Supporting information
Crystallographic Information File (CIF) https://doi.org/10.1107/S1600536804015004/wn6256sup1.cif | |
Structure factor file (CIF format) https://doi.org/10.1107/S1600536804015004/wn6256Isup2.hkl |
CCDC reference: 245158
Data collection: CAD-4 EXPRESS (Enraf–Nonius, 1994); cell refinement: CAD-4 EXPRESS; data reduction: XCAD4 (Harms & Wocadlo, 1995); program(s) used to solve structure: SHELXS97 (Sheldrick, 1997); 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 publication routines (Farrugia, 1999).
(C6H18N2)[V2Cl5(C6H16N2)2](C24H20B)·C4H8O | Z = 2 |
Mr = 1021.08 | F(000) = 1080 |
Triclinic, P1 | Dx = 1.287 Mg m−3 |
Hall symbol: -P 1 | Mo Kα radiation, λ = 0.71073 Å |
a = 9.3902 (17) Å | Cell parameters from 25 reflections |
b = 14.9426 (13) Å | θ = 7.3–10° |
c = 19.455 (4) Å | µ = 0.65 mm−1 |
α = 102.125 (14)° | T = 173 K |
β = 98.065 (17)° | Prism, green |
γ = 92.267 (11)° | 0.3 × 0.3 × 0.1 mm |
V = 2635.8 (8) Å3 |
Enraf-Nonius CAD-4 diffractometer | 6586 reflections with I > 2σ(I) |
Radiation source: Enraf Nonius FR590 | Rint = 0 |
Graphite monochromator | θmax = 25.0°, θmin = 2.2° |
non–profiled ω/2θ scans | h = 0→11 |
Absorption correction: ψ scan (North et al., 1968) | k = −17→17 |
Tmin = 0.88, Tmax = 0.94 | l = −23→22 |
9241 measured reflections | 2 standard reflections every 60 min |
9241 independent reflections | intensity decay: 4% |
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)] = 0.046 | Hydrogen site location: inferred from neighbouring sites |
wR(F2) = 0.118 | H atoms treated by a mixture of independent and constrained refinement |
S = 0.98 | w = 1/[σ2(Fo2) + (0.058P)2 + 1.5496P] where P = (Fo2 + 2Fc2)/3 |
9241 reflections | (Δ/σ)max = 0.001 |
586 parameters | Δρmax = 0.37 e Å−3 |
0 restraints | Δρmin = −0.48 e Å−3 |
Experimental. Number of psi-scan sets used was 1 Theta correction was applied. Averaged transmission function was used. No Fourier smoothing was applied. |
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) | |
V1 | 0.11493 (6) | 0.71094 (4) | 0.21680 (3) | 0.02443 (14) | |
V2 | 0.30908 (6) | 0.81288 (4) | 0.35489 (3) | 0.02486 (14) | |
Cl1 | 0.35737 (9) | 0.79419 (6) | 0.22963 (4) | 0.0297 (2) | |
Cl2 | 0.05382 (9) | 0.83816 (6) | 0.31252 (5) | 0.0328 (2) | |
Cl3 | 0.00784 (9) | 0.79098 (6) | 0.12430 (4) | 0.0309 (2) | |
Cl4 | 0.37687 (9) | 0.97999 (5) | 0.38278 (4) | 0.0300 (2) | |
Cl5 | 0.23155 (10) | 0.64638 (6) | 0.31682 (5) | 0.0350 (2) | |
O1 | 0.2350 (3) | 0.33060 (18) | 0.44624 (16) | 0.0505 (7) | |
N1 | 0.1646 (3) | 0.59156 (19) | 0.13345 (15) | 0.0347 (7) | |
N2 | −0.0899 (3) | 0.6227 (2) | 0.20585 (17) | 0.0398 (8) | |
N3 | 0.5346 (3) | 0.78822 (19) | 0.39911 (15) | 0.0301 (7) | |
N4 | 0.2728 (3) | 0.8148 (2) | 0.46781 (15) | 0.0352 (7) | |
N5 | 0.2297 (3) | 0.9420 (2) | 0.11912 (14) | 0.0271 (6) | |
H5 | 0.181 (4) | 0.891 (3) | 0.128 (2) | 0.047 (12)* | |
N6 | 0.1594 (3) | 1.0724 (2) | 0.29794 (15) | 0.0295 (7) | |
H6 | 0.211 (4) | 1.032 (3) | 0.320 (2) | 0.041 (11)* | |
