Supporting information
Crystallographic Information File (CIF) https://doi.org/10.1107/S1600536805035397/hb6284sup1.cif | |
Structure factor file (CIF format) https://doi.org/10.1107/S1600536805035397/hb6284Isup2.hkl |
CCDC reference: 293899
Key indicators
- Single-crystal X-ray study
- T = 200 K
- Mean (C-C) = 0.010 Å
- Disorder in solvent or counterion
- R factor = 0.034
- wR factor = 0.080
- Data-to-parameter ratio = 12.5
checkCIF/PLATON results
No syntax errors found
Alert level B PLAT331_ALERT_2_B Small Average Phenyl C-C Dist. C61A -C66A 1.36 Ang.
Alert level C PLAT041_ALERT_1_C Calc. and Rep. SumFormula Strings Differ .... ? PLAT042_ALERT_1_C Calc. and Rep. MoietyFormula Strings Differ .... ? PLAT045_ALERT_1_C Calculated and Reported Z Differ by ............ 0.50 Ratio PLAT243_ALERT_4_C High 'Solvent' Ueq as Compared to Neighbors for C64A PLAT244_ALERT_4_C Low 'Solvent' Ueq as Compared to Neighbors for C51A PLAT244_ALERT_4_C Low 'Solvent' Ueq as Compared to Neighbors for C62A PLAT302_ALERT_4_C Anion/Solvent Disorder ......................... 50.00 Perc. PLAT331_ALERT_2_C Small Average Phenyl C-C Dist. C51A -C56A 1.36 Ang. PLAT331_ALERT_2_C Small Average Phenyl C-C Dist. C51B -C56B 1.37 Ang. PLAT342_ALERT_3_C Low Bond Precision on C-C bonds (x 1000) Ang ... 10 PLAT380_ALERT_4_C Check Incorrectly? Oriented X(sp2)-Methyl Moiety C57A PLAT380_ALERT_4_C Check Incorrectly? Oriented X(sp2)-Methyl Moiety C67A
0 ALERT level A = In general: serious problem 1 ALERT level B = Potentially serious problem 12 ALERT level C = Check and explain 0 ALERT level G = General alerts; check 3 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 1 ALERT type 3 Indicator that the structure quality may be low 6 ALERT type 4 Improvement, methodology, query or suggestion
Data collection: Please provide; cell refinement: Please provide; data reduction: Please provide; 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 (Farrugia, 1999).
[W2(C6H6NO)4]·1.5C7H8 | F(000) = 1804 |
Mr = 938.37 | Dx = 1.884 Mg m−3 |
Monoclinic, P21/c | Mo Kα radiation, λ = 0.71073 Å |
Hall symbol: -P 2ybc | Cell parameters from 6111 reflections |
a = 15.563 (2) Å | θ = 2.0–25.0° |
b = 12.975 (2) Å | µ = 6.99 mm−1 |
c = 16.486 (3) Å | T = 200 K |
β = 96.48 (1)° | Plate, red |
V = 3307.8 (9) Å3 | 0.19 × 0.08 × 0.04 mm |
Z = 4 |
Nonius KappaCCD diffractometer | 4480 reflections with I > 2σ(I) |
Graphite monochromator | Rint = 0.082 |
φ and ω scans | θmax = 25.0°, θmin = 2.1° |
Absorption correction: multi-scan (SCALEPACK; Otwinowski & Minor, 1997) | h = −18→18 |
Tmin = 0.553, Tmax = 0.756 | k = −15→15 |
51699 measured reflections | l = −19→19 |
5840 independent reflections |
Refinement on F2 | Primary atom site location: heavy-atom method |
Least-squares matrix: full | Secondary atom site location: difference Fourier map |
R[F2 > 2σ(F2)] = 0.034 | Hydrogen site location: inferred from neighbouring sites |
wR(F2) = 0.081 | H-atom parameters constrained |
S = 1.04 | w = 1/[σ2(Fo2) + (0.0387P)2 + 6.3721P] where P = (Fo2 + 2Fc2)/3 |
5840 reflections | (Δ/σ)max = 0.028 |
