Supporting information
Crystallographic Information File (CIF) https://doi.org/10.1107/S1600536806033216/cv2098sup1.cif | |
Structure factor file (CIF format) https://doi.org/10.1107/S1600536806033216/cv2098Isup2.hkl |
CCDC reference: 620948
Data collection: SMART (Bruker, 1997); cell refinement: SMART; data reduction: SAINT (Bruker, 1998); program(s) used to solve structure: SHELXS97 (Sheldrick, 1997); program(s) used to refine structure: SHELXL97 (Sheldrick, 1997); molecular graphics: SHELXTL (Bruker, 1998); software used to prepare material for publication: SHELXTL.
C30H26N42+·2PF6−·3C2H3N | F(000) = 1752 |
Mr = 855.65 | Dx = 1.415 Mg m−3 |
Monoclinic, P21/c | Mo Kα radiation, λ = 0.71073 Å |
a = 8.643 (2) Å | Cell parameters from 3267 reflections |
b = 22.391 (6) Å | θ = 2.6–21.1° |
c = 20.983 (5) Å | µ = 0.20 mm−1 |
β = 98.506 (5)° | T = 294 K |
V = 4015.9 (18) Å3 | Block, yellow |
Z = 4 | 0.40 × 0.22 × 0.18 mm |
Bruker SMART CCD area-detector diffractometer | 7086 independent reflections |
Radiation source: fine-focus sealed tube | 3197 reflections with I > 2σ(I) |
Graphite monochromator | Rint = 0.058 |
φ and ω scans | θmax = 25.0°, θmin = 1.3° |
Absorption correction: multi-scan (SADABS; Sheldrick, 1996) | h = −10→9 |
Tmin = 0.949, Tmax = 0.965 | k = −26→25 |
20280 measured reflections | l = −24→16 |
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)] = 0.054 | Hydrogen site location: inferred from neighbouring sites |
wR(F2) = 0.179 | H-atom parameters constrained |
S = 1.03 | w = 1/[σ2(Fo2) + (0.0813P)2 + 0.3116P] where P = (Fo2 + 2Fc2)/3 |
7086 reflections | (Δ/σ)max = 0.005 |
627 parameters | Δρmax = 0.26 e Å−3 |
282 restraints | Δρmin = −0.23 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 | Occ. (<1) | |
N1 | 0.31769 (5) | 0.20021 (2) | 0.76432 (2) | 0.05763 (17) | |
N2 | 0.06948 (5) | 0.20296 (2) | 0.76325 (2) | 0.06008 (17) | |
N3 | 0.04000 (5) | 0.47948 (2) | 0.75493 (2) | 0.06113 (18) | |
N4 | 0.28406 (5) | 0.489922 (19) | 0.75031 (2) | 0.05270 (16) | |
C1 | 0.18940 (6) | 0.23054 (3) | 0.74398 (3) | 0.0598 (2) | |
H1 | 0.1841 | 0.2656 | 0.7200 | 0.072* | |
C2 | 0.27765 (8) | 0.15102 (3) | 0.79687 (3) | 0.0719 (2) | |
H2 | 0.3455 | 0.1217 | 0.8158 | 0.086* | |
C3 | 0.12416 (8) | 0.15290 (3) | 0.79641 (3) | 0.0700 (2) | |
H3 | 0.0646 | 0.1252 | 0.8152 | 0.084* | |
C4 | −0.09118 (7) | 0.22742 (3) | 0.75532 (3) | 0.0740 (3) | |
H4A | −0.1600 | 0.1992 | 0.7722 | 0.089* | |
H4B | −0.1289 | 0.2332 | 0.7099 | 0.089* | |
C5 | −0.09480 (6) | 0.28581 (3) | 0.79008 (3) | 0.0613 (2) | |
C6 | −0.07709 (9) | 0.28737 (3) | 0.85588 (3) | 0.0919 (3) | |
H6 | −0.0683 | 0.2519 | 0.8793 | 0.110* | |
C7 | −0.07226 (11) | 0.34103 (3) | 0.88741 (4) | 0.1172 (4) | |
H7 | −0.0594 | 0.3417 | 0.9322 | 0.141* | |
C8 | −0.08601 (9) | 0.39382 (3) | 0.85398 (3) | 0.0959 (3) | |
H8 | −0.0828 | 0.4299 | 0.8761 | 0.115* | |
C9 | −0.10452 (7) | 0.39349 (3) | 0.78793 (3) | 0.0639 (2) | |
C10 | −0.10949 (6) | 0.33929 (3) | 0.75669 (3) | 0.0600 (2) | |
H10 | −0.1231 | 0.3386 | 0.7119 | 0.072* | |
C11 | −0.11519 (7) | 0.45062 (3) | 0.74997 (4) | 0.0784 (3) | |
H11A | −0.1542 | 0.4422 | 0.7051 | 0.094* | |
