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
Key indicators
- Single-crystal X-ray study
- T = 173 K
- Mean (C-C) = 0.005 Å
- R factor = 0.046
- wR factor = 0.118
- Data-to-parameter ratio = 15.8
checkCIF/PLATON results
No syntax errors found
Alert level B PLAT027_ALERT_3_B _diffrn_reflns_theta_full (too) Low ............ 24.98 Deg.
Alert level C PLAT042_ALERT_1_C Calc. and Rep. MoietyFormula Strings Differ .... ? PLAT241_ALERT_2_C Check High U(eq) as Compared to Neighbors .... C1 PLAT241_ALERT_2_C Check High U(eq) as Compared to Neighbors .... C1A PLAT242_ALERT_2_C Check Low U(eq) as Compared to Neighbors .... N1 PLAT301_ALERT_3_C Main Residue Disorder ......................... 8.00 Perc. PLAT720_ALERT_4_C Number of Unusual/Non-Standard Label(s) ........ 10
Alert level G FORMU01_ALERT_1_G There is a discrepancy between the atom counts in the _chemical_formula_sum and _chemical_formula_moiety. This is usually due to the moiety formula being in the wrong format. Atom count from _chemical_formula_sum: C46 H78 B1 Cl5 N6 O1 V2 Atom count from _chemical_formula_moiety:C46 H78 B1 Cl5 N6 V2
0 ALERT level A = In general: serious problem 1 ALERT level B = Potentially serious problem 6 ALERT level C = Check and explain 1 ALERT level G = General alerts; check 2 ALERT type 1 CIF construction/syntax error, inconsistent or missing data 3 ALERT type 2 Indicator that the structure model may be wrong or deficient 2 ALERT type 3 Indicator that the structure quality may be low 1 ALERT type 4 Improvement, methodology, query or suggestion
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 |