Supporting information
Crystallographic Information File (CIF) https://doi.org/10.1107/S1600536803004094/lh6039sup1.cif | |
Structure factor file (CIF format) https://doi.org/10.1107/S1600536803004094/lh6039Isup2.hkl |
CCDC reference: 206747
Data collection: SMART (Bruker, 1999); cell refinement: SAINT (Bruker, 1999); data reduction: SAINT; program(s) used to solve structure: SHELXS97 (Sheldrick, 1990); program(s) used to refine structure: SHELXL97 (Sheldrick, 1997); molecular graphics: ORTEP-3 (Farrugia, 1997) and ATOMS (Dowty, 1999); software used to prepare material for publication: SHELXL97.
[Re(C12H12N2)(C18H24N2)2(CO)6](PF6)2·2CH2Cl2 | F(000) = 1692 |
Mr = 1721.28 | Dx = 1.791 Mg m−3 |
Monoclinic, P21/n | Mo Kα radiation, λ = 0.71073 Å |
Hall symbol: -P 2yn | Cell parameters from 6778 reflections |
a = 12.0280 (7) Å | θ = 5.1–62.8° |
b = 10.2060 (6) Å | µ = 4.09 mm−1 |
c = 26.1366 (14) Å | T = 110 K |
β = 95.695 (2)° | Prism, light yellow |
V = 3192.6 (3) Å3 | 0.35 × 0.24 × 0.18 mm |
Z = 2 |
Bruker SMART Apex CCD diffractometer | 7907 independent reflections |
Radiation source: fine-focus sealed tube | 7044 reflections with I > 2σ(I) |
Graphite monochromator | Rint = 0.033 |
ω scans | θmax = 28.3°, θmin = 1.8° |
Absorption correction: multi-scan (SADABS; Sheldrick, 1996) | h = −16→15 |
Tmin = 0.342, Tmax = 0.479 | k = −13→13 |
32788 measured reflections | l = −34→34 |
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)] = 0.035 | Hydrogen site location: inferred from neighbouring sites |
wR(F2) = 0.099 | H-atom parameters constrained |
S = 1.05 | w = 1/[σ2(Fo2) + (0.0534P)2 + 12.0416P] where P = (Fo2 + 2Fc2)/3 |
7907 reflections | (Δ/σ)max = 0.003 |
403 parameters | Δρmax = 2.62 e Å−3 |
0 restraints | Δρmin = −1.61 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. |
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 | ||
Re1 | 0.21451 (1) | 0.29153 (2) | 0.79394 (1) | 0.01789 (6) | |
C1 | 0.2654 (3) | 0.3586 (4) | 0.73119 (16) | 0.0214 (8) | |
O1 | 0.2957 (3) | 0.3944 (3) | 0.69372 (13) | 0.0291 (7) | |
C2 | 0.1185 (4) | 0.1724 (4) | 0.75334 (17) | 0.0219 (8) | |