H11B | −0.1882 | 0.4775 | 0.7662 | 0.094* | |
C12 | 0.08681 (7) | 0.53064 (3) | 0.78782 (3) | 0.0683 (2) | |
H12 | 0.0245 | 0.5561 | 0.8082 | 0.082* | |
C13 | 0.23964 (7) | 0.53701 (3) | 0.78499 (3) | 0.0645 (2) | |
H13 | 0.3038 | 0.5678 | 0.8032 | 0.077* | |
C14 | 0.16111 (6) | 0.45565 (3) | 0.73253 (3) | 0.0584 (2) | |
H14 | 0.1599 | 0.4208 | 0.7084 | 0.070* | |
C15 | 0.44488 (6) | 0.47660 (2) | 0.73930 (3) | 0.0594 (2) | |
H15A | 0.5187 | 0.4973 | 0.7711 | 0.071* | |
H15B | 0.4599 | 0.4907 | 0.6969 | 0.071* | |
C16 | 0.47477 (6) | 0.41040 (2) | 0.74405 (3) | 0.04751 (19) | |
C17 | 0.46887 (6) | 0.38192 (3) | 0.80294 (3) | 0.0512 (2) | |
C18 | 0.45183 (7) | 0.41443 (3) | 0.85971 (3) | 0.0692 (2) | |
H18 | 0.4488 | 0.4559 | 0.8584 | 0.083* | |
C19 | 0.43994 (9) | 0.38580 (3) | 0.91545 (3) | 0.0893 (3) | |
H19 | 0.4264 | 0.4079 | 0.9517 | 0.107* | |
C20 | 0.44760 (9) | 0.32369 (3) | 0.91951 (3) | 0.0950 (3) | |
H20 | 0.4402 | 0.3048 | 0.9584 | 0.114* | |
C21 | 0.46566 (8) | 0.29078 (3) | 0.86726 (3) | 0.0763 (3) | |
H21 | 0.4717 | 0.2494 | 0.8709 | 0.092* | |
C22 | 0.47565 (6) | 0.31802 (3) | 0.80672 (3) | 0.0533 (2) | |
C23 | 0.48902 (6) | 0.28476 (2) | 0.75121 (3) | 0.05025 (19) | |
C24 | 0.50832 (6) | 0.31296 (2) | 0.69371 (3) | 0.04952 (19) | |
C25 | 0.53633 (7) | 0.28147 (3) | 0.63734 (3) | 0.0717 (2) | |
H25 | 0.5385 | 0.2399 | 0.6381 | 0.086* | |
C26 | 0.55955 (9) | 0.30999 (3) | 0.58355 (3) | 0.0917 (3) | |
H26 | 0.5783 | 0.2881 | 0.5478 | 0.110* | |
C27 | 0.55590 (9) | 0.37184 (3) | 0.58048 (3) | 0.0920 (3) | |
H27 | 0.5754 | 0.3909 | 0.5431 | 0.110* | |
C28 | 0.52456 (7) | 0.40490 (3) | 0.63078 (3) | 0.0694 (2) | |
H28 | 0.5181 | 0.4462 | 0.6269 | 0.083* | |
C29 | 0.50126 (6) | 0.37734 (2) | 0.68980 (3) | 0.04805 (19) | |
C30 | 0.47742 (6) | 0.21771 (3) | 0.75480 (3) | 0.0701 (2) | |
H30A | 0.5021 | 0.2001 | 0.7153 | 0.084* | |
H30B | 0.5523 | 0.2029 | 0.7903 | 0.084* | |
P1 | 0.26736 (2) | 0.603967 (8) | 0.597190 (8) | 0.07065 (7) | |
P2 | 0.28659 (2) | 0.408383 (8) | 0.102339 (9) | 0.06710 (6) | |
F1 | 0.36670 (15) | 0.55203 (5) | 0.57483 (6) | 0.1373 (5) | 0.3571 (3) |
F2 | 0.41510 (12) | 0.64165 (5) | 0.58128 (5) | 0.1000 (4) | 0.3571 (3) |
F3 | 0.19544 (18) | 0.66224 (5) | 0.61787 (8) | 0.1638 (6) | 0.3571 (3) |
F4 | 0.14031 (12) | 0.56558 (6) | 0.62125 (6) | 0.1136 (5) | 0.3571 (3) |
F5 | 0.18262 (15) | 0.61130 (6) | 0.52661 (5) | 0.1226 (5) | 0.3571 (3) |
F6 | 0.37645 (13) | 0.59947 (5) | 0.66615 (4) | 0.0918 (4) | 0.3571 (3) |
F1' | 0.41611 (9) | 0.56856 (4) | 0.59362 (5) | 0.1662 (4) | 0.6429 (3) |
F2' | 0.33500 (9) | 0.66460 (3) | 0.57934 (4) | 0.1252 (3) | 0.6429 (3) |
F3' | 0.10150 (8) | 0.63530 (3) | 0.59970 (4) | 0.1219 (3) | 0.6429 (3) |
F4' | 0.19023 (8) | 0.54187 (3) | 0.61196 (3) | 0.1047 (3) | 0.6429 (3) |
F5' | 0.20880 (8) | 0.59029 (3) | 0.52393 (3) | 0.1044 (3) | 0.6429 (3) |
F6' | 0.30777 (9) | 0.61625 (3) | 0.67084 (3) | 0.1264 (3) | 0.6429 (3) |
F7 | 0.24020 (9) | 0.46823 (3) | 0.13356 (4) | 0.1555 (3) | 0.6578 (4) |
F8 | 0.15471 (7) | 0.37902 (3) | 0.13402 (3) | 0.1253 (3) | 0.6578 (4) |
F9 | 0.34400 (9) | 0.34987 (3) | 0.07576 (4) | 0.1332 (3) | 0.6578 (4) |
