
O3 | 0.7465 (3) | 0.1639 (3) | 0.1002 (5) | 0.051 (1) | |
O4 | 0.7479 (3) | 0.1672 (3) | 0.4038 (6) | 0.060 (1) | |
O5 | 0.6688 (4) | 0.0472 (4) | 0.2507 (6) | 0.083 (2) | |
N1 | 0.5286 (2) | 0.2771 (3) | 0.7356 (5) | 0.0261 (8) | |
C1 | 0.7485 (3) | 0.5186 (4) | 0.7783 (9) | 0.044 (1) | |
C2 | 0.7311 (3) | 0.4494 (5) | 0.9057 (7) | 0.044 (1) | |
C3 | 0.7257 (3) | 0.3525 (4) | 0.8342 (6) | 0.033 (1) | |
C4 | 0.7382 (3) | 0.3607 (4) | 0.6628 (6) | 0.030 (1) | |
C5 | 0.7535 (3) | 0.4644 (5) | 0.6291 (7) | 0.038 (1) | |
C6 | 0.5860 (3) | 0.5337 (4) | 0.8423 (9) | 0.051 (2) | |
C7 | 0.6056 (3) | 0.4944 (4) | 0.5246 (7) | 0.037 (1) | |
C8 | 0.5716 (3) | 0.3443 (3) | 0.7314 (5) | 0.0233 (9) | |
C9 | 0.5379 (4) | 0.0596 (5) | 0.7339 (9) | 0.051 (2) | |
C10 | 0.4116 (4) | 0.1725 (5) | 0.9229 (9) | 0.049 (2) | |
C11 | 0.4090 (3) | 0.1766 (5) | 0.5402 (9) | 0.049 (2) | |
C12 | 0.6309 (4) | 0.2376 (7) | 0.2442 (7) | 0.057 (2) | |
H1 | 0.7557 | 0.5897 | 0.7909 | 0.0443* | |
H2 | 0.7242 | 0.4656 | 1.0196 | 0.0437* | |
H3 | 0.7152 | 0.2912 | 0.8923 | 0.0327* | |
H4 | 0.7367 | 0.3066 | 0.5839 | 0.0301* | |
H5 | 0.7651 | 0.4923 | 0.5233 | 0.0383* | |
H6 | 0.5107 | −0.0033 | 0.7332 | 0.0515* | |
H7 | 0.5681 | 0.0637 | 0.6374 | 0.0515* | |
H8 | 0.5704 | 0.0633 | 0.8311 | 0.0515* | |
H9 | 0.4452 | 0.1733 | 1.0188 | 0.0495* | |
H10 | 0.3814 | 0.2328 | 0.9205 | 0.0495* | |
H11 | 0.3787 | 0.1148 | 0.9276 | 0.0495* | |
H12 | 0.3796 | 0.2374 | 0.5429 | 0.0495* | |
H13 | 0.4414 | 0.1778 | 0.4468 | 0.0495* | |
H14 | 0.3754 | 0.1195 | 0.5311 | 0.0495* |
U11 | U22 | U33 | U12 | U13 | U23 | |
Fe1 | 0.0169 (3) | 0.0183 (3) | 0.0305 (4) | −0.0025 (2) | 0.0017 (2) | −0.0011 (3) |
S1 | 0.0637 (9) | 0.0241 (6) | 0.0295 (6) | −0.0115 (6) | −0.0026 (6) | 0.0010 (5) |
Si1 | 0.0195 (6) | 0.0224 (6) | 0.0450 (8) | −0.0055 (5) | 0.0043 (5) | −0.0048 (6) |
F1 | 0.118 (4) | 0.055 (3) | 0.071 (3) | 0.043 (3) | 0.022 (3) | 0.009 (2) |
F2 | 0.070 (3) | 0.185 (6) | 0.065 (3) | 0.000 (4) | 0.040 (2) | −0.003 (3) |
F3 | 0.061 (3) | 0.215 (7) | 0.060 (3) | 0.038 (4) | −0.023 (2) | −0.020 (4) |
O1 | 0.070 (4) | 0.064 (3) | 0.128 (5) | −0.001 (3) | 0.041 (3) | −0.051 (3) |
O2 | 0.048 (3) | 0.072 (3) | 0.057 (3) | 0.002 (2) | −0.012 (2) | 0.032 (2) |
O3 | 0.068 (3) | 0.036 (2) | 0.049 (2) | 0.013 (2) | 0.018 (2) | 0.004 (2) |
O4 | 0.088 (4) | 0.043 (2) | 0.048 (3) | 0.010 (2) | −0.027 (2) | −0.005 (2) |
O5 | 0.143 (5) | 0.046 (3) | 0.060 (3) | −0.056 (3) | −0.005 (3) | 0.003 (2) |
N1 | 0.018 (2) | 0.029 (2) | 0.031 (2) | −0.007 (2) | 0.000 (1) | 0.000 (2) |