466 parameters | Δρmax = 1.43 e Å−3 |
334 restraints | Δρmin = −1.30 e Å−3 |
Experimental. All work was done at 200 K using an Oxford Cryosystems Cryostream Cooler. The data collection strategy was set up to measure a quadrant of reciprocal space with a redundancy factor of 4.1, which means that 90% of the reflections were measured 4.1 times. A combination of phi and omega scans with a frame width of 1.0 degree was used. Data integration was done with DENZO. Scaling and merging of the data was done with SCALEPACK. |
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. |
x | y | z | Uiso*/Ueq | Occ. (<1) | |
W1 | 0.240278 (18) | 0.11123 (2) | 0.171820 (15) | 0.02990 (10) | |
W2 | 0.373034 (18) | 0.14165 (2) | 0.152580 (15) | 0.02943 (10) | |
O1 | 0.4188 (3) | 0.1231 (3) | 0.2737 (2) | 0.0331 (11) | |
O2 | 0.2513 (3) | −0.0450 (3) | 0.1560 (3) | 0.0361 (11) | |
O3 | 0.2118 (3) | 0.2637 (3) | 0.1922 (2) | 0.0327 (10) | |
O4 | 0.3442 (3) | 0.1643 (3) | 0.0289 (2) | 0.0292 (10) | |
N1 | 0.2796 (4) | 0.0906 (4) | 0.2999 (3) | 0.0329 (13) | |
N2 | 0.3926 (4) | −0.0195 (4) | 0.1331 (3) | 0.0314 (13) | |
N3 | 0.3527 (4) | 0.3023 (4) | 0.1746 (3) | 0.0297 (13) | |
N4 | 0.2025 (3) | 0.1341 (4) | 0.0450 (3) | 0.0294 (12) | |
C11 | 0.3649 (5) | 0.1002 (5) | 0.3271 (4) | 0.0344 (16) | |
C12 | 0.3950 (5) | 0.0854 (5) | 0.4100 (4) | 0.0413 (18) | |
H12 | 0.455 | 0.0909 | 0.4282 | 0.05* | |
C13 | 0.3372 (6) | 0.0632 (6) | 0.4638 (4) | 0.054 (2) | |
H13 | 0.3568 | 0.0527 | 0.5199 | 0.065* | |
C14 | 0.2498 (6) | 0.0558 (6) | 0.4365 (4) | 0.053 (2) | |
H14 | 0.2092 | 0.0417 | 0.474 | 0.064* | |
C15 | 0.2223 (5) | 0.0690 (5) | 0.3562 (4) | 0.0389 (17) | |
C16 | 0.1313 (5) | 0.0613 (7) | 0.3226 (5) | 0.058 (2) | |
H16A | 0.1244 | 0.0051 | 0.2827 | 0.087* | |
H16B | 0.1128 | 0.1263 | 0.2958 | 0.087* | |
H16C | 0.0958 | 0.0473 | 0.3668 | 0.087* | |
C21 | 0.3256 (5) | −0.0851 (5) | 0.1422 (4) | 0.0330 (16) | |
C22 | 0.3352 (5) | −0.1921 (5) | 0.1344 (4) | 0.0437 (18) | |
H22 | 0.2881 | −0.2369 | 0.1407 | 0.052* | |
C23 | 0.4122 (6) | −0.2311 (6) | 0.1177 (5) | 0.056 (2) | |
H23 | 0.4196 | −0.3035 | 0.1134 | 0.068* | |
C24 | 0.4806 (5) | −0.1646 (6) | 0.1067 (4) | 0.0463 (19) | |
H24 | 0.5341 | −0.1916 | 0.0935 | 0.056* | |
C25 | 0.4704 (5) | −0.0605 (5) | 0.1151 (4) | 0.0364 (16) | |
C26 | 0.5391 (5) | 0.0152 (5) | 0.1028 (4) | 0.0406 (17) | |
H26A | 0.5553 | 0.0528 | 0.1538 | 0.061* | |
H26B | 0.5176 | 0.0638 | 0.0598 | 0.061* | |
H26C | 0.5898 | −0.0211 | 0.0868 | 0.061* | |
C31 | 0.2723 (4) | 0.3339 (5) | 0.1905 (4) | 0.0294 (15) | |
C32 | 0.2544 (5) | 0.4371 (5) | 0.2059 (4) | 0.0388 (17) | |
H32 | 0.198 | 0.4577 | 0.2161 | 0.047* | |
C33 | 0.3198 (5) | 0.5085 (5) | 0.2061 (4) | 0.0426 (18) | |
H33 | 0.3091 | 0.5789 | 0.2169 | 0.051* | |
C34 | 0.4017 (5) | 0.4769 (5) | 0.1903 (4) | 0.0410 (18) | |
H34 | 0.447 | 0.5259 | 0.1901 | 0.049* | |
C35 | 0.4171 (5) | 0.3751 (5) | 0.1751 (4) | 0.0341 (17) | |
C36 | 0.5031 (5) | 0.3360 (6) | 0.1592 (5) | 0.0453 (19) | |
H36A | 0.5256 | 0.2895 | 0.2034 | 0.068* | |