F10 | 0.41276 (7) | 0.44284 (3) | 0.07083 (3) | 0.1174 (3) | 0.6578 (4) |
F11 | 0.16952 (8) | 0.41836 (4) | 0.04036 (4) | 0.1414 (3) | 0.6578 (4) |
F12 | 0.41625 (7) | 0.39921 (3) | 0.16446 (3) | 0.1084 (3) | 0.6578 (4) |
F7' | 0.16290 (13) | 0.46003 (5) | 0.10290 (6) | 0.1277 (5) | 0.3422 (4) |
F8' | 0.19632 (13) | 0.35501 (5) | 0.13179 (6) | 0.1141 (5) | 0.3422 (4) |
F9' | 0.41047 (15) | 0.36154 (7) | 0.09097 (9) | 0.1694 (7) | 0.3422 (4) |
F10' | 0.39003 (15) | 0.45706 (5) | 0.07740 (7) | 0.1274 (5) | 0.3422 (4) |
F11' | 0.19825 (15) | 0.38928 (5) | 0.03506 (5) | 0.1146 (5) | 0.3422 (4) |
F12' | 0.35463 (16) | 0.42317 (6) | 0.17236 (5) | 0.1244 (5) | 0.3422 (4) |
N5 | 0.10404 (8) | 0.33843 (3) | 0.62968 (3) | 0.1066 (3) | |
C33 | 0.78555 (9) | 0.53968 (3) | 0.57477 (4) | 0.1062 (3) | |
N7 | 0.78125 (10) | 0.34258 (3) | 0.09987 (5) | 0.1602 (4) | |
N6 | 0.77573 (10) | 0.52640 (3) | 0.62429 (4) | 0.1475 (4) | |
C31 | 0.08016 (10) | 0.30883 (3) | 0.58791 (4) | 0.0984 (3) | |
C35 | 0.78060 (9) | 0.38313 (4) | 0.06853 (4) | 0.1085 (4) | |
C36 | 0.78050 (10) | 0.43712 (4) | 0.03178 (4) | 0.1259 (4) | |
H36A | 0.7047 | 0.4643 | 0.0444 | 0.189* | |
H36B | 0.7544 | 0.4281 | −0.0133 | 0.189* | |
H36C | 0.8824 | 0.4551 | 0.0396 | 0.189* | |
C32 | 0.04586 (14) | 0.26820 (4) | 0.53403 (4) | 0.1746 (6) | |
H32A | 0.0538 | 0.2278 | 0.5494 | 0.262* | |
H32B | 0.1193 | 0.2744 | 0.5045 | 0.262* | |
H32C | −0.0583 | 0.2754 | 0.5124 | 0.262* | |
C34 | 0.80130 (13) | 0.55765 (4) | 0.51028 (5) | 0.1661 (5) | |
H34A | 0.7895 | 0.6002 | 0.5064 | 0.249* | |
H34B | 0.7221 | 0.5384 | 0.4803 | 0.249* | |
H34C | 0.9028 | 0.5463 | 0.5010 | 0.249* |
U11 | U22 | U33 | U12 | U13 | U23 | |
N1 | 0.0556 (3) | 0.0417 (3) | 0.0777 (3) | −0.0008 (2) | 0.0171 (3) | 0.0019 (3) |
N2 | 0.0479 (3) | 0.0565 (3) | 0.0772 (3) | −0.0098 (2) | 0.0135 (2) | −0.0031 (3) |
N3 | 0.0414 (3) | 0.0638 (3) | 0.0782 (3) | 0.0146 (2) | 0.0086 (3) | 0.0082 (3) |
N4 | 0.0491 (3) | 0.0423 (2) | 0.0687 (3) | 0.0038 (2) | 0.0153 (2) | −0.0008 (2) |
C1 | 0.0528 (3) | 0.0522 (3) | 0.0745 (4) | −0.0073 (3) | 0.0095 (3) | 0.0073 (3) |
C2 | 0.0769 (4) | 0.0443 (3) | 0.0969 (5) | −0.0011 (3) | 0.0216 (4) | 0.0102 (3) |
C3 | 0.0755 (4) | 0.0515 (4) | 0.0866 (4) | −0.0107 (3) | 0.0235 (4) | 0.0034 (3) |
C4 | 0.0460 (4) | 0.0814 (4) | 0.0940 (5) | −0.0098 (4) | 0.0084 (3) | 0.0011 (4) |
C5 | 0.0417 (3) | 0.0684 (4) | 0.0751 (4) | −0.0028 (3) | 0.0135 (3) | 0.0016 (3) |
C6 | 0.1181 (6) | 0.0812 (5) | 0.0816 (5) | 0.0093 (5) | 0.0322 (4) | 0.0146 (4) |
C7 | 0.1896 (8) | 0.0949 (6) | 0.0756 (5) | 0.0273 (6) | 0.0475 (5) | 0.0120 (4) |
C8 | 0.1191 (6) | 0.0819 (5) | 0.0924 (5) | 0.0216 (4) | 0.0347 (4) | −0.0063 (4) |
C9 | 0.0422 (3) | 0.0669 (4) | 0.0846 (4) | 0.0098 (3) | 0.0161 (3) | 0.0089 (4) |
C10 | 0.0315 (3) | 0.0851 (4) | 0.0627 (4) | 0.0004 (3) | 0.0044 (3) | 0.0064 (3) |
C11 | 0.0444 (4) | 0.0794 (4) | 0.1099 (5) | 0.0140 (4) | 0.0063 (4) | 0.0117 (4) |
C12 | 0.0704 (4) | 0.0541 (4) | 0.0833 (4) | 0.0172 (3) | 0.0211 (3) | −0.0024 (3) |
C13 | 0.0693 (4) | 0.0480 (3) | 0.0787 (4) | 0.0038 (3) | 0.0196 (3) | −0.0075 (3) |
