Supporting information
Crystallographic Information File (CIF) https://doi.org/10.1107/S0108270110037017/mx3029sup1.cif | |
Structure factor file (CIF format) https://doi.org/10.1107/S0108270110037017/mx3029I_150Ksup2.hkl | |
Structure factor file (CIF format) https://doi.org/10.1107/S0108270110037017/mx3029I_200Ksup3.hkl |
CCDC references: 798587; 798588
For background on group 6 metal halide clusters see Kepert & Vrieze (1967) and Prokopuk & Shriver (1999). For background on the photochemical and electrochemical properties of tungsten(II) halide clusters see Maverick et al. (1983), Nocera & Gray (1984), Zietlow et al. (1985), Zietlow, Nocera et al. 1986), Mussell & Nocera (1990), Jackson et al. (1990), Arratia-Pérez & Hernández-Acevedo (1997), and Gray (2009); For previous structures see Zietlow, Schaefer et al. (1986) and Venkataraman et al. (1999). For synthesis Hogue & McCarley (1970), Dorman & McCarley (1974), Kolesnichenko & Messerle (1998), and Ströbele et al. (2009).
The tungsten(II) chloride cluster was prepared via the reduction of tungsten(VI) chloride with bismuth using published procedures (Kolesnichenko & Messerle, 1998). The hydronium salt was converted to the tetrabutylammonium salt by methathesis with tetrabutylammonium chloride in ethanol solution. The crude product was recrystallized by slow evaporation of an acetone solution.
The asymmetric unit consists of two tetrabutylammonium cations and two half octahedrons of the [W6Cl14]2- cluster anion, with each octahedron containing a crystallographic inversion center.
Not surprisingly, the two low-temperature structures determined at 200 and 150 K are perfectly identical. In both cases one of the hydrocarbon chains was found to be disordered and was modeled with two sites for each of the last three carbon atoms of the n-butyl chain. The ratio of occupancy of the two disorder components was refined freely and converged at 0.555 (11) for the 200 K structure and 0.616 (10) for the 150 K structure; the sum of the site-occupancy factors for each disorder was constrained to unity. The major component of the disordered chain contains atoms C14, C15 and C16, while the minor component consists of C14A, C15A and C16A.
Similarity restraints on 1-2 and 1-3 distances (standard uncertainties 0.02 and 0.04 Å, respectively) were used to geometrically relate the two components of the disordered n-butyl chain to one another and also to the remaining three butyl chains of the first tetrabutylammonium ion. In addition, similarity restraints on displacement parameters (standard uncertainty 0.04 Å2, 0.08 Å2 for terminal atoms) as well as rigid bond restraints for anisotropic displacement parameters (standard uncertainy 0.01 Å2) were applied to all disordered atoms as well as to C13.
The top four peaks in the final difference electron-density map range from 1.09 to 1.20 e Å-3 (150 K data) and from 1.62 to 2.35 e Å-3 (200 K data). All of these peaks are located within 1.5 Å of a tungsten atom and are presumably Fourier truncation artifacts due to the presence of multiple heavy atoms.
For both compounds, data collection: COLLECT (Nonius, 2000). Cell refinement: SCALEPACK (Otwinowski & Minor, 1997) for I_150K; HKL SCALEPACK (Otwinowski & Minor, 1997) for I_200K. Data reduction: DENZO and SCALEPACK (Otwinowski & Minor, 1997) for I_150K; HKL DENZO and SCALEPACK (Otwinowski & Minor, 1997) for I_200K. For both compounds, program(s) used to solve structure: SHELXS97 (Sheldrick, 2008); program(s) used to refine structure: SHELXL97 (Sheldrick, 2008); molecular graphics: ORTEP-3 for Windows (Farrugia, 1997), Mercury (Macrae et al., 2008), POV-RAY (Cason, 2004); software used to prepare material for publication: WinGX publication routines (Farrugia, 1999).
(C16H36N)2[W6Cl14] | F(000) = 3840 |
Mr = 2084.32 | Dx = 2.57 Mg m−3 |
Monoclinic, P21/c | Mo Kα radiation, λ = 0.71073 Å |
Hall symbol: -P 2ybc | Cell parameters from 12939 reflections |
a = 22.3152 (2) Å | θ = 2.0–27.5° |
b = 11.7220 (1) Å | µ = 13.48 mm−1 |
c = 22.2786 (1) Å | T = 150 K |
β = 112.415 (1)° | Chunk, yellow |
V = 5387.31 (7) Å3 | 0.31 × 0.27 × 0.23 mm |
Z = 4 |
Nonius KappaCCD diffractometer | 12352 independent reflections |
Radiation source: Enraf–Nonius FR590 | 9499 reflections with I > 2σ(I) |
Graphite monochromator | Rint = 0.086 |
Detector resolution: 9 pixels mm-1 | θmax = 27.5°, θmin = 2.5° |
ϕ and ω scans | h = −28→28 |
Absorption correction: multi-scan (SADABS; Bruker, 2008) | k = −15→15 |
Tmin = 0.484, Tmax = 0.746 | l = −28→28 |
137050 measured reflections |
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)] = 0.031 | Hydrogen site location: inferred from neighbouring sites |
wR(F2) = 0.054 | H-atom parameters constrained |
S = 1.07 | w = 1/[σ2(Fo2) + (0.0257P)2 + 0.5516P] where P = (Fo2 + 2Fc2)/3 |
12352 reflections | (Δ/σ)max = 0.001 |
515 parameters | Δρmax = 1.20 e Å−3 |
148 restraints | Δρmin = −1.69 e Å−3 |
(C16H36N)2[W6Cl14] | V = 5387.31 (7) Å3 |
Mr = 2084.32 | Z = 4 |
Monoclinic, P21/c | Mo Kα radiation |
a = 22.3152 (2) Å | µ = 13.48 mm−1 |
b = 11.7220 (1) Å | T = 150 K |
c = 22.2786 (1) Å | 0.31 × 0.27 × 0.23 mm |
β = 112.415 (1)° |
Nonius KappaCCD diffractometer | 12352 independent reflections |
Absorption correction: multi-scan (SADABS; Bruker, 2008) | 9499 reflections with I > 2σ(I) |
Tmin = 0.484, Tmax = 0.746 | Rint = 0.086 |
137050 measured reflections |
R[F2 > 2σ(F2)] = 0.031 | 148 restraints |
wR(F2) = 0.054 | H-atom parameters constrained |
S = 1.07 | Δρmax = 1.20 e Å−3 |
12352 reflections | Δρmin = −1.69 e Å−3 |
515 parameters |
Experimental. Examination of the diffraction pattern on a Nonius Kappa CCD diffractometer indicated a monoclinic crystal system. All work was done at 150 K using an Oxford Cryosystems Cryostream Cooler. The data collection strategy was set up to measure a hemisphere of reciprocal space with a redundancy factor of 3.4, which means that 90% of the reflections were measured at least 3.4 times. Phi and omega scans with a frame width of 1.0 degree were used. Data integration was done with Denzo (Otwinowski & Minor, 1997), and an absorption correction, with scaling and merging of the data was done with SADABS (Bruker, 2008). The structure was solved by the direct methods procedure in SHELXS-97(Sheldrick, 2008). Full-matrix least-squares refinements based on F2 were performed in SHELXL-97(Sheldrick, 2008), as incorporated in the WinGX package(Farrugia, 1999). |
Geometry. All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. |
Refinement. For the methyl groups, the hydrogen atoms were added at calculated positions using a riding model with C—H=0.98 Å and U(H)=1.5*Ueq(bonded carbon atom). The remaining hydrogen atoms were included in the model at calculated positions using a riding model with a C—H distance of 0.99 Å and U(H)=1.2*Ueq(bonded carbon atom). 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) | |
W1 | 0.062410 (10) | 0.422481 (19) | 0.066914 (10) | 0.01082 (5) | |
W2 | −0.000429 (10) | 0.613152 (19) | 0.057738 (10) | 0.01117 (5) | |
W3 | −0.064400 (10) | 0.423422 (19) | 0.016818 (10) | 0.01086 (5) | |
Cl1 | 0.14602 (6) | 0.32756 (12) | 0.15623 (6) | 0.0206 (3) | |
Cl2 | 0.00190 (6) | 0.75560 (12) | 0.13779 (6) | 0.0218 (3) | |
