Supporting information
Crystallographic Information File (CIF) https://doi.org/10.1107/S1600536805005003/cf6407sup1.cif | |
Structure factor file (CIF format) https://doi.org/10.1107/S1600536805005003/cf6407Isup2.hkl |
CCDC reference: 269403
Data collection: CAD-4 EXPRESS (Enraf–Nonius, 1992); cell refinement: CAD-4 EXPRESS; data reduction: XCAD4 (Harms, 1996); program(s) used to solve structure: SHELXS97 (Sheldrick, 1997); program(s) used to refine structure: SHELXL97 (Sheldrick, 1997); molecular graphics: PLATON (Spek, 2003); software used to prepare material for publication: SHELXL97.
[Re(C2F3O2)(C20H24N2)(CO)3] | F(000) = 1320 |
Mr = 675.66 | Dx = 1.690 Mg m−3 |
Monoclinic, P21/c | Mo Kα radiation, λ = 0.71073 Å |
Hall symbol: -P 2ybc | Cell parameters from 25 reflections |
a = 12.818 (3) Å | θ = 14.0–15.9° |
b = 13.026 (3) Å | µ = 4.63 mm−1 |
c = 16.554 (4) Å | T = 293 K |
β = 106.07 (2)° | Block, dark red |
V = 2655.9 (11) Å3 | 0.55 × 0.30 × 0.30 mm |
Z = 4 |
Enraf–Nonius CAD-4 diffractometer | 2977 reflections with I > 2σ(I) |
Radiation source: fine-focus sealed X-ray tube | Rint = 0.015 |
Graphite monochromator | θmax = 26.3°, θmin = 2.6° |
ω–2θ scans | h = 0→15 |
Absorption correction: ψ scan (DATCOR; Reibenspies, 1989) | k = 0→16 |
Tmin = 0.137, Tmax = 0.250 | l = −20→19 |
5775 measured reflections | 3 standard reflections every 60 min |
5369 independent reflections | intensity decay: 3% |
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)] = 0.042 | Hydrogen site location: inferred from neighbouring sites |
wR(F2) = 0.087 | H-atom parameters constrained |
S = 0.92 | w = 1/[σ2(Fo2) + (0.0422P)2] where P = (Fo2 + 2Fc2)/3 |
5369 reflections | (Δ/σ)max = 0.004 |
335 parameters | Δρmax = 0.76 e Å−3 |
0 restraints | Δρmin = −0.63 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. Least-squares planes (x,y,z in crystal coordinates) and deviations from them (* indicates atom used to define plane) - 1.6263 (0.0298) x + 9.3049 (0.0251) y + 11.5288 (0.0329) z = 4.1307 (0.0086) * 0.0101 (0.0041) N1 * 0.0068 (0.0057) C2 * 0.0060 (0.0060) C3 * -0.0168 (0.0041) N4 * -0.0149 (0.0039) C2A * 0.0088 (0.0039) C3A 0.1421 (0.0074) Re1 Rms deviation of fitted atoms = 0.0113 - 0.9022 (0.0308) x + 10.3125 (0.0171) y + 9.9760 (0.0277) z = 4.3039 (0.0065) Angle to previous plane (with approximate e.s.d.) = 7.20 (0.34) * -0.0149 (0.0031) N1 * 0.0150 (0.0031) N4 * 0.0143 (0.0029) C5 * -0.0144 (0.0030) C6 - 