O2 | 0.0571 (3) | 0.1042 (3) | 0.72950 (13) | 0.0312 (7) | |
C3 | 0.3330 (4) | 0.1620 (4) | 0.79719 (17) | 0.0228 (8) | |
O3 | 0.4015 (3) | 0.0841 (3) | 0.80028 (14) | 0.0313 (7) | |
C4 | 0.2329 (4) | 0.1850 (5) | 0.90675 (19) | 0.0282 (9) | |
H4 | 0.3078 | 0.2053 | 0.9051 | 0.034* | |
N1 | 0.1583 (3) | 0.2145 (3) | 0.86650 (15) | 0.0219 (7) | |
C5 | 0.2012 (4) | 0.1255 (5) | 0.95036 (19) | 0.0309 (10) | |
H5 | 0.2545 | 0.1083 | 0.9778 | 0.037* | |
C6 | 0.0524 (4) | 0.1851 (5) | 0.87012 (18) | 0.0284 (9) | |
H6 | 0.0002 | 0.2064 | 0.8427 | 0.034* | |
C7 | 0.0152 (4) | 0.1244 (5) | 0.91234 (19) | 0.0320 (10) | |
H7 | −0.0603 | 0.1059 | 0.9132 | 0.038* | |
C8 | 0.0918 (4) | 0.0912 (5) | 0.95366 (18) | 0.0288 (9) | |
C9 | 0.0598 (4) | 0.0206 (6) | 1.00082 (18) | 0.0339 (11) | |
H9A | 0.1063 | −0.0568 | 1.0061 | 0.041* | |
H9B | 0.0767 | 0.0773 | 1.0304 | 0.041* | |
N2 | 0.0898 (3) | 0.4417 (3) | 0.80076 (13) | 0.0189 (7) | |
N3 | 0.2979 (3) | 0.4403 (3) | 0.84296 (13) | 0.0190 (7) | |
C10 | −0.0156 (4) | 0.4373 (4) | 0.77867 (17) | 0.0237 (8) | |
H10 | −0.0375 | 0.3644 | 0.7588 | 0.028* | |
C11 | −0.0933 (4) | 0.5345 (4) | 0.78362 (17) | 0.0245 (8) | |
H11 | −0.1657 | 0.5257 | 0.7679 | 0.029* | |
C12 | −0.0628 (3) | 0.6455 (4) | 0.81231 (16) | 0.0224 (8) | |
C13 | 0.0470 (3) | 0.6507 (4) | 0.83518 (16) | 0.0214 (8) | |
H13 | 0.0710 | 0.7237 | 0.8545 | 0.026* | |
C14 | 0.1208 (3) | 0.5489 (4) | 0.82947 (15) | 0.0184 (7) | |
C15 | 0.2383 (3) | 0.5483 (4) | 0.85309 (15) | 0.0184 (7) | |
C16 | 0.2853 (3) | 0.6500 (4) | 0.88320 (16) | 0.0211 (8) | |
H16 | 0.2422 | 0.7231 | 0.8892 | 0.025* | |
C17 | 0.3960 (3) | 0.6444 (4) | 0.90456 (15) | 0.0208 (8) | |
C18 | 0.4557 (3) | 0.5313 (4) | 0.89428 (16) | 0.0226 (8) | |
H18 | 0.5295 | 0.5218 | 0.9082 | 0.027* | |
C19 | 0.4051 (3) | 0.4337 (4) | 0.86351 (16) | 0.0217 (8) | |
H19 | 0.4469 | 0.3602 | 0.8567 | 0.026* | |
C20 | −0.1429 (4) | 0.7596 (5) | 0.82037 (19) | 0.0273 (9) | |
C21 | −0.2608 (4) | 0.7318 (6) | 0.7947 (2) | 0.0337 (11) | |
H21A | −0.2882 | 0.6518 | 0.8082 | 0.051* | |
H21B | −0.2585 | 0.7233 | 0.7583 | 0.051* | |
H21C | −0.3096 | 0.8027 | 0.8017 | 0.051* | |