C14 | 0.0529 (3) | 0.0549 (3) | 0.0670 (4) | 0.0051 (3) | 0.0077 (3) | −0.0025 (3) |
C15 | 0.0500 (3) | 0.0482 (3) | 0.0837 (4) | −0.0050 (3) | 0.0223 (3) | −0.0031 (3) |
C16 | 0.0357 (3) | 0.0427 (3) | 0.0652 (4) | −0.0045 (3) | 0.0110 (3) | −0.0056 (3) |
C17 | 0.0380 (3) | 0.0541 (3) | 0.0606 (4) | −0.0039 (3) | 0.0040 (3) | −0.0033 (3) |
C18 | 0.0731 (4) | 0.0731 (4) | 0.0601 (4) | 0.0040 (4) | 0.0053 (3) | −0.0093 (3) |
C19 | 0.1019 (5) | 0.1020 (5) | 0.0634 (4) | 0.0083 (5) | 0.0104 (4) | −0.0075 (4) |
C20 | 0.1089 (6) | 0.1175 (6) | 0.0581 (4) | 0.0018 (5) | 0.0105 (4) | 0.0186 (4) |
C21 | 0.0756 (4) | 0.0808 (4) | 0.0707 (4) | 0.0004 (4) | 0.0051 (4) | 0.0163 (4) |
C22 | 0.0382 (3) | 0.0573 (3) | 0.0629 (4) | −0.0006 (3) | 0.0029 (3) | 0.0058 (3) |
C23 | 0.0343 (3) | 0.0401 (3) | 0.0772 (4) | −0.0001 (3) | 0.0112 (3) | −0.0025 (3) |
C24 | 0.0304 (3) | 0.0534 (3) | 0.0657 (4) | −0.0022 (3) | 0.0102 (3) | −0.0081 (3) |
C25 | 0.0683 (4) | 0.0658 (4) | 0.0848 (4) | −0.0031 (4) | 0.0238 (3) | −0.0190 (4) |
C26 | 0.1060 (5) | 0.1008 (5) | 0.0757 (4) | −0.0030 (5) | 0.0377 (4) | −0.0251 (4) |
C27 | 0.1132 (5) | 0.0969 (5) | 0.0768 (4) | −0.0098 (5) | 0.0502 (4) | −0.0042 (4) |
C28 | 0.0728 (4) | 0.0708 (4) | 0.0702 (4) | −0.0057 (4) | 0.0288 (3) | 0.0047 (3) |
C29 | 0.0343 (3) | 0.0498 (3) | 0.0616 (4) | −0.0044 (3) | 0.0121 (3) | −0.0030 (3) |
C30 | 0.0490 (4) | 0.0579 (4) | 0.1068 (5) | 0.0026 (3) | 0.0227 (3) | 0.0056 (4) |
P1 | 0.08036 (12) | 0.07039 (11) | 0.06361 (11) | −0.00682 (10) | 0.01862 (9) | −0.00671 (10) |
P2 | 0.06623 (11) | 0.06613 (10) | 0.07064 (11) | 0.00215 (9) | 0.01573 (9) | −0.00472 (9) |
F1 | 0.1329 (9) | 0.1137 (8) | 0.1595 (10) | 0.0288 (8) | 0.0026 (8) | −0.0571 (7) |
F2 | 0.1093 (8) | 0.1029 (8) | 0.0858 (7) | −0.0242 (7) | 0.0079 (6) | 0.0066 (6) |
F3 | 0.1785 (11) | 0.1382 (10) | 0.1804 (11) | 0.0607 (8) | 0.0457 (9) | −0.0407 (8) |
F4 | 0.0841 (7) | 0.1513 (10) | 0.1084 (8) | −0.0201 (7) | 0.0239 (6) | 0.0124 (7) |
F5 | 0.1133 (9) | 0.1353 (9) | 0.1094 (9) | 0.0328 (8) | −0.0160 (7) | 0.0230 (8) |
F6 | 0.1081 (8) | 0.0953 (7) | 0.0658 (6) | −0.0336 (6) | −0.0071 (6) | 0.0139 (6) |
F1' | 0.1044 (5) | 0.1873 (7) | 0.2023 (8) | 0.0454 (5) | 0.0079 (5) | −0.0321 (6) |
F2' | 0.1505 (6) | 0.0917 (4) | 0.1325 (6) | −0.0474 (4) | 0.0178 (5) | 0.0162 (4) |
F3' | 0.1059 (5) | 0.1250 (5) | 0.1415 (5) | 0.0122 (4) | 0.0406 (4) | −0.0265 (5) |
F4' | 0.1352 (5) | 0.0830 (4) | 0.0960 (4) | −0.0338 (4) | 0.0173 (4) | −0.0056 (4) |
F5' | 0.1297 (5) | 0.1224 (5) | 0.0631 (4) | −0.0221 (4) | 0.0214 (4) | −0.0152 (4) |
F6' | 0.1702 (6) | 0.1300 (5) | 0.0786 (4) | −0.0496 (5) | 0.0174 (4) | −0.0264 (4) |
F7 | 0.1567 (6) | 0.1295 (5) | 0.1872 (6) | 0.0447 (5) | 0.0487 (5) | −0.0561 (5) |
F8 | 0.0947 (4) | 0.1414 (5) | 0.1469 (5) | −0.0237 (4) | 0.0414 (4) | 0.0158 (5) |
F9 | 0.1209 (5) | 0.0892 (4) | 0.1847 (6) | 0.0133 (4) | 0.0071 (5) | −0.0620 (4) |
F10 | 0.1181 (4) | 0.1182 (5) | 0.1313 (5) | −0.0193 (4) | 0.0692 (3) | 0.0004 (4) |
F11 | 0.1152 (5) | 0.1628 (6) | 0.1288 (6) | 0.0188 (5) | −0.0395 (5) | 0.0289 (5) |
F12 | 0.0968 (4) | 0.1279 (5) | 0.0901 (4) | −0.0080 (4) | −0.0205 (4) | 0.0135 (4) |