0.0684 (0.0033) Re1 0.1363 (0.0087) C2 0.1688 (0.0091) C3 Rms deviation of fitted atoms = 0.0146 2.5347 (0.0379) x + 9.5766 (0.0308) y - 11.2199 (0.0425) z = 1.3603 (0.0146) Angle to previous plane (with approximate e.s.d.) = 79.94 (0.17) * -0.0008 (0.0053) C11 * 0.0055 (0.0052) C12 * -0.0083 (0.0057) C13 * 0.0060 (0.0061) C14 * -0.0012 (0.0065) C15 * -0.0013 (0.0059) C16 Rms deviation of fitted atoms = 0.0048 - 2.2442 (0.1026) x + 9.6505 (0.0276) y + 11.1169 (0.0404) z = 4.0982 (0.0185) Angle to previous plane (with approximate e.s.d.) = 84.86 (0.22) * 0.0000 (0.0000) Re1 * 0.0000 (0.0000) N1 * 0.0000 (0.0000) C2 Rms deviation of fitted atoms = 0.0000 5.2381 (0.0431) x + 7.9671 (0.0443) y - 12.6485 (0.0461) z = 1.4195 (0.0299) Angle to previous plane (with approximate e.s.d.) = 86.69 (0.29) * 0.0102 (0.0063) C21_a * 0.0044 (0.0078) C22_a * -0.0027 (0.0089) C23_a * -0.0148 (0.0084) C24_a * 0.0299 (0.0076) C25_a * -0.0270 (0.0063) C26_a Rms deviation of fitted atoms = 0.0182 - 0.4186 (0.0861) x + 9.3460 (0.0519) y + 11.2180 (0.0424) z = 4.4705 (0.0189) Angle to previous plane (with approximate e.s.d.) = 87.37 (0.30) * 0.0000 (0.0000) Re1 * 0.0000 (0.0000) N4 * 0.0000 (0.0000) C3 Rms deviation of fitted atoms = 0.0000 |
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 | Occ. (<1) | |
Re1 | 0.22160 (2) | 0.18855 (2) | 0.249699 (16) | 0.05297 (11) | |
F1 | 0.2107 (7) | 0.4698 (4) | 0.4842 (4) | 0.185 (3) | |
F2 | 0.3182 (10) | 0.5000 (7) | 0.4193 (7) | 0.258 (7) | |
F3 | 0.1603 (12) | 0.5073 (7) | 0.3587 (6) | 0.271 (7) | |
O1 | 0.2349 (4) | 0.3334 (3) | 0.3149 (3) | 0.0715 (15) | |
O2 | 0.2327 (6) | 0.2774 (5) | 0.4417 (4) | 0.106 (2) | |
O5 | 0.0366 (4) | 0.1144 (4) | 0.3187 (4) | 0.0939 (19) | |
O6 | 0.3878 (5) | 0.0757 (5) | 0.3897 (3) | 0.106 (2) | |
O7 | 0.1974 (5) | −0.0142 (4) | 0.1544 (4) | 0.0971 (19) | |
N1 | 0.1286 (4) | 0.2835 (4) | 0.1485 (3) | 0.0502 (14) | |
N4 | 0.3364 (4) | 0.2606 (5) | 0.1939 (3) | 0.0547 (14) | |
C2 | 0.1806 (6) | 0.3401 (5) | 0.1099 (4) | 0.0566 (19) | |
C2A | 0.1294 (6) | 0.4136 (6) | 0.0415 (5) | 0.082 (2) | |
H2A1 | 0.0520 | 0.4121 | 0.0316 | 0.123* | 0.50 |
H2A2 | 0.1474 | 0.3944 | −0.0090 | 0.123* | 0.50 |
H2A3 | 0.1558 | 0.4816 | 0.0577 | 0.123* | 0.50 |
H2A4 | 0.1848 | 0.4466 | 0.0219 | 0.123* | 0.50 |
H2A5 | 0.0894 | 0.4644 | 0.0626 | 0.123* | 0.50 |
H2A6 | 0.0810 | 0.3771 | −0.0042 | 0.123* | 0.50 |
C3 | 0.3004 (6) | 0.3280 (6) | 0.1365 (4) | 0.062 (2) | |