H36B | 0.543 | 0.3941 | 0.1565 | 0.068* | |
H36C | 0.4977 | 0.2987 | 0.1072 | 0.068* | |
C41 | 0.2647 (4) | 0.1577 (5) | −0.0050 (4) | 0.0284 (15) | |
C42 | 0.2423 (5) | 0.1757 (5) | −0.0887 (4) | 0.0370 (17) | |
H42 | 0.2863 | 0.1912 | −0.1223 | 0.044* | |
C43 | 0.1584 (5) | 0.1713 (6) | −0.1225 (4) | 0.0418 (18) | |
H43 | 0.1437 | 0.1836 | −0.1791 | 0.05* | |
C44 | 0.0940 (5) | 0.1480 (6) | −0.0718 (4) | 0.0446 (19) | |
H44 | 0.0348 | 0.146 | −0.0936 | 0.054* | |
C45 | 0.1176 (5) | 0.1279 (5) | 0.0106 (4) | 0.0341 (16) | |
C46 | 0.0539 (4) | 0.1004 (6) | 0.0685 (4) | 0.0425 (18) | |
H46A | −0.0042 | 0.0967 | 0.0388 | 0.064* | |
H46B | 0.055 | 0.1531 | 0.1112 | 0.064* | |
H46C | 0.0692 | 0.0334 | 0.0935 | 0.064* | |
C51A | 0.8478 (7) | 0.2303 (9) | 0.2109 (7) | 0.060 (3) | 0.698 (8) |
C52A | 0.7789 (8) | 0.2904 (10) | 0.1821 (7) | 0.061 (3) | 0.698 (8) |
H52A | 0.7691 | 0.3547 | 0.207 | 0.073* | 0.698 (8) |
C53A | 0.7248 (9) | 0.2567 (10) | 0.1175 (8) | 0.072 (3) | 0.698 (8) |
H53A | 0.6769 | 0.2984 | 0.0974 | 0.086* | 0.698 (8) |
C54A | 0.7370 (9) | 0.1630 (10) | 0.0794 (8) | 0.071 (3) | 0.698 (8) |
H54A | 0.6988 | 0.14 | 0.034 | 0.085* | 0.698 (8) |
C55A | 0.8057 (8) | 0.1063 (10) | 0.1099 (8) | 0.068 (3) | 0.698 (8) |
H55A | 0.8168 | 0.0426 | 0.0845 | 0.081* | 0.698 (8) |
C56A | 0.8598 (10) | 0.1373 (10) | 0.1759 (8) | 0.066 (3) | 0.698 (8) |
H56A | 0.9059 | 0.0939 | 0.1977 | 0.08* | 0.698 (8) |
C57A | 0.9103 (11) | 0.2675 (15) | 0.2827 (10) | 0.104 (5) | 0.698 (8) |
H57A | 0.892 | 0.3355 | 0.3002 | 0.156* | 0.698 (8) |
H57B | 0.9686 | 0.2724 | 0.2661 | 0.156* | 0.698 (8) |
H57C | 0.9103 | 0.2186 | 0.328 | 0.156* | 0.698 (8) |
C51B | 0.7889 (14) | 0.2105 (17) | 0.1457 (13) | 0.065 (4) | 0.302 (8) |
C52B | 0.8404 (16) | 0.1248 (18) | 0.1477 (16) | 0.063 (5) | 0.302 (8) |
H52B | 0.8315 | 0.0752 | 0.1052 | 0.075* | 0.302 (8) |
C53B | 0.9051 (16) | 0.1101 (18) | 0.2107 (15) | 0.066 (5) | 0.302 (8) |
H53B | 0.9399 | 0.0498 | 0.2115 | 0.08* | 0.302 (8) |
C54B | 0.9199 (16) | 0.1805 (19) | 0.2717 (15) | 0.066 (5) | 0.302 (8) |
H54B | 0.9659 | 0.1718 | 0.3141 | 0.079* | 0.302 (8) |
C55B | 0.8659 (18) | 0.265 (2) | 0.2699 (17) | 0.067 (5) | 0.302 (8) |
H55B | 0.8736 | 0.3132 | 0.3132 | 0.08* | 0.302 (8) |
C56B | 0.802 (2) | 0.281 (2) | 0.2077 (16) | 0.061 (5) | 0.302 (8) |
H56B | 0.7662 | 0.3402 | 0.2075 | 0.074* | 0.302 (8) |
C57B | 0.717 (2) | 0.230 (3) | 0.0785 (18) | 0.080 (8) | 0.302 (8) |
H57D | 0.7145 | 0.1742 | 0.0385 | 0.12* | 0.302 (8) |
H57E | 0.7268 | 0.2958 | 0.0516 | 0.12* | 0.302 (8) |
H57F | 0.6614 | 0.2337 | 0.1018 | 0.12* | 0.302 (8) |
C61A | 0.0255 (10) | 0.5557 (11) | −0.0013 (9) | 0.076 (5)* | 0.5 |
C62A | 0.0654 (10) | 0.4944 (11) | 0.0577 (9) | 0.056 (5)* | 0.5 |
H62A | 0.1169 | 0.5157 | 0.0898 | 0.068* | 0.5 |
C63A | 0.0288 (11) | 0.4007 (12) | 0.0693 (10) | 0.082 (6)* | 0.5 |
H63A | 0.0557 | 0.3566 | 0.1106 | 0.099* | 0.5 |
C64A | −0.0443 (15) | 0.3683 (15) | 0.0244 (15) | 0.105 (9)* | 0.5 |
H64A | −0.0687 | 0.3028 | 0.0337 | 0.126* | 0.5 |
C65A | −0.0822 (11) | 0.4335 (13) | −0.0353 (11) | 0.092 (6)* | 0.5 |