Cl3 | −0.15157 (6) | 0.32924 (12) | 0.03771 (6) | 0.0193 (3) | |
Cl4 | −0.00262 (6) | 0.45944 (12) | 0.13495 (6) | 0.0161 (3) | |
Cl5 | 0.12036 (6) | 0.60846 (11) | 0.10193 (6) | 0.0142 (3) | |
Cl6 | −0.00059 (6) | 0.24393 (11) | 0.02466 (6) | 0.0156 (3) | |
Cl7 | 0.12143 (6) | 0.38916 (11) | −0.00662 (6) | 0.0144 (3) | |
W4 | 0.488900 (10) | 0.865237 (19) | 0.037565 (10) | 0.01246 (6) | |
W5 | 0.555949 (10) | 1.05123 (2) | 0.080045 (10) | 0.01317 (6) | |
W6 | 0.430835 (10) | 1.063373 (19) | 0.014454 (10) | 0.01212 (5) | |
Cl8 | 0.47659 (7) | 0.68889 (13) | 0.08856 (7) | 0.0268 (4) | |
Cl9 | 0.63157 (7) | 1.11536 (15) | 0.18472 (7) | 0.0321 (4) | |
Cl10 | 0.33893 (6) | 1.14388 (13) | 0.03308 (7) | 0.0225 (3) | |
Cl11 | 0.50183 (6) | 0.76171 (12) | −0.05457 (6) | 0.0194 (3) | |
Cl12 | 0.60857 (6) | 0.85873 (12) | 0.09836 (6) | 0.0190 (3) | |
Cl13 | 0.36975 (6) | 0.88193 (12) | −0.02733 (6) | 0.0164 (3) | |
Cl14 | 0.47631 (6) | 0.98205 (12) | 0.12580 (6) | 0.0180 (3) | |
N1 | 0.34302 (19) | 0.4721 (4) | 0.13039 (19) | 0.0169 (11) | |
C1 | 0.3137 (3) | 0.4096 (5) | 0.1725 (3) | 0.0198 (13) | |
H1A | 0.2694 | 0.4393 | 0.1622 | 0.024* | |
H1B | 0.3396 | 0.4283 | 0.2185 | 0.024* | |
C2 | 0.3099 (3) | 0.2799 (5) | 0.1654 (3) | 0.0241 (14) | |
H2A | 0.2705 | 0.2585 | 0.1276 | 0.029* | |
H2B | 0.3481 | 0.2513 | 0.1578 | 0.029* | |
C3 | 0.3078 (3) | 0.2261 (5) | 0.2267 (3) | 0.0290 (15) | |
H3A | 0.3511 | 0.2332 | 0.2620 | 0.035* | |
H3B | 0.2765 | 0.2686 | 0.2399 | 0.035* | |
C4 | 0.2887 (3) | 0.1019 (6) | 0.2182 (3) | 0.049 (2) | |
H4A | 0.2879 | 0.0720 | 0.2589 | 0.073* | |
H4B | 0.3201 | 0.0588 | 0.2062 | 0.073* | |
H4C | 0.2455 | 0.0943 | 0.1838 | 0.073* | |
C5 | 0.2989 (2) | 0.4548 (5) | 0.0596 (2) | 0.0181 (13) | |
H5A | 0.2546 | 0.4783 | 0.0542 | 0.022* | |
H5B | 0.2975 | 0.3722 | 0.0500 | 0.022* | |
C6 | 0.3172 (2) | 0.5182 (5) | 0.0087 (2) | 0.0209 (14) | |
H6A | 0.2766 | 0.5398 | −0.0277 | 0.025* | |
H6B | 0.3396 | 0.5897 | 0.0286 | 0.025* | |
C7 | 0.3600 (3) | 0.4538 (5) | −0.0193 (3) | 0.0275 (15) | |
H7A | 0.4040 | 0.4453 | 0.0147 | 0.033* | |
H7B | 0.3420 | 0.3765 | −0.0327 | 0.033* | |
C8 | 0.3645 (3) | 0.5158 (6) | −0.0772 (3) | 0.0394 (18) | |
H8A | 0.3912 | 0.4713 | −0.0948 | 0.059* | |
H8B | 0.3842 | 0.5909 | −0.0636 | 0.059* | |
H8C | 0.3209 | 0.5251 | −0.1107 | 0.059* | |
C9 | 0.3491 (2) | 0.5973 (4) | 0.1492 (3) | 0.0175 (13) | |
H9A | 0.3713 | 0.6373 | 0.1244 | 0.021* | |
H9B | 0.3772 | 0.6035 | 0.1958 | 0.021* | |
C10 | 0.2856 (2) | 0.6591 (5) | 0.1380 (3) | 0.0210 (14) | |
H10A | 0.2654 | 0.6262 | 0.1666 | 0.025* | |
H10B | 0.2554 | 0.6480 | 0.0924 | 0.025* | |
C11 | 0.2972 (3) | 0.7865 (5) | 0.1519 (3) | 0.0255 (15) | |
H11A | 0.2571 | 0.8216 | 0.1525 | 0.031* | |
H11B | 0.3317 | 0.7968 | 0.1955 | 0.031* | |
C12 | 0.3168 (3) | 0.8483 (5) | 0.1019 (3) | 0.0366 (17) | |
H12A | 0.3235 | 0.9294 | 0.1131 | 0.055* | |
H12B | 0.2825 | 0.8398 | 0.0588 | 0.055* | |
H12C | 0.3571 | 0.8153 | 0.1018 | 0.055* | |
C13 | 0.4102 (2) | 0.4276 (5) | 0.1412 (2) | 0.0219 (14) | |
H13A | 0.4322 | 0.4841 | 0.1237 | 0.033* | 0.616 (10) |
H13B | 0.4055 | 0.3564 | 0.1159 | 0.033* | 0.616 (10) |
H13C | 0.4252 | 0.4637 | 0.1092 | 0.033* | 0.384 (10) |
H13D | 0.4075 | 0.3443 | 0.1331 | 0.033* | 0.384 (10) |
C14 | 0.4543 (5) | 0.4028 (10) | 0.2127 (5) | 0.019 (3) | 0.616 (10) |
H14A | 0.4618 | 0.4744 | 0.2381 | 0.023* | 0.616 (10) |
H14B | 0.4322 | 0.3483 | 0.2314 | 0.023* | 0.616 (10) |
C15 | 0.5188 (6) | 0.3534 (12) | 0.2181 (12) | 0.024 (4) | 0.616 (10) |
H15A | 0.5107 | 0.2829 | 0.1917 | 0.029* | 0.616 (10) |
H15B | 0.5435 | 0.3318 | 0.2639 | 0.029* | 0.616 (10) |
C16 | 0.5600 (4) | 0.4332 (9) | 0.1963 (5) | 0.038 (3) | 0.616 (10) |
H16A | 0.5999 | 0.3941 | 0.1995 | 0.058* | 0.616 (10) |
H16B | 0.5710 | 0.5010 | 0.2242 | 0.058* | 0.616 (10) |
H16C | 0.5358 | 0.4563 | 0.1512 | 0.058* | 0.616 (10) |
C14A | 0.4607 (8) | 0.4504 (16) | 0.2102 (7) | 0.027 (5) | 0.384 (10) |
H14C | 0.4731 | 0.5320 | 0.2148 | 0.032* | 0.384 (10) |
H14D | 0.4420 | 0.4320 | 0.2428 | 0.032* | 0.384 (10) |
C15A | 0.5203 (9) | 0.3766 (19) | 0.2217 (18) | 0.031 (7) | 0.384 (10) |
H15C | 0.5355 | 0.3887 | 0.1858 | 0.038* | 0.384 (10) |
H15D | 0.5555 | 0.4006 | 0.2626 | 0.038* | 0.384 (10) |
C16A | 0.5066 (8) | 0.2503 (14) | 0.2259 (8) | 0.047 (6) | 0.384 (10) |
H16D | 0.5461 | 0.2063 | 0.2330 | 0.070* | 0.384 (10) |
H16E | 0.4723 | 0.2258 | 0.1853 | 0.070* | 0.384 (10) |
H16F | 0.4927 | 0.2376 | 0.2621 | 0.070* | 0.384 (10) |
N2 | 0.14102 (19) | 0.5121 (4) | 0.3565 (2) | 0.0143 (10) | |
C17 | 0.1520 (2) | 0.3964 (4) | 0.3315 (2) | 0.0156 (12) | |
H17A | 0.1251 | 0.3395 | 0.3425 | 0.019* | |
H17B | 0.1360 | 0.4004 | 0.2835 | 0.019* | |
C18 | 0.2212 (2) | 0.3532 (5) | 0.3566 (3) | 0.0228 (14) | |
H18A | 0.2411 | 0.3628 | 0.4043 | 0.027* | |
H18B | 0.2467 | 0.3983 | 0.3372 | 0.027* | |
C19 | 0.2224 (3) | 0.2268 (5) | 0.3393 (3) | 0.0207 (14) | |
H19A | 0.2679 | 0.2035 | 0.3497 | 0.025* | |
H19B | 0.1987 | 0.2175 | 0.2919 | 0.025* | |
C20 | 0.1923 (3) | 0.1469 (5) | 0.3748 (3) | 0.0284 (15) | |
H20A | 0.1941 | 0.0681 | 0.3609 | 0.043* | |
H20B | 0.1471 | 0.1686 | 0.3644 | 0.043* | |
H20C | 0.2166 | 0.1530 | 0.4217 | 0.043* | |
C21 | 0.1638 (2) | 0.5128 (5) | 0.4303 (2) | 0.0174 (13) | |
H21A | 0.2116 | 0.5050 | 0.4489 | 0.021* | |
H21B | 0.1532 | 0.5881 | 0.4438 | 0.021* | |
C22 | 0.1356 (3) | 0.4211 (5) | 0.4601 (2) | 0.0258 (15) | |
H22A | 0.1481 | 0.3449 | 0.4496 | 0.031* | |
H22B | 0.0877 | 0.4262 | 0.4414 | 0.031* | |
C23 | 0.1605 (3) | 0.4359 (5) | 0.5340 (3) | 0.0247 (14) | |
H23A | 0.1497 | 0.3665 | 0.5531 | 0.030* | |
H23B | 0.2084 | 0.4425 | 0.5512 | 0.030* | |
C24 | 0.1331 (3) | 0.5390 (5) | 0.5559 (3) | 0.0372 (17) | |
H24A | 0.1511 | 0.5426 | 0.6035 | 0.056* | |
H24B | 0.0858 | 0.5324 | 0.5402 | 0.056* | |
H24C | 0.1447 | 0.6085 | 0.5384 | 0.056* | |
C25 | 0.0685 (2) | 0.5332 (5) | 0.3238 (2) | 0.0164 (13) | |
H25A | 0.0561 | 0.5253 | 0.2764 | 0.020* | |
H25B | 0.0459 | 0.4719 | 0.3375 | 0.020* | |
C26 | 0.0430 (2) | 0.6466 (5) | 0.3364 (3) | 0.0208 (14) | |
H26A | 0.0662 | 0.7096 | 0.3249 | 0.025* | |
H26B | 0.0506 | 0.6534 | 0.3830 | 0.025* | |
C27 | −0.0290 (3) | 0.6550 (5) | 0.2960 (3) | 0.0238 (14) | |
H27A | −0.0361 | 0.6420 | 0.2498 | 0.029* | |
H27B | −0.0438 | 0.7333 | 0.2997 | 0.029* | |
C28 | −0.0699 (3) | 0.5705 (5) | 0.3157 (3) | 0.0391 (18) | |
H28A | −0.1156 | 0.5800 | 0.2874 | 0.059* | |
H28B | −0.0644 | 0.5845 | 0.3608 | 0.059* | |
H28C | −0.0561 | 0.4926 | 0.3115 | 0.059* | |
C29 | 0.1801 (3) | 0.6055 (5) | 0.3410 (2) | 0.0183 (13) | |
H29A | 0.1742 | 0.6770 | 0.3617 | 0.022* | |
H29B | 0.2266 | 0.5848 | 0.3610 | 0.022* | |
C30 | 0.1635 (3) | 0.6293 (5) | 0.2693 (2) | 0.0213 (14) | |
H30A | 0.1164 | 0.6431 | 0.2474 | 0.026* | |
H30B | 0.1748 | 0.5621 | 0.2488 | 0.026* | |
C31 | 0.2008 (3) | 0.7333 (5) | 0.2615 (3) | 0.0282 (15) | |
H31A | 0.2477 | 0.7191 | 0.2852 | 0.034* | |
H31B | 0.1931 | 0.7421 | 0.2150 | 0.034* | |
C32 | 0.1835 (3) | 0.8431 (5) | 0.2856 (3) | 0.049 (2) | |
H32A | 0.2097 | 0.9052 | 0.2788 | 0.074* | |
H32B | 0.1921 | 0.8363 | 0.3320 | 0.074* | |
H32C | 0.1375 | 0.8595 | 0.2616 | 0.074* |
U11 | U22 | U33 | U12 | U13 | U23 | |
W1 | 0.00963 (11) | 0.01247 (12) | 0.00929 (11) | 0.00084 (9) | 0.00242 (9) | 0.00115 (9) |