F7' | 0.1152 (8) | 0.1255 (9) | 0.1485 (10) | 0.0598 (7) | 0.0392 (7) | −0.0089 (8) |
F8' | 0.1357 (9) | 0.1077 (8) | 0.0974 (8) | −0.0560 (7) | 0.0120 (7) | 0.0295 (6) |
F9' | 0.1324 (11) | 0.1465 (11) | 0.2222 (14) | 0.0606 (9) | 0.0022 (10) | −0.0072 (10) |
F10' | 0.1476 (10) | 0.0793 (7) | 0.1564 (11) | −0.0420 (7) | 0.0258 (8) | 0.0192 (7) |
F11' | 0.1341 (10) | 0.1309 (9) | 0.0779 (7) | −0.0209 (8) | 0.0128 (7) | −0.0379 (7) |
F12' | 0.1456 (10) | 0.1269 (9) | 0.0901 (8) | −0.0403 (8) | −0.0183 (8) | −0.0187 (7) |
N5 | 0.1129 (5) | 0.1193 (5) | 0.0862 (4) | −0.0112 (4) | 0.0107 (4) | −0.0123 (4) |
C33 | 0.0956 (5) | 0.0604 (4) | 0.1496 (7) | −0.0105 (4) | −0.0249 (5) | 0.0102 (5) |
N7 | 0.1228 (6) | 0.1230 (6) | 0.2330 (10) | −0.0107 (5) | 0.0204 (6) | 0.0198 (6) |
N6 | 0.1724 (7) | 0.1040 (5) | 0.1587 (7) | −0.0232 (5) | −0.0005 (6) | 0.0303 (5) |
C31 | 0.1251 (6) | 0.0961 (5) | 0.0697 (5) | 0.0003 (5) | −0.0004 (5) | 0.0068 (4) |
C35 | 0.0741 (5) | 0.1131 (6) | 0.1368 (7) | −0.0023 (5) | 0.0105 (5) | −0.0244 (6) |
C36 | 0.1063 (6) | 0.1524 (8) | 0.1174 (7) | 0.0097 (6) | 0.0105 (6) | 0.0157 (6) |
C32 | 0.2809 (14) | 0.1239 (8) | 0.1016 (7) | −0.0034 (9) | −0.0294 (9) | −0.0183 (6) |
C34 | 0.2075 (11) | 0.1517 (8) | 0.1201 (8) | −0.0390 (8) | −0.0378 (8) | 0.0088 (7) |
N1—C1 | 1.3163 (7) | C23—C30 | 1.5073 (9) |
N1—C2 | 1.3673 (8) | C24—C25 | 1.4281 (9) |
N1—C30 | 1.4767 (8) | C24—C29 | 1.4446 (9) |
N2—C1 | 1.3202 (8) | C25—C26 | 1.3377 (10) |
N2—C3 | 1.3663 (8) | C25—H25 | 0.9300 |
N2—C4 | 1.4789 (8) | C26—C27 | 1.3865 (11) |
N3—C14 | 1.3216 (8) | C26—H26 | 0.9300 |
N3—C12 | 1.3674 (8) | C27—C28 | 1.3490 (10) |
N3—C11 | 1.4786 (8) | C27—H27 | 0.9300 |
N4—C14 | 1.3192 (7) | C28—C29 | 1.4244 (9) |
N4—C13 | 1.3679 (8) | C28—H28 | 0.9300 |
N4—C15 | 1.4728 (8) | C30—H30A | 0.9700 |
C1—H1 | 0.9300 | C30—H30B | 0.9700 |
C2—C3 | 1.3259 (10) | P1—F1' | 1.5216 (9) |
C2—H2 | 0.9300 | P1—F3 | 1.5353 (14) |
C3—H3 | 0.9300 | P1—F4 | 1.5374 (12) |
C4—C5 | 1.4997 (10) | P1—F2' | 1.5459 (8) |
C4—H4A | 0.9700 | P1—F6' | 1.5577 (7) |
C4—H4B | 0.9700 | P1—F1 | 1.5584 (12) |
C5—C6 | 1.3669 (10) | P1—F5 | 1.5606 (11) |
C5—C10 | 1.3836 (9) | P1—F5' | 1.5756 (7) |
C6—C7 | 1.3692 (11) | P1—F4' | 1.5921 (7) |
C6—H6 | 0.9300 | P1—F3' | 1.6038 (8) |
C7—C8 | 1.3707 (11) | P1—F2 | 1.6062 (12) |
C7—H7 | 0.9300 | P1—F6 | 1.6090 (9) |
C8—C9 | 1.3714 (10) | P2—F9 | 1.5347 (7) |
C8—H8 | 0.9300 | P2—F12' | 1.5358 (12) |
C9—C10 | 1.3768 (9) | P2—F11 | 1.5414 (8) |
C9—C11 | 1.5025 (10) | P2—F9' | 1.5423 (15) |
C10—H10 | 0.9300 | P2—F8 | 1.5483 (8) |
C11—H11A | 0.9700 | P2—F10' | 1.5489 (13) |
C11—H11B | 0.9700 | P2—F10 | 1.5603 (7) |
C12—C13 | 1.3385 (9) | P2—F11' | 1.5621 (11) |
C12—H12 | 0.9300 | P2—F7 | 1.5694 (8) |
C13—H13 | 0.9300 | P2—F7' | 1.5760 (12) |
C14—H14 | 0.9300 | P2—F8' | 1.6004 (13) |
C15—C16 | 1.5052 (8) | P2—F12 | 1.6016 (7) |
C15—H15A | 0.9700 | N5—C31 | 1.0938 (10) |
C15—H15B | 0.9700 | C33—N6 | 1.0960 (13) |
C16—C17 | 1.3983 (8) | C33—C34 | 1.4374 (14) |
C16—C29 | 1.4047 (8) | N7—C35 | 1.1206 (13) |
C17—C18 | 1.4219 (9) | C31—C32 | 1.4472 (12) |
C17—C22 | 1.4337 (9) | C35—C36 | 1.4337 (13) |