H65A | −0.1337 | 0.4129 | −0.0678 | 0.11* | 0.5 |
C66A | −0.0462 (11) | 0.5277 (13) | −0.0482 (11) | 0.069 (6)* | 0.5 |
H66A | −0.0719 | 0.5723 | −0.0898 | 0.083* | 0.5 |
C67A | 0.0690 (16) | 0.6539 (19) | −0.0168 (14) | 0.092 (8)* | 0.5 |
H67A | 0.1201 | 0.6624 | 0.0231 | 0.138* | 0.5 |
H67B | 0.029 | 0.7113 | −0.0119 | 0.138* | 0.5 |
H67C | 0.0867 | 0.653 | −0.072 | 0.138* | 0.5 |
U11 | U22 | U33 | U12 | U13 | U23 | |
W1 | 0.03606 (17) | 0.02863 (16) | 0.02599 (16) | −0.00196 (12) | 0.00780 (12) | 0.00131 (11) |
W2 | 0.03441 (17) | 0.02764 (16) | 0.02676 (16) | −0.00080 (12) | 0.00573 (12) | 0.00136 (11) |
O1 | 0.039 (3) | 0.036 (3) | 0.024 (2) | 0.000 (2) | 0.000 (2) | 0.0027 (19) |
O2 | 0.041 (3) | 0.030 (3) | 0.039 (3) | −0.002 (2) | 0.008 (2) | 0.003 (2) |
O3 | 0.043 (3) | 0.024 (2) | 0.030 (2) | 0.000 (2) | 0.005 (2) | −0.0006 (19) |
O4 | 0.034 (3) | 0.030 (3) | 0.024 (2) | −0.001 (2) | 0.006 (2) | 0.0032 (18) |
N1 | 0.041 (4) | 0.030 (3) | 0.028 (3) | −0.003 (3) | 0.006 (3) | 0.002 (2) |
N2 | 0.046 (4) | 0.022 (3) | 0.025 (3) | 0.003 (3) | 0.002 (3) | 0.000 (2) |
N3 | 0.040 (4) | 0.023 (3) | 0.026 (3) | −0.002 (3) | 0.004 (2) | 0.005 (2) |
N4 | 0.030 (3) | 0.027 (3) | 0.031 (3) | −0.005 (2) | 0.004 (2) | 0.000 (2) |
C11 | 0.053 (5) | 0.021 (4) | 0.029 (4) | −0.002 (3) | 0.005 (3) | 0.001 (3) |
C12 | 0.053 (5) | 0.038 (4) | 0.030 (4) | −0.001 (4) | −0.004 (3) | 0.000 (3) |
C13 | 0.086 (7) | 0.050 (5) | 0.026 (4) | −0.002 (5) | 0.009 (4) | 0.003 (3) |
C14 | 0.063 (6) | 0.062 (5) | 0.038 (5) | −0.013 (4) | 0.018 (4) | 0.004 (4) |
C15 | 0.056 (5) | 0.031 (4) | 0.030 (4) | −0.005 (3) | 0.005 (3) | 0.002 (3) |
C16 | 0.079 (7) | 0.054 (5) | 0.045 (5) | −0.009 (5) | 0.023 (4) | 0.009 (4) |
C21 | 0.043 (5) | 0.027 (4) | 0.029 (4) | −0.005 (3) | 0.005 (3) | 0.004 (3) |
C22 | 0.051 (5) | 0.027 (4) | 0.052 (5) | 0.001 (4) | 0.002 (4) | 0.007 (3) |
C23 | 0.073 (6) | 0.030 (4) | 0.065 (5) | 0.009 (4) | 0.005 (5) | 0.007 (4) |
C24 | 0.052 (5) | 0.036 (5) | 0.052 (5) | 0.013 (4) | 0.016 (4) | 0.003 (3) |
C25 | 0.040 (4) | 0.040 (4) | 0.030 (4) | 0.004 (3) | 0.006 (3) | 0.005 (3) |
C26 | 0.043 (4) | 0.043 (4) | 0.036 (4) | 0.004 (3) | 0.004 (3) | 0.001 (3) |
C31 | 0.038 (4) | 0.028 (4) | 0.021 (3) | 0.003 (3) | −0.002 (3) | −0.002 (3) |
C32 | 0.046 (5) | 0.037 (4) | 0.032 (4) | 0.004 (4) | 0.000 (3) | 0.000 (3) |
C33 | 0.064 (6) | 0.028 (4) | 0.035 (4) | 0.003 (4) | 0.003 (4) | −0.002 (3) |
C34 | 0.064 (5) | 0.029 (4) | 0.029 (4) | −0.013 (4) | 0.001 (3) | 0.000 (3) |
C35 | 0.051 (5) | 0.029 (4) | 0.020 (3) | −0.004 (3) | −0.005 (3) | 0.004 (3) |
C36 | 0.040 (5) | 0.039 (4) | 0.057 (5) | −0.012 (3) | 0.003 (4) | 0.005 (4) |
C41 | 0.036 (4) | 0.020 (3) | 0.027 (3) | 0.000 (3) | −0.001 (3) | −0.002 (3) |
C42 | 0.049 (5) | 0.035 (4) | 0.030 (4) | −0.008 (3) | 0.015 (3) | 0.001 (3) |
C43 | 0.051 (5) | 0.046 (5) | 0.027 (4) | −0.003 (4) | 0.001 (3) | 0.001 (3) |
C44 | 0.049 (5) | 0.050 (5) | 0.032 (4) | 0.004 (4) | −0.007 (3) | 0.000 (3) |
C45 | 0.044 (4) | 0.029 (4) | 0.031 (4) | −0.004 (3) | 0.008 (3) | −0.001 (3) |