C3A | 0.3703 (6) | 0.3911 (7) | 0.0956 (5) | 0.089 (3) | |
H3A1 | 0.4453 | 0.3741 | 0.1201 | 0.133* | 0.50 |
H3A2 | 0.3593 | 0.4628 | 0.1042 | 0.133* | 0.50 |
H3A3 | 0.3509 | 0.3768 | 0.0364 | 0.133* | 0.50 |
H3A4 | 0.3250 | 0.4350 | 0.0537 | 0.133* | 0.50 |
H3A5 | 0.4110 | 0.3463 | 0.0696 | 0.133* | 0.50 |
H3A6 | 0.4194 | 0.4323 | 0.1374 | 0.133* | 0.50 |
C5 | 0.1065 (6) | 0.1436 (6) | 0.2940 (5) | 0.0614 (19) | |
C6 | 0.3228 (7) | 0.1175 (6) | 0.3377 (5) | 0.070 (2) | |
C7 | 0.2063 (6) | 0.0640 (6) | 0.1878 (5) | 0.064 (2) | |
C8 | 0.2346 (7) | 0.3425 (7) | 0.3917 (6) | 0.080 (3) | |
C9 | 0.2362 (16) | 0.4553 (10) | 0.4178 (8) | 0.140 (5) | |
C11 | 0.0109 (5) | 0.2880 (5) | 0.1271 (4) | 0.0520 (18) | |
C12 | −0.0506 (6) | 0.2293 (5) | 0.0626 (4) | 0.0612 (19) | |
C13 | −0.1619 (6) | 0.2381 (6) | 0.0462 (5) | 0.076 (2) | |
H13 | −0.2052 | 0.1977 | 0.0036 | 0.091* | |
C14 | −0.2120 (7) | 0.3026 (7) | 0.0887 (6) | 0.082 (2) | |
C15 | −0.1486 (7) | 0.3594 (7) | 0.1521 (6) | 0.093 (3) | |
H15 | −0.1808 | 0.4032 | 0.1826 | 0.111* | |
C16 | −0.0357 (6) | 0.3531 (6) | 0.1722 (5) | 0.081 (2) | |
H16 | 0.0074 | 0.3925 | 0.2156 | 0.097* | |
C121 | −0.0026 (8) | 0.1595 (7) | 0.0109 (6) | 0.117 (3) | |
H12A | −0.0598 | 0.1263 | −0.0309 | 0.175* | 0.50 |
H12B | 0.0415 | 0.1087 | 0.0465 | 0.175* | 0.50 |
H12C | 0.0414 | 0.1988 | −0.0163 | 0.175* | 0.50 |
H12D | 0.0752 | 0.1629 | 0.0304 | 0.175* | 0.50 |
H12E | −0.0261 | 0.1805 | −0.0470 | 0.175* | 0.50 |
H12F | −0.0260 | 0.0904 | 0.0159 | 0.175* | 0.50 |
C141 | −0.3354 (7) | 0.3117 (7) | 0.0654 (7) | 0.123 (4) | |
H14A | −0.3671 | 0.2651 | 0.0204 | 0.185* | 0.50 |
H14B | −0.3564 | 0.3807 | 0.0479 | 0.185* | 0.50 |
H14C | −0.3603 | 0.2949 | 0.1134 | 0.185* | 0.50 |
H14D | −0.3554 | 0.3620 | 0.1008 | 0.185* | 0.50 |
H14E | −0.3661 | 0.2465 | 0.0732 | 0.185* | 0.50 |
H14F | −0.3622 | 0.3322 | 0.0077 | 0.185* | 0.50 |
C21 | 0.4503 (6) | 0.2414 (6) | 0.2254 (4) | 0.065 (2) | |
C22 | 0.4939 (7) | 0.1602 (9) | 0.1929 (6) | 0.114 (4) | |
H22 | 0.4506 | 0.1205 | 0.1499 | 0.137* | 0.349 (15) |
C221 | 0.4364 (12) | 0.1134 (15) | 0.1093 (11) | 0.195 (12) | 0.651 (15) |
H22A | 0.4792 | 0.0580 | 0.0973 | 0.293* | 0.325 (8) |
H22B | 0.4264 | 0.1646 | 0.0661 | 0.293* | 0.325 (8) |
H22C | 0.3670 | 0.0877 | 0.1112 | 0.293* | 0.325 (8) |
H22D | 0.3692 | 0.1488 | 0.0858 | 0.293* | 0.325 (8) |
H22E | 0.4220 | 0.0422 | 0.1170 | 0.293* | 0.325 (8) |