C1 | 0.022 (2) | 0.032 (3) | 0.079 (4) | −0.011 (2) | −0.002 (3) | −0.003 (3) |
C2 | 0.045 (3) | 0.057 (4) | 0.029 (3) | −0.002 (3) | −0.011 (2) | −0.012 (3) |
C3 | 0.026 (2) | 0.035 (3) | 0.037 (3) | 0.000 (2) | −0.003 (2) | 0.010 (2) |
C4 | 0.021 (2) | 0.039 (3) | 0.030 (2) | 0.006 (2) | −0.001 (2) | −0.002 (2) |
C5 | 0.021 (2) | 0.054 (3) | 0.040 (3) | 0.003 (2) | 0.007 (2) | 0.022 (3) |
C6 | 0.035 (3) | 0.035 (3) | 0.083 (5) | −0.009 (2) | 0.019 (3) | −0.025 (3) |
C7 | 0.025 (2) | 0.038 (3) | 0.048 (3) | −0.002 (2) | 0.001 (2) | 0.015 (2) |
C8 | 0.021 (2) | 0.024 (2) | 0.025 (2) | −0.002 (2) | 0.001 (2) | −0.001 (2) |
C9 | 0.043 (3) | 0.030 (3) | 0.081 (5) | 0.005 (3) | 0.003 (3) | −0.002 (3) |
C10 | 0.041 (3) | 0.044 (3) | 0.066 (4) | −0.014 (3) | 0.025 (3) | −0.005 (3) |
C11 | 0.032 (3) | 0.050 (3) | 0.066 (4) | −0.006 (3) | −0.012 (3) | −0.017 (3) |
C12 | 0.045 (3) | 0.100 (6) | 0.026 (3) | 0.009 (4) | 0.008 (2) | −0.001 (3) |
Fe1—C1 | 2.079 (6) | N1—C8 | 1.157 (6) |
Fe1—C2 | 2.088 (6) | C1—C2 | 1.406 (9) |
Fe1—C3 | 2.099 (5) | C1—C5 | 1.396 (9) |
Fe1—C4 | 2.090 (5) | C1—H1 | 0.947 |
Fe1—C5 | 2.088 (5) | C2—C3 | 1.398 (8) |
Fe1—C6 | 1.786 (6) | C2—H2 | 0.948 |
Fe1—C7 | 1.791 (6) | C3—C4 | 1.401 (7) |
Fe1—C8 | 1.862 (4) | C3—H3 | 0.950 |
S1—O3 | 1.430 (5) | C4—C5 | 1.414 (8) |
S1—O4 | 1.436 (5) | C4—H4 | 0.951 |
S1—O5 | 1.426 (6) | C5—H5 | 0.951 |
S1—C12 | 1.810 (8) | C9—H6 | 0.951 |
Si1—N1 | 1.794 (4) | C9—H7 | 0.950 |
Si1—C9 | 1.842 (6) | C9—H8 | 0.950 |
Si1—C10 | 1.840 (7) | C10—H9 | 0.951 |
Si1—C11 | 1.842 (7) | C10—H10 | 0.949 |
F1—C12 | 1.343 (10) | C10—H11 | 0.951 |
F2—C12 | 1.309 (8) | C11—H12 | 0.948 |
F3—C12 | 1.325 (8) | C11—H13 | 0.950 |
O1—C6 | 1.134 (9) | C11—H14 | 0.951 |
O2—C7 | 1.143 (7) | ||
F1···C2i | 3.391 (7) | O2···C6ii | 3.529 (8) |
F1···C3i | 3.528 (7) | O3···C5v | 3.200 (7) |
F3···N1i | 3.174 (6) | O3···C3i | 3.279 (7) |
F3···C8i | 3.368 (7) | O3···C11vi | 3.560 (8) |
F3···O1ii | 3.384 (9) | O3···C7v | 3.567 (7) |
F3···C10i | 3.426 (8) | O3···C1v | 3.586 (8) |
O1···O1iii | 3.22 (1) | O4···C1vii | 3.207 (8) |
O1···C10iii | 3.443 (9) | O4···C2vii | 3.256 (8) |
O1···C6iii | 3.492 (9) | O4···C10vi | 3.537 (8) |
O2···C8ii | 3.339 (7) | O5···C2vii | 3.457 (8) |
O2···C7ii | 3.355 (7) | O5···C10viii | 3.477 (8) |
O2···O2ii | 3.404 (10) | O5···C5v | 3.539 (8) |
O2···N1ii | 3.420 (6) | C3···C11ix | 3.562 (8) |
O2···O3iv | 3.504 (7) | ||
C1—Fe1—C2 | 39.4 (2) | Fe1—C2—H2 | 124.5 |
C1—Fe1—C3 | 65.6 (2) | C1—C2—C3 | 107.7 (5) |
C1—Fe1—C4 | 66.1 (2) | C1—C2—H2 | 126.2 |
C1—Fe1—C5 | 39.2 (2) | C3—C2—H2 | 126.2 |