C46 | 0.034 (4) | 0.057 (5) | 0.036 (4) | −0.005 (4) | 0.003 (3) | 0.001 (3) |
C51A | 0.061 (6) | 0.066 (6) | 0.054 (6) | −0.010 (5) | 0.011 (5) | 0.005 (4) |
C52A | 0.074 (7) | 0.051 (6) | 0.062 (7) | 0.001 (5) | 0.020 (5) | −0.009 (5) |
C53A | 0.063 (7) | 0.082 (7) | 0.071 (8) | 0.010 (6) | 0.006 (5) | 0.006 (6) |
C54A | 0.087 (8) | 0.082 (8) | 0.044 (6) | −0.027 (6) | 0.007 (5) | −0.006 (5) |
C55A | 0.088 (8) | 0.057 (6) | 0.067 (7) | −0.012 (5) | 0.044 (5) | −0.012 (5) |
C56A | 0.073 (7) | 0.057 (6) | 0.071 (7) | 0.008 (5) | 0.020 (5) | 0.017 (5) |
C57A | 0.094 (11) | 0.124 (12) | 0.088 (10) | −0.033 (10) | −0.014 (7) | 0.000 (8) |
C51B | 0.074 (8) | 0.062 (7) | 0.062 (7) | −0.002 (6) | 0.017 (6) | 0.002 (6) |
C52B | 0.074 (10) | 0.054 (8) | 0.064 (11) | −0.006 (8) | 0.022 (8) | −0.002 (8) |
C53B | 0.068 (11) | 0.058 (10) | 0.076 (11) | −0.004 (8) | 0.022 (8) | 0.008 (8) |
C54B | 0.060 (10) | 0.065 (10) | 0.072 (10) | −0.007 (8) | 0.009 (8) | 0.008 (8) |
C55B | 0.068 (11) | 0.063 (10) | 0.071 (10) | −0.006 (9) | 0.012 (8) | 0.000 (8) |
C56B | 0.068 (10) | 0.054 (9) | 0.065 (9) | 0.002 (8) | 0.017 (8) | 0.000 (7) |
C57B | 0.093 (16) | 0.085 (18) | 0.062 (15) | 0.007 (13) | 0.008 (11) | −0.002 (14) |
W1—W2 | 2.1617 (5) | C42—C43 | 1.360 (10) |
W2—O1 | 2.056 (4) | C42—H42 | 0.95 |
W1—O2 | 2.054 (4) | C43—C44 | 1.409 (10) |
W1—O3 | 2.063 (4) | C43—H43 | 0.95 |
W2—O4 | 2.060 (4) | C44—C45 | 1.390 (9) |
W1—N1 | 2.147 (5) | C44—H44 | 0.95 |
W2—N2 | 2.142 (5) | C45—C46 | 1.495 (9) |
W2—N3 | 2.146 (5) | C46—H46A | 0.98 |
W1—N4 | 2.129 (5) | C46—H46B | 0.98 |
O1—C11 | 1.317 (8) | C46—H46C | 0.98 |
O2—C21 | 1.311 (8) | C51A—C56A | 1.359 (11) |
O3—C31 | 1.313 (8) | C51A—C52A | 1.368 (11) |
O4—C41 | 1.301 (7) | C51A—C57A | 1.522 (17) |
N1—C11 | 1.359 (9) | C52A—C53A | 1.354 (12) |
N1—C15 | 1.386 (9) | C52A—H52A | 0.95 |
N2—C21 | 1.368 (8) | C53A—C54A | 1.391 (12) |
N2—C25 | 1.386 (9) | C53A—H53A | 0.95 |
N3—C31 | 1.369 (8) | C54A—C55A | 1.348 (12) |
N3—C35 | 1.376 (8) | C54A—H54A | 0.95 |
N4—C41 | 1.374 (8) | C55A—C56A | 1.359 (12) |
N4—C45 | 1.380 (9) | C55A—H55A | 0.95 |
C11—C12 | 1.406 (9) | C56A—H56A | 0.95 |
C12—C13 | 1.364 (10) | C57A—H57A | 0.98 |
C12—H12 | 0.95 | C57A—H57B | 0.98 |
C13—C14 | 1.387 (11) | C57A—H57C | 0.98 |
C13—H13 | 0.95 | C51B—C56B | 1.366 (14) |
C14—C15 | 1.355 (9) | C51B—C52B | 1.369 (14) |
C14—H14 | 0.95 | C51B—C57B | 1.51 (2) |
C15—C16 | 1.465 (11) | C52B—C53B | 1.375 (14) |
C16—H16A | 0.98 | C52B—H52B | 0.95 |
C16—H16B | 0.98 | C53B—C54B | 1.359 (14) |
C16—H16C | 0.98 | C53B—H53B | 0.95 |
C21—C22 | 1.404 (10) | C54B—C55B | 1.377 (14) |
C22—C23 | 1.358 (11) | C54B—H54B | 0.95 |
C22—H22 | 0.95 | C55B—C56B | 1.363 (14) |
C23—C24 | 1.398 (11) | C55B—H55B | 0.95 |
C23—H23 | 0.95 | C56B—H56B | 0.95 |
C24—C25 | 1.368 (10) | C57B—H57D | 0.98 |
C24—H24 | 0.95 | C57B—H57E | 0.98 |
C25—C26 | 1.482 (10) | C57B—H57F | 0.98 |
C26—H26A | 0.98 | C61A—C66A | 1.335 (13) |
C26—H26B | 0.98 | C61A—C62A | 1.352 (13) |
C26—H26C | 0.98 | C61A—C67A | 1.48 (3) |
C31—C32 | 1.397 (9) | C62A—C63A | 1.365 (15) |