W2 | 0.01083 (11) | 0.01222 (12) | 0.01014 (11) | 0.00045 (9) | 0.00363 (9) | −0.00092 (9) |
W3 | 0.00956 (11) | 0.01235 (12) | 0.01035 (11) | −0.00023 (9) | 0.00344 (9) | 0.00087 (9) |
Cl1 | 0.0169 (7) | 0.0255 (9) | 0.0162 (7) | 0.0042 (6) | 0.0027 (6) | 0.0075 (6) |
Cl2 | 0.0238 (8) | 0.0215 (8) | 0.0176 (7) | 0.0042 (6) | 0.0050 (6) | −0.0077 (6) |
Cl3 | 0.0151 (7) | 0.0208 (8) | 0.0228 (8) | −0.0018 (6) | 0.0080 (6) | 0.0059 (6) |
Cl4 | 0.0172 (7) | 0.0213 (8) | 0.0106 (7) | 0.0010 (6) | 0.0062 (6) | 0.0020 (6) |
Cl5 | 0.0107 (6) | 0.0165 (8) | 0.0124 (7) | −0.0024 (6) | 0.0012 (5) | −0.0030 (6) |
Cl6 | 0.0155 (7) | 0.0121 (7) | 0.0172 (7) | 0.0003 (6) | 0.0040 (6) | 0.0021 (6) |
Cl7 | 0.0108 (7) | 0.0161 (7) | 0.0167 (7) | 0.0025 (6) | 0.0055 (5) | −0.0008 (6) |
W4 | 0.01252 (12) | 0.01421 (13) | 0.01126 (12) | −0.00061 (10) | 0.00522 (9) | 0.00229 (9) |
W5 | 0.01240 (12) | 0.01827 (13) | 0.00806 (11) | −0.00306 (10) | 0.00304 (9) | −0.00097 (9) |
W6 | 0.01145 (11) | 0.01473 (13) | 0.01100 (11) | −0.00027 (10) | 0.00522 (9) | 0.00060 (10) |
Cl8 | 0.0273 (8) | 0.0205 (8) | 0.0369 (9) | 0.0013 (7) | 0.0171 (7) | 0.0135 (7) |
Cl9 | 0.0308 (9) | 0.0485 (11) | 0.0118 (7) | −0.0179 (8) | 0.0022 (6) | −0.0066 (7) |
Cl10 | 0.0202 (8) | 0.0250 (9) | 0.0266 (8) | 0.0043 (7) | 0.0136 (6) | 0.0010 (7) |
Cl11 | 0.0214 (8) | 0.0151 (8) | 0.0244 (8) | −0.0034 (6) | 0.0120 (6) | −0.0057 (6) |
Cl12 | 0.0132 (7) | 0.0227 (8) | 0.0190 (7) | 0.0035 (6) | 0.0037 (6) | 0.0089 (6) |
Cl13 | 0.0108 (7) | 0.0215 (8) | 0.0163 (7) | −0.0039 (6) | 0.0043 (6) | −0.0005 (6) |
Cl14 | 0.0199 (7) | 0.0263 (8) | 0.0088 (7) | −0.0026 (6) | 0.0068 (6) | 0.0011 (6) |
N1 | 0.014 (2) | 0.020 (3) | 0.019 (3) | −0.004 (2) | 0.008 (2) | −0.004 (2) |
C1 | 0.023 (3) | 0.024 (4) | 0.016 (3) | −0.004 (3) | 0.012 (3) | 0.000 (3) |
C2 | 0.037 (4) | 0.021 (4) | 0.021 (3) | −0.001 (3) | 0.019 (3) | −0.004 (3) |
C3 | 0.034 (4) | 0.034 (4) | 0.025 (4) | 0.000 (3) | 0.018 (3) | 0.003 (3) |
C4 | 0.075 (6) | 0.035 (5) | 0.043 (5) | −0.007 (4) | 0.030 (4) | 0.004 (4) |
C5 | 0.013 (3) | 0.024 (4) | 0.013 (3) | −0.001 (3) | −0.001 (2) | −0.007 (3) |
C6 | 0.022 (3) | 0.027 (4) | 0.010 (3) | −0.004 (3) | 0.001 (2) | 0.001 (3) |
C7 | 0.031 (4) | 0.034 (4) | 0.020 (3) | 0.000 (3) | 0.013 (3) | 0.001 (3) |
C8 | 0.043 (4) | 0.054 (5) | 0.026 (4) | −0.006 (4) | 0.019 (3) | 0.004 (4) |
C9 | 0.009 (3) | 0.026 (4) | 0.015 (3) | −0.003 (3) | 0.001 (2) | 0.000 (3) |
C10 | 0.013 (3) | 0.026 (4) | 0.024 (3) | −0.001 (3) | 0.007 (3) | −0.002 (3) |
C11 | 0.026 (3) | 0.029 (4) | 0.025 (3) | −0.001 (3) | 0.012 (3) | −0.003 (3) |
C12 | 0.037 (4) | 0.029 (4) | 0.054 (5) | 0.006 (3) | 0.029 (4) | 0.006 (4) |
C13 | 0.015 (3) | 0.034 (4) | 0.018 (3) | 0.006 (3) | 0.008 (2) | −0.002 (3) |
C14 | 0.018 (5) | 0.023 (7) | 0.015 (5) | −0.004 (5) | 0.006 (4) | −0.004 (5) |
C15 | 0.024 (6) | 0.022 (8) | 0.024 (8) | 0.009 (5) | 0.008 (5) | −0.005 (6) |
C16 | 0.019 (5) | 0.051 (8) | 0.040 (7) | −0.001 (5) | 0.004 (5) | 0.006 (6) |
C14A | 0.018 (8) | 0.036 (11) | 0.021 (8) | −0.002 (8) | 0.003 (6) | 0.000 (9) |
C15A | 0.031 (10) | 0.049 (12) | 0.009 (11) | 0.011 (9) | 0.001 (8) | −0.004 (11) |
C16A | 0.050 (12) | 0.046 (11) | 0.041 (11) | 0.023 (10) | 0.013 (9) | 0.002 (10) |
N2 | 0.018 (2) | 0.013 (3) | 0.012 (2) | 0.001 (2) | 0.005 (2) | 0.000 (2) |
C17 | 0.016 (3) | 0.016 (3) | 0.013 (3) | 0.004 (2) | 0.003 (2) | −0.002 (2) |
C18 | 0.016 (3) | 0.022 (4) | 0.029 (4) | 0.001 (3) | 0.009 (3) | 0.002 (3) |
C19 | 0.021 (3) | 0.020 (4) | 0.019 (3) | 0.005 (3) | 0.006 (3) | 0.002 (3) |
C20 | 0.039 (4) | 0.019 (4) | 0.029 (4) | 0.012 (3) | 0.015 (3) | 0.009 (3) |
C21 | 0.022 (3) | 0.020 (3) | 0.006 (3) | −0.004 (3) | 0.001 (2) | −0.004 (2) |
C22 | 0.042 (4) | 0.024 (4) | 0.012 (3) | −0.009 (3) | 0.012 (3) | 0.001 (3) |
C23 | 0.023 (3) | 0.025 (4) | 0.026 (3) | 0.001 (3) | 0.009 (3) | 0.011 (3) |
C24 | 0.049 (4) | 0.039 (5) | 0.029 (4) | 0.005 (4) | 0.022 (3) | 0.004 (3) |
C25 | 0.013 (3) | 0.019 (3) | 0.016 (3) | 0.003 (2) | 0.005 (2) | 0.003 (3) |
C26 | 0.021 (3) | 0.019 (3) | 0.023 (3) | 0.002 (3) | 0.010 (3) | −0.004 (3) |
C27 | 0.024 (3) | 0.020 (4) | 0.025 (3) | 0.009 (3) | 0.007 (3) | −0.004 (3) |
C28 | 0.019 (3) | 0.029 (4) | 0.060 (5) | 0.002 (3) | 0.005 (3) | −0.001 (4) |
C29 | 0.024 (3) | 0.018 (3) | 0.014 (3) | −0.002 (3) | 0.008 (3) | 0.001 (3) |
C30 | 0.029 (3) | 0.019 (3) | 0.018 (3) | −0.006 (3) | 0.010 (3) | −0.004 (3) |
C31 | 0.029 (4) | 0.033 (4) | 0.023 (3) | −0.007 (3) | 0.010 (3) | 0.004 (3) |
C32 | 0.077 (6) | 0.023 (4) | 0.061 (5) | −0.007 (4) | 0.041 (5) | 0.002 (4) |
W1—W2 | 2.6048 (3) | C12—H12A | 0.9800 |
W1—W2i | 2.6212 (3) | C12—H12B | 0.9800 |
W1—W3 | 2.6163 (3) | C12—H12C | 0.9800 |
W1—W3i | 2.6091 (3) | C13—C14A | 1.544 (12) |
W2—W3 | 2.6120 (3) | C13—C14 | 1.547 (9) |
W2—W3i | 2.6207 (3) | C13—H13A | 0.9900 |
W1—Cl1 | 2.4181 (13) | C13—H13B | 0.9900 |
W2—Cl2 | 2.4292 (13) | C13—H13C | 0.9900 |
W3—Cl3 | 2.4310 (13) | C13—H13D | 0.9900 |
W1—Cl4 | 2.5037 (12) | C14—C15 | 1.513 (10) |
W1—Cl5 | 2.5028 (13) | C14—H14A | 0.9900 |
W1—Cl6 | 2.4968 (13) | C14—H14B | 0.9900 |
W1—Cl7 | 2.4934 (12) | C15—C16 | 1.517 (13) |
W2—Cl4 | 2.5044 (13) | C15—H15A | 0.9900 |
W2—Cl5 | 2.4927 (12) | C15—H15B | 0.9900 |
W2—Cl6i | 2.4919 (13) | C16—H16A | 0.9800 |
W2—Cl7i | 2.4987 (12) | C16—H16B | 0.9800 |
W3—Cl4 | 2.4977 (13) | C16—H16C | 0.9800 |
W3—Cl5i | 2.4856 (12) | C14A—C15A | 1.524 (13) |
W3—Cl6 | 2.5090 (13) | C14A—H14C | 0.9900 |
W3—Cl7i | 2.5055 (13) | C14A—H14D | 0.9900 |
W4—W5 | 2.6092 (3) | C15A—C16A | 1.521 (16) |
W4—W5ii | 2.6127 (3) | C15A—H15C | 0.9900 |
W4—W6 | 2.6133 (3) | C15A—H15D | 0.9900 |
W4—W6ii | 2.6143 (3) | C16A—H16D | 0.9800 |
W5—W6 | 2.6152 (3) | C16A—H16E | 0.9800 |
W5—W6ii | 2.6071 (3) | C16A—H16F | 0.9800 |
W4—Cl8 | 2.4243 (14) | N2—C29 | 1.520 (6) |
W5—Cl9 | 2.4187 (13) | N2—C17 | 1.521 (6) |
W6—Cl10 | 2.4328 (13) | N2—C25 | 1.521 (6) |
W4—Cl11 | 2.4941 (13) | N2—C21 | 1.524 (6) |
W4—Cl12 | 2.4926 (13) | C17—C18 | 1.515 (7) |
W4—Cl13 | 2.5034 (12) | C17—H17A | 0.9900 |
W4—Cl14 | 2.4979 (13) | C17—H17B | 0.9900 |
W5—Cl11ii | 2.4969 (14) | C18—C19 | 1.534 (7) |
W5—Cl12 | 2.5044 (14) | C18—H18A | 0.9900 |
W5—Cl13ii | 2.4954 (13) | C18—H18B | 0.9900 |
W5—Cl14 | 2.4974 (13) | C19—C20 | 1.535 (7) |
W6—Cl11ii | 2.4972 (13) | C19—H19A | 0.9900 |
W6—Cl12ii | 2.4978 (13) | C19—H19B | 0.9900 |
W6—Cl13 | 2.5062 (14) | C20—H20A | 0.9800 |
W6—Cl14 | 2.4844 (13) | C20—H20B | 0.9800 |
N1—C9 | 1.517 (6) | C20—H20C | 0.9800 |
N1—C13 | 1.517 (6) | C21—C22 | 1.519 (7) |
N1—C1 | 1.521 (6) | C21—H21A | 0.9900 |
N1—C5 | 1.521 (6) | C21—H21B | 0.9900 |
C1—C2 | 1.528 (7) | C22—C23 | 1.533 (7) |
C1—H1A | 0.9900 | C22—H22A | 0.9900 |
C1—H1B | 0.9900 | C22—H22B | 0.9900 |
C2—C3 | 1.520 (6) | C23—C24 | 1.518 (8) |
C2—H2A | 0.9900 | C23—H23A | 0.9900 |
C2—H2B | 0.9900 | C23—H23B | 0.9900 |
C3—C4 | 1.508 (7) | C24—H24A | 0.9800 |
C3—H3A | 0.9900 | C24—H24B | 0.9800 |
C3—H3B | 0.9900 | C24—H24C | 0.9800 |
C4—H4A | 0.9800 | C25—C26 | 1.513 (7) |
C4—H4B | 0.9800 | C25—H25A | 0.9900 |
C4—H4C | 0.9800 | C25—H25B | 0.9900 |
C5—C6 | 1.534 (6) | C26—C27 | 1.515 (7) |
C5—H5A | 0.9900 | C26—H26A | 0.9900 |
C5—H5B | 0.9900 | C26—H26B | 0.9900 |
C6—C7 | 1.525 (6) | C27—C28 | 1.521 (8) |