C18—C19 | 1.3510 (10) | C36—H36A | 0.9600 |
C18—H18 | 0.9300 | C36—H36B | 0.9600 |
C19—C20 | 1.3942 (11) | C36—H36C | 0.9600 |
C19—H19 | 0.9300 | C32—H32A | 0.9600 |
C20—C21 | 1.3490 (10) | C32—H32B | 0.9600 |
C20—H20 | 0.9300 | C32—H32C | 0.9600 |
C21—C22 | 1.4233 (9) | C34—H34A | 0.9600 |
C21—H21 | 0.9300 | C34—H34B | 0.9600 |
C22—C23 | 1.4016 (9) | C34—H34C | 0.9600 |
C23—C24 | 1.3934 (9) | ||
C1—N1—C2 | 108.31 (5) | F1—P1—F5 | 89.71 (7) |
C1—N1—C30 | 125.37 (5) | F1'—P1—F5' | 90.15 (5) |
C2—N1—C30 | 126.30 (5) | F3—P1—F5' | 110.84 (6) |
C1—N2—C3 | 108.16 (5) | F4—P1—F5' | 94.00 (5) |
C1—N2—C4 | 123.98 (5) | F2'—P1—F5' | 90.73 (4) |
C3—N2—C4 | 127.54 (5) | F6'—P1—F5' | 174.13 (4) |
C14—N3—C12 | 109.09 (5) | F1—P1—F5' | 70.92 (5) |
C14—N3—C11 | 123.81 (5) | F5—P1—F5' | 19.40 (5) |
C12—N3—C11 | 126.82 (5) | F1'—P1—F4' | 86.32 (5) |
C14—N4—C13 | 108.73 (5) | F3—P1—F4' | 119.24 (7) |
C14—N4—C15 | 125.25 (5) | F4—P1—F4' | 26.85 (5) |
C13—N4—C15 | 125.82 (5) | F2'—P1—F4' | 176.68 (4) |
N1—C1—N2 | 108.74 (5) | F6'—P1—F4' | 89.99 (4) |
N1—C1—H1 | 125.6 | F1—P1—F4' | 70.86 (6) |
N2—C1—H1 | 125.6 | F5—P1—F4' | 97.20 (5) |
C3—C2—N1 | 107.32 (5) | F5'—P1—F4' | 86.38 (4) |
C3—C2—H2 | 126.3 | F1'—P1—F3' | 174.44 (4) |
N1—C2—H2 | 126.3 | F3—P1—F3' | 38.53 (6) |
C2—C3—N2 | 107.46 (6) | F4—P1—F3' | 63.16 (5) |
C2—C3—H3 | 126.3 | F2'—P1—F3' | 89.75 (4) |
N2—C3—H3 | 126.3 | F6'—P1—F3' | 87.74 (4) |
N2—C4—C5 | 110.79 (5) | F1—P1—F3' | 150.60 (5) |
N2—C4—H4A | 109.5 | F5—P1—F3' | 71.87 (6) |
C5—C4—H4A | 109.5 | F5'—P1—F3' | 87.55 (4) |
N2—C4—H4B | 109.5 | F4'—P1—F3' | 88.49 (4) |
C5—C4—H4B | 109.5 | F1'—P1—F2 | 63.90 (6) |
H4A—C4—H4B | 108.1 | F3—P1—F2 | 88.85 (7) |
C6—C5—C10 | 118.51 (6) | F4—P1—F2 | 172.03 (6) |
C6—C5—C4 | 120.41 (6) | F2'—P1—F2 | 31.53 (5) |
C10—C5—C4 | 121.02 (6) | F6'—P1—F2 | 92.58 (5) |
C5—C6—C7 | 120.09 (7) | F1—P1—F2 | 80.74 (6) |
C5—C6—H6 | 120.0 | F5—P1—F2 | 91.34 (6) |
C7—C6—H6 | 120.0 | F5'—P1—F2 | 92.85 (5) |
C6—C7—C8 | 121.02 (7) | F4'—P1—F2 | 150.21 (5) |
C6—C7—H7 | 119.5 | F3'—P1—F2 | 121.26 (5) |
C8—C7—H7 | 119.5 | F1'—P1—F6 | 67.96 (5) |
C7—C8—C9 | 120.05 (7) | F3—P1—F6 | 90.40 (7) |
C7—C8—H8 | 120.0 | F4—P1—F6 | 91.24 (6) |
C9—C8—H8 | 120.0 | F2'—P1—F6 | 94.62 (5) |
C8—C9—C10 | 118.47 (6) | F6'—P1—F6 | 26.28 (5) |
C8—C9—C11 | 121.33 (6) | F1—P1—F6 | 87.04 (6) |
C10—C9—C11 | 120.19 (6) | F5—P1—F6 | 171.98 (6) |
C9—C10—C5 | 121.85 (6) | F5'—P1—F6 | 157.83 (5) |
C9—C10—H10 | 119.1 | F4'—P1—F6 | 88.67 (4) |
C5—C10—H10 | 119.1 | F3'—P1—F6 | 113.93 (5) |
N3—C11—C9 | 110.54 (5) | F2—P1—F6 | 80.90 (6) |
N3—C11—H11A | 109.5 | F9—P2—F12' | 115.66 (6) |
C9—C11—H11A | 109.5 | F9—P2—F11 | 91.39 (4) |
N3—C11—H11B | 109.5 | F12'—P2—F11 | 152.46 (6) |
C9—C11—H11B | 109.5 | F9—P2—F9' | 25.07 (6) |
H11A—C11—H11B | 108.1 | F12'—P2—F9' | 96.79 (8) |
C13—C12—N3 | 106.68 (5) | F11—P2—F9' | 110.62 (7) |
C13—C12—H12 | 126.7 | F9—P2—F8 | 95.26 (4) |
N3—C12—H12 | 126.7 | F12'—P2—F8 | 83.27 (6) |
C12—C13—N4 | 107.33 (5) | F11—P2—F8 | 89.47 (4) |
C12—C13—H13 | 126.3 | F9'—P2—F8 | 110.46 (7) |
N4—C13—H13 | 126.3 | F9—P2—F10' | 104.13 (6) |
N4—C14—N3 | 108.17 (5) | F12'—P2—F10' | 90.75 (7) |