C22 | −0.0983 (4) | 0.8851 (5) | 0.7969 (2) | 0.0381 (12) | |
H22A | −0.1477 | 0.9567 | 0.8020 | 0.057* | |
H22B | −0.0942 | 0.8723 | 0.7607 | 0.057* | |
H22C | −0.0252 | 0.9045 | 0.8133 | 0.057* | |
C23 | −0.1480 (5) | 0.7800 (6) | 0.8781 (2) | 0.0375 (12) | |
H23A | −0.1748 | 0.7014 | 0.8930 | 0.056* | |
H23B | −0.1977 | 0.8511 | 0.8835 | 0.056* | |
H23C | −0.0747 | 0.8001 | 0.8941 | 0.056* | |
C24 | 0.4519 (4) | 0.7553 (5) | 0.93672 (18) | 0.0262 (9) | |
C25 | 0.4925 (6) | 0.7007 (6) | 0.9904 (2) | 0.0444 (14) | |
H25A | 0.5283 | 0.7693 | 1.0111 | 0.067* | |
H25B | 0.5447 | 0.6309 | 0.9869 | 0.067* | |
H25C | 0.4298 | 0.6681 | 1.0065 | 0.067* | |
C26 | 0.5525 (6) | 0.8042 (6) | 0.9104 (3) | 0.0463 (15) | |
H26A | 0.5277 | 0.8342 | 0.8763 | 0.069* | |
H26B | 0.6049 | 0.7339 | 0.9083 | 0.069* | |
H26C | 0.5879 | 0.8750 | 0.9299 | 0.069* | |
C27 | 0.3723 (5) | 0.8697 (6) | 0.9431 (3) | 0.0490 (15) | |
H27A | 0.4107 | 0.9366 | 0.9638 | 0.073* | |
H27B | 0.3093 | 0.8394 | 0.9597 | 0.073* | |
H27C | 0.3470 | 0.9050 | 0.9099 | 0.073* | |
P1 | 0.67141 (12) | 0.19133 (14) | 0.87212 (6) | 0.0349 (3) | |
F1 | 0.6693 (3) | 0.3340 (4) | 0.89769 (16) | 0.0600 (10) | |
F2 | 0.7363 (3) | 0.1347 (4) | 0.92414 (14) | 0.0565 (10) | |
F3 | 0.7890 (3) | 0.2230 (4) | 0.85094 (16) | 0.0566 (10) | |
F4 | 0.6720 (3) | 0.0496 (4) | 0.84669 (15) | 0.0549 (9) | |
F5 | 0.6071 (3) | 0.2484 (4) | 0.82040 (13) | 0.0441 (8) | |
F6 | 0.5547 (3) | 0.1604 (4) | 0.89377 (13) | 0.0437 (8) | |
C28 | 0.8517 (8) | 0.4152 (9) | 0.9797 (4) | 0.080 (3) | |
H28A | 0.7971 | 0.3521 | 0.9651 | 0.096* | |
H28B | 0.8971 | 0.4417 | 0.9528 | 0.096* | |
Cl1 | 0.93614 (16) | 0.3422 (2) | 1.02952 (8) | 0.0671 (5) | |
Cl2 | 0.7824 (2) | 0.5526 (2) | 1.00162 (13) | 0.0985 (9) |
U11 | U22 | U33 | U12 | U13 | U23 | |
Re1 | 0.01677 (9) | 0.01731 (9) | 0.01945 (9) | 0.00098 (5) | 0.00106 (6) | −0.00150 (6) |
C1 | 0.0214 (19) | 0.020 (2) | 0.023 (2) | −0.0006 (15) | 0.0038 (15) | −0.0018 (15) |
O1 | 0.0339 (18) | 0.0274 (17) | 0.0265 (16) | −0.0011 (13) | 0.0068 (13) | −0.0010 (13) |
C2 | 0.023 (2) | 0.0205 (19) | 0.022 (2) | 0.0017 (16) | 0.0021 (16) | −0.0004 (16) |