C32—C33 | 1.376 (10) | C62A—H62A | 0.95 |
C32—H32 | 0.95 | C63A—C64A | 1.353 (15) |
C33—C34 | 1.390 (10) | C63A—H63A | 0.95 |
C33—H33 | 0.95 | C64A—C65A | 1.379 (15) |
C34—C35 | 1.370 (9) | C64A—H64A | 0.95 |
C34—H34 | 0.95 | C65A—C66A | 1.371 (15) |
C35—C36 | 1.483 (10) | C65A—H65A | 0.95 |
C36—H36A | 0.98 | C66A—H66A | 0.95 |
C36—H36B | 0.98 | C67A—H67A | 0.98 |
C36—H36C | 0.98 | C67A—H67B | 0.98 |
C41—C42 | 1.405 (9) | C67A—H67C | 0.98 |
O2—W1—O3 | 171.82 (18) | C35—C36—H36C | 109.5 |
O1—W2—O4 | 172.31 (17) | H36A—C36—H36C | 109.5 |
N4—W1—N1 | 179.0 (2) | H36B—C36—H36C | 109.5 |
N2—W2—N3 | 178.80 (19) | O4—C41—N4 | 117.2 (5) |
O2—W1—N4 | 91.76 (18) | O4—C41—C42 | 121.9 (6) |
O3—W1—N4 | 89.20 (17) | N4—C41—C42 | 120.8 (6) |
O2—W1—N1 | 89.02 (18) | C43—C42—C41 | 121.0 (6) |
O3—W1—N1 | 90.10 (18) | C43—C42—H42 | 119.5 |
O2—W1—W2 | 93.83 (13) | C41—C42—H42 | 119.5 |
O3—W1—W2 | 94.31 (13) | C42—C43—C44 | 118.7 (6) |
N1—W1—W2 | 89.79 (15) | C42—C43—H43 | 120.6 |
N4—W1—W2 | 89.61 (14) | C44—C43—H43 | 120.6 |
O1—W2—N2 | 89.55 (17) | C45—C44—C43 | 119.4 (7) |
O4—W2—N2 | 90.54 (17) | C45—C44—H44 | 120.3 |
O1—W2—N3 | 89.47 (17) | C43—C44—H44 | 120.3 |
O4—W2—N3 | 90.52 (17) | N4—C45—C44 | 121.7 (6) |
O1—W2—W1 | 93.90 (13) | N4—C45—C46 | 115.1 (6) |
O4—W2—W1 | 93.79 (12) | C44—C45—C46 | 123.2 (7) |
N2—W2—W1 | 89.90 (15) | C45—C46—H46A | 109.5 |
N3—W2—W1 | 89.48 (15) | C45—C46—H46B | 109.5 |
C11—O1—W2 | 120.0 (4) | H46A—C46—H46B | 109.5 |
C21—O2—W1 | 120.1 (4) | C45—C46—H46C | 109.5 |
C31—O3—W1 | 119.7 (4) | H46A—C46—H46C | 109.5 |
C41—O4—W2 | 120.4 (4) | H46B—C46—H46C | 109.5 |
C11—N1—C15 | 118.4 (6) | C56A—C51A—C52A | 119.9 (11) |
C11—N1—W1 | 118.2 (4) | C56A—C51A—C57A | 120.4 (12) |
C15—N1—W1 | 123.4 (5) | C52A—C51A—C57A | 119.8 (11) |
C21—N2—C25 | 118.7 (6) | C53A—C52A—C51A | 118.9 (11) |
C21—N2—W2 | 117.9 (4) | C53A—C52A—H52A | 120.6 |
C25—N2—W2 | 123.4 (4) | C51A—C52A—H52A | 120.6 |
C31—N3—C35 | 118.3 (5) | C52A—C53A—C54A | 122.2 (12) |
C31—N3—W2 | 118.6 (4) | C52A—C53A—H53A | 118.9 |
C35—N3—W2 | 123.1 (5) | C54A—C53A—H53A | 118.9 |
C41—N4—C45 | 118.2 (5) | C55A—C54A—C53A | 116.9 (11) |
C41—N4—W1 | 119.0 (4) | C55A—C54A—H54A | 121.6 |
C45—N4—W1 | 122.8 (4) | C53A—C54A—H54A | 121.6 |
O1—C11—N1 | 118.1 (6) | C54A—C55A—C56A | 122.0 (12) |
O1—C11—C12 | 120.9 (7) | C54A—C55A—H55A | 119 |
N1—C11—C12 | 121.0 (6) | C56A—C55A—H55A | 119 |
C13—C12—C11 | 119.3 (7) | C51A—C56A—C55A | 120.1 (12) |
C13—C12—H12 | 120.4 | C51A—C56A—H56A | 120 |
C11—C12—H12 | 120.4 | C55A—C56A—H56A | 120 |
C12—C13—C14 | 119.9 (7) | C51A—C57A—H57A | 109.5 |
C12—C13—H13 | 120.1 | C51A—C57A—H57B | 109.5 |
C14—C13—H13 | 120.1 | H57A—C57A—H57B | 109.5 |
C15—C14—C13 | 119.9 (7) | C51A—C57A—H57C | 109.5 |
C15—C14—H14 | 120.1 | H57A—C57A—H57C | 109.5 |
C13—C14—H14 | 120.1 | H57B—C57A—H57C | 109.5 |
C14—C15—N1 | 121.6 (7) | C56B—C51B—C52B | 119.2 (17) |
C14—C15—C16 | 123.1 (7) | C56B—C51B—C57B | 118.1 (19) |
N1—C15—C16 | 115.3 (6) | C52B—C51B—C57B | 122.8 (19) |
C15—C16—H16A | 109.5 | C51B—C52B—C53B | 120.5 (19) |
C15—C16—H16B | 109.5 | C51B—C52B—H52B | 119.8 |