N4—C14—H14 | 125.9 | F11—P2—F10' | 87.28 (6) |
N3—C14—H14 | 125.9 | F9'—P2—F10' | 88.72 (8) |
N4—C15—C16 | 110.23 (4) | F8—P2—F10' | 160.41 (6) |
N4—C15—H15A | 109.6 | F9—P2—F10 | 89.10 (4) |
C16—C15—H15A | 109.6 | F12'—P2—F10 | 96.09 (6) |
N4—C15—H15B | 109.6 | F11—P2—F10 | 89.06 (4) |
C16—C15—H15B | 109.6 | F9'—P2—F10 | 74.10 (7) |
H15A—C15—H15B | 108.1 | F8—P2—F10 | 175.43 (4) |
C17—C16—C29 | 120.49 (5) | F10'—P2—F10 | 15.10 (5) |
C17—C16—C15 | 118.64 (5) | F9—P2—F11' | 65.10 (5) |
C29—C16—C15 | 120.82 (5) | F12'—P2—F11' | 172.08 (7) |
C16—C17—C18 | 121.91 (6) | F11—P2—F11' | 26.50 (5) |
C16—C17—C22 | 119.83 (5) | F9'—P2—F11' | 86.08 (8) |
C18—C17—C22 | 118.23 (5) | F8—P2—F11' | 88.81 (6) |
C19—C18—C17 | 120.85 (6) | F10'—P2—F11' | 96.70 (7) |
C19—C18—H18 | 119.6 | F10—P2—F11' | 91.79 (6) |
C17—C18—H18 | 119.6 | F9—P2—F7 | 175.40 (4) |
C18—C19—C20 | 121.14 (7) | F12'—P2—F7 | 60.13 (6) |
C18—C19—H19 | 119.4 | F11—P2—F7 | 92.98 (4) |
C20—C19—H19 | 119.4 | F9'—P2—F7 | 150.60 (6) |
C21—C20—C19 | 120.36 (7) | F8—P2—F7 | 86.19 (4) |
C21—C20—H20 | 119.8 | F10'—P2—F7 | 74.70 (6) |
C19—C20—H20 | 119.8 | F10—P2—F7 | 89.57 (4) |
C20—C21—C22 | 121.39 (7) | F11'—P2—F7 | 119.35 (5) |
C20—C21—H21 | 119.3 | F9—P2—F7' | 152.27 (5) |
C22—C21—H21 | 119.3 | F12'—P2—F7' | 89.93 (7) |
C23—C22—C21 | 122.51 (6) | F11—P2—F7' | 62.53 (5) |
C23—C22—C17 | 119.48 (5) | F9'—P2—F7' | 170.85 (8) |
C21—C22—C17 | 118.01 (6) | F8—P2—F7' | 76.41 (6) |
C24—C23—C22 | 120.92 (5) | F10'—P2—F7' | 84.97 (7) |
C24—C23—C30 | 120.80 (5) | F10—P2—F7' | 99.08 (6) |
C22—C23—C30 | 118.26 (5) | F11'—P2—F7' | 88.07 (6) |
C23—C24—C25 | 123.36 (6) | F7—P2—F7' | 32.32 (5) |
C23—C24—C29 | 119.47 (5) | F9—P2—F8' | 72.85 (6) |
C25—C24—C29 | 117.16 (5) | F12'—P2—F8' | 86.05 (7) |
C26—C25—C24 | 121.88 (6) | F11—P2—F8' | 97.90 (5) |
C26—C25—H25 | 119.1 | F9'—P2—F8' | 86.63 (8) |
C24—C25—H25 | 119.1 | F8—P2—F8' | 23.84 (5) |
C25—C26—C27 | 120.71 (7) | F10'—P2—F8' | 174.00 (6) |
C25—C26—H26 | 119.6 | F10—P2—F8' | 160.72 (5) |
C27—C26—H26 | 119.6 | F11'—P2—F8' | 86.76 (6) |
C28—C27—C26 | 121.18 (7) | F7—P2—F8' | 107.89 (6) |
C28—C27—H27 | 119.4 | F7'—P2—F8' | 100.08 (7) |
C26—C27—H27 | 119.4 | F9—P2—F12 | 87.79 (4) |
C27—C28—C29 | 120.86 (6) | F12'—P2—F12 | 29.09 (6) |
C27—C28—H28 | 119.6 | F11—P2—F12 | 176.65 (4) |
C29—C28—H28 | 119.6 | F9'—P2—F12 | 67.70 (7) |
C16—C29—C28 | 122.48 (5) | F8—P2—F12 | 93.85 (4) |
C16—C29—C24 | 119.37 (5) | F10'—P2—F12 | 89.76 (6) |
C28—C29—C24 | 118.14 (5) | F10—P2—F12 | 87.68 (4) |
N1—C30—C23 | 109.96 (5) | F11'—P2—F12 | 152.88 (5) |
N1—C30—H30A | 109.7 | F7—P2—F12 | 87.76 (4) |
C23—C30—H30A | 109.7 | F7'—P2—F12 | 118.80 (5) |
N1—C30—H30B | 109.7 | F8'—P2—F12 | 84.97 (5) |
C23—C30—H30B | 109.7 | N6—C33—C34 | 178.88 (10) |
H30A—C30—H30B | 108.2 | N5—C31—C32 | 177.95 (10) |
F1'—P1—F3 | 146.83 (7) | N7—C35—C36 | 176.64 (10) |
F1'—P1—F4 | 112.00 (6) | C35—C36—H36A | 109.5 |
F3—P1—F4 | 92.50 (8) | C35—C36—H36B | 109.5 |
F1'—P1—F2' | 95.34 (5) | H36A—C36—H36B | 109.5 |
F3—P1—F2' | 60.36 (7) | C35—C36—H36C | 109.5 |
F4—P1—F2' | 152.20 (6) | H36A—C36—H36C | 109.5 |
F1'—P1—F6' | 94.23 (5) | H36B—C36—H36C | 109.5 |