H22F | 0.4815 | 0.1191 | 0.0718 | 0.293* | 0.325 (8) |
C23 | 0.6041 (9) | 0.1384 (10) | 0.2253 (7) | 0.142 (5) | |
H23 | 0.6333 | 0.0837 | 0.2026 | 0.170* | |
C24 | 0.6686 (7) | 0.1917 (12) | 0.2866 (7) | 0.114 (4) | |
C241 | 0.7906 (7) | 0.1702 (10) | 0.3168 (7) | 0.172 (6) | |
H24A | 0.8236 | 0.2147 | 0.3630 | 0.258* | 0.5 |
H24B | 0.8226 | 0.1823 | 0.2716 | 0.258* | 0.5 |
H24C | 0.8023 | 0.1000 | 0.3346 | 0.258* | 0.5 |
H24D | 0.8087 | 0.1166 | 0.2831 | 0.258* | 0.5 |
H24E | 0.8097 | 0.1490 | 0.3746 | 0.258* | 0.5 |
H24F | 0.8300 | 0.2314 | 0.3115 | 0.258* | 0.5 |
C25 | 0.6258 (9) | 0.2732 (10) | 0.3166 (7) | 0.111 (4) | |
H25 | 0.6720 | 0.3150 | 0.3564 | 0.134* | |
C26 | 0.5154 (7) | 0.2974 (6) | 0.2907 (5) | 0.079 (2) | |
H26 | 0.4869 | 0.3495 | 0.3165 | 0.095* | 0.651 (15) |
C261 | 0.493 (2) | 0.3883 (17) | 0.3185 (15) | 0.098 (10) | 0.349 (15) |
H26A | 0.5523 | 0.4102 | 0.3643 | 0.148* | 0.175 (8) |
H26B | 0.4285 | 0.3825 | 0.3375 | 0.148* | 0.175 (8) |
H26C | 0.4804 | 0.4377 | 0.2738 | 0.148* | 0.175 (8) |
H26D | 0.4218 | 0.4100 | 0.2861 | 0.148* | 0.175 (8) |
H26E | 0.5456 | 0.4377 | 0.3130 | 0.148* | 0.175 (8) |
H26F | 0.4937 | 0.3825 | 0.3766 | 0.148* | 0.175 (8) |
U11 | U22 | U33 | U12 | U13 | U23 | |
Re1 | 0.05039 (17) | 0.06053 (18) | 0.05120 (16) | 0.00330 (18) | 0.01940 (11) | −0.00117 (18) |
F1 | 0.365 (10) | 0.107 (5) | 0.145 (5) | −0.040 (5) | 0.173 (7) | −0.047 (4) |
F2 | 0.424 (17) | 0.186 (8) | 0.250 (11) | −0.201 (11) | 0.239 (13) | −0.115 (8) |
F3 | 0.48 (2) | 0.110 (6) | 0.170 (8) | 0.085 (9) | 0.012 (9) | −0.059 (6) |
O1 | 0.104 (4) | 0.054 (4) | 0.068 (3) | −0.011 (3) | 0.044 (3) | −0.014 (3) |
O2 | 0.180 (7) | 0.085 (5) | 0.072 (4) | −0.006 (4) | 0.065 (4) | 0.005 (3) |
O5 | 0.070 (4) | 0.102 (5) | 0.123 (5) | −0.004 (3) | 0.050 (4) | 0.014 (4) |
O6 | 0.099 (5) | 0.133 (6) | 0.081 (4) | 0.031 (4) | 0.015 (3) | 0.034 (4) |
O7 | 0.136 (5) | 0.065 (4) | 0.090 (4) | 0.003 (4) | 0.031 (4) | −0.010 (3) |
N1 | 0.050 (3) | 0.051 (4) | 0.052 (3) | 0.007 (3) | 0.019 (3) | −0.002 (3) |
N4 | 0.045 (3) | 0.074 (4) | 0.048 (3) | −0.002 (3) | 0.018 (3) | −0.010 (3) |
C2 | 0.064 (5) | 0.059 (5) | 0.046 (4) | 0.005 (4) | 0.013 (4) | 0.002 (3) |
C2A | 0.086 (6) | 0.077 (6) | 0.084 (6) | 0.008 (5) | 0.025 (5) | 0.017 (5) |
C3 | 0.073 (5) | 0.067 (5) | 0.050 (4) | −0.002 (4) | 0.022 (4) | −0.005 (4) |
C3A | 0.073 (5) | 0.119 (8) | 0.078 (5) | −0.024 (5) | 0.029 (4) | 0.019 (5) |