C3 | 0.1824 (6) | 0.6148 (3) | 0.0658 (2) | 0.0691 (16) | |
H3A | 0.098 | 0.6453 | 0.0489 | 0.104* | |
H3B | 0.1919 | 0.5587 | 0.0307 | 0.104* | |
H3C | 0.2692 | 0.6562 | 0.0724 | 0.104* | |
C4 | 0.2930 (5) | 0.5463 (3) | 0.1560 (2) | 0.0579 (13) | |
H4A | 0.2846 | 0.5292 | 0.2013 | 0.087* | |
H4B | 0.3788 | 0.5883 | 0.1619 | 0.087* | |
H4C | 0.3015 | 0.491 | 0.1198 | 0.087* | |
C7 | 0.5387 (4) | 0.8148 (3) | 0.47737 (19) | 0.0443 (10) | |
H7A | 0.5465 | 0.8825 | 0.4927 | 0.053* | |
H7B | 0.6248 | 0.7913 | 0.5014 | 0.053* | |
C8 | 0.4054 (5) | 0.7768 (3) | 0.4990 (2) | 0.0444 (10) | |
H8A | 0.3971 | 0.7091 | 0.483 | 0.053* | |
H8B | 0.4139 | 0.7919 | 0.5515 | 0.053* | |
C9 | 0.6500 (4) | 0.8448 (3) | 0.3800 (2) | 0.0453 (10) | |
H9A | 0.6309 | 0.9098 | 0.3926 | 0.068* | |
H9B | 0.6521 | 0.8269 | 0.3287 | 0.068* | |
H9C | 0.7433 | 0.8352 | 0.406 | 0.068* | |
C10 | 0.5715 (4) | 0.6923 (2) | 0.3784 (2) | 0.0409 (9) | |
H10A | 0.4982 | 0.6515 | 0.3898 | 0.061* | |
H10B | 0.6658 | 0.6849 | 0.4045 | 0.061* | |
H10C | 0.5749 | 0.6767 | 0.3272 | 0.061* | |
C11 | 0.2570 (5) | 0.9069 (3) | 0.5102 (2) | 0.0455 (10) | |
H11A | 0.3393 | 0.9483 | 0.5084 | 0.068* | |
H11B | 0.2537 | 0.9033 | 0.5597 | 0.068* | |
H11C | 0.1676 | 0.9304 | 0.4909 | 0.068* | |
C12 | 0.1464 (5) | 0.7567 (3) | 0.4728 (2) | 0.0504 (11) | |
H12A | 0.1515 | 0.6946 | 0.4447 | 0.076* | |
H12B | 0.0583 | 0.7825 | 0.4545 | 0.076* | |
H12C | 0.1449 | 0.7542 | 0.5227 | 0.076* | |
C13 | 0.2643 (4) | 1.0066 (2) | 0.18977 (18) | 0.0294 (8) | |
H13A | 0.3142 | 1.0638 | 0.1844 | 0.035* | |
H13B | 0.3298 | 0.9785 | 0.2224 | 0.035* | |
C14 | 0.1276 (4) | 1.0288 (2) | 0.22093 (18) | 0.0317 (8) | |
H14A | 0.0742 | 1.0708 | 0.1953 | 0.038* | |
H14B | 0.0653 | 0.9717 | 0.2142 | 0.038* | |
C15 | 0.1334 (4) | 0.9805 (3) | 0.0672 (2) | 0.0415 (10) | |
H15A | 0.0467 | 0.9998 | 0.0874 | 0.062* | |
H15B | 0.1059 | 0.9337 | 0.0233 | 0.062* | |
H15C | 0.184 | 1.0336 | 0.0568 | 0.062* | |
C16 | 0.3629 (4) | 0.9115 (2) | 0.0910 (2) | 0.0353 (9) | |
H16A | 0.4239 | 0.8863 | 0.1265 | 0.053* | |
H16B | 0.4156 | 0.9639 | 0.0808 | 0.053* | |
H16C | 0.3372 | 0.8641 | 0.0472 | 0.053* | |
C17 | 0.2514 (5) | 1.1590 (3) | 0.3126 (2) | 0.0461 (10) | |
H17A | 0.2694 | 1.1847 | 0.3639 | 0.069* | |
H17B | 0.2025 | 1.2029 | 0.2882 | 0.069* | |
H17C | 0.3434 | 1.1467 | 0.2953 | 0.069* | |
C18 | 0.0230 (4) | 1.0856 (3) | 0.3282 (2) | 0.0475 (11) | |
H18A | 0.0453 | 1.1139 | 0.379 | 0.071* | |
H18B | −0.0304 | 1.026 | 0.3217 | 0.071* | |
H18C | −0.0357 | 1.1256 | 0.3037 | 0.071* | |
C19 | 0.7139 (3) | 0.1411 (2) | 0.19446 (17) | 0.0248 (7) | |
C20 | 0.6471 (4) | 0.1176 (2) | 0.24901 (19) | 0.0311 (8) | |
H20 | 0.6053 | 0.1644 | 0.2793 | 0.037* | |
C21 | 0.6393 (4) | 0.0292 (3) | 0.2608 (2) | 0.0381 (9) | |
H21 | 0.5946 | 0.0169 | 0.2991 | 0.046* | |
C22 | 0.6962 (4) | −0.0406 (3) | 0.2174 (2) | 0.0403 (10) | |
H22 | 0.6912 | −0.1012 | 0.2252 | 0.048* | |
C23 | 0.7607 (4) | −0.0209 (2) | 0.1623 (2) | 0.0353 (9) | |