F3—P1—F6' | 67.06 (7) | C31—C32—H32A | 109.5 |
F4—P1—F6' | 80.74 (5) | C31—C32—H32B | 109.5 |
F2'—P1—F6' | 92.75 (4) | H32A—C32—H32B | 109.5 |
F1'—P1—F1 | 24.40 (5) | C31—C32—H32C | 109.5 |
F3—P1—F1 | 169.54 (8) | H32A—C32—H32C | 109.5 |
F4—P1—F1 | 97.69 (7) | H32B—C32—H32C | 109.5 |
F2'—P1—F1 | 109.72 (6) | C33—C34—H34A | 109.5 |
F6'—P1—F1 | 112.20 (5) | C33—C34—H34B | 109.5 |
F1'—P1—F5 | 106.83 (6) | H34A—C34—H34B | 109.5 |
F3—P1—F5 | 91.49 (8) | C33—C34—H34C | 109.5 |
F4—P1—F5 | 96.47 (7) | H34A—C34—H34C | 109.5 |
F2'—P1—F5 | 79.57 (6) | H34B—C34—H34C | 109.5 |
F6'—P1—F5 | 158.09 (6) | ||
C2—N1—C1—N2 | 0.95 (7) | C15—C16—C17—C18 | −6.67 (8) |
C30—N1—C1—N2 | −177.53 (5) | C29—C16—C17—C22 | −5.69 (8) |
C3—N2—C1—N1 | −0.70 (7) | C15—C16—C17—C22 | 171.55 (5) |
C4—N2—C1—N1 | 173.20 (5) | C16—C17—C18—C19 | 177.25 (6) |
C1—N1—C2—C3 | −0.84 (7) | C22—C17—C18—C19 | −1.00 (9) |
C30—N1—C2—C3 | 177.63 (6) | C17—C18—C19—C20 | 1.50 (10) |
N1—C2—C3—N2 | 0.40 (7) | C18—C19—C20—C21 | −0.65 (11) |
C1—N2—C3—C2 | 0.17 (7) | C19—C20—C21—C22 | −0.69 (11) |
C4—N2—C3—C2 | −173.46 (6) | C20—C21—C22—C23 | −177.76 (6) |
C1—N2—C4—C5 | −60.35 (8) | C20—C21—C22—C17 | 1.13 (9) |
C3—N2—C4—C5 | 112.35 (7) | C16—C17—C22—C23 | 0.35 (8) |
N2—C4—C5—C6 | −72.17 (8) | C18—C17—C22—C23 | 178.63 (5) |
N2—C4—C5—C10 | 105.10 (6) | C16—C17—C22—C21 | −178.58 (5) |
C10—C5—C6—C7 | −0.79 (10) | C18—C17—C22—C21 | −0.29 (8) |
C4—C5—C6—C7 | 176.55 (7) | C21—C22—C23—C24 | −175.97 (5) |
C5—C6—C7—C8 | 0.44 (13) | C17—C22—C23—C24 | 5.15 (8) |
C6—C7—C8—C9 | −0.18 (13) | C21—C22—C23—C30 | 5.72 (8) |
C7—C8—C9—C10 | 0.29 (11) | C17—C22—C23—C30 | −173.15 (5) |
C7—C8—C9—C11 | −178.19 (7) | C22—C23—C24—C25 | 174.29 (5) |
C8—C9—C10—C5 | −0.67 (9) | C30—C23—C24—C25 | −7.45 (8) |
C11—C9—C10—C5 | 177.82 (5) | C22—C23—C24—C29 | −5.25 (7) |
C6—C5—C10—C9 | 0.92 (9) | C30—C23—C24—C29 | 173.01 (5) |
C4—C5—C10—C9 | −176.41 (5) | C23—C24—C25—C26 | −177.72 (6) |
C14—N3—C11—C9 | 64.07 (8) | C29—C24—C25—C26 | 1.83 (8) |
C12—N3—C11—C9 | −109.08 (7) | C24—C25—C26—C27 | −0.53 (10) |
C8—C9—C11—N3 | 73.67 (8) | C25—C26—C27—C28 | −1.90 (11) |
C10—C9—C11—N3 | −104.78 (6) | C26—C27—C28—C29 | 2.91 (10) |
C14—N3—C12—C13 | −0.28 (7) | C17—C16—C29—C28 | −173.25 (5) |
C11—N3—C12—C13 | 173.71 (6) | C15—C16—C29—C28 | 9.57 (8) |
N3—C12—C13—N4 | 0.22 (7) | C17—C16—C29—C24 | 5.57 (7) |
C14—N4—C13—C12 | −0.09 (7) | C15—C16—C29—C24 | −171.61 (5) |
C15—N4—C13—C12 | −175.20 (5) | C27—C28—C29—C16 | 177.34 (6) |
C13—N4—C14—N3 | −0.08 (6) | C27—C28—C29—C24 | −1.50 (8) |
C15—N4—C14—N3 | 175.06 (5) | C23—C24—C29—C16 | −0.11 (7) |
C12—N3—C14—N4 | 0.22 (7) | C25—C24—C29—C16 | −179.68 (5) |
C11—N3—C14—N4 | −173.99 (5) | C23—C24—C29—C28 | 178.76 (5) |
C14—N4—C15—C16 | −34.62 (7) | C25—C24—C29—C28 | −0.81 (7) |
C13—N4—C15—C16 | 139.70 (5) | C1—N1—C30—C23 | 29.28 (8) |
N4—C15—C16—C17 | −63.26 (6) | C2—N1—C30—C23 | −148.93 (6) |
N4—C15—C16—C29 | 113.98 (6) | C24—C23—C30—N1 | −111.55 (6) |
C29—C16—C17—C18 | 176.09 (5) | C22—C23—C30—N1 | 66.75 (6) |
D—H···A | D—H | H···A | D···A | D—H···A |
C1—H1···N5 | 0.93 | 2.52 | 3.407 (3) | 160 |
C14—H14···N5 | 0.93 | 2.47 | 3.387 (3) | 167 |