C6—H6A | 0.9900 | C27—H27A | 0.9900 |
C6—H6B | 0.9900 | C27—H27B | 0.9900 |
C7—C8 | 1.517 (7) | C28—H28A | 0.9800 |
C7—H7A | 0.9900 | C28—H28B | 0.9800 |
C7—H7B | 0.9900 | C28—H28C | 0.9800 |
C8—H8A | 0.9800 | C29—C30 | 1.520 (7) |
C8—H8B | 0.9800 | C29—H29A | 0.9900 |
C8—H8C | 0.9800 | C29—H29B | 0.9900 |
C9—C10 | 1.523 (6) | C30—C31 | 1.524 (7) |
C9—H9A | 0.9900 | C30—H30A | 0.9900 |
C9—H9B | 0.9900 | C30—H30B | 0.9900 |
C10—C11 | 1.527 (7) | C31—C32 | 1.499 (8) |
C10—H10A | 0.9900 | C31—H31A | 0.9900 |
C10—H10B | 0.9900 | C31—H31B | 0.9900 |
C11—C12 | 1.525 (7) | C32—H32A | 0.9800 |
C11—H11A | 0.9900 | C32—H32B | 0.9800 |
C11—H11B | 0.9900 | C32—H32C | 0.9800 |
Cl1—W1—Cl7 | 91.92 (4) | W6—Cl14—W5 | 63.33 (3) |
Cl1—W1—Cl6 | 94.09 (5) | W6—Cl14—W4 | 63.27 (3) |
Cl7—W1—Cl6 | 89.06 (4) | W5—Cl14—W4 | 62.98 (3) |
Cl1—W1—Cl5 | 89.97 (4) | C9—N1—C13 | 108.1 (4) |
Cl7—W1—Cl5 | 90.10 (4) | C9—N1—C1 | 108.0 (4) |
Cl6—W1—Cl5 | 175.87 (4) | C13—N1—C1 | 111.5 (4) |
Cl1—W1—Cl4 | 91.43 (4) | C9—N1—C5 | 111.7 (4) |
Cl7—W1—Cl4 | 176.59 (4) | C13—N1—C5 | 109.1 (4) |
Cl6—W1—Cl4 | 90.01 (4) | C1—N1—C5 | 108.4 (4) |
Cl5—W1—Cl4 | 90.60 (4) | N1—C1—C2 | 115.9 (4) |
Cl1—W1—W2 | 133.06 (4) | N1—C1—H1A | 108.3 |
Cl7—W1—W2 | 119.10 (3) | C2—C1—H1A | 108.3 |
Cl6—W1—W2 | 118.74 (3) | N1—C1—H1B | 108.3 |
Cl5—W1—W2 | 58.38 (3) | C2—C1—H1B | 108.3 |
Cl4—W1—W2 | 58.67 (3) | H1A—C1—H1B | 107.4 |
Cl1—W1—W3i | 133.53 (3) | C3—C2—C1 | 109.9 (4) |
Cl7—W1—W3i | 58.76 (3) | C3—C2—H2A | 109.7 |
Cl6—W1—W3i | 118.13 (3) | C1—C2—H2A | 109.7 |
Cl5—W1—W3i | 58.14 (3) | C3—C2—H2B | 109.7 |
Cl4—W1—W3i | 119.00 (3) | C1—C2—H2B | 109.7 |
W2—W1—W3i | 60.348 (8) | H2A—C2—H2B | 108.2 |
Cl1—W1—W3 | 136.27 (3) | C4—C3—C2 | 113.1 (5) |
Cl7—W1—W3 | 118.48 (3) | C4—C3—H3A | 109.0 |
Cl6—W1—W3 | 58.72 (3) | C2—C3—H3A | 109.0 |
Cl5—W1—W3 | 118.39 (3) | C4—C3—H3B | 109.0 |
Cl4—W1—W3 | 58.35 (3) | C2—C3—H3B | 109.0 |
W2—W1—W3 | 60.037 (8) | H3A—C3—H3B | 107.8 |
W3i—W1—W3 | 90.149 (9) | C3—C4—H4A | 109.5 |
Cl1—W1—W2i | 136.75 (4) | C3—C4—H4B | 109.5 |
Cl7—W1—W2i | 58.43 (3) | H4A—C4—H4B | 109.5 |
Cl6—W1—W2i | 58.21 (3) | C3—C4—H4C | 109.5 |
Cl5—W1—W2i | 118.05 (3) | H4A—C4—H4C | 109.5 |
Cl4—W1—W2i | 118.39 (3) | H4B—C4—H4C | 109.5 |
W2—W1—W2i | 90.159 (9) | N1—C5—C6 | 116.9 (4) |
W3i—W1—W2i | 59.921 (8) | N1—C5—H5A | 108.1 |
W3—W1—W2i | 60.050 (8) | C6—C5—H5A | 108.1 |
Cl2—W2—Cl6i | 94.31 (5) | N1—C5—H5B | 108.1 |
Cl2—W2—Cl5 | 90.46 (4) | C6—C5—H5B | 108.1 |
Cl6i—W2—Cl5 | 89.63 (4) | H5A—C5—H5B | 107.3 |
Cl2—W2—Cl7i | 93.38 (4) | C7—C6—C5 | 116.5 (5) |
Cl6i—W2—Cl7i | 89.05 (4) | C7—C6—H6A | 108.2 |
Cl5—W2—Cl7i | 176.03 (4) | C5—C6—H6A | 108.2 |
Cl2—W2—Cl4 | 89.48 (5) | C7—C6—H6B | 108.2 |
Cl6i—W2—Cl4 | 176.19 (4) | C5—C6—H6B | 108.2 |
Cl5—W2—Cl4 | 90.81 (4) | H6A—C6—H6B | 107.3 |
Cl7i—W2—Cl4 | 90.26 (4) | C8—C7—C6 | 111.4 (5) |
Cl2—W2—W1 | 132.22 (3) | C8—C7—H7A | 109.3 |
Cl6i—W2—W1 | 118.61 (3) | C6—C7—H7A | 109.3 |
Cl5—W2—W1 | 58.76 (3) | C8—C7—H7B | 109.3 |
Cl7i—W2—W1 | 118.84 (3) | C6—C7—H7B | 109.3 |
Cl4—W2—W1 | 58.65 (3) | H7A—C7—H7B | 108.0 |
Cl2—W2—W3 | 134.22 (3) | C7—C8—H8A | 109.5 |
Cl6i—W2—W3 | 118.21 (3) | C7—C8—H8B | 109.5 |
Cl5—W2—W3 | 118.93 (3) | H8A—C8—H8B | 109.5 |
Cl7i—W2—W3 | 58.66 (3) | C7—C8—H8C | 109.5 |
Cl4—W2—W3 | 58.39 (3) | H8A—C8—H8C | 109.5 |
W1—W2—W3 | 60.199 (8) | H8B—C8—H8C | 109.5 |
Cl2—W2—W3i | 135.67 (3) | N1—C9—C10 | 115.8 (4) |
Cl6i—W2—W3i | 58.72 (3) | N1—C9—H9A | 108.3 |
Cl5—W2—W3i | 58.10 (3) | C10—C9—H9A | 108.3 |
Cl7i—W2—W3i | 118.11 (3) | N1—C9—H9B | 108.3 |
Cl4—W2—W3i | 118.53 (3) | C10—C9—H9B | 108.3 |
W1—W2—W3i | 59.908 (8) | H9A—C9—H9B | 107.4 |
W3—W2—W3i | 89.989 (9) | C9—C10—C11 | 111.0 (4) |
Cl2—W2—W1i | 137.93 (3) | C9—C10—H10A | 109.4 |
Cl6i—W2—W1i | 58.39 (3) | C11—C10—H10A | 109.4 |
Cl5—W2—W1i | 117.98 (3) | C9—C10—H10B | 109.4 |
Cl7i—W2—W1i | 58.23 (3) | C11—C10—H10B | 109.4 |
Cl4—W2—W1i | 118.20 (3) | H10A—C10—H10B | 108.0 |
W1—W2—W1i | 89.840 (9) | C12—C11—C10 | 112.9 (5) |
W3—W2—W1i | 59.814 (8) | C12—C11—H11A | 109.0 |
W3i—W2—W1i | 59.882 (8) | C10—C11—H11A | 109.0 |
Cl3—W3—Cl5i | 91.24 (4) | C12—C11—H11B | 109.0 |
Cl3—W3—Cl4 | 92.03 (4) | C10—C11—H11B | 109.0 |
Cl5i—W3—Cl4 | 176.69 (4) | H11A—C11—H11B | 107.8 |
Cl3—W3—Cl7i | 89.98 (4) | C11—C12—H12A | 109.5 |
Cl5i—W3—Cl7i | 90.21 (4) | C11—C12—H12B | 109.5 |
Cl4—W3—Cl7i | 90.26 (4) | H12A—C12—H12B | 109.5 |
Cl3—W3—Cl6 | 94.59 (4) | C11—C12—H12C | 109.5 |
Cl5i—W3—Cl6 | 89.40 (4) | H12A—C12—H12C | 109.5 |
Cl4—W3—Cl6 | 89.87 (4) | H12B—C12—H12C | 109.5 |
Cl7i—W3—Cl6 | 175.41 (4) | N1—C13—C14A | 113.6 (8) |
Cl3—W3—W1i | 133.18 (3) | N1—C13—C14 | 115.5 (6) |
Cl5i—W3—W1i | 58.78 (3) | N1—C13—H13A | 108.4 |
Cl4—W3—W1i | 118.90 (3) | C14A—C13—H13A | 89.6 |
Cl7i—W3—W1i | 58.31 (3) | C14—C13—H13A | 108.4 |
Cl6—W3—W1i | 117.80 (3) | N1—C13—H13B | 108.4 |
Cl3—W3—W2 | 133.68 (4) | C14A—C13—H13B | 126.3 |
Cl5i—W3—W2 | 119.04 (3) | C14—C13—H13B | 108.4 |
Cl4—W3—W2 | 58.65 (3) | H13A—C13—H13B | 107.5 |
Cl7i—W3—W2 | 58.41 (3) | N1—C13—H13C | 108.8 |
Cl6—W3—W2 | 118.01 (3) | C14A—C13—H13C | 108.8 |
W1i—W3—W2 | 60.267 (8) | C14—C13—H13C | 124.3 |
Cl3—W3—W1 | 136.94 (3) | H13B—C13—H13C | 86.7 |
Cl5i—W3—W1 | 118.43 (3) | N1—C13—H13D | 108.8 |
Cl4—W3—W1 | 58.57 (3) | C14A—C13—H13D | 108.8 |
Cl7i—W3—W1 | 118.15 (3) | C14—C13—H13D | 88.5 |
Cl6—W3—W1 | 58.26 (3) | H13A—C13—H13D | 126.3 |
W1i—W3—W1 | 89.851 (9) | H13C—C13—H13D | 107.7 |
W2—W3—W1 | 59.764 (8) | C15—C14—C13 | 111.5 (11) |
Cl3—W3—W2i | 136.26 (4) | C15—C14—H14A | 109.3 |
Cl5i—W3—W2i | 58.37 (3) | C13—C14—H14A | 109.3 |
Cl4—W3—W2i | 118.63 (3) | C15—C14—H14B | 109.3 |
Cl7i—W3—W2i | 118.04 (3) | C13—C14—H14B | 109.3 |
Cl6—W3—W2i | 58.08 (3) | H14A—C14—H14B | 108.0 |
W1i—W3—W2i | 59.742 (8) | C14—C15—C16 | 114.4 (10) |
W2—W3—W2i | 90.012 (9) | C14—C15—H15A | 108.7 |
W1—W3—W2i | 60.068 (8) | C16—C15—H15A | 108.7 |
W3—Cl4—W1 | 63.08 (3) | C14—C15—H15B | 108.7 |
W3—Cl4—W2 | 62.96 (3) | C16—C15—H15B | 108.7 |
W1—Cl4—W2 | 62.68 (3) | H15A—C15—H15B | 107.6 |
W3i—Cl5—W2 | 63.53 (3) | C15—C16—H16A | 109.5 |
W3i—Cl5—W1 | 63.07 (3) | C15—C16—H16B | 109.5 |
W2—Cl5—W1 | 62.86 (3) | H16A—C16—H16B | 109.5 |
W2i—Cl6—W1 | 63.39 (3) | C15—C16—H16C | 109.5 |
W2i—Cl6—W3 | 63.21 (3) | H16A—C16—H16C | 109.5 |
W1—Cl6—W3 | 63.02 (3) | H16B—C16—H16C | 109.5 |
W1—Cl7—W2i | 63.34 (3) | C15A—C14A—C13 | 109.2 (15) |
W1—Cl7—W3i | 62.92 (3) | C15A—C14A—H14C | 109.8 |
W2i—Cl7—W3i | 62.93 (3) | C13—C14A—H14C | 109.8 |
Cl8—W4—Cl12 | 90.49 (5) | C15A—C14A—H14D | 109.8 |
Cl8—W4—Cl11 | 92.30 (5) | C13—C14A—H14D | 109.8 |
Cl12—W4—Cl11 | 89.78 (4) | H14C—C14A—H14D | 108.3 |
Cl8—W4—Cl14 | 91.82 (5) | C16A—C15A—C14A | 112.3 (15) |
Cl12—W4—Cl14 | 90.45 (4) | C16A—C15A—H15C | 109.1 |
Cl11—W4—Cl14 | 175.87 (5) | C14A—C15A—H15C | 109.1 |
Cl8—W4—Cl13 | 92.99 (5) | C16A—C15A—H15D | 109.1 |
Cl12—W4—Cl13 | 176.49 (4) | C14A—C15A—H15D | 109.1 |
Cl11—W4—Cl13 | 89.62 (4) | H15C—C15A—H15D | 107.9 |
Cl14—W4—Cl13 | 89.90 (4) | C15A—C16A—H16D | 109.5 |
Cl8—W4—W5 | 133.97 (4) | C15A—C16A—H16E | 109.5 |
Cl12—W4—W5 | 58.74 (3) | H16D—C16A—H16E | 109.5 |
Cl11—W4—W5 | 118.35 (3) | C15A—C16A—H16F | 109.5 |
Cl14—W4—W5 | 58.50 (3) | H16D—C16A—H16F | 109.5 |
Cl13—W4—W5 | 118.69 (3) | H16E—C16A—H16F | 109.5 |
Cl8—W4—W5ii | 136.14 (4) | C29—N2—C17 | 111.8 (4) |
Cl12—W4—W5ii | 118.54 (3) | C29—N2—C25 | 111.8 (4) |