H23 | 0.8 | −0.0685 | 0.1316 | 0.042* | |
C24 | 0.7686 (4) | 0.0674 (2) | 0.15160 (19) | 0.0301 (8) | |
H24 | 0.8135 | 0.0787 | 0.1131 | 0.036* | |
C25 | 0.6022 (3) | 0.2419 (2) | 0.10517 (17) | 0.0249 (7) | |
C26 | 0.5971 (4) | 0.3143 (2) | 0.06915 (19) | 0.0348 (8) | |
H26 | 0.6665 | 0.365 | 0.0859 | 0.042* | |
C27 | 0.4959 (4) | 0.3150 (3) | 0.0105 (2) | 0.0414 (10) | |
H27 | 0.4956 | 0.3662 | −0.0113 | 0.05* | |
C28 | 0.3949 (4) | 0.2417 (3) | −0.01659 (19) | 0.0386 (9) | |
H28 | 0.3256 | 0.2418 | −0.0572 | 0.046* | |
C29 | 0.3970 (4) | 0.1689 (3) | 0.01635 (19) | 0.0361 (9) | |
H29 | 0.3289 | 0.1177 | −0.0017 | 0.043* | |
C30 | 0.4980 (3) | 0.1700 (2) | 0.07581 (18) | 0.0282 (8) | |
H30 | 0.4961 | 0.1189 | 0.0977 | 0.034* | |
C31 | 0.6800 (3) | 0.3217 (2) | 0.24366 (17) | 0.0238 (7) | |
C32 | 0.5795 (3) | 0.3869 (2) | 0.23794 (18) | 0.0270 (7) | |
H32 | 0.526 | 0.3855 | 0.1925 | 0.032* | |
C33 | 0.5536 (4) | 0.4533 (2) | 0.29470 (19) | 0.0302 (8) | |
H33 | 0.4836 | 0.496 | 0.2878 | 0.036* | |
C34 | 0.6290 (4) | 0.4577 (2) | 0.36141 (19) | 0.0322 (8) | |
H34 | 0.6138 | 0.5047 | 0.4004 | 0.039* | |
C35 | 0.7264 (4) | 0.3937 (2) | 0.37101 (18) | 0.0327 (8) | |
H35 | 0.7772 | 0.3949 | 0.4171 | 0.039* | |
C36 | 0.7501 (4) | 0.3277 (2) | 0.31380 (18) | 0.0297 (8) | |
H36 | 0.8174 | 0.2838 | 0.3218 | 0.036* | |
C37 | 0.8838 (3) | 0.2673 (2) | 0.16115 (17) | 0.0234 (7) | |
C38 | 0.9225 (4) | 0.2424 (2) | 0.09245 (18) | 0.0311 (8) | |
H38 | 0.8486 | 0.2177 | 0.0537 | 0.037* | |
C39 | 1.0624 (4) | 0.2520 (3) | 0.0785 (2) | 0.0363 (9) | |
H39 | 1.0823 | 0.2327 | 0.0313 | 0.044* | |
C40 | 1.1727 (4) | 0.2892 (2) | 0.13258 (19) | 0.0320 (8) | |
H40 | 1.2691 | 0.2949 | 0.1236 | 0.038* | |
C41 | 1.1396 (4) | 0.3180 (2) | 0.20019 (19) | 0.0328 (8) | |
H41 | 1.2135 | 0.3458 | 0.2381 | 0.039* | |
C42 | 0.9997 (4) | 0.3067 (2) | 0.21343 (18) | 0.0294 (8) | |
H42 | 0.9815 | 0.3268 | 0.2608 | 0.035* | |
C43 | 0.3427 (4) | 0.3841 (3) | 0.4264 (2) | 0.0438 (10) | |
H43A | 0.3635 | 0.3546 | 0.3786 | 0.053* | |
H43B | 0.4326 | 0.3898 | 0.4608 | 0.053* | |
C44 | 0.2889 (4) | 0.4773 (3) | 0.4255 (2) | 0.0466 (10) | |
H44A | 0.3315 | 0.5228 | 0.469 | 0.056* | |
H44B | 0.3116 | 0.499 | 0.3833 | 0.056* | |
C45 | 0.1290 (4) | 0.4616 (3) | 0.4224 (2) | 0.0489 (11) | |
H45A | 0.0892 | 0.5154 | 0.4503 | 0.059* | |
H45B | 0.079 | 0.4489 | 0.3727 | 0.059* | |
C46 | 0.1143 (5) | 0.3802 (3) | 0.4543 (3) | 0.0622 (13) | |
H46A | 0.1065 | 0.4001 | 0.5054 | 0.075* | |
H46B | 0.0262 | 0.3415 | 0.4301 | 0.075* | |
B1 | 0.7193 (4) | 0.2441 (3) | 0.1769 (2) | 0.0244 (8) | |
C1 | 0.0384 (5) | 0.5250 (3) | 0.1225 (3) | 0.0677 (15) | 0.564 (13) |
H1A | 0.0281 | 0.4879 | 0.0733 | 0.081* | 0.564 (13) |
H1B | 0.0596 | 0.4826 | 0.155 | 0.081* | 0.564 (13) |
C2 | −0.0984 (8) | 0.5616 (5) | 0.1334 (5) | 0.046 (3) | 0.564 (13) |
H2A | −0.1722 | 0.5103 | 0.1279 | 0.056* | 0.564 (13) |
H2B | −0.1284 | 0.5969 | 0.0967 | 0.056* | 0.564 (13) |
C5 | −0.2253 (12) | 0.6806 (8) | 0.1994 (6) | 0.045 (3) | 0.564 (13) |