H16A—C16—H16B | 109.5 | C53B—C52B—H52B | 119.8 |
C15—C16—H16C | 109.5 | C54B—C53B—C52B | 121 (2) |
H16A—C16—H16C | 109.5 | C54B—C53B—H53B | 119.5 |
H16B—C16—H16C | 109.5 | C52B—C53B—H53B | 119.5 |
O2—C21—N2 | 118.1 (6) | C53B—C54B—C55B | 117.7 (18) |
O2—C21—C22 | 120.9 (6) | C53B—C54B—H54B | 121.1 |
N2—C21—C22 | 121.0 (6) | C55B—C54B—H54B | 121.1 |
C23—C22—C21 | 119.5 (7) | C56B—C55B—C54B | 122 (2) |
C23—C22—H22 | 120.2 | C56B—C55B—H55B | 119 |
C21—C22—H22 | 120.2 | C54B—C55B—H55B | 119 |
C22—C23—C24 | 119.9 (7) | C55B—C56B—C51B | 120 (2) |
C22—C23—H23 | 120.1 | C55B—C56B—H56B | 120.2 |
C24—C23—H23 | 120.1 | C51B—C56B—H56B | 120.2 |
C25—C24—C23 | 119.9 (7) | C51B—C57B—H57D | 109.5 |
C25—C24—H24 | 120.1 | C51B—C57B—H57E | 109.5 |
C23—C24—H24 | 120.1 | H57D—C57B—H57E | 109.5 |
C24—C25—N2 | 121.0 (7) | C51B—C57B—H57F | 109.5 |
C24—C25—C26 | 123.2 (7) | H57D—C57B—H57F | 109.5 |
N2—C25—C26 | 115.8 (6) | H57E—C57B—H57F | 109.5 |
C25—C26—H26A | 109.5 | C66A—C61A—C62A | 122.9 (12) |
C25—C26—H26B | 109.5 | C66A—C61A—C67A | 120.2 (11) |
H26A—C26—H26B | 109.5 | C62A—C61A—C67A | 116.7 (11) |
C25—C26—H26C | 109.5 | C61A—C62A—C63A | 117.4 (10) |
H26A—C26—H26C | 109.5 | C61A—C62A—H62A | 121.3 |
H26B—C26—H26C | 109.5 | C63A—C62A—H62A | 121.3 |
O3—C31—N3 | 118.0 (5) | C64A—C63A—C62A | 122.6 (10) |
O3—C31—C32 | 120.2 (6) | C64A—C63A—H63A | 118.7 |
N3—C31—C32 | 121.8 (6) | C62A—C63A—H63A | 118.7 |
C33—C32—C31 | 118.8 (7) | C63A—C64A—C65A | 117.7 (12) |
C33—C32—H32 | 120.6 | C63A—C64A—H64A | 121.1 |
C31—C32—H32 | 120.6 | C65A—C64A—H64A | 121.1 |
C32—C33—C34 | 119.7 (7) | C66A—C65A—C64A | 120.6 (10) |
C32—C33—H33 | 120.2 | C66A—C65A—H65A | 119.7 |
C34—C33—H33 | 120.2 | C64A—C65A—H65A | 119.7 |
C35—C34—C33 | 120.1 (7) | C61A—C66A—C65A | 118.8 (10) |
C35—C34—H34 | 120 | C61A—C66A—H66A | 120.6 |
C33—C34—H34 | 120 | C65A—C66A—H66A | 120.6 |
C34—C35—N3 | 121.3 (7) | C61A—C67A—H67A | 109.5 |
C34—C35—C36 | 122.8 (7) | C61A—C67A—H67B | 109.5 |
N3—C35—C36 | 115.8 (6) | H67A—C67A—H67B | 109.5 |
C35—C36—H36A | 109.5 | C61A—C67A—H67C | 109.5 |
C35—C36—H36B | 109.5 | H67A—C67A—H67C | 109.5 |
H36A—C36—H36B | 109.5 | H67B—C67A—H67C | 109.5 |
O2—W1—W2—O1 | −88.78 (16) | C25—N2—C21—O2 | −177.3 (5) |
O3—W1—W2—O1 | 90.32 (16) | W2—N2—C21—O2 | 5.3 (7) |
N4—W1—W2—O1 | 179.49 (18) | C25—N2—C21—C22 | 0.6 (9) |
N1—W1—W2—O1 | 0.23 (18) | W2—N2—C21—C22 | −176.8 (5) |
O2—W1—W2—O4 | 91.30 (16) | O2—C21—C22—C23 | 178.0 (6) |
O3—W1—W2—O4 | −89.60 (16) | N2—C21—C22—C23 | 0.2 (10) |
N4—W1—W2—O4 | −0.43 (17) | C21—C22—C23—C24 | −1.3 (11) |
N1—W1—W2—O4 | −179.69 (18) | C22—C23—C24—C25 | 1.8 (11) |
O2—W1—W2—N2 | 0.77 (17) | C23—C24—C25—N2 | −1.0 (10) |
O3—W1—W2—N2 | 179.87 (17) | C23—C24—C25—C26 | −178.7 (7) |
N4—W1—W2—N2 | −90.97 (19) | C21—N2—C25—C24 | −0.2 (9) |
N1—W1—W2—N2 | 89.78 (19) | W2—N2—C25—C24 | 177.1 (5) |
O2—W1—W2—N3 | −178.21 (17) | C21—N2—C25—C26 | 177.7 (5) |
O3—W1—W2—N3 | 0.89 (16) | W2—N2—C25—C26 | −5.1 (7) |
N4—W1—W2—N3 | 90.06 (19) | W1—O3—C31—N3 | 0.3 (7) |
N1—W1—W2—N3 | −89.20 (19) | W1—O3—C31—C32 | −178.7 (4) |
N2—W2—O1—C11 | −89.7 (4) | C35—N3—C31—O3 | −178.1 (5) |