Cl11—W4—W5ii | 58.48 (3) | C17—N2—C25 | 105.0 (4) |
Cl14—W4—W5ii | 117.96 (3) | C29—N2—C21 | 105.0 (4) |
Cl13—W4—W5ii | 58.34 (3) | C17—N2—C21 | 111.5 (4) |
W5—W4—W5ii | 89.885 (9) | C25—N2—C21 | 111.8 (4) |
Cl8—W4—W6 | 135.55 (4) | C18—C17—N2 | 116.5 (4) |
Cl12—W4—W6 | 118.83 (3) | C18—C17—H17A | 108.2 |
Cl11—W4—W6 | 118.33 (3) | N2—C17—H17A | 108.2 |
Cl14—W4—W6 | 58.11 (3) | C18—C17—H17B | 108.2 |
Cl13—W4—W6 | 58.61 (3) | N2—C17—H17B | 108.2 |
W5—W4—W6 | 60.100 (8) | H17A—C17—H17B | 107.3 |
W5ii—W4—W6 | 59.855 (8) | C17—C18—C19 | 110.0 (4) |
Cl8—W4—W6ii | 134.42 (4) | C17—C18—H18A | 109.7 |
Cl12—W4—W6ii | 58.50 (3) | C19—C18—H18A | 109.7 |
Cl11—W4—W6ii | 58.48 (3) | C17—C18—H18B | 109.7 |
Cl14—W4—W6ii | 118.36 (3) | C19—C18—H18B | 109.7 |
Cl13—W4—W6ii | 118.38 (3) | H18A—C18—H18B | 108.2 |
W5—W4—W6ii | 59.884 (8) | C18—C19—C20 | 114.0 (5) |
W5ii—W4—W6ii | 60.043 (8) | C18—C19—H19A | 108.8 |
W6—W4—W6ii | 90.012 (9) | C20—C19—H19A | 108.8 |
Cl9—W5—Cl13ii | 90.67 (5) | C18—C19—H19B | 108.8 |
Cl9—W5—Cl11ii | 93.22 (5) | C20—C19—H19B | 108.8 |
Cl13ii—W5—Cl11ii | 89.74 (4) | H19A—C19—H19B | 107.6 |
Cl9—W5—Cl14 | 92.92 (5) | C19—C20—H20A | 109.5 |
Cl13ii—W5—Cl14 | 176.38 (4) | C19—C20—H20B | 109.5 |
Cl11ii—W5—Cl14 | 89.53 (4) | H20A—C20—H20B | 109.5 |
Cl9—W5—Cl12 | 90.66 (5) | C19—C20—H20C | 109.5 |
Cl13ii—W5—Cl12 | 90.30 (4) | H20A—C20—H20C | 109.5 |
Cl11ii—W5—Cl12 | 176.12 (4) | H20B—C20—H20C | 109.5 |
Cl14—W5—Cl12 | 90.19 (4) | C22—C21—N2 | 116.4 (4) |
Cl9—W5—W6ii | 133.36 (4) | C22—C21—H21A | 108.2 |
Cl13ii—W5—W6ii | 58.78 (3) | N2—C21—H21A | 108.2 |
Cl11ii—W5—W6ii | 118.46 (3) | C22—C21—H21B | 108.2 |
Cl14—W5—W6ii | 118.65 (3) | N2—C21—H21B | 108.2 |
Cl12—W5—W6ii | 58.46 (3) | H21A—C21—H21B | 107.4 |
Cl9—W5—W4 | 134.60 (4) | C21—C22—C23 | 110.3 (5) |
Cl13ii—W5—W4 | 118.93 (3) | C21—C22—H22A | 109.6 |
Cl11ii—W5—W4 | 118.45 (3) | C23—C22—H22A | 109.6 |
Cl14—W5—W4 | 58.52 (3) | C21—C22—H22B | 109.6 |
Cl12—W5—W4 | 58.30 (3) | C23—C22—H22B | 109.6 |
W6ii—W5—W4 | 60.156 (8) | H22A—C22—H22B | 108.1 |
Cl9—W5—W4ii | 135.24 (4) | C24—C23—C22 | 114.2 (5) |
Cl13ii—W5—W4ii | 58.64 (3) | C24—C23—H23A | 108.7 |
Cl11ii—W5—W4ii | 58.38 (3) | C22—C23—H23A | 108.7 |
Cl14—W5—W4ii | 118.10 (3) | C24—C23—H23B | 108.7 |
Cl12—W5—W4ii | 118.53 (3) | C22—C23—H23B | 108.7 |
W6ii—W5—W4ii | 60.087 (8) | H23A—C23—H23B | 107.6 |
W4—W5—W4ii | 90.115 (9) | C23—C24—H24A | 109.5 |
Cl9—W5—W6 | 136.51 (4) | C23—C24—H24B | 109.5 |
Cl13ii—W5—W6 | 118.64 (3) | H24A—C24—H24B | 109.5 |
Cl11ii—W5—W6 | 58.43 (3) | C23—C24—H24C | 109.5 |
Cl14—W5—W6 | 58.09 (3) | H24A—C24—H24C | 109.5 |
Cl12—W5—W6 | 118.32 (3) | H24B—C24—H24C | 109.5 |
W6ii—W5—W6 | 90.129 (9) | C26—C25—N2 | 117.4 (4) |
W4—W5—W6 | 60.029 (8) | C26—C25—H25A | 107.9 |
W4ii—W5—W6 | 60.010 (8) | N2—C25—H25A | 107.9 |
Cl10—W6—Cl14 | 91.63 (4) | C26—C25—H25B | 107.9 |
Cl10—W6—Cl11ii | 92.97 (5) | N2—C25—H25B | 107.9 |
Cl14—W6—Cl11ii | 89.82 (4) | H25A—C25—H25B | 107.2 |
Cl10—W6—Cl12ii | 91.93 (5) | C25—C26—C27 | 109.6 (4) |
Cl14—W6—Cl12ii | 176.42 (4) | C25—C26—H26A | 109.8 |
Cl11ii—W6—Cl12ii | 89.59 (5) | C27—C26—H26A | 109.8 |
Cl10—W6—Cl13 | 91.03 (5) | C25—C26—H26B | 109.8 |
Cl14—W6—Cl13 | 90.14 (4) | C27—C26—H26B | 109.8 |
Cl11ii—W6—Cl13 | 175.99 (4) | H26A—C26—H26B | 108.2 |
Cl12ii—W6—Cl13 | 90.20 (4) | C26—C27—C28 | 113.8 (5) |
Cl10—W6—W5ii | 134.42 (3) | C26—C27—H27A | 108.8 |
Cl14—W6—W5ii | 118.66 (3) | C28—C27—H27A | 108.8 |
Cl11ii—W6—W5ii | 118.30 (3) | C26—C27—H27B | 108.8 |
Cl12ii—W6—W5ii | 58.71 (3) | C28—C27—H27B | 108.8 |
Cl13—W6—W5ii | 58.38 (3) | H27A—C27—H27B | 107.7 |
Cl10—W6—W4 | 134.27 (4) | C27—C28—H28A | 109.5 |
Cl14—W6—W4 | 58.62 (3) | C27—C28—H28B | 109.5 |
Cl11ii—W6—W4 | 118.28 (3) | H28A—C28—H28B | 109.5 |
Cl12ii—W6—W4 | 118.75 (3) | C27—C28—H28C | 109.5 |
Cl13—W6—W4 | 58.50 (3) | H28A—C28—H28C | 109.5 |
W5ii—W6—W4 | 60.061 (8) | H28B—C28—H28C | 109.5 |
Cl10—W6—W4ii | 135.73 (4) | C30—C29—N2 | 116.1 (4) |
Cl14—W6—W4ii | 118.52 (3) | C30—C29—H29A | 108.3 |
Cl11ii—W6—W4ii | 58.36 (3) | N2—C29—H29A | 108.3 |
Cl12ii—W6—W4ii | 58.31 (3) | C30—C29—H29B | 108.3 |
Cl13—W6—W4ii | 118.33 (3) | N2—C29—H29B | 108.3 |
W5ii—W6—W4ii | 59.958 (8) | H29A—C29—H29B | 107.4 |
W4—W6—W4ii | 89.988 (9) | C29—C30—C31 | 110.0 (4) |
Cl10—W6—W5 | 135.70 (3) | C29—C30—H30A | 109.7 |
Cl14—W6—W5 | 58.58 (3) | C31—C30—H30A | 109.7 |
Cl11ii—W6—W5 | 58.42 (3) | C29—C30—H30B | 109.7 |
Cl12ii—W6—W5 | 118.25 (3) | C31—C30—H30B | 109.7 |
Cl13—W6—W5 | 118.36 (3) | H30A—C30—H30B | 108.2 |
W5ii—W6—W5 | 89.872 (9) | C32—C31—C30 | 114.8 (5) |
W4—W6—W5 | 59.871 (8) | C32—C31—H31A | 108.6 |
W4ii—W6—W5 | 59.948 (8) | C30—C31—H31A | 108.6 |
W4—Cl11—W5ii | 63.13 (3) | C32—C31—H31B | 108.6 |
W4—Cl11—W6ii | 63.17 (3) | C30—C31—H31B | 108.6 |
W5ii—Cl11—W6ii | 63.16 (3) | H31A—C31—H31B | 107.5 |
W4—Cl12—W6ii | 63.18 (3) | C31—C32—H32A | 109.5 |
W4—Cl12—W5 | 62.95 (3) | C31—C32—H32B | 109.5 |
W6ii—Cl12—W5 | 62.83 (3) | H32A—C32—H32B | 109.5 |
W5ii—Cl13—W4 | 63.02 (3) | C31—C32—H32C | 109.5 |
W5ii—Cl13—W6 | 62.84 (3) | H32A—C32—H32C | 109.5 |
W4—Cl13—W6 | 62.89 (3) | H32B—C32—H32C | 109.5 |
Cl1—W1—W2—Cl2 | −2.64 (7) | Cl8—W4—W5—Cl14 | −57.36 (6) |
Cl7—W1—W2—Cl2 | −127.56 (6) | Cl12—W4—W5—Cl14 | −112.50 (5) |
Cl6—W1—W2—Cl2 | 125.96 (6) | Cl11—W4—W5—Cl14 | 176.92 (5) |
Cl5—W1—W2—Cl2 | −57.46 (6) | Cl13—W4—W5—Cl14 | 70.26 (5) |
Cl4—W1—W2—Cl2 | 55.43 (6) | W5ii—W4—W5—Cl14 | 123.44 (4) |
W3i—W1—W2—Cl2 | −126.19 (5) | W6—W4—W5—Cl14 | 68.76 (4) |
W3—W1—W2—Cl2 | 124.44 (5) | W6ii—W4—W5—Cl14 | 178.26 (4) |
W2i—W1—W2—Cl2 | 179.14 (5) | Cl8—W4—W5—Cl12 | 55.14 (6) |
Cl1—W1—W2—Cl6i | 124.98 (6) | Cl11—W4—W5—Cl12 | −70.57 (5) |
Cl7—W1—W2—Cl6i | 0.06 (5) | Cl14—W4—W5—Cl12 | 112.50 (5) |
Cl6—W1—W2—Cl6i | −106.42 (4) | Cl13—W4—W5—Cl12 | −177.23 (5) |
Cl5—W1—W2—Cl6i | 70.16 (5) | W5ii—W4—W5—Cl12 | −124.06 (4) |
Cl4—W1—W2—Cl6i | −176.95 (5) | W6—W4—W5—Cl12 | −178.74 (4) |
W3i—W1—W2—Cl6i | 1.43 (3) | W6ii—W4—W5—Cl12 | −69.24 (4) |
W3—W1—W2—Cl6i | −107.94 (3) | Cl8—W4—W5—W6ii | 124.38 (5) |
W2i—W1—W2—Cl6i | −53.24 (3) | Cl12—W4—W5—W6ii | 69.24 (4) |
Cl1—W1—W2—Cl5 | 54.82 (6) | Cl11—W4—W5—W6ii | −1.34 (4) |
Cl7—W1—W2—Cl5 | −70.10 (5) | Cl14—W4—W5—W6ii | −178.26 (4) |
Cl6—W1—W2—Cl5 | −176.58 (5) | Cl13—W4—W5—W6ii | −108.00 (3) |
Cl4—W1—W2—Cl5 | 112.89 (5) | W5ii—W4—W5—W6ii | −54.823 (8) |
W3i—W1—W2—Cl5 | −68.73 (3) | W6—W4—W5—W6ii | −109.502 (9) |
W3—W1—W2—Cl5 | −178.10 (3) | Cl8—W4—W5—W4ii | 179.20 (5) |
W2i—W1—W2—Cl5 | −123.40 (3) | Cl12—W4—W5—W4ii | 124.06 (4) |
Cl1—W1—W2—Cl7i | −128.84 (6) | Cl11—W4—W5—W4ii | 53.49 (4) |
Cl7—W1—W2—Cl7i | 106.24 (4) | Cl14—W4—W5—W4ii | −123.44 (4) |
Cl6—W1—W2—Cl7i | −0.24 (5) | Cl13—W4—W5—W4ii | −53.17 (3) |
Cl5—W1—W2—Cl7i | 176.34 (5) | W5ii—W4—W5—W4ii | 0.0 |
Cl4—W1—W2—Cl7i | −70.77 (5) | W6—W4—W5—W4ii | −54.679 (8) |
W3i—W1—W2—Cl7i | 107.61 (3) | W6ii—W4—W5—W4ii | 54.824 (8) |
W3—W1—W2—Cl7i | −1.76 (3) | Cl8—W4—W5—W6 | −126.12 (5) |
W2i—W1—W2—Cl7i | 52.94 (3) | Cl12—W4—W5—W6 | 178.74 (4) |
Cl1—W1—W2—Cl4 | −58.07 (6) | Cl11—W4—W5—W6 | 108.17 (4) |
Cl7—W1—W2—Cl4 | 177.01 (5) | Cl14—W4—W5—W6 | −68.76 (4) |
Cl6—W1—W2—Cl4 | 70.52 (5) | Cl13—W4—W5—W6 | 1.51 (3) |
Cl5—W1—W2—Cl4 | −112.89 (5) | W5ii—W4—W5—W6 | 54.680 (8) |
W3i—W1—W2—Cl4 | 178.38 (3) | W6ii—W4—W5—W6 | 109.502 (9) |