H5A | −0.2198 | 0.7151 | 0.1621 | 0.068* | 0.564 (13) |
H5B | −0.2272 | 0.7234 | 0.2449 | 0.068* | 0.564 (13) |
H5C | −0.3131 | 0.6393 | 0.1872 | 0.068* | 0.564 (13) |
C6 | −0.107 (2) | 0.5734 (11) | 0.2587 (10) | 0.060 (4) | 0.564 (13) |
H6A | −0.1012 | 0.6163 | 0.3048 | 0.09* | 0.564 (13) |
H6B | −0.031 | 0.5307 | 0.2611 | 0.09* | 0.564 (13) |
H6C | −0.2015 | 0.5389 | 0.247 | 0.09* | 0.564 (13) |
C1A | 0.0384 (5) | 0.5250 (3) | 0.1225 (3) | 0.0677 (15) | 0.436 (13) |
H1A1 | −0.0244 | 0.5313 | 0.0787 | 0.081* | 0.436 (13) |
H1A2 | 0.0741 | 0.4628 | 0.1128 | 0.081* | 0.436 (13) |
C2A | −0.0458 (12) | 0.5278 (7) | 0.1735 (7) | 0.052 (4) | 0.436 (13) |
H2A1 | 0.0059 | 0.5022 | 0.2122 | 0.062* | 0.436 (13) |
H2A2 | −0.1343 | 0.4874 | 0.1531 | 0.062* | 0.436 (13) |
C5A | −0.2149 (19) | 0.6430 (12) | 0.1695 (11) | 0.064 (5) | 0.436 (13) |
H5A1 | −0.2394 | 0.7044 | 0.1917 | 0.096* | 0.436 (13) |
H5A2 | −0.2927 | 0.5978 | 0.1705 | 0.096* | 0.436 (13) |
H5A3 | −0.2025 | 0.6414 | 0.1201 | 0.096* | 0.436 (13) |
C6A | −0.120 (3) | 0.6104 (14) | 0.2804 (12) | 0.058 (5) | 0.436 (13) |
H6A1 | −0.0328 | 0.5926 | 0.3065 | 0.088* | 0.436 (13) |
H6A2 | −0.1981 | 0.5625 | 0.2742 | 0.088* | 0.436 (13) |
H6A3 | −0.1487 | 0.6683 | 0.3071 | 0.088* | 0.436 (13) |
U11 | U22 | U33 | U12 | U13 | U23 | |
V1 | 0.0273 (3) | 0.0231 (3) | 0.0213 (3) | −0.0006 (2) | −0.0017 (2) | 0.0053 (2) |
V2 | 0.0294 (3) | 0.0236 (3) | 0.0201 (3) | −0.0005 (2) | −0.0014 (2) | 0.0053 (2) |
Cl1 | 0.0301 (4) | 0.0329 (5) | 0.0243 (4) | −0.0024 (3) | 0.0013 (3) | 0.0055 (3) |
Cl2 | 0.0300 (5) | 0.0365 (5) | 0.0289 (5) | 0.0032 (4) | 0.0015 (4) | 0.0021 (4) |
Cl3 | 0.0315 (5) | 0.0308 (4) | 0.0287 (5) | −0.0010 (4) | −0.0052 (4) | 0.0097 (4) |
Cl4 | 0.0328 (5) | 0.0256 (4) | 0.0283 (4) | 0.0010 (3) | −0.0057 (4) | 0.0058 (3) |
Cl5 | 0.0468 (5) | 0.0267 (4) | 0.0287 (5) | −0.0036 (4) | −0.0077 (4) | 0.0098 (4) |
O1 | 0.0501 (18) | 0.0407 (16) | 0.071 (2) | 0.0095 (13) | 0.0236 (16) | 0.0247 (15) |
N1 | 0.0425 (18) | 0.0290 (16) | 0.0303 (17) | 0.0054 (13) | −0.0006 (14) | 0.0053 (13) |
N2 | 0.0336 (18) | 0.0395 (18) | 0.045 (2) | −0.0068 (14) | 0.0027 (15) | 0.0096 (15) |
N3 | 0.0329 (16) | 0.0260 (15) | 0.0296 (16) | 0.0063 (12) | −0.0006 (13) | 0.0046 (13) |
N4 | 0.0445 (19) | 0.0319 (17) | 0.0282 (16) | −0.0011 (14) | 0.0042 (14) | 0.0059 (13) |
N5 | 0.0276 (16) | 0.0301 (16) | 0.0235 (15) | −0.0006 (13) | 0.0015 (12) | 0.0078 (12) |
N6 | 0.0317 (17) | 0.0288 (16) | 0.0242 (15) | 0.0088 (13) | −0.0034 (13) | 0.0014 (13) |
C3 | 0.129 (5) | 0.051 (3) | 0.035 (2) | 0.030 (3) | 0.032 (3) | 0.008 (2) |
C4 | 0.057 (3) | 0.053 (3) | 0.053 (3) | 0.021 (2) | −0.004 (2) | −0.006 (2) |
C7 | 0.051 (3) | 0.047 (2) | 0.028 (2) | 0.015 (2) | −0.0091 (18) | 0.0015 (18) |
C8 | 0.061 (3) | 0.048 (2) | 0.028 (2) | 0.011 (2) | 0.0023 (19) | 0.0180 (18) |
C9 | 0.035 (2) | 0.045 (2) | 0.055 (3) | 0.0026 (18) | −0.0046 (19) | 0.014 (2) |
C10 | 0.042 (2) | 0.031 (2) | 0.045 (2) | 0.0098 (17) | −0.0035 (18) | 0.0038 (17) |