C1—Fe1—C6 | 96.5 (3) | Fe1—C3—C2 | 70.0 (3) |
C1—Fe1—C7 | 109.9 (3) | Fe1—C3—C4 | 70.1 (3) |
C1—Fe1—C8 | 154.0 (2) | Fe1—C3—H3 | 125.9 |
C2—Fe1—C3 | 39.0 (2) | C2—C3—C4 | 108.7 (5) |
C2—Fe1—C4 | 66.0 (2) | C2—C3—H3 | 125.6 |
C2—Fe1—C5 | 65.9 (2) | C4—C3—H3 | 125.7 |
C2—Fe1—C6 | 91.6 (3) | Fe1—C4—C3 | 70.8 (3) |
C2—Fe1—C7 | 149.3 (2) | Fe1—C4—C5 | 70.2 (3) |
C2—Fe1—C8 | 116.5 (2) | Fe1—C4—H4 | 124.3 |
C3—Fe1—C4 | 39.1 (2) | C3—C4—C5 | 107.3 (5) |
C3—Fe1—C5 | 65.6 (2) | C3—C4—H4 | 126.2 |
C3—Fe1—C6 | 121.9 (3) | C5—C4—H4 | 126.4 |
C3—Fe1—C7 | 143.2 (2) | Fe1—C5—C1 | 70.1 (3) |
C3—Fe1—C8 | 88.8 (2) | Fe1—C5—C4 | 70.3 (3) |
C4—Fe1—C5 | 39.6 (2) | Fe1—C5—H5 | 125.3 |
C4—Fe1—C6 | 157.6 (2) | C1—C5—C4 | 108.1 (5) |
C4—Fe1—C7 | 104.5 (2) | C1—C5—H5 | 126.0 |
C4—Fe1—C8 | 97.3 (2) | C4—C5—H5 | 126.0 |
C5—Fe1—C6 | 131.8 (3) | Fe1—C6—O1 | 178.8 (6) |
C5—Fe1—C7 | 88.1 (2) | Fe1—C7—O2 | 178.8 (5) |
C5—Fe1—C8 | 134.8 (2) | Fe1—C8—N1 | 178.2 (4) |
C6—Fe1—C7 | 94.6 (3) | Si1—C9—H6 | 109.5 |
C6—Fe1—C8 | 93.2 (2) | Si1—C9—H7 | 109.5 |
C7—Fe1—C8 | 93.1 (2) | Si1—C9—H8 | 109.5 |
O3—S1—O4 | 116.2 (3) | H6—C9—H7 | 109.4 |
O3—S1—O5 | 113.9 (3) | H6—C9—H8 | 109.4 |
O3—S1—C12 | 102.5 (3) | H7—C9—H8 | 109.5 |
O4—S1—O5 | 114.2 (3) | Si1—C10—H9 | 109.5 |
O4—S1—C12 | 102.4 (3) | Si1—C10—H10 | 109.6 |
O5—S1—C12 | 105.5 (4) | Si1—C10—H11 | 109.5 |
N1—Si1—C9 | 103.8 (2) | H9—C10—H10 | 109.5 |
N1—Si1—C10 | 106.3 (2) | H9—C10—H11 | 109.3 |
N1—Si1—C11 | 104.8 (2) | H10—C10—H11 | 109.5 |
C9—Si1—C10 | 113.8 (3) | Si1—C11—H12 | 109.5 |
C9—Si1—C11 | 114.1 (3) | Si1—C11—H13 | 109.4 |
C10—Si1—C11 | 112.8 (3) | Si1—C11—H14 | 109.4 |
Si1—N1—C8 | 174.7 (4) | H12—C11—H13 | 109.6 |
Fe1—C1—C2 | 70.6 (3) | H12—C11—H14 | 109.5 |
Fe1—C1—C5 | 70.8 (3) | H13—C11—H14 | 109.3 |
Fe1—C1—H1 | 124.4 | S1—C12—F1 | 110.5 (5) |
C2—C1—C5 | 108.2 (5) | S1—C12—F2 | 112.9 (6) |
C2—C1—H1 | 126.2 | S1—C12—F3 | 111.3 (6) |
C5—C1—H1 | 125.6 | F1—C12—F2 | 105.9 (6) |
Fe1—C2—C1 | 70.0 (3) | F1—C12—F3 | 107.3 (6) |
Fe1—C2—C3 | 71.0 (3) | F2—C12—F3 | 108.6 (5) |
F1—C12—S1—O3 | −61.4 (4) | F2—C12—S1—O5 | 60.8 (6) |
F1—C12—S1—O4 | 59.4 (5) | F3—C12—S1—O3 | 57.8 (6) |
F1—C12—S1—O5 | 179.2 (4) | F3—C12—S1—O4 | 178.5 (5) |
F2—C12—S1—O3 | −179.7 (5) | F3—C12—S1—O5 | −61.7 (6) |
F2—C12—S1—O4 | −59.0 (6) |
Symmetry codes: (i) x, y, z−1; (ii) −x+1, −y+1, −z+1; (iii) −x+1, −y+1, −z+2; (iv) −x+3/2, y+1/2, −z+1/2; (v) −x+3/2, y−1/2, −z+1/2; (vi) x+1/2, −y+1/2, z−1/2; (vii) −x+3/2, y−1/2, −z+3/2; (viii) −x+1, −y, −z+1; (ix) x+1/2, −y+1/2, z+1/2. |
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