O2 | 0.0277 (17) | 0.0320 (18) | 0.0331 (18) | −0.0034 (14) | −0.0004 (14) | −0.0078 (14) |
C3 | 0.0198 (19) | 0.024 (2) | 0.025 (2) | −0.0015 (16) | 0.0013 (16) | −0.0038 (16) |
O3 | 0.0254 (16) | 0.0280 (17) | 0.0393 (19) | 0.0074 (13) | −0.0028 (14) | −0.0086 (14) |
C4 | 0.026 (2) | 0.030 (2) | 0.027 (2) | −0.0005 (18) | −0.0020 (18) | 0.0052 (18) |
N1 | 0.0207 (17) | 0.0217 (17) | 0.0226 (17) | 0.0025 (13) | −0.0010 (14) | −0.0003 (13) |
C5 | 0.029 (2) | 0.035 (2) | 0.028 (2) | −0.001 (2) | −0.0043 (18) | 0.0072 (19) |
C6 | 0.026 (2) | 0.035 (2) | 0.023 (2) | −0.0019 (18) | 0.0003 (17) | 0.0043 (18) |
C7 | 0.023 (2) | 0.043 (3) | 0.030 (2) | −0.003 (2) | 0.0031 (18) | 0.010 (2) |
C8 | 0.029 (2) | 0.033 (2) | 0.024 (2) | −0.0024 (18) | 0.0026 (18) | 0.0039 (18) |
C9 | 0.032 (3) | 0.046 (3) | 0.023 (2) | −0.002 (2) | 0.0020 (19) | 0.010 (2) |
N2 | 0.0178 (16) | 0.0218 (17) | 0.0169 (15) | 0.0003 (13) | 0.0000 (12) | −0.0001 (13) |
N3 | 0.0164 (15) | 0.0196 (17) | 0.0212 (16) | 0.0003 (13) | 0.0022 (13) | −0.0011 (13) |
C10 | 0.022 (2) | 0.023 (2) | 0.025 (2) | −0.0007 (16) | −0.0030 (16) | −0.0029 (16) |
C11 | 0.0183 (19) | 0.027 (2) | 0.027 (2) | 0.0003 (16) | −0.0020 (16) | −0.0002 (17) |
C12 | 0.0181 (19) | 0.025 (2) | 0.023 (2) | 0.0063 (16) | 0.0006 (15) | 0.0001 (16) |
C13 | 0.0175 (19) | 0.022 (2) | 0.025 (2) | 0.0015 (15) | 0.0013 (15) | −0.0022 (16) |
C14 | 0.0168 (18) | 0.0212 (19) | 0.0175 (18) | 0.0004 (15) | 0.0028 (14) | 0.0014 (15) |
C15 | 0.0148 (17) | 0.0208 (19) | 0.0196 (18) | 0.0007 (14) | 0.0026 (14) | 0.0005 (15) |
C16 | 0.0198 (19) | 0.021 (2) | 0.0228 (19) | 0.0010 (15) | 0.0012 (15) | −0.0018 (15) |
C17 | 0.0208 (19) | 0.024 (2) | 0.0178 (18) | −0.0018 (16) | 0.0005 (15) | −0.0007 (15) |
C18 | 0.0160 (18) | 0.028 (2) | 0.024 (2) | 0.0022 (16) | −0.0001 (15) | −0.0002 (17) |
C19 | 0.0183 (19) | 0.022 (2) | 0.025 (2) | 0.0052 (15) | 0.0001 (15) | 0.0011 (16) |
C20 | 0.019 (2) | 0.031 (2) | 0.031 (2) | 0.0097 (18) | −0.0015 (17) | −0.0029 (19) |
C21 | 0.020 (2) | 0.043 (3) | 0.037 (3) | 0.009 (2) | −0.0027 (19) | −0.005 (2) |
C22 | 0.034 (3) | 0.029 (3) | 0.052 (3) | 0.008 (2) | 0.001 (2) | −0.001 (2) |