C11 | 0.064 (3) | 0.042 (2) | 0.031 (2) | 0.000 (2) | 0.014 (2) | 0.0050 (18) |
C12 | 0.060 (3) | 0.053 (3) | 0.039 (2) | −0.013 (2) | 0.014 (2) | 0.012 (2) |
C13 | 0.0274 (18) | 0.0301 (18) | 0.0278 (19) | 0.0008 (15) | −0.0012 (15) | 0.0039 (15) |
C14 | 0.032 (2) | 0.0336 (19) | 0.0249 (19) | 0.0036 (15) | −0.0053 (15) | 0.0017 (15) |
C15 | 0.046 (2) | 0.052 (2) | 0.029 (2) | 0.0106 (19) | 0.0007 (18) | 0.0161 (18) |
C16 | 0.034 (2) | 0.036 (2) | 0.036 (2) | 0.0009 (16) | 0.0106 (17) | 0.0053 (17) |
C17 | 0.055 (3) | 0.033 (2) | 0.041 (2) | 0.0016 (19) | −0.009 (2) | 0.0008 (18) |
C18 | 0.040 (2) | 0.063 (3) | 0.035 (2) | 0.019 (2) | 0.0029 (18) | −0.001 (2) |
C19 | 0.0173 (16) | 0.0297 (18) | 0.0248 (18) | 0.0015 (13) | −0.0037 (14) | 0.0052 (14) |
C20 | 0.0226 (18) | 0.036 (2) | 0.034 (2) | 0.0009 (15) | 0.0020 (15) | 0.0087 (16) |
C21 | 0.031 (2) | 0.045 (2) | 0.041 (2) | −0.0046 (17) | −0.0013 (17) | 0.0215 (19) |
C22 | 0.038 (2) | 0.030 (2) | 0.051 (3) | −0.0042 (17) | −0.0093 (19) | 0.0163 (18) |
C23 | 0.029 (2) | 0.0284 (19) | 0.043 (2) | 0.0030 (15) | −0.0073 (17) | 0.0026 (17) |
C24 | 0.0258 (18) | 0.0311 (19) | 0.0310 (19) | 0.0007 (15) | −0.0010 (15) | 0.0055 (15) |
C25 | 0.0222 (17) | 0.0288 (18) | 0.0234 (18) | 0.0043 (14) | 0.0056 (14) | 0.0030 (14) |
C26 | 0.033 (2) | 0.034 (2) | 0.035 (2) | 0.0011 (16) | 0.0002 (17) | 0.0085 (16) |
C27 | 0.043 (2) | 0.048 (2) | 0.038 (2) | 0.0135 (19) | 0.0019 (18) | 0.0200 (19) |
C28 | 0.0265 (19) | 0.063 (3) | 0.0232 (19) | 0.0047 (18) | −0.0046 (15) | 0.0085 (18) |
C29 | 0.0241 (19) | 0.051 (2) | 0.029 (2) | −0.0013 (16) | 0.0002 (15) | 0.0043 (18) |
C30 | 0.0246 (18) | 0.0327 (19) | 0.0268 (18) | 0.0010 (14) | 0.0030 (15) | 0.0060 (15) |
C31 | 0.0196 (16) | 0.0248 (17) | 0.0278 (18) | 0.0010 (13) | 0.0066 (14) | 0.0056 (14) |
C32 | 0.0224 (17) | 0.0312 (18) | 0.0266 (18) | 0.0022 (14) | 0.0004 (14) | 0.0064 (15) |
C33 | 0.0262 (18) | 0.0294 (19) | 0.036 (2) | 0.0098 (15) | 0.0058 (16) | 0.0082 (16) |
C34 | 0.032 (2) | 0.034 (2) | 0.030 (2) | 0.0069 (16) | 0.0088 (16) | 0.0023 (16) |
C35 | 0.032 (2) | 0.042 (2) | 0.0229 (18) | 0.0044 (16) | 0.0034 (15) | 0.0046 (16) |
C36 | 0.0253 (18) | 0.036 (2) | 0.0280 (19) | 0.0068 (15) | 0.0033 (15) | 0.0080 (16) |
C37 | 0.0275 (18) | 0.0206 (16) | 0.0227 (17) | 0.0051 (13) | 0.0016 (14) | 0.0065 (13) |
C38 | 0.0285 (19) | 0.037 (2) | 0.0242 (18) | 0.0013 (15) | −0.0006 (15) | 0.0013 (15) |
C39 | 0.036 (2) | 0.045 (2) | 0.028 (2) | 0.0034 (17) | 0.0118 (17) | 0.0038 (17) |
C40 | 0.0241 (18) | 0.036 (2) | 0.039 (2) | 0.0021 (15) | 0.0075 (16) | 0.0132 (17) |
C41 | 0.0275 (19) | 0.035 (2) | 0.034 (2) | −0.0046 (15) | −0.0027 (16) | 0.0092 (16) |
C42 | 0.0311 (19) | 0.0318 (19) | 0.0243 (18) | 0.0024 (15) | −0.0002 (15) | 0.0067 (15) |
C43 | 0.035 (2) | 0.040 (2) | 0.059 (3) | 0.0059 (17) | 0.008 (2) | 0.016 (2) |
C44 | 0.045 (2) | 0.044 (2) | 0.057 (3) | 0.0081 (19) | 0.012 (2) | 0.022 (2) |
C45 | 0.041 (2) | 0.045 (2) | 0.063 (3) | 0.0076 (19) | 0.008 (2) | 0.015 (2) |