N3—W2—O1—C11 | 89.6 (4) | W2—N3—C31—O3 | 0.6 (7) |
W1—W2—O1—C11 | 0.2 (4) | C35—N3—C31—C32 | 0.9 (8) |
N4—W1—O2—C21 | 91.4 (4) | W2—N3—C31—C32 | 179.6 (4) |
N1—W1—O2—C21 | −88.1 (5) | O3—C31—C32—C33 | 178.1 (6) |
W2—W1—O2—C21 | 1.7 (4) | N3—C31—C32—C33 | −0.9 (9) |
N4—W1—O3—C31 | −90.5 (4) | C31—C32—C33—C34 | 0.6 (10) |
N1—W1—O3—C31 | 88.8 (4) | C32—C33—C34—C35 | −0.3 (10) |
W2—W1—O3—C31 | −1.0 (4) | C33—C34—C35—N3 | 0.3 (10) |
N2—W2—O4—C41 | 90.7 (4) | C33—C34—C35—C36 | −179.0 (6) |
N3—W2—O4—C41 | −88.7 (4) | C31—N3—C35—C34 | −0.6 (9) |
W1—W2—O4—C41 | 0.8 (4) | W2—N3—C35—C34 | −179.3 (5) |
O2—W1—N1—C11 | 93.1 (5) | C31—N3—C35—C36 | 178.8 (5) |
O3—W1—N1—C11 | −95.0 (5) | W2—N3—C35—C36 | 0.1 (7) |
W2—W1—N1—C11 | −0.7 (5) | W2—O4—C41—N4 | −0.7 (7) |
O2—W1—N1—C15 | −87.5 (5) | W2—O4—C41—C42 | 178.0 (5) |
O3—W1—N1—C15 | 84.3 (5) | C45—N4—C41—O4 | 179.2 (5) |
W2—W1—N1—C15 | 178.6 (5) | W1—N4—C41—O4 | 0.2 (7) |
O1—W2—N2—C21 | 90.6 (4) | C45—N4—C41—C42 | 0.5 (9) |
O4—W2—N2—C21 | −97.1 (4) | W1—N4—C41—C42 | −178.5 (5) |
W1—W2—N2—C21 | −3.3 (4) | O4—C41—C42—C43 | −178.1 (6) |
O1—W2—N2—C25 | −86.7 (5) | N4—C41—C42—C43 | 0.6 (10) |
O4—W2—N2—C25 | 85.6 (5) | C41—C42—C43—C44 | −0.1 (11) |
W1—W2—N2—C25 | 179.4 (4) | C42—C43—C44—C45 | −1.5 (11) |
O1—W2—N3—C31 | −95.0 (4) | C41—N4—C45—C44 | −2.1 (9) |
O4—W2—N3—C31 | 92.7 (4) | W1—N4—C45—C44 | 176.9 (5) |
W1—W2—N3—C31 | −1.1 (4) | C41—N4—C45—C46 | 179.1 (6) |
O1—W2—N3—C35 | 83.7 (4) | W1—N4—C45—C46 | −1.9 (8) |
O4—W2—N3—C35 | −88.7 (4) | C43—C44—C45—N4 | 2.6 (10) |
W1—W2—N3—C35 | 177.6 (4) | C43—C44—C45—C46 | −178.7 (7) |
O2—W1—N4—C41 | −93.5 (4) | C56A—C51A—C52A—C53A | −1.6 (14) |
O3—W1—N4—C41 | 94.6 (4) | C57A—C51A—C52A—C53A | 179.1 (12) |
W2—W1—N4—C41 | 0.3 (4) | C51A—C52A—C53A—C54A | 0.0 (15) |
O2—W1—N4—C45 | 87.5 (5) | C52A—C53A—C54A—C55A | 0.1 (19) |
O3—W1—N4—C45 | −84.4 (5) | C53A—C54A—C55A—C56A | 1 (2) |
W2—W1—N4—C45 | −178.7 (5) | C52A—C51A—C56A—C55A | 3.2 (19) |
W2—O1—C11—N1 | −0.7 (7) | C57A—C51A—C56A—C55A | −177.5 (13) |
W2—O1—C11—C12 | 178.9 (5) | C54A—C55A—C56A—C51A | −3 (2) |
C15—N1—C11—O1 | −178.4 (5) | C56B—C51B—C52B—C53B | −1 (2) |
W1—N1—C11—O1 | 0.9 (8) | C57B—C51B—C52B—C53B | −180 (2) |
C15—N1—C11—C12 | 2.0 (9) | C51B—C52B—C53B—C54B | −1 (2) |
W1—N1—C11—C12 | −178.6 (5) | C52B—C53B—C54B—C55B | 2 (3) |
O1—C11—C12—C13 | 179.1 (6) | C53B—C54B—C55B—C56B | −3 (5) |
N1—C11—C12—C13 | −1.3 (10) | C54B—C55B—C56B—C51B | 1 (5) |
C11—C12—C13—C14 | −0.3 (11) | C52B—C51B—C56B—C55B | 1 (4) |
C12—C13—C14—C15 | 1.2 (12) | C57B—C51B—C56B—C55B | 179 (3) |
C13—C14—C15—N1 | −0.5 (11) | C66A—C61A—C62A—C63A | −1 (2) |
C13—C14—C15—C16 | 179.3 (7) | C67A—C61A—C62A—C63A | −176.1 (16) |
C11—N1—C15—C14 | −1.1 (10) | C61A—C62A—C63A—C64A | 0 (2) |
W1—N1—C15—C14 | 179.6 (5) | C62A—C63A—C64A—C65A | 0 (3) |
C11—N1—C15—C16 | 179.1 (6) | C63A—C64A—C65A—C66A | 0 (4) |
W1—N1—C15—C16 | −0.2 (8) | C62A—C61A—C66A—C65A | 1 (3) |
W1—O2—C21—N2 | −4.5 (7) | C67A—C61A—C66A—C65A | 176 (2) |
W1—O2—C21—C22 | 177.5 (5) | C64A—C65A—C66A—C61A | −1 (3) |
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