W3—W1—W2—Cl4 | 69.01 (3) | Cl8—W4—W6—Cl10 | −2.26 (7) |
W2i—W1—W2—Cl4 | 123.71 (4) | Cl12—W4—W6—Cl10 | −127.37 (6) |
Cl1—W1—W2—W3 | −127.08 (5) | Cl11—W4—W6—Cl10 | 125.66 (6) |
Cl7—W1—W2—W3 | 108.00 (3) | Cl14—W4—W6—Cl10 | −56.76 (6) |
Cl6—W1—W2—W3 | 1.52 (3) | Cl13—W4—W6—Cl10 | 55.40 (6) |
Cl5—W1—W2—W3 | 178.10 (3) | W5—W4—W6—Cl10 | −126.14 (5) |
Cl4—W1—W2—W3 | −69.01 (3) | W5ii—W4—W6—Cl10 | 124.51 (5) |
W3i—W1—W2—W3 | 109.368 (8) | W6ii—W4—W6—Cl10 | 179.23 (5) |
W2i—W1—W2—W3 | 54.700 (7) | Cl8—W4—W6—Cl14 | 54.49 (6) |
Cl1—W1—W2—W3i | 123.55 (5) | Cl12—W4—W6—Cl14 | −70.62 (5) |
Cl7—W1—W2—W3i | −1.37 (3) | Cl11—W4—W6—Cl14 | −177.58 (5) |
Cl6—W1—W2—W3i | −107.85 (4) | Cl13—W4—W6—Cl14 | 112.16 (5) |
Cl5—W1—W2—W3i | 68.73 (3) | W5—W4—W6—Cl14 | −69.39 (4) |
Cl4—W1—W2—W3i | −178.38 (3) | W5ii—W4—W6—Cl14 | −178.73 (4) |
W3—W1—W2—W3i | −109.368 (8) | W6ii—W4—W6—Cl14 | −124.01 (4) |
W2i—W1—W2—W3i | −54.668 (7) | Cl8—W4—W6—Cl11ii | 125.08 (6) |
Cl1—W1—W2—W1i | 178.22 (5) | Cl12—W4—W6—Cl11ii | −0.03 (5) |
Cl7—W1—W2—W1i | 53.30 (3) | Cl11—W4—W6—Cl11ii | −106.99 (4) |
Cl6—W1—W2—W1i | −53.19 (3) | Cl14—W4—W6—Cl11ii | 70.59 (5) |
Cl5—W1—W2—W1i | 123.40 (3) | Cl13—W4—W6—Cl11ii | −177.25 (5) |
Cl4—W1—W2—W1i | −123.71 (4) | W5—W4—W6—Cl11ii | 1.20 (4) |
W3i—W1—W2—W1i | 54.666 (7) | W5ii—W4—W6—Cl11ii | −108.15 (4) |
W3—W1—W2—W1i | −54.702 (7) | W6ii—W4—W6—Cl11ii | −53.43 (4) |
W2i—W1—W2—W1i | 0.0 | Cl8—W4—W6—Cl12ii | −128.31 (6) |
Cl2—W2—W3—Cl3 | 6.24 (7) | Cl12—W4—W6—Cl12ii | 106.58 (4) |
Cl6i—W2—W3—Cl3 | −123.61 (6) | Cl11—W4—W6—Cl12ii | −0.38 (5) |
Cl5—W2—W3—Cl3 | 129.65 (6) | Cl14—W4—W6—Cl12ii | 177.19 (5) |
Cl7i—W2—W3—Cl3 | −54.01 (6) | Cl13—W4—W6—Cl12ii | −70.65 (5) |
Cl4—W2—W3—Cl3 | 58.38 (6) | W5—W4—W6—Cl12ii | 107.81 (4) |
W1—W2—W3—Cl3 | 127.79 (5) | W5ii—W4—W6—Cl12ii | −1.54 (4) |
W3i—W2—W3—Cl3 | −177.49 (5) | W6ii—W4—W6—Cl12ii | 53.18 (4) |
W1i—W2—W3—Cl3 | −122.97 (5) | Cl8—W4—W6—Cl13 | −57.67 (6) |
Cl2—W2—W3—Cl5i | 130.59 (6) | Cl12—W4—W6—Cl13 | 177.22 (5) |
Cl6i—W2—W3—Cl5i | 0.74 (5) | Cl11—W4—W6—Cl13 | 70.26 (5) |
Cl5—W2—W3—Cl5i | −106.00 (4) | Cl14—W4—W6—Cl13 | −112.16 (5) |
Cl7i—W2—W3—Cl5i | 70.34 (5) | W5—W4—W6—Cl13 | 178.45 (3) |
Cl4—W2—W3—Cl5i | −177.27 (5) | W5ii—W4—W6—Cl13 | 69.11 (3) |
W1—W2—W3—Cl5i | −107.86 (3) | W6ii—W4—W6—Cl13 | 123.83 (4) |
W3i—W2—W3—Cl5i | −53.15 (3) | Cl8—W4—W6—W5ii | −126.77 (5) |
W1i—W2—W3—Cl5i | 1.38 (3) | Cl12—W4—W6—W5ii | 108.12 (4) |
Cl2—W2—W3—Cl4 | −52.14 (6) | Cl11—W4—W6—W5ii | 1.15 (3) |
Cl6i—W2—W3—Cl4 | 178.01 (5) | Cl14—W4—W6—W5ii | 178.73 (4) |
Cl5—W2—W3—Cl4 | 71.27 (5) | Cl13—W4—W6—W5ii | −69.11 (3) |
Cl7i—W2—W3—Cl4 | −112.39 (5) | W5—W4—W6—W5ii | 109.345 (9) |
W1—W2—W3—Cl4 | 69.41 (3) | W6ii—W4—W6—W5ii | 54.720 (8) |
W3i—W2—W3—Cl4 | 124.12 (3) | Cl8—W4—W6—W4ii | 178.51 (5) |
W1i—W2—W3—Cl4 | 178.65 (3) | Cl12—W4—W6—W4ii | 53.40 (4) |
Cl2—W2—W3—Cl7i | 60.25 (6) | Cl11—W4—W6—W4ii | −53.56 (3) |
Cl6i—W2—W3—Cl7i | −69.60 (5) | Cl14—W4—W6—W4ii | 124.01 (4) |
Cl5—W2—W3—Cl7i | −176.34 (5) | Cl13—W4—W6—W4ii | −123.83 (4) |
Cl4—W2—W3—Cl7i | 112.39 (5) | W5—W4—W6—W4ii | 54.627 (8) |
W1—W2—W3—Cl7i | −178.20 (3) | W5ii—W4—W6—W4ii | −54.718 (8) |
W3i—W2—W3—Cl7i | −123.49 (3) | W6ii—W4—W6—W4ii | 0.0 |
W1i—W2—W3—Cl7i | −68.96 (3) | Cl8—W4—W6—W5 | 123.88 (5) |
Cl2—W2—W3—Cl6 | −123.05 (6) | Cl12—W4—W6—W5 | −1.23 (4) |
Cl6i—W2—W3—Cl6 | 107.10 (4) | Cl11—W4—W6—W5 | −108.19 (4) |
Cl5—W2—W3—Cl6 | 0.36 (5) | Cl14—W4—W6—W5 | 69.39 (4) |
Cl7i—W2—W3—Cl6 | 176.70 (5) | Cl13—W4—W6—W5 | −178.45 (3) |
Cl4—W2—W3—Cl6 | −70.91 (5) | W5ii—W4—W6—W5 | −109.345 (9) |
W1—W2—W3—Cl6 | −1.50 (3) | W6ii—W4—W6—W5 | −54.625 (8) |
W3i—W2—W3—Cl6 | 53.21 (3) | Cl9—W5—W6—Cl10 | −0.62 (8) |
W1i—W2—W3—Cl6 | 107.73 (3) | Cl13ii—W5—W6—Cl10 | −127.14 (6) |
Cl2—W2—W3—W1i | 129.21 (5) | Cl11ii—W5—W6—Cl10 | −57.12 (6) |
Cl6i—W2—W3—W1i | −0.63 (3) | Cl14—W5—W6—Cl10 | 54.67 (6) |
Cl5—W2—W3—W1i | −107.38 (3) | Cl12—W5—W6—Cl10 | 125.34 (6) |
Cl7i—W2—W3—W1i | 68.96 (3) | W6ii—W5—W6—Cl10 | 178.97 (5) |
Cl4—W2—W3—W1i | −178.65 (3) | W4—W5—W6—Cl10 | 124.12 (5) |
W1—W2—W3—W1i | −109.234 (8) | W4ii—W5—W6—Cl10 | −126.28 (5) |
W3i—W2—W3—W1i | −54.522 (7) | Cl9—W5—W6—Cl14 | −55.30 (7) |
Cl2—W2—W3—W1 | −121.55 (5) | Cl13ii—W5—W6—Cl14 | 178.19 (5) |
Cl6i—W2—W3—W1 | 108.60 (3) | Cl11ii—W5—W6—Cl14 | −111.79 (5) |
Cl5—W2—W3—W1 | 1.86 (3) | Cl12—W5—W6—Cl14 | 70.67 (5) |
Cl7i—W2—W3—W1 | 178.20 (3) | W6ii—W5—W6—Cl14 | 124.30 (4) |
Cl4—W2—W3—W1 | −69.41 (3) | W4—W5—W6—Cl14 | 69.45 (4) |
W3i—W2—W3—W1 | 54.712 (7) | W4ii—W5—W6—Cl14 | 179.05 (4) |
W1i—W2—W3—W1 | 109.234 (8) | Cl9—W5—W6—Cl11ii | 56.50 (7) |
Cl2—W2—W3—W2i | −176.27 (5) | Cl13ii—W5—W6—Cl11ii | −70.02 (5) |
Cl6i—W2—W3—W2i | 53.89 (3) | Cl14—W5—W6—Cl11ii | 111.79 (5) |
Cl5—W2—W3—W2i | −52.86 (3) | Cl12—W5—W6—Cl11ii | −177.54 (5) |
Cl7i—W2—W3—W2i | 123.48 (3) | W6ii—W5—W6—Cl11ii | −123.91 (4) |
Cl4—W2—W3—W2i | −124.13 (3) | W4—W5—W6—Cl11ii | −178.76 (4) |
W1—W2—W3—W2i | −54.713 (7) | W4ii—W5—W6—Cl11ii | −69.16 (4) |
W3i—W2—W3—W2i | 0.0 | Cl9—W5—W6—Cl12ii | 126.62 (7) |
W1i—W2—W3—W2i | 54.520 (7) | Cl13ii—W5—W6—Cl12ii | 0.11 (5) |
Cl1—W1—W3—Cl3 | −0.65 (7) | Cl11ii—W5—W6—Cl12ii | 70.13 (5) |
Cl7—W1—W3—Cl3 | 127.82 (6) | Cl14—W5—W6—Cl12ii | −178.08 (5) |
Cl6—W1—W3—Cl3 | 58.40 (6) | Cl12—W5—W6—Cl12ii | −107.42 (4) |
Cl5—W1—W3—Cl3 | −125.00 (6) | W6ii—W5—W6—Cl12ii | −53.79 (4) |
Cl4—W1—W3—Cl3 | −53.62 (6) | W4—W5—W6—Cl12ii | −108.63 (4) |
W2—W1—W3—Cl3 | −123.16 (5) | W4ii—W5—W6—Cl12ii | 0.97 (4) |
W3i—W1—W3—Cl3 | −178.23 (5) | Cl9—W5—W6—Cl13 | −126.24 (7) |
W2i—W1—W3—Cl3 | 127.22 (5) | Cl13ii—W5—W6—Cl13 | 107.24 (4) |
Cl1—W1—W3—Cl5i | −128.62 (6) | Cl11ii—W5—W6—Cl13 | 177.26 (5) |
Cl7—W1—W3—Cl5i | −0.16 (5) | Cl14—W5—W6—Cl13 | −70.95 (5) |
Cl6—W1—W3—Cl5i | −69.58 (5) | Cl12—W5—W6—Cl13 | −0.28 (5) |
Cl5—W1—W3—Cl5i | 107.02 (4) | W6ii—W5—W6—Cl13 | 53.35 (3) |
Cl4—W1—W3—Cl5i | 178.40 (5) | W4—W5—W6—Cl13 | −1.50 (3) |
W2—W1—W3—Cl5i | 108.86 (4) | W4ii—W5—W6—Cl13 | 108.10 (3) |
W3i—W1—W3—Cl5i | 53.79 (4) | Cl9—W5—W6—W5ii | −179.59 (6) |
W2i—W1—W3—Cl5i | −0.76 (4) | Cl13ii—W5—W6—W5ii | 53.89 (4) |
Cl1—W1—W3—Cl4 | 52.98 (6) | Cl11ii—W5—W6—W5ii | 123.91 (4) |
Cl7—W1—W3—Cl4 | −178.56 (5) | Cl14—W5—W6—W5ii | −124.30 (4) |
Cl6—W1—W3—Cl4 | 112.02 (5) | Cl12—W5—W6—W5ii | −53.63 (4) |
Cl5—W1—W3—Cl4 | −71.38 (5) | W6ii—W5—W6—W5ii | 0.0 |
W2—W1—W3—Cl4 | −69.54 (4) | W4—W5—W6—W5ii | −54.848 (8) |
W3i—W1—W3—Cl4 | −124.61 (4) | W4ii—W5—W6—W5ii | 54.754 (8) |
W2i—W1—W3—Cl4 | −179.16 (4) | Cl9—W5—W6—W4 | −124.74 (6) |
Cl1—W1—W3—Cl7i | 124.25 (6) | Cl13ii—W5—W6—W4 | 108.74 (4) |
Cl7—W1—W3—Cl7i | −107.28 (4) | Cl11ii—W5—W6—W4 | 178.76 (4) |
Cl6—W1—W3—Cl7i | −176.70 (5) | Cl14—W5—W6—W4 | −69.45 (4) |
Cl5—W1—W3—Cl7i | −0.10 (5) | Cl12—W5—W6—W4 | 1.22 (4) |
Cl4—W1—W3—Cl7i | 71.28 (5) | W6ii—W5—W6—W4 | 54.847 (8) |
W2—W1—W3—Cl7i | 1.74 (3) | W4ii—W5—W6—W4 | 109.602 (9) |
W3i—W1—W3—Cl7i | −53.33 (3) | Cl9—W5—W6—W4ii | 125.65 (6) |
W2i—W1—W3—Cl7i | −107.88 (3) | Cl13ii—W5—W6—W4ii | −0.86 (4) |
Cl1—W1—W3—Cl6 | −59.04 (6) | Cl11ii—W5—W6—W4ii | 69.16 (4) |
Cl7—W1—W3—Cl6 | 69.42 (5) | Cl14—W5—W6—W4ii | −179.05 (4) |
Cl5—W1—W3—Cl6 | 176.60 (5) | Cl12—W5—W6—W4ii | −108.38 (4) |
Cl4—W1—W3—Cl6 | −112.02 (5) | W6ii—W5—W6—W4ii | −54.755 (8) |
W2—W1—W3—Cl6 | 178.44 (4) | W4—W5—W6—W4ii | −109.602 (9) |
W3i—W1—W3—Cl6 | 123.37 (4) | Cl8—W4—Cl11—W5ii | 145.27 (4) |