C5 | 0.049 (4) | 0.064 (5) | 0.074 (5) | 0.007 (4) | 0.022 (4) | −0.007 (4) |
C6 | 0.071 (5) | 0.074 (6) | 0.078 (6) | 0.004 (4) | 0.043 (5) | 0.001 (5) |
C7 | 0.067 (5) | 0.060 (5) | 0.068 (5) | −0.008 (4) | 0.022 (4) | 0.012 (4) |
C8 | 0.110 (7) | 0.077 (7) | 0.072 (6) | −0.024 (5) | 0.054 (5) | −0.028 (5) |
C9 | 0.245 (16) | 0.112 (11) | 0.103 (9) | −0.012 (11) | 0.113 (11) | −0.004 (8) |
C11 | 0.042 (4) | 0.056 (5) | 0.058 (4) | 0.004 (3) | 0.014 (3) | 0.000 (3) |
C12 | 0.058 (5) | 0.061 (5) | 0.066 (5) | 0.007 (4) | 0.019 (4) | −0.013 (4) |
C13 | 0.060 (5) | 0.074 (5) | 0.083 (6) | −0.001 (4) | 0.003 (4) | −0.004 (5) |
C14 | 0.060 (5) | 0.091 (7) | 0.097 (6) | 0.013 (5) | 0.024 (5) | 0.006 (6) |
C15 | 0.066 (6) | 0.121 (8) | 0.096 (7) | 0.028 (6) | 0.031 (5) | −0.015 (6) |
C16 | 0.066 (5) | 0.092 (6) | 0.085 (6) | 0.013 (5) | 0.021 (5) | −0.028 (5) |
C121 | 0.086 (6) | 0.135 (9) | 0.117 (7) | 0.015 (6) | 0.009 (6) | −0.050 (6) |
C141 | 0.057 (5) | 0.143 (9) | 0.174 (10) | 0.010 (6) | 0.039 (6) | 0.006 (8) |
C21 | 0.054 (5) | 0.089 (6) | 0.059 (5) | 0.010 (4) | 0.025 (4) | 0.001 (4) |
C22 | 0.061 (6) | 0.186 (11) | 0.093 (7) | 0.011 (7) | 0.018 (5) | −0.056 (7) |
C221 | 0.078 (11) | 0.25 (2) | 0.23 (2) | 0.040 (13) | −0.007 (12) | −0.177 (19) |
C23 | 0.068 (7) | 0.245 (14) | 0.114 (8) | 0.047 (8) | 0.026 (6) | −0.063 (9) |
C24 | 0.047 (5) | 0.194 (13) | 0.103 (8) | 0.011 (8) | 0.023 (5) | 0.034 (9) |
C241 | 0.035 (5) | 0.327 (18) | 0.144 (9) | 0.018 (8) | 0.009 (5) | 0.050 (11) |
C25 | 0.069 (7) | 0.140 (10) | 0.101 (8) | −0.029 (7) | −0.016 (6) | 0.021 (7) |
C26 | 0.076 (6) | 0.073 (7) | 0.075 (5) | −0.010 (5) | −0.001 (4) | −0.008 (5) |
C21A | 0.054 (5) | 0.089 (6) | 0.059 (5) | 0.010 (4) | 0.025 (4) | 0.001 (4) |
C22A | 0.061 (6) | 0.186 (11) | 0.093 (7) | 0.011 (7) | 0.018 (5) | −0.056 (7) |
C23A | 0.068 (7) | 0.245 (14) | 0.114 (8) | 0.047 (8) | 0.026 (6) | −0.063 (9) |
C24A | 0.047 (5) | 0.194 (13) | 0.103 (8) | 0.011 (8) | 0.023 (5) | 0.034 (9) |
C242 | 0.035 (5) | 0.327 (18) | 0.144 (9) | 0.018 (8) | 0.009 (5) | 0.050 (11) |
C25A | 0.069 (7) | 0.140 (10) | 0.101 (8) | −0.029 (7) | −0.016 (6) | 0.021 (7) |
C26A | 0.076 (6) | 0.073 (7) | 0.075 (5) | −0.010 (5) | −0.001 (4) | −0.008 (5) |
C261 | 0.11 (2) | 0.055 (17) | 0.11 (2) | 0.007 (14) | 0.009 (16) | −0.038 (15) |
Re1—C7 | 1.900 (9) | C15—H15 | 0.93 |
Re1—C6 | 1.901 (9) | C16—H16 | 0.93 |
Re1—C5 | 1.912 (8) | C121—H12A | 0.96 |
Re1—N4 | 2.156 (5) | C121—H12B | 0.96 |