C23 | 0.031 (3) | 0.051 (3) | 0.031 (3) | 0.017 (2) | 0.001 (2) | −0.007 (2) |
C24 | 0.022 (2) | 0.027 (2) | 0.029 (2) | −0.0033 (17) | −0.0004 (17) | −0.0071 (18) |
C25 | 0.050 (3) | 0.046 (3) | 0.034 (3) | −0.001 (3) | −0.010 (3) | −0.007 (2) |
C26 | 0.046 (3) | 0.042 (3) | 0.053 (4) | −0.018 (3) | 0.010 (3) | −0.005 (3) |
C27 | 0.040 (3) | 0.039 (3) | 0.064 (4) | 0.002 (2) | −0.011 (3) | −0.024 (3) |
P1 | 0.0293 (6) | 0.0424 (8) | 0.0330 (7) | 0.0142 (5) | 0.0026 (5) | 0.0008 (5) |
F1 | 0.060 (2) | 0.052 (2) | 0.065 (3) | 0.0078 (19) | −0.0077 (19) | −0.0170 (19) |
F2 | 0.0414 (19) | 0.084 (3) | 0.0429 (19) | 0.0211 (19) | −0.0013 (15) | 0.0160 (19) |
F3 | 0.0306 (17) | 0.077 (3) | 0.062 (2) | 0.0101 (17) | 0.0073 (16) | 0.018 (2) |
F4 | 0.063 (2) | 0.047 (2) | 0.056 (2) | 0.0194 (18) | 0.0135 (18) | −0.0058 (17) |
F5 | 0.0368 (17) | 0.0559 (19) | 0.0386 (17) | 0.0125 (16) | −0.0008 (14) | 0.0077 (16) |
F6 | 0.0353 (17) | 0.057 (2) | 0.0395 (17) | 0.0129 (15) | 0.0069 (13) | 0.0026 (15) |
C28 | 0.083 (6) | 0.064 (5) | 0.084 (6) | 0.005 (4) | −0.035 (5) | 0.002 (4) |
Cl1 | 0.0579 (10) | 0.0827 (13) | 0.0602 (11) | 0.0101 (9) | 0.0035 (8) | 0.0113 (10) |
Cl2 | 0.0854 (16) | 0.0706 (14) | 0.145 (2) | 0.0225 (12) | 0.0412 (16) | 0.0296 (15) |
Re1—C2 | 1.922 (4) | C17—C18 | 1.399 (6) |
Re1—C1 | 1.932 (4) | C17—C24 | 1.525 (6) |
Re1—C3 | 1.939 (4) | C18—C19 | 1.383 (6) |
Re1—N2 | 2.164 (3) | C18—H18 | 0.9300 |
Re1—N3 | 2.167 (3) | C19—H19 | 0.9300 |
Re1—N1 | 2.220 (4) | C20—C23 | 1.531 (7) |
C1—O1 | 1.138 (5) | C20—C21 | 1.534 (7) |
C2—O2 | 1.152 (5) | C20—C22 | 1.539 (8) |
C3—O3 | 1.143 (5) | C21—H21A | 0.9600 |
C4—N1 | 1.347 (6) | C21—H21B | 0.9600 |
C4—C5 | 1.378 (7) | C21—H21C | 0.9600 |
C4—H4 | 0.9300 | C22—H22A | 0.9600 |
N1—C6 | 1.321 (6) | C22—H22B | 0.9600 |
C5—C8 | 1.373 (7) | C22—H22C | 0.9600 |
C5—H5 | 0.9300 | C23—H23A | 0.9600 |
C6—C7 | 1.378 (6) | C23—H23B | 0.9600 |
C6—H6 | 0.9300 | C23—H23C | 0.9600 |
C7—C8 | 1.390 (7) | C24—C27 | 1.529 (7) |
C7—H7 | 0.9300 | C24—C26 | 1.534 (7) |
C8—C9 | 1.510 (6) | C24—C25 | 1.542 (7) |
C9—C9i | 1.495 (10) | C25—H25A | 0.9600 |
C9—H9A | 0.9700 | C25—H25B | 0.9600 |