C46 | 0.040 (3) | 0.062 (3) | 0.099 (4) | 0.009 (2) | 0.027 (3) | 0.037 (3) |
B1 | 0.0230 (19) | 0.026 (2) | 0.024 (2) | 0.0040 (15) | 0.0018 (16) | 0.0058 (16) |
C1 | 0.059 (3) | 0.040 (3) | 0.085 (4) | −0.008 (2) | 0.005 (3) | −0.023 (2) |
C2 | 0.044 (5) | 0.036 (4) | 0.047 (5) | −0.014 (3) | −0.011 (4) | −0.004 (4) |
C5 | 0.022 (4) | 0.054 (7) | 0.060 (7) | −0.009 (5) | 0.001 (5) | 0.019 (5) |
C6 | 0.054 (7) | 0.064 (10) | 0.063 (11) | −0.019 (7) | −0.001 (7) | 0.028 (7) |
C1A | 0.059 (3) | 0.040 (3) | 0.085 (4) | −0.008 (2) | 0.005 (3) | −0.023 (2) |
C2A | 0.047 (6) | 0.032 (5) | 0.068 (8) | −0.013 (5) | −0.007 (6) | 0.006 (5) |
C5A | 0.046 (7) | 0.061 (11) | 0.090 (14) | −0.003 (8) | 0.015 (9) | 0.026 (9) |
C6A | 0.053 (9) | 0.072 (14) | 0.056 (13) | −0.029 (11) | 0.008 (8) | 0.034 (10) |
V1—N2 | 2.247 (3) | C3—H3C | 0.980 |
V1—N1 | 2.257 (3) | C4—H4A | 0.980 |
V1—Cl3 | 2.4843 (11) | C4—H4B | 0.980 |
V1—Cl5 | 2.4882 (11) | C4—H4C | 0.981 |
V1—Cl1 | 2.5056 (11) | C5—H5A | 0.980 |
V1—Cl2 | 2.5121 (11) | C5—H5B | 0.980 |
V1—V2 | 3.0901 (10) | C5—H5C | 0.980 |
V2—N3 | 2.246 (3) | C6—H6A | 0.980 |
V2—N4 | 2.264 (3) | C6—H6B | 0.979 |
V2—Cl4 | 2.4785 (10) | C6—H6C | 0.981 |
V2—Cl5 | 2.4899 (10) | C7—H7A | 0.989 |
V2—Cl2 | 2.4932 (11) | C7—H7B | 0.990 |
V2—Cl1 | 2.5014 (11) | C8—H8A | 0.990 |
O1—C46 | 1.387 (5) | C8—H8B | 0.990 |
O1—C43 | 1.410 (4) | C9—H9A | 0.981 |
N1—C3 | 1.459 (5) | C9—H9B | 0.981 |
N1—C4 | 1.464 (5) | C9—H9C | 0.980 |
N1—C1 | 1.479 (5) | C9—H9B | 0.981 |
N2—C6 | 1.41 (2) | C10—H10A | 0.980 |
N2—C2 | 1.500 (8) | C10—H10B | 0.979 |
N2—C5 | 1.570 (12) | C10—H10C | 0.980 |
N3—C10 | 1.474 (4) | C11—H11A | 0.980 |
N3—C9 | 1.484 (5) | C11—H11B | 0.980 |
N3—C7 | 1.485 (5) | C11—H11C | 0.979 |
N4—C12 | 1.470 (5) | C12—H12A | 0.980 |
N4—C11 | 1.473 (5) | C12—H12B | 0.980 |
N4—C8 | 1.493 (5) | C12—H12C | 0.981 |
N5—C15 | 1.483 (4) | C13—H13A | 0.990 |
N5—C16 | 1.484 (4) | C13—H13B | 0.990 |
N5—C13 | 1.490 (4) | C14—H14A | 0.990 |
N6—C17 | 1.480 (5) | C14—H14B | 0.990 |
N6—C14 | 1.486 (4) | C15—H15A | 0.980 |
N6—C18 | 1.486 (5) | C15—H15B | 0.979 |
C7—C8 | 1.502 (6) | C15—H15C | 0.980 |
C13—C14 | 1.515 (5) | C16—H16A | 0.981 |
C19—C24 | 1.397 (5) | C16—H16B | 0.980 |
C19—C20 | 1.403 (5) | C16—H16C | 0.980 |
C19—B1 | 1.646 (5) | C17—H17A | 0.979 |
C20—C21 | 1.390 (5) | C17—H17B | 0.980 |
C21—C22 | 1.373 (5) | C17—H17C | 0.981 |
C22—C23 | 1.379 (5) | C18—H18A | 0.979 |
C23—C24 | 1.380 (5) | C18—H18B | 0.980 |
C25—C30 | 1.393 (4) | C18—H18C | 0.980 |
C25—C26 | 1.405 (5) | C43—H43A | 0.991 |
C25—B1 | 1.644 (5) | C43—H43B | 0.990 |
C26—C27 | 1.381 (5) | C44—H44A | 0.990 |
C27—C28 | 1.382 (5) | C44—H44B | 0.990 |
C28—C29 | 1.373 (5) | C45—H45A | 0.989 |
C29—C30 | 1.387 (5) | C45—H45B | 0.990 |
C31—C32 | 1.394 (4) | C46—H46A | 0.990 |
C31—C36 | 1.412 (5) | C46—H46B | 0.989 |
C31—B1 | 1.644 (5) | C20—H20 | 0.951 |
C32—C33 | 1.377 (5) | C21—H21 | 0.951 |
C33—C34 | 1.376 (5) | C22—H22 | 0.950 |
C34—C35 | 1.373 (5) | C23—H23 | 0.950 |