Re1—N1 | 2.157 (5) | C121—H12C | 0.96 |
Re1—O1 | 2.157 (4) | C121—H12D | 0.96 |
F1—C9 | 1.245 (10) | C121—H12E | 0.96 |
F2—C9 | 1.196 (17) | C121—H12F | 0.96 |
F3—C9 | 1.356 (16) | C141—H14A | 0.96 |
O1—C8 | 1.278 (9) | C141—H14B | 0.96 |
O2—C8 | 1.190 (9) | C141—H14C | 0.96 |
O5—C5 | 1.149 (7) | C141—H14D | 0.96 |
O7—C7 | 1.149 (8) | C141—H14E | 0.96 |
O6—C6 | 1.155 (8) | C141—H14F | 0.96 |
N1—C2 | 1.277 (8) | C21—C22 | 1.374 (11) |
N1—C11 | 1.452 (8) | C21—C26 | 1.377 (10) |
N4—C3 | 1.282 (8) | C22—C23 | 1.395 (12) |
N4—C21 | 1.430 (8) | C22—C221 | 1.505 (15) |
C2—C3 | 1.484 (10) | C221—H22A | 0.96 |
C2—C2A | 1.490 (9) | C221—H22B | 0.96 |
C2A—H2A1 | 0.96 | C221—H22C | 0.96 |
C2A—H2A2 | 0.96 | C221—H22D | 0.96 |
C2A—H2A3 | 0.96 | C221—H22E | 0.96 |
C2A—H2A4 | 0.96 | C221—H22F | 0.96 |
C2A—H2A5 | 0.96 | C23—C24 | 1.316 (14) |
C2A—H2A6 | 0.96 | C23—H23 | 0.93 |
C3—C3A | 1.508 (9) | C24—C25 | 1.351 (13) |
C3A—H3A1 | 0.96 | C24—C241 | 1.530 (12) |
C3A—H3A2 | 0.96 | C241—H24A | 0.96 |
C3A—H3A3 | 0.96 | C241—H24B | 0.96 |
C3A—H3A4 | 0.96 | C241—H24C | 0.96 |
C3A—H3A5 | 0.96 | C241—H24D | 0.96 |
C3A—H3A6 | 0.96 | C241—H24E | 0.96 |
C8—C9 | 1.530 (14) | C241—H24F | 0.96 |
C11—C12 | 1.371 (9) | C25—C26 | 1.396 (13) |
C11—C16 | 1.372 (9) | C25—H25 | 0.93 |
C12—C13 | 1.380 (9) | C26—H26 | 0.93 |
C12—C121 | 1.493 (10) | C261—H26A | 0.96 |
C13—C14 | 1.366 (10) | C261—H26B | 0.96 |
C13—H13 | 0.93 | C261—H26C | 0.96 |
C14—C15 | 1.356 (11) | C261—H26D | 0.96 |
C14—C141 | 1.525 (11) | C261—H26E | 0.96 |
C15—C16 | 1.395 (10) | C261—H26F | 0.96 |
C7—Re1—C6 | 86.8 (3) | C14—C15—H15 | 119.6 |
C7—Re1—C5 | 88.3 (3) | C16—C15—H15 | 119.6 |
C6—Re1—C5 | 89.6 (3) | C11—C16—C15 | 119.1 (7) |
C7—Re1—N4 | 97.0 (2) | C11—C16—H16 | 120.5 |
C6—Re1—N4 | 98.0 (3) | C15—C16—H16 | 120.5 |
C5—Re1—N4 | 171.0 (3) | C12—C121—H12A | 109.5 |
C7—Re1—N1 | 96.8 (2) | C12—C121—H12B | 109.5 |
C6—Re1—N1 | 170.9 (3) | H12A—C121—H12B | 109.5 |
C5—Re1—N1 | 98.9 (3) | C12—C121—H12C | 109.5 |
N4—Re1—N1 | 73.4 (2) | H12A—C121—H12C | 109.5 |
C7—Re1—O1 | 177.4 (2) | H12B—C121—H12C | 109.5 |
C6—Re1—O1 | 95.7 (3) | C12—C121—H12D | 109.5 |
C5—Re1—O1 | 92.2 (2) | C12—C121—H12E | 109.5 |
N4—Re1—O1 | 82.22 (19) | H12D—C121—H12E | 109.5 |
N1—Re1—O1 | 80.61 (18) | C12—C121—H12F | 109.5 |
C8—O1—Re1 | 123.8 (5) | H12D—C121—H12F | 109.5 |
C2—N1—C11 | 120.4 (6) | H12E—C121—H12F | 109.5 |
C2—N1—Re1 | 117.8 (5) | C14—C141—H14A | 109.5 |
C11—N1—Re1 | 121.7 (4) | C14—C141—H14B | 109.5 |