C9—H9B | 0.9700 | C25—H25C | 0.9600 |
N2—C10 | 1.340 (5) | C26—H26A | 0.9600 |
N2—C14 | 1.358 (5) | C26—H26B | 0.9600 |
N3—C19 | 1.348 (5) | C26—H26C | 0.9600 |
N3—C15 | 1.355 (5) | C27—H27A | 0.9600 |
C10—C11 | 1.378 (6) | C27—H27B | 0.9600 |
C10—H10 | 0.9300 | C27—H27C | 0.9600 |
C11—C12 | 1.388 (6) | P1—F4 | 1.592 (4) |
C11—H11 | 0.9300 | P1—F6 | 1.597 (4) |
C12—C13 | 1.396 (6) | P1—F5 | 1.599 (3) |
C12—C20 | 1.540 (6) | P1—F3 | 1.602 (4) |
C13—C14 | 1.384 (6) | P1—F1 | 1.603 (4) |
C13—H13 | 0.9300 | P1—F2 | 1.607 (4) |
C14—C15 | 1.484 (5) | C28—Cl1 | 1.738 (8) |
C15—C16 | 1.389 (6) | C28—Cl2 | 1.757 (10) |
C16—C17 | 1.393 (6) | C28—H28A | 0.9700 |
C16—H16 | 0.9300 | C28—H28B | 0.9700 |
C2—Re1—C1 | 88.79 (18) | C17—C18—H18 | 120.0 |
C2—Re1—C3 | 89.52 (18) | N3—C19—C18 | 123.0 (4) |
C1—Re1—C3 | 89.16 (18) | N3—C19—H19 | 118.5 |
C2—Re1—N2 | 96.31 (16) | C18—C19—H19 | 118.5 |
C1—Re1—N2 | 95.71 (15) | C23—C20—C21 | 109.3 (4) |
C3—Re1—N2 | 172.47 (15) | C23—C20—C22 | 109.3 (4) |
C2—Re1—N3 | 170.71 (16) | C21—C20—C22 | 108.9 (4) |
C1—Re1—N3 | 94.97 (16) | C23—C20—C12 | 108.9 (4) |
C3—Re1—N3 | 99.01 (16) | C21—C20—C12 | 111.3 (4) |
N2—Re1—N3 | 74.89 (13) | C22—C20—C12 | 109.1 (4) |
C2—Re1—N1 | 91.74 (16) | C20—C21—H21A | 109.5 |
C1—Re1—N1 | 179.27 (16) | C20—C21—H21B | 109.5 |
C3—Re1—N1 | 90.35 (16) | H21A—C21—H21B | 109.5 |
N2—Re1—N1 | 84.72 (13) | C20—C21—H21C | 109.5 |
N3—Re1—N1 | 84.58 (13) | H21A—C21—H21C | 109.5 |
O1—C1—Re1 | 177.9 (4) | H21B—C21—H21C | 109.5 |
O2—C2—Re1 | 177.1 (4) | C20—C22—H22A | 109.5 |
O3—C3—Re1 | 178.0 (4) | C20—C22—H22B | 109.5 |
N1—C4—C5 | 121.8 (4) | H22A—C22—H22B | 109.5 |
N1—C4—H4 | 119.1 | C20—C22—H22C | 109.5 |
C5—C4—H4 | 119.1 | H22A—C22—H22C | 109.5 |
C6—N1—C4 | 117.7 (4) | H22B—C22—H22C | 109.5 |
C6—N1—Re1 | 121.3 (3) | C20—C23—H23A | 109.5 |
C4—N1—Re1 | 120.7 (3) | C20—C23—H23B | 109.5 |
C8—C5—C4 | 120.6 (4) | H23A—C23—H23B | 109.5 |
C8—C5—H5 | 119.7 | C20—C23—H23C | 109.5 |
C4—C5—H5 | 119.7 | H23A—C23—H23C | 109.5 |
N1—C6—C7 | 123.4 (4) | H23B—C23—H23C | 109.5 |
N1—C6—H6 | 118.3 | C17—C24—C27 | 112.4 (4) |
C7—C6—H6 | 118.3 | C17—C24—C26 | 108.5 (4) |