C35—C36 | 1.373 (5) | C24—H24 | 0.950 |
C37—C42 | 1.398 (4) | C26—H26 | 0.950 |
C37—C38 | 1.413 (5) | C27—H27 | 0.949 |
C37—B1 | 1.654 (5) | C28—H28 | 0.951 |
C38—C39 | 1.386 (5) | C29—H29 | 0.950 |
C39—C40 | 1.375 (5) | C30—H30 | 0.950 |
C40—C41 | 1.378 (5) | C32—H32 | 0.949 |
C41—C42 | 1.384 (5) | C33—H33 | 0.950 |
C43—C44 | 1.503 (5) | C34—H34 | 0.951 |
C44—C45 | 1.501 (5) | C35—H35 | 0.951 |
C45—C46 | 1.486 (6) | C36—H36 | 0.950 |
C1—C2 | 1.441 (9) | C38—H38 | 0.950 |
C1—H1A | 0.990 | C39—H39 | 0.950 |
C1—H1B | 0.992 | C40—H40 | 0.950 |
C2—H2A | 0.991 | C41—H41 | 0.950 |
C2—H2B | 0.990 | C42—H42 | 0.949 |
C3—H3A | 0.981 | N5—H5 | 0.93 (4) |
C3—H3B | 0.980 | N6—H6 | 0.92 (4) |
N2—V1—N1 | 81.65 (12) | O1—C43—C44 | 108.2 (3) |
N2—V1—Cl3 | 91.86 (9) | C45—C44—C43 | 103.3 (3) |
N1—V1—Cl3 | 91.59 (8) | C46—C45—C44 | 103.7 (3) |
N2—V1—Cl5 | 92.17 (9) | O1—C46—C45 | 108.5 (3) |
N1—V1—Cl5 | 93.13 (8) | C31—B1—C25 | 109.9 (3) |
Cl3—V1—Cl5 | 174.20 (4) | C31—B1—C19 | 111.2 (3) |
N2—V1—Cl1 | 173.87 (9) | C25—B1—C19 | 108.1 (3) |
N1—V1—Cl1 | 94.11 (9) | C31—B1—C37 | 110.4 (3) |
Cl3—V1—Cl1 | 92.69 (4) | C25—B1—C37 | 109.6 (3) |
Cl5—V1—Cl1 | 83.61 (4) | C19—B1—C37 | 107.6 (3) |
N2—V1—Cl2 | 96.09 (9) | C2—C1—N1 | 117.2 (4) |
N1—V1—Cl2 | 177.12 (8) | C1—C2—N2 | 111.4 (6) |
Cl3—V1—Cl2 | 90.27 (4) | N1—C1A—H1A | 108.04 |
Cl5—V1—Cl2 | 85.15 (4) | N1—C1A—H1B | 107.97 |
Cl1—V1—Cl2 | 88.00 (4) | N2—C2—H2A | 109.37 |
N2—V1—V2 | 128.10 (9) | N2—C2—H2B | 109.44 |
N1—V1—V2 | 128.68 (8) | N2—C5—H5A | 109.44 |
Cl3—V1—V2 | 122.57 (3) | N2—C5—H5B | 109.39 |
Cl5—V1—V2 | 51.65 (3) | N2—C5—H5C | 109.40 |
Cl1—V1—V2 | 51.83 (3) | N2—C6—H6A | 109.46 |
Cl2—V1—V2 | 51.60 (3) | N2—C6—H6B | 109.66 |
N3—V2—N4 | 82.04 (11) | N2—C6—H6C | 109.37 |
N3—V2—Cl4 | 89.51 (8) | N3—C7—H7A | 109.49 |
N4—V2—Cl4 | 92.50 (8) | N3—C7—H7B | 109.43 |
N3—V2—Cl5 | 93.73 (8) | N3—C9—H9A | 109.51 |
N4—V2—Cl5 | 91.45 (8) | N3—C9—H9B | 109.53 |
Cl4—V2—Cl5 | 175.20 (4) | N3—C9—H9C | 109.48 |
N3—V2—Cl2 | 176.48 (8) | N3—C10—H10A | 109.43 |
N4—V2—Cl2 | 94.53 (9) | N3—C10—H10B | 109.48 |
Cl4—V2—Cl2 | 91.45 (4) | N3—C10—H10C | 109.51 |
Cl5—V2—Cl2 | 85.52 (4) | N4—C11—H11A | 109.52 |
N3—V2—Cl1 | 94.82 (8) | N4—C11—H11B | 109.44 |
N4—V2—Cl1 | 174.04 (8) | N4—C11—H11C | 109.56 |
Cl4—V2—Cl1 | 92.55 (4) | N4—C12—H12A | 109.54 |
Cl5—V2—Cl1 | 83.66 (4) | N4—C12—H12B | 109.54 |
Cl2—V2—Cl1 | 88.52 (4) | N4—C12—H12C | 109.48 |
N3—V2—V1 | 129.60 (8) | N5—C15—H15A | 109.37 |
N4—V2—V1 | 126.80 (8) | N5—C15—H15B | 109.41 |
Cl4—V2—V1 | 123.63 (3) | N5—C15—H15C | 109.42 |
Cl5—V2—V1 | 51.60 (3) | N5—C13—H13A | 109.55 |
Cl2—V2—V1 | 52.15 (3) | N5—C13—H13B | 109.57 |
Cl1—V2—V1 | 51.95 (3) | N5—C16—H16A | 109.45 |
V2—Cl1—V1 | 76.22 (3) | N5—C16—H16B | 109.47 |
V2—Cl2—V1 | 76.25 (3) | N5—C16—H16C | 109.50 |
V1—Cl5—V2 | 76.74 (3) | N6—C14—H14A | 109.27 |
C46—O1—C43 | 109.6 (3) | N6—C14—H14B | 109.39 |
C3—N1—C4 | 107.2 (4) | N6—C17—H17A | 109.51 |
C3—N1—C1 | 109.3 (4) | N6—C17—H17B | 109.48 |
C4—N1—C1 | 107.8 (3) | N6—C17—H17C | 109.45 |