C3—N4—C21 | 120.8 (6) | H14A—C141—H14B | 109.5 |
C3—N4—Re1 | 117.9 (5) | C14—C141—H14C | 109.5 |
C21—N4—Re1 | 121.1 (5) | H14A—C141—H14C | 109.5 |
N1—C2—C3 | 115.5 (6) | H14B—C141—H14C | 109.5 |
N1—C2—C2A | 124.8 (7) | C14—C141—H14D | 109.5 |
C3—C2—C2A | 119.7 (7) | C14—C141—H14E | 109.5 |
C2—C2A—H2A1 | 109.5 | H14D—C141—H14E | 109.5 |
C2—C2A—H2A2 | 109.5 | C14—C141—H14F | 109.5 |
H2A1—C2A—H2A2 | 109.5 | H14D—C141—H14F | 109.5 |
C2—C2A—H2A3 | 109.5 | H14E—C141—H14F | 109.5 |
H2A1—C2A—H2A3 | 109.5 | C22—C21—C26 | 119.4 (8) |
H2A2—C2A—H2A3 | 109.5 | C22—C21—N4 | 118.5 (7) |
C2—C2A—H2A4 | 109.5 | C26—C21—N4 | 122.0 (7) |
C2—C2A—H2A5 | 109.5 | C21—C22—C23 | 119.0 (9) |
H2A4—C2A—H2A5 | 109.5 | C21—C22—C221 | 121.6 (10) |
C2—C2A—H2A6 | 109.5 | C23—C22—C221 | 117.2 (9) |
H2A4—C2A—H2A6 | 109.5 | C22—C221—H22A | 109.5 |
H2A5—C2A—H2A6 | 109.5 | C22—C221—H22B | 109.5 |
N4—C3—C2 | 115.0 (6) | H22A—C221—H22B | 109.5 |
N4—C3—C3A | 124.8 (7) | C22—C221—H22C | 109.5 |
C2—C3—C3A | 120.2 (7) | H22A—C221—H22C | 109.5 |
C3—C3A—H3A1 | 109.5 | H22B—C221—H22C | 109.5 |
C3—C3A—H3A2 | 109.5 | C22—C221—H22D | 109.5 |
H3A1—C3A—H3A2 | 109.5 | C22—C221—H22E | 109.5 |
C3—C3A—H3A3 | 109.5 | H22D—C221—H22E | 109.5 |
H3A1—C3A—H3A3 | 109.5 | C22—C221—H22F | 109.5 |
H3A2—C3A—H3A3 | 109.5 | H22D—C221—H22F | 109.5 |
C3—C3A—H3A4 | 109.5 | H22E—C221—H22F | 109.5 |
C3—C3A—H3A5 | 109.5 | C24—C23—C22 | 122.8 (10) |
H3A4—C3A—H3A5 | 109.5 | C24—C23—H23 | 118.6 |
C3—C3A—H3A6 | 109.5 | C22—C23—H23 | 118.6 |
H3A4—C3A—H3A6 | 109.5 | C23—C24—C25 | 117.8 (10) |
H3A5—C3A—H3A6 | 109.5 | C23—C24—C241 | 121.5 (13) |
O5—C5—Re1 | 177.9 (7) | C25—C24—C241 | 120.4 (12) |
O7—C7—Re1 | 176.2 (6) | C24—C241—H24A | 109.5 |
O6—C6—Re1 | 177.0 (7) | C24—C241—H24B | 109.5 |
O2—C8—O1 | 129.3 (8) | H24A—C241—H24B | 109.5 |
O2—C8—C9 | 119.2 (8) | C24—C241—H24C | 109.5 |
O1—C8—C9 | 111.5 (8) | H24A—C241—H24C | 109.5 |
F2—C9—F1 | 110.7 (15) | H24B—C241—H24C | 109.5 |
F2—C9—F3 | 102.8 (12) | C24—C241—H24D | 109.5 |
F1—C9—F3 | 104.5 (14) | C24—C241—H24E | 109.5 |
F2—C9—C8 | 114.6 (13) | H24D—C241—H24E | 109.5 |
F1—C9—C8 | 114.2 (10) | C24—C241—H24F | 109.5 |
F3—C9—C8 | 109.0 (13) | H24D—C241—H24F | 109.5 |
C12—C11—C16 | 121.7 (7) | H24E—C241—H24F | 109.5 |
C12—C11—N1 | 120.2 (6) | C24—C25—C26 | 123.0 (10) |
C16—C11—N1 | 118.1 (6) | C24—C25—H25 | 118.5 |
C11—C12—C13 | 116.6 (6) | C26—C25—H25 | 118.5 |
C11—C12—C121 | 123.1 (7) | C21—C26—C25 | 117.7 (9) |