C6—C7—C8 | 119.3 (4) | C27—C24—C26 | 109.3 (5) |
C6—C7—H7 | 120.3 | C17—C24—C25 | 108.4 (4) |
C8—C7—H7 | 120.3 | C27—C24—C25 | 108.8 (5) |
C5—C8—C7 | 117.0 (4) | C26—C24—C25 | 109.4 (5) |
C5—C8—C9 | 119.7 (4) | C24—C25—H25A | 109.5 |
C7—C8—C9 | 123.2 (4) | C24—C25—H25B | 109.5 |
C9i—C9—C8 | 115.7 (5) | H25A—C25—H25B | 109.5 |
C9i—C9—H9A | 108.4 | C24—C25—H25C | 109.5 |
C8—C9—H9A | 108.4 | H25A—C25—H25C | 109.5 |
C9i—C9—H9B | 108.4 | H25B—C25—H25C | 109.5 |
C8—C9—H9B | 108.4 | C24—C26—H26A | 109.5 |
H9A—C9—H9B | 107.4 | C24—C26—H26B | 109.5 |
C10—N2—C14 | 117.5 (4) | H26A—C26—H26B | 109.5 |
C10—N2—Re1 | 125.1 (3) | C24—C26—H26C | 109.5 |
C14—N2—Re1 | 117.5 (3) | H26A—C26—H26C | 109.5 |
C19—N3—C15 | 117.8 (4) | H26B—C26—H26C | 109.5 |
C19—N3—Re1 | 124.7 (3) | C24—C27—H27A | 109.5 |
C15—N3—Re1 | 117.5 (3) | C24—C27—H27B | 109.5 |
N2—C10—C11 | 123.8 (4) | H27A—C27—H27B | 109.5 |
N2—C10—H10 | 118.1 | C24—C27—H27C | 109.5 |
C11—C10—H10 | 118.1 | H27A—C27—H27C | 109.5 |
C10—C11—C12 | 119.5 (4) | H27B—C27—H27C | 109.5 |
C10—C11—H11 | 120.2 | F4—P1—F6 | 90.5 (2) |
C12—C11—H11 | 120.2 | F4—P1—F5 | 90.0 (2) |
C11—C12—C13 | 116.8 (4) | F6—P1—F5 | 90.18 (19) |
C11—C12—C20 | 123.8 (4) | F4—P1—F3 | 89.9 (2) |
C13—C12—C20 | 119.4 (4) | F6—P1—F3 | 179.4 (2) |
C14—C13—C12 | 121.0 (4) | F5—P1—F3 | 90.2 (2) |
C14—C13—H13 | 119.5 | F4—P1—F1 | 179.3 (2) |
C12—C13—H13 | 119.5 | F6—P1—F1 | 88.9 (2) |
N2—C14—C13 | 121.3 (4) | F5—P1—F1 | 89.7 (2) |
N2—C14—C15 | 115.1 (3) | F3—P1—F1 | 90.7 (2) |
C13—C14—C15 | 123.5 (4) | F4—P1—F2 | 90.3 (2) |
N3—C15—C16 | 121.7 (4) | F6—P1—F2 | 89.97 (19) |
N3—C15—C14 | 115.0 (4) | F5—P1—F2 | 179.7 (3) |
C16—C15—C14 | 123.3 (4) | F3—P1—F2 | 89.6 (2) |
C15—C16—C17 | 121.0 (4) | F1—P1—F2 | 90.0 (2) |
C15—C16—H16 | 119.5 | Cl1—C28—Cl2 | 111.0 (5) |
C17—C16—H16 | 119.5 | Cl1—C28—H28A | 109.4 |
C16—C17—C18 | 116.4 (4) | Cl2—C28—H28A | 109.4 |
C16—C17—C24 | 122.8 (4) | Cl1—C28—H28B | 109.4 |
C18—C17—C24 | 120.7 (4) | Cl2—C28—H28B | 109.4 |
C19—C18—C17 | 120.1 (4) | H28A—C28—H28B | 108.0 |
C19—C18—H18 | 120.0 | ||
C5—C4—N1—C6 | 0.4 (7) | C10—C11—C12—C20 | −179.9 (4) |
C5—C4—N1—Re1 | −173.7 (4) | C11—C12—C13—C14 | −0.4 (6) |