C3—N1—V1 | 114.1 (2) | N6—C18—H18A | 109.42 |
C4—N1—V1 | 113.8 (2) | N6—C18—H18B | 109.45 |
C1—N1—V1 | 104.3 (2) | N6—C18—H18C | 109.39 |
C6—N2—C2 | 112.7 (7) | C7—C8—H8A | 109.28 |
C6—N2—C5 | 106.2 (10) | C7—C8—H8B | 109.29 |
C2—N2—C5 | 104.2 (5) | C15—N5—H5 | 109 (2) |
C6—N2—V1 | 118.8 (8) | H13A—C13—H13B | 108.18 |
C2—N2—V1 | 103.2 (3) | H6—N6—C14 | 107 (2) |
C5—N2—V1 | 111.0 (4) | H6—N6—C17 | 107 (3) |
C10—N3—C9 | 105.9 (3) | H6—N6—C18 | 108 (2) |
C10—N3—C7 | 110.1 (3) | O1—C43—H43A | 110.03 |
C9—N3—C7 | 107.9 (3) | O1—C43—H43B | 110.07 |
C10—N3—V2 | 114.0 (2) | O1—C46—H46A | 110.00 |
C9—N3—V2 | 115.0 (2) | O1—C46—H46B | 109.98 |
C7—N3—V2 | 103.9 (2) | C19—C20—H20 | 118.46 |
C12—N4—C11 | 106.6 (3) | C19—C24—H24 | 118.31 |
C12—N4—C8 | 108.7 (3) | C20—C21—H21 | 119.93 |
C11—N4—C8 | 109.8 (3) | C21—C22—H22 | 120.61 |
C12—N4—V2 | 114.0 (2) | C21—C20—H20 | 118.50 |
C11—N4—V2 | 114.2 (2) | C22—C21—H21 | 119.84 |
C8—N4—V2 | 103.4 (2) | C23—C22—H22 | 119.73 |
C15—N5—C16 | 111.6 (3) | C23—C24—H24 | 118.36 |
C15—N5—C13 | 112.3 (3) | C24—C23—H23 | 119.86 |
C16—N5—C13 | 111.2 (3) | C25—C26—H26 | 118.50 |
C17—N6—C14 | 112.7 (3) | C25—C30—H30 | 118.23 |
C17—N6—C18 | 111.8 (3) | C26—C27—H27 | 119.76 |
C14—N6—C18 | 110.2 (3) | C27—C26—H26 | 118.52 |
N3—C7—C8 | 111.0 (3) | C27—C28—H28 | 120.59 |
N4—C8—C7 | 111.6 (3) | C28—C27—H27 | 119.81 |
N5—C13—C14 | 110.3 (3) | C28—C29—H29 | 119.82 |
N6—C14—C13 | 111.6 (3) | C29—C28—H28 | 120.82 |
C24—C19—C20 | 114.3 (3) | C29—C30—H30 | 118.20 |
C24—C19—B1 | 121.2 (3) | C30—C29—H29 | 120.00 |
C20—C19—B1 | 124.3 (3) | C31—C32—H32 | 118.26 |
C21—C20—C19 | 123.0 (3) | C31—C36—H36 | 118.21 |
C22—C21—C20 | 120.2 (4) | C32—C33—H33 | 120.00 |
C21—C22—C23 | 118.8 (3) | C33—C32—H32 | 118.23 |
C22—C23—C24 | 120.4 (4) | C33—C34—H34 | 120.26 |
C23—C24—C19 | 123.3 (3) | C34—C33—H33 | 119.99 |
C30—C25—C26 | 114.2 (3) | C34—C35—H35 | 120.18 |
C30—C25—B1 | 123.4 (3) | C35—C34—H34 | 120.41 |
C26—C25—B1 | 122.3 (3) | C35—C36—H36 | 118.25 |
C27—C26—C25 | 123.0 (3) | C36—C35—H35 | 120.08 |
C26—C27—C28 | 120.4 (4) | C37—C38—H38 | 118.18 |
C29—C28—C27 | 118.6 (3) | C37—C42—H42 | 118.11 |
C28—C29—C30 | 120.2 (3) | C38—C39—H39 | 118.82 |
C29—C30—C25 | 123.6 (3) | C39—C38—H38 | 118.22 |
C32—C31—C36 | 113.8 (3) | C39—C40—H40 | 120.92 |
C32—C31—B1 | 125.1 (3) | C40—C39—H39 | 119.75 |
C36—C31—B1 | 121.1 (3) | C40—C41—H41 | 119.72 |
C33—C32—C31 | 123.5 (3) | C41—C40—H40 | 120.86 |
C34—C33—C32 | 120.0 (3) | C41—C42—H42 | 118.07 |
C35—C34—C33 | 119.3 (3) | C42—C41—H41 | 119.66 |
C34—C35—C36 | 119.7 (3) | C43—C44—H44A | 111.17 |
C35—C36—C31 | 123.6 (3) | C43—C44—H44B | 111.15 |
C42—C37—C38 | 113.2 (3) | C44—C43—H43A | 110.05 |
C42—C37—B1 | 124.6 (3) | C44—C43—H43B | 110.01 |
C38—C37—B1 | 122.0 (3) | C44—C45—H45A | 111.01 |
C39—C38—C37 | 123.6 (3) | C44—C45—H45B | 111.08 |
C40—C39—C38 | 120.5 (3) | C45—C46—H46A | 110.03 |
C39—C40—C41 | 118.2 (3) | C45—C46—H46B | 109.88 |
C40—C41—C42 | 120.6 (3) | C46—C45—H45A | 110.96 |
C41—C42—C37 | 123.8 (3) | C46—C45—H45B | 110.03 |