C13—C12—C121 | 120.3 (7) | C21—C26—H26 | 121.2 |
C14—C13—C12 | 123.8 (8) | C25—C26—H26 | 121.2 |
C14—C13—H13 | 118.1 | H26A—C261—H26B | 109.5 |
C12—C13—H13 | 118.1 | H26A—C261—H26C | 109.5 |
C15—C14—C13 | 117.9 (8) | H26B—C261—H26C | 109.5 |
C15—C14—C141 | 120.7 (8) | H26D—C261—H26E | 109.5 |
C13—C14—C141 | 121.4 (9) | H26D—C261—H26F | 109.5 |
C14—C15—C16 | 120.8 (8) | H26E—C261—H26F | 109.5 |
C6—Re1—O1—C8 | −45.0 (7) | O2—C8—C9—F3 | −131.9 (12) |
C5—Re1—O1—C8 | 44.7 (7) | O1—C8—C9—F3 | 47.7 (17) |
N4—Re1—O1—C8 | −142.3 (7) | C2—N1—C11—C12 | 85.8 (8) |
N1—Re1—O1—C8 | 143.4 (7) | Re1—N1—C11—C12 | −97.5 (7) |
C7—Re1—N1—C2 | −100.4 (5) | C2—N1—C11—C16 | −93.3 (8) |
C5—Re1—N1—C2 | 170.3 (5) | Re1—N1—C11—C16 | 83.4 (7) |
N4—Re1—N1—C2 | −5.1 (5) | C16—C11—C12—C13 | −0.9 (11) |
O1—Re1—N1—C2 | 79.6 (5) | N1—C11—C12—C13 | −179.9 (6) |
C7—Re1—N1—C11 | 82.9 (5) | C16—C11—C12—C121 | 178.5 (8) |
C5—Re1—N1—C11 | −6.5 (5) | N1—C11—C12—C121 | −0.5 (11) |
N4—Re1—N1—C11 | 178.2 (5) | C11—C12—C13—C14 | 1.7 (12) |
O1—Re1—N1—C11 | −97.2 (5) | C121—C12—C13—C14 | −177.7 (8) |
C7—Re1—N4—C3 | 100.8 (5) | C12—C13—C14—C15 | −1.8 (13) |
C6—Re1—N4—C3 | −171.4 (5) | C12—C13—C14—C141 | 177.8 (8) |
N1—Re1—N4—C3 | 5.8 (5) | C13—C14—C15—C16 | 1.0 (14) |
O1—Re1—N4—C3 | −76.7 (5) | C141—C14—C15—C16 | −178.5 (8) |
C7—Re1—N4—C21 | −85.1 (5) | C12—C11—C16—C15 | 0.3 (12) |
C6—Re1—N4—C21 | 2.7 (6) | N1—C11—C16—C15 | 179.3 (7) |
N1—Re1—N4—C21 | 179.9 (5) | C14—C15—C16—C11 | −0.3 (13) |
O1—Re1—N4—C21 | 97.4 (5) | C3—N4—C21—C22 | −97.1 (10) |
C11—N1—C2—C3 | −179.3 (5) | Re1—N4—C21—C22 | 89.0 (8) |
Re1—N1—C2—C3 | 3.9 (7) | C3—N4—C21—C26 | 87.1 (9) |
C11—N1—C2—C2A | −0.2 (10) | Re1—N4—C21—C26 | −86.8 (8) |
Re1—N1—C2—C2A | −177.0 (5) | C26—C21—C22—C23 | −1.7 (15) |
C21—N4—C3—C2 | −179.9 (6) | N4—C21—C22—C23 | −177.6 (9) |
Re1—N4—C3—C2 | −5.8 (8) | C26—C21—C22—C221 | −164.4 (13) |
C21—N4—C3—C3A | 1.1 (11) | N4—C21—C22—C221 | 19.7 (16) |
Re1—N4—C3—C3A | 175.3 (5) | C21—C22—C23—C24 | 0.6 (19) |
N1—C2—C3—N4 | 1.3 (9) | C221—C22—C23—C24 | 164.0 (15) |
C2A—C2—C3—N4 | −177.9 (6) | C22—C23—C24—C25 | −2 (2) |
N1—C2—C3—C3A | −179.7 (6) | C22—C23—C24—C241 | −175.9 (10) |
Re1—O1—C8—C9 | −175.5 (9) | C23—C24—C25—C26 | 5.6 (18) |
O2—C8—C9—F2 | 113.6 (13) | C241—C24—C25—C26 | 179.2 (9) |
O1—C8—C9—F2 | −66.8 (18) | C22—C21—C26—C25 | 4.6 (13) |
O2—C8—C9—F1 | −16 (2) | N4—C21—C26—C25 | −179.6 (7) |
O1—C8—C9—F1 | 164.0 (13) | C24—C25—C26—C21 | −6.8 (15) |