C2—Re1—N1—C6 | −40.4 (4) | C20—C12—C13—C14 | 178.9 (4) |
C3—Re1—N1—C6 | −129.9 (4) | C10—N2—C14—C13 | −0.8 (6) |
N2—Re1—N1—C6 | 55.8 (4) | Re1—N2—C14—C13 | 178.9 (3) |
N3—Re1—N1—C6 | 131.1 (4) | C10—N2—C14—C15 | 179.9 (4) |
C2—Re1—N1—C4 | 133.5 (4) | Re1—N2—C14—C15 | −0.4 (4) |
C3—Re1—N1—C4 | 43.9 (4) | C12—C13—C14—N2 | 1.2 (6) |
N2—Re1—N1—C4 | −130.4 (4) | C12—C13—C14—C15 | −179.6 (4) |
N3—Re1—N1—C4 | −55.1 (3) | C19—N3—C15—C16 | 0.6 (6) |
N1—C4—C5—C8 | 1.6 (8) | Re1—N3—C15—C16 | −178.6 (3) |
C4—N1—C6—C7 | −1.0 (7) | C19—N3—C15—C14 | −179.8 (4) |
Re1—N1—C6—C7 | 173.0 (4) | Re1—N3—C15—C14 | 1.0 (4) |
N1—C6—C7—C8 | −0.2 (8) | N2—C14—C15—N3 | −0.4 (5) |
C4—C5—C8—C7 | −2.7 (8) | C13—C14—C15—N3 | −179.7 (4) |
C4—C5—C8—C9 | 177.2 (5) | N2—C14—C15—C16 | 179.3 (4) |
C6—C7—C8—C5 | 2.0 (8) | C13—C14—C15—C16 | 0.0 (6) |
C6—C7—C8—C9 | −177.9 (5) | N3—C15—C16—C17 | −0.5 (6) |
C5—C8—C9—C9i | −175.9 (6) | C14—C15—C16—C17 | 179.9 (4) |
C7—C8—C9—C9i | 4.0 (9) | C15—C16—C17—C18 | −0.4 (6) |
C2—Re1—N2—C10 | −2.6 (4) | C15—C16—C17—C24 | 178.4 (4) |
C1—Re1—N2—C10 | 86.8 (4) | C16—C17—C18—C19 | 1.2 (6) |
N3—Re1—N2—C10 | −179.6 (4) | C24—C17—C18—C19 | −177.6 (4) |
N1—Re1—N2—C10 | −93.8 (4) | C15—N3—C19—C18 | 0.3 (6) |
C2—Re1—N2—C14 | 177.7 (3) | Re1—N3—C19—C18 | 179.4 (3) |
C1—Re1—N2—C14 | −92.9 (3) | C17—C18—C19—N3 | −1.2 (7) |
N3—Re1—N2—C14 | 0.7 (3) | C11—C12—C20—C23 | 123.1 (5) |
N1—Re1—N2—C14 | 86.5 (3) | C13—C12—C20—C23 | −56.2 (6) |
C1—Re1—N3—C19 | −85.5 (4) | C11—C12—C20—C21 | 2.5 (6) |
C3—Re1—N3—C19 | 4.4 (4) | C13—C12—C20—C21 | −176.8 (4) |
N2—Re1—N3—C19 | 179.9 (4) | C11—C12—C20—C22 | −117.7 (5) |
N1—Re1—N3—C19 | 93.9 (3) | C13—C12—C20—C22 | 63.0 (5) |
C1—Re1—N3—C15 | 93.6 (3) | C16—C17—C24—C27 | 0.9 (7) |
C3—Re1—N3—C15 | −176.4 (3) | C18—C17—C24—C27 | 179.7 (5) |
N2—Re1—N3—C15 | −1.0 (3) | C16—C17—C24—C26 | −120.1 (5) |
N1—Re1—N3—C15 | −86.9 (3) | C18—C17—C24—C26 | 58.7 (6) |
C14—N2—C10—C11 | −0.3 (6) | C16—C17—C24—C25 | 121.1 (5) |
Re1—N2—C10—C11 | −179.9 (3) | C18—C17—C24—C25 | −60.1 (6) |
N2—C10—C11—C12 | 1.0 (7) | C8—C9—C9i—C8i | 180.000 (3) |
C10—C11—C12—C13 | −0.6 (6) |
Symmetry code: (i) −x, −y, −z+2. |