W2i—W1—W3—Cl6 | 68.82 (3) | Cl12—W4—Cl11—W5ii | −124.25 (4) |
Cl1—W1—W3—W1i | 177.59 (5) | Cl14—W4—Cl11—W5ii | −31.1 (6) |
Cl7—W1—W3—W1i | −53.95 (4) | Cl13—W4—Cl11—W5ii | 52.29 (4) |
Cl6—W1—W3—W1i | −123.37 (4) | W5—W4—Cl11—W5ii | −70.52 (3) |
Cl5—W1—W3—W1i | 53.23 (3) | W6—W4—Cl11—W5ii | −1.17 (4) |
Cl4—W1—W3—W1i | 124.61 (4) | W6ii—W4—Cl11—W5ii | −71.88 (2) |
W2—W1—W3—W1i | 55.073 (8) | Cl8—W4—Cl11—W6ii | −142.85 (4) |
W3i—W1—W3—W1i | 0.0 | Cl12—W4—Cl11—W6ii | −52.37 (4) |
W2i—W1—W3—W1i | −54.552 (8) | Cl14—W4—Cl11—W6ii | 40.8 (6) |
Cl1—W1—W3—W2 | 122.51 (5) | Cl13—W4—Cl11—W6ii | 124.17 (4) |
Cl7—W1—W3—W2 | −109.02 (4) | W5—W4—Cl11—W6ii | 1.36 (4) |
Cl6—W1—W3—W2 | −178.44 (4) | W5ii—W4—Cl11—W6ii | 71.88 (2) |
Cl5—W1—W3—W2 | −1.84 (3) | W6—W4—Cl11—W6ii | 70.71 (3) |
Cl4—W1—W3—W2 | 69.54 (4) | Cl8—W4—Cl12—W6ii | 144.65 (4) |
W3i—W1—W3—W2 | −55.072 (8) | Cl11—W4—Cl12—W6ii | 52.35 (4) |
W2i—W1—W3—W2 | −109.625 (9) | Cl14—W4—Cl12—W6ii | −123.53 (4) |
Cl1—W1—W3—W2i | −127.86 (5) | Cl13—W4—Cl12—W6ii | −27.8 (8) |
Cl7—W1—W3—W2i | 0.61 (4) | W5—W4—Cl12—W6ii | −71.55 (2) |
Cl6—W1—W3—W2i | −68.82 (3) | W5ii—W4—Cl12—W6ii | −0.99 (4) |
Cl5—W1—W3—W2i | 107.79 (3) | W6—W4—Cl12—W6ii | −70.30 (3) |
Cl4—W1—W3—W2i | 179.16 (4) | Cl8—W4—Cl12—W5 | −143.80 (4) |
W2—W1—W3—W2i | 109.625 (9) | Cl11—W4—Cl12—W5 | 123.90 (4) |
W3i—W1—W3—W2i | 54.554 (8) | Cl14—W4—Cl12—W5 | −51.98 (4) |
Cl3—W3—Cl4—W1 | 146.63 (4) | Cl13—W4—Cl12—W5 | 43.7 (8) |
Cl5i—W3—Cl4—W1 | −25.2 (8) | W5ii—W4—Cl12—W5 | 70.56 (3) |
Cl7i—W3—Cl4—W1 | −123.37 (4) | W6—W4—Cl12—W5 | 1.25 (4) |
Cl6—W3—Cl4—W1 | 52.04 (4) | W6ii—W4—Cl12—W5 | 71.55 (2) |
W1i—W3—Cl4—W1 | −70.07 (3) | Cl9—W5—Cl12—W4 | 144.91 (4) |
W2—W3—Cl4—W1 | −71.41 (2) | Cl13ii—W5—Cl12—W4 | −124.42 (4) |
W2i—W3—Cl4—W1 | −0.83 (4) | Cl11ii—W5—Cl12—W4 | −33.9 (7) |
Cl3—W3—Cl4—W2 | −141.95 (4) | Cl14—W5—Cl12—W4 | 51.99 (3) |
Cl5i—W3—Cl4—W2 | 46.2 (8) | W6ii—W5—Cl12—W4 | −72.11 (2) |
Cl7i—W3—Cl4—W2 | −51.96 (3) | W4ii—W5—Cl12—W4 | −70.55 (3) |
Cl6—W3—Cl4—W2 | 123.45 (4) | W6—W5—Cl12—W4 | −1.24 (4) |
W1i—W3—Cl4—W2 | 1.34 (3) | Cl9—W5—Cl12—W6ii | −142.99 (4) |
W1—W3—Cl4—W2 | 71.41 (2) | Cl13ii—W5—Cl12—W6ii | −52.32 (3) |
W2i—W3—Cl4—W2 | 70.59 (3) | Cl11ii—W5—Cl12—W6ii | 38.2 (7) |
Cl1—W1—Cl4—W3 | −146.49 (4) | Cl14—W5—Cl12—W6ii | 124.10 (3) |
Cl7—W1—Cl4—W3 | 21.8 (8) | W4—W5—Cl12—W6ii | 72.11 (2) |
Cl6—W1—Cl4—W3 | −52.40 (4) | W4ii—W5—Cl12—W6ii | 1.56 (4) |
Cl5—W1—Cl4—W3 | 123.52 (4) | W6—W5—Cl12—W6ii | 70.87 (3) |
W2—W1—Cl4—W3 | 71.84 (2) | Cl8—W4—Cl13—W5ii | −144.69 (4) |
W3i—W1—Cl4—W3 | 70.23 (3) | Cl12—W4—Cl13—W5ii | 27.8 (8) |
W2i—W1—Cl4—W3 | 0.82 (4) | Cl11—W4—Cl13—W5ii | −52.41 (4) |
Cl1—W1—Cl4—W2 | 141.66 (4) | Cl14—W4—Cl13—W5ii | 123.49 (4) |
Cl7—W1—Cl4—W2 | −50.0 (8) | W5—W4—Cl13—W5ii | 70.12 (3) |
Cl6—W1—Cl4—W2 | −124.24 (3) | W6—W4—Cl13—W5ii | 71.64 (2) |
Cl5—W1—Cl4—W2 | 51.68 (3) | W6ii—W4—Cl13—W5ii | 0.88 (4) |
W3i—W1—Cl4—W2 | −1.61 (3) | Cl8—W4—Cl13—W6 | 143.66 (4) |
W3—W1—Cl4—W2 | −71.84 (2) | Cl12—W4—Cl13—W6 | −43.9 (8) |
W2i—W1—Cl4—W2 | −71.02 (3) | Cl11—W4—Cl13—W6 | −124.05 (4) |
Cl2—W2—Cl4—W3 | 145.54 (4) | Cl14—W4—Cl13—W6 | 51.85 (4) |
Cl6i—W2—Cl4—W3 | −27.4 (6) | W5—W4—Cl13—W6 | −1.53 (3) |
Cl5—W2—Cl4—W3 | −124.01 (3) | W5ii—W4—Cl13—W6 | −71.64 (2) |
Cl7i—W2—Cl4—W3 | 52.16 (3) | W6ii—W4—Cl13—W6 | −70.77 (3) |
W1—W2—Cl4—W3 | −72.04 (2) | Cl10—W6—Cl13—W5ii | 144.19 (4) |
W3i—W2—Cl4—W3 | −70.44 (3) | Cl14—W6—Cl13—W5ii | −124.18 (4) |
W1i—W2—Cl4—W3 | −1.33 (3) | Cl11ii—W6—Cl13—W5ii | −34.8 (6) |
Cl2—W2—Cl4—W1 | −142.42 (4) | Cl12ii—W6—Cl13—W5ii | 52.26 (4) |
Cl6i—W2—Cl4—W1 | 44.7 (6) | W4—W6—Cl13—W5ii | −71.93 (2) |
Cl5—W2—Cl4—W1 | −51.98 (3) | W4ii—W6—Cl13—W5ii | −1.24 (4) |
Cl7i—W2—Cl4—W1 | 124.20 (4) | W5—W6—Cl13—W5ii | −70.41 (3) |
W3—W2—Cl4—W1 | 72.04 (2) | Cl10—W6—Cl13—W4 | −143.88 (4) |
W3i—W2—Cl4—W1 | 1.60 (3) | Cl14—W6—Cl13—W4 | −52.24 (3) |
W1i—W2—Cl4—W1 | 70.71 (3) | Cl11ii—W6—Cl13—W4 | 37.2 (6) |
Cl2—W2—Cl5—W3i | −146.89 (4) | Cl12ii—W6—Cl13—W4 | 124.19 (4) |
Cl6i—W2—Cl5—W3i | −52.58 (4) | W5ii—W6—Cl13—W4 | 71.93 (2) |
Cl7i—W2—Cl5—W3i | 18.0 (7) | W4ii—W6—Cl13—W4 | 70.69 (3) |
Cl4—W2—Cl5—W3i | 123.63 (4) | W5—W6—Cl13—W4 | 1.52 (3) |
W1—W2—Cl5—W3i | 71.75 (2) | Cl10—W6—Cl14—W5 | −145.25 (4) |
W3—W2—Cl5—W3i | 69.86 (3) | Cl11ii—W6—Cl14—W5 | −52.28 (4) |
W1i—W2—Cl5—W3i | 0.77 (4) | Cl12ii—W6—Cl14—W5 | 28.2 (8) |
Cl2—W2—Cl5—W1 | 141.37 (4) | Cl13—W6—Cl14—W5 | 123.72 (4) |
Cl6i—W2—Cl5—W1 | −124.33 (4) | W5ii—W6—Cl14—W5 | 70.31 (3) |
Cl7i—W2—Cl5—W1 | −53.8 (7) | W4—W6—Cl14—W5 | 71.56 (2) |
Cl4—W2—Cl5—W1 | 51.89 (4) | W4ii—W6—Cl14—W5 | 0.94 (4) |
W3—W2—Cl5—W1 | −1.88 (3) | Cl10—W6—Cl14—W4 | 143.19 (4) |
W3i—W2—Cl5—W1 | −71.75 (2) | Cl11ii—W6—Cl14—W4 | −123.84 (4) |
W1i—W2—Cl5—W1 | −70.98 (3) | Cl12ii—W6—Cl14—W4 | −43.4 (8) |
Cl1—W1—Cl5—W3i | 144.21 (4) | Cl13—W6—Cl14—W4 | 52.16 (3) |
Cl7—W1—Cl5—W3i | 52.30 (3) | W5ii—W6—Cl14—W4 | −1.25 (4) |
Cl6—W1—Cl5—W3i | −25.9 (6) | W4ii—W6—Cl14—W4 | −70.62 (3) |
Cl4—W1—Cl5—W3i | −124.36 (3) | W5—W6—Cl14—W4 | −71.56 (2) |
W2—W1—Cl5—W3i | −72.46 (2) | Cl9—W5—Cl14—W6 | 145.49 (5) |
W3—W1—Cl5—W3i | −70.58 (3) | Cl13ii—W5—Cl14—W6 | −26.1 (8) |
W2i—W1—Cl5—W3i | −1.38 (3) | Cl11ii—W5—Cl14—W6 | 52.29 (4) |
Cl1—W1—Cl5—W2 | −143.33 (4) | Cl12—W5—Cl14—W6 | −123.83 (4) |
Cl7—W1—Cl5—W2 | 124.75 (3) | W6ii—W5—Cl14—W6 | −70.29 (3) |
Cl6—W1—Cl5—W2 | 46.6 (6) | W4—W5—Cl14—W6 | −72.01 (2) |
Cl4—W1—Cl5—W2 | −51.90 (3) | W4ii—W5—Cl14—W6 | −0.93 (4) |
W3i—W1—Cl5—W2 | 72.46 (2) | Cl9—W5—Cl14—W4 | −142.49 (5) |
W3—W1—Cl5—W2 | 1.87 (3) | Cl13ii—W5—Cl14—W4 | 45.9 (8) |
W2i—W1—Cl5—W2 | 71.08 (3) | Cl11ii—W5—Cl14—W4 | 124.30 (4) |
Cl1—W1—Cl6—W2i | −144.56 (4) | Cl12—W5—Cl14—W4 | −51.82 (4) |
Cl7—W1—Cl6—W2i | −52.71 (3) | W6ii—W5—Cl14—W4 | 1.72 (4) |
Cl5—W1—Cl6—W2i | 25.5 (6) | W4ii—W5—Cl14—W4 | 71.08 (3) |
Cl4—W1—Cl6—W2i | 124.00 (3) | W6—W5—Cl14—W4 | 72.01 (2) |
W2—W1—Cl6—W2i | 70.36 (3) | Cl8—W4—Cl14—W6 | −145.23 (4) |
W3i—W1—Cl6—W2i | 0.64 (3) | Cl12—W4—Cl14—W6 | 124.27 (4) |
W3—W1—Cl6—W2i | 71.90 (2) | Cl11—W4—Cl14—W6 | 31.1 (6) |
Cl1—W1—Cl6—W3 | 143.54 (4) | Cl13—W4—Cl14—W6 | −52.24 (4) |
Cl7—W1—Cl6—W3 | −124.61 (3) | W5—W4—Cl14—W6 | 72.10 (2) |
Cl5—W1—Cl6—W3 | −46.4 (6) | W5ii—W4—Cl14—W6 | 1.24 (3) |
Cl4—W1—Cl6—W3 | 52.11 (3) | W6ii—W4—Cl14—W6 | 70.39 (3) |
W2—W1—Cl6—W3 | −1.54 (3) | Cl8—W4—Cl14—W5 | 142.67 (4) |
W3i—W1—Cl6—W3 | −71.25 (3) | Cl12—W4—Cl14—W5 | 52.17 (4) |
W2i—W1—Cl6—W3 | −71.90 (2) | Cl11—W4—Cl14—W5 | −41.0 (6) |
Cl3—W3—Cl6—W2i | 143.50 (4) | Cl13—W4—Cl14—W5 | −124.34 (4) |
Cl5i—W3—Cl6—W2i | 52.31 (3) | W5ii—W4—Cl14—W5 | −70.86 (3) |
Cl4—W3—Cl6—W2i | −124.47 (3) | W6—W4—Cl14—W5 | −72.10 (2) |
Cl7i—W3—Cl6—W2i | −32.8 (5) | W6ii—W4—Cl14—W5 | −1.71 (4) |
W1i—W3—Cl6—W2i | −1.43 (3) | C9—N1—C1—C2 | −174.2 (4) |
W2—W3—Cl6—W2i | −70.66 (3) | C13—N1—C1—C2 | −55.6 (6) |
W1—W3—Cl6—W2i | −72.19 (2) | C5—N1—C1—C2 | 64.6 (6) |
Cl3—W3—Cl6—W1 | −144.31 (4) | N1—C1—C2—C3 | 156.0 (5) |
Cl5i—W3—Cl6—W1 | 124.49 (4) | C1—C2—C3—C4 | 166.7 (5) |
Cl4—W3—Cl6—W1 | −52.28 (3) | C9—N1—C5—C6 | 56.9 (6) |
Cl7i—W3—Cl6—W1 | 39.4 (5) | C13—N1—C5—C6 | −62.6 (6) |
W1i—W3—Cl6—W1 | 70.75 (3) | C1—N1—C5—C6 | 175.8 (4) |
W2—W3—Cl6—W1 | 1.52 (3) | N1—C5—C6—C7 | 92.1 (6) |
W2i—W3—Cl6—W1 | 72.19 (2) | C5—C6—C7—C8 | 169.6 (5) |
Cl1—W1—Cl7—W2i | 146.60 (4) | C13—N1—C9—C10 | 176.7 (4) |
Cl6—W1—Cl7—W2i | 52.53 (3) | C1—N1—C9—C10 | −62.5 (5) |
Cl5—W1—Cl7—W2i | −123.43 (4) | C5—N1—C9—C10 | 56.6 (6) |
Cl4—W1—Cl7—W2i | −21.7 (8) | N1—C9—C10—C11 | −174.0 (4) |
W2—W1—Cl7—W2i | −70.23 (3) | C9—C10—C11—C12 | 69.5 (6) |
W3i—W1—Cl7—W2i | −71.62 (2) | C9—N1—C13—C14A | 53.3 (10) |
W3—W1—Cl7—W2i | −0.62 (4) | C1—N1—C13—C14A | −65.4 (10) |
Cl1—W1—Cl7—W3i | −141.78 (4) | C5—N1—C13—C14A | 174.9 (9) |
Cl6—W1—Cl7—W3i | 124.15 (3) | C9—N1—C13—C14 | 77.2 (7) |
Cl5—W1—Cl7—W3i | −51.81 (3) | C1—N1—C13—C14 | −41.5 (8) |
Cl4—W1—Cl7—W3i | 49.9 (8) | C5—N1—C13—C14 | −161.2 (6) |
W2—W1—Cl7—W3i | 1.39 (3) | N1—C13—C14—C15 | 177.2 (8) |
W3—W1—Cl7—W3i | 71.00 (3) | C14A—C13—C14—C15 | −93 (3) |
W2i—W1—Cl7—W3i | 71.62 (2) | C13—C14—C15—C16 | 64.0 (17) |
Cl8—W4—W5—Cl9 | 1.30 (7) | N1—C13—C14A—C15A | 165.1 (13) |
Cl12—W4—W5—Cl9 | −53.84 (7) | C14—C13—C14A—C15A | 65 (3) |
Cl11—W4—W5—Cl9 | −124.42 (7) | C13—C14A—C15A—C16A | −69 (3) |
Cl14—W4—W5—Cl9 | 58.66 (7) | C29—N2—C17—C18 | 58.6 (6) |
Cl13—W4—W5—Cl9 | 128.92 (6) | C25—N2—C17—C18 | −179.9 (4) |
W5ii—W4—W5—Cl9 | −177.90 (6) | C21—N2—C17—C18 | −58.6 (6) |
W6—W4—W5—Cl9 | 127.42 (6) | N2—C17—C18—C19 | 167.6 (4) |
W6ii—W4—W5—Cl9 | −123.08 (6) | C17—C18—C19—C20 | −67.5 (6) |
Cl8—W4—W5—Cl13ii | 125.61 (6) | C29—N2—C21—C22 | −176.0 (5) |
Cl12—W4—W5—Cl13ii | 70.47 (5) | C17—N2—C21—C22 | −54.7 (6) |
Cl11—W4—W5—Cl13ii | −0.10 (5) | C25—N2—C21—C22 | 62.6 (6) |
Cl14—W4—W5—Cl13ii | −177.03 (5) | N2—C21—C22—C23 | −177.5 (4) |
Cl13—W4—W5—Cl13ii | −106.76 (4) | C21—C22—C23—C24 | 70.9 (6) |
W5ii—W4—W5—Cl13ii | −53.59 (4) | C29—N2—C25—C26 | −55.0 (6) |
W6—W4—W5—Cl13ii | −108.27 (4) | C17—N2—C25—C26 | −176.4 (4) |
W6ii—W4—W5—Cl13ii | 1.23 (4) | C21—N2—C25—C26 | 62.4 (6) |
Cl8—W4—W5—Cl11ii | −127.32 (6) | N2—C25—C26—C27 | 175.8 (4) |
Cl12—W4—W5—Cl11ii | 177.54 (5) | C25—C26—C27—C28 | 66.5 (6) |
Cl11—W4—W5—Cl11ii | 106.96 (4) | C17—N2—C29—C30 | 63.1 (6) |
Cl14—W4—W5—Cl11ii | −69.96 (5) | C25—N2—C29—C30 | −54.4 (6) |
Cl13—W4—W5—Cl11ii | 0.30 (5) | C21—N2—C29—C30 | −175.8 (5) |
W5ii—W4—W5—Cl11ii | 53.48 (4) | N2—C29—C30—C31 | 173.5 (4) |
W6—W4—W5—Cl11ii | −1.20 (4) | C29—C30—C31—C32 | −64.5 (7) |
W6ii—W4—W5—Cl11ii | 108.30 (4) |
Symmetry codes: (i) −x, −y+1, −z; (ii) −x+1, −y+2, −z. |
(C16H36N)2[W6Cl14] | F(000) = 3840 |
Mr = 2084.32 | Dx = 2.55 Mg m−3 |
Monoclinic, P21/c | Mo Kα radiation, λ = 0.71073 Å |
Hall symbol: -P 2ybc | Cell parameters from 12989 reflections |
a = 22.3689 (2) Å | θ = 2.0–27.5° |
b = 11.7596 (1) Å | µ = 13.38 mm−1 |
c = 22.3108 (2) Å | T = 200 K |
β = 112.320 (1)° | Chunk, yellow |
V = 5429.13 (8) Å3 | 0.27 × 0.19 × 0.19 mm |
Z = 4 |
Nonius KappaCCD diffractometer | 12422 independent reflections |
Radiation source: Enraf–Nonius FR590 | 9227 reflections with I > 2σ(I) |
Graphite monochromator | Rint = 0.063 |
Detector resolution: 9 pixels mm-1 | θmax = 27.5°, θmin = 2.2° |
ϕ and ω scans | h = −29→28 |
Absorption correction: multi-scan (HKL SCALEPACK; Otwinowski & Minor, 1997) | k = −15→15 |
Tmin = 0.055, Tmax = 0.079 | l = −28→28 |
101212 measured reflections |
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)] = 0.031 | Hydrogen site location: inferred from neighbouring sites |
wR(F2) = 0.064 | H-atom parameters constrained |
S = 1.03 | w = 1/[σ2(Fo2) + (0.0257P)2 + 0.5516P] where P = (Fo2 + 2Fc2)/3 |
12422 reflections | (Δ/σ)max = 0.001 |
515 parameters | Δρmax = 2.36 e Å−3 |
148 restraints | Δρmin = −2.11 e Å−3 |
(C16H36N)2[W6Cl14] | V = 5429.13 (8) Å3 |
Mr = 2084.32 | Z = 4 |
Monoclinic, P21/c | Mo Kα radiation |
a = 22.3689 (2) Å | µ = 13.38 mm−1 |
b = 11.7596 (1) Å | T = 200 K |
c = 22.3108 (2) Å | 0.27 × 0.19 × 0.19 mm |
β = 112.320 (1)° |
Nonius KappaCCD diffractometer | 12422 independent reflections |
Absorption correction: multi-scan (HKL SCALEPACK; Otwinowski & Minor, 1997) | 9227 reflections with I > 2σ(I) |
Tmin = 0.055, Tmax = 0.079 | Rint = 0.063 |
101212 measured reflections |
R[F2 > 2σ(F2)] = 0.031 | 148 restraints |
wR(F2) = 0.064 | H-atom parameters constrained |
S = 1.03 | Δρmax = 2.36 e Å−3 |
12422 reflections | Δρmin = −2.11 e Å−3 |
515 parameters |
Experimental. Examination of the diffraction pattern on a Nonius Kappa CCD diffractometer indicated a monoclinic crystal system. 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 4.3, which means that 90% of the reflections were measured at least 4.3 times. Phi and omega scans with a frame width of 1.0 degree were used. Data integration was done with Denzo (Otwinowski & Minor, 1997), and scaling and merging of the data was done with Scalepack (Otwinowski & Minor, 1997). The structure was solved by the direct methods procedure in SHELXS-97(Sheldrick, 2008). Full-matrix least-squares refinements based on F2 were performed in SHELXL-97(Sheldrick, 2008), as incorporated in the WinGX package(Farrugia, 1999). |
Geometry. All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. |
Refinement. For the methyl groups, the hydrogen atoms were added at calculated positions using a riding model with C—H=0.98 Å and U(H)=1.5*Ueq(bonded carbon atom). The remaining hydrogen atoms were included in the model at calculated positions using a riding model with a C—H distance of 0.99 Å and U(H)=1.2*Ueq(bonded carbon atom). 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) | |
W1 | 0.062258 (11) | 0.42355 (2) | 0.067138 (10) | 0.02029 (6) | |
W2 | −0.000658 (11) | 0.61364 (2) | 0.057169 (10) | 0.02090 (6) | |
W3 | −0.064295 (11) | 0.42407 (2) | 0.017128 (10) | 0.01980 (6) | |
Cl1 | 0.14558 (7) | 0.32943 (14) | 0.15639 (7) | 0.0358 (4) | |
Cl2 | 0.00138 (8) | 0.75644 (14) | 0.13658 (7) | 0.0381 (4) | |
Cl3 | −0.15104 (7) | 0.33055 (14) | 0.03837 (7) | 0.0326 (4) | |
Cl4 | −0.00275 (7) | 0.46106 (13) | 0.13481 (6) | 0.0285 (4) | |
Cl5 | 0.11965 (6) | 0.60874 (13) | 0.10147 (6) | 0.0260 (3) | |
Cl6 | −0.00047 (7) | 0.24526 (12) | 0.02539 (7) | 0.0279 (3) | |
Cl7 | 0.12119 (6) | 0.38933 (12) | −0.00637 (6) | 0.0250 (3) | |
W4 | 0.489027 (11) | 0.86558 (2) | 0.037684 (10) | 0.02094 (6) | |
W5 | 0.556063 (11) | 1.05107 (2) | 0.079812 (10) | 0.02201 (6) | |
W6 | 0.431115 (11) | 1.06340 (2) | 0.014804 (10) | 0.02046 (6) | |
Cl8 | 0.47681 (8) | 0.69039 (14) | 0.08869 (8) | 0.0422 (4) | |
Cl9 | 0.63153 (8) | 1.11456 (16) | 0.18417 (7) | 0.0481 (5) | |
Cl10 | 0.33976 (7) | 1.14363 (14) | 0.03380 (7) | 0.0345 (4) | |
Cl11 | 0.50170 (7) | 0.76229 (13) | −0.05435 (7) | 0.0302 (4) | |
Cl12 | 0.60829 (7) | 0.85910 (13) | 0.09760 (6) | 0.0302 (4) | |
Cl13 | 0.37024 (7) | 0.88263 (13) | −0.02667 (6) | 0.0268 (3) | |
Cl14 | 0.47682 (7) | 0.98226 (13) | 0.12583 (6) | 0.0285 (4) | |
N1 | 0.3435 (2) | 0.4729 (4) | 0.1301 (2) | 0.0263 (12) | |
C1 | 0.3147 (3) | 0.4108 (5) | 0.1725 (3) | 0.0346 (16) | |
H1A | 0.2706 | 0.4406 | 0.1625 | 0.042* | |
H1B | 0.3408 | 0.4296 | 0.2183 | 0.042* | |
C2 | 0.3107 (3) | 0.2810 (5) | 0.1656 (3) | 0.0440 (19) | |
H2A | 0.2716 | 0.2599 | 0.1277 | 0.053* | |
H2B | 0.3489 | 0.2524 | 0.1582 | 0.053* | |
C3 | 0.3080 (3) | 0.2265 (6) | 0.2260 (3) | 0.0443 (19) | |
H3A | 0.3504 | 0.2365 | 0.2620 | 0.053* | |
H3B | 0.2753 | 0.2670 | 0.2380 | 0.053* | |
C4 | 0.2917 (4) | 0.1028 (6) | 0.2190 (3) | 0.077 (3) | |
H4A | 0.2911 | 0.0736 | 0.2599 | 0.115* | |
H4B | 0.3242 | 0.0616 | 0.2081 | 0.115* | |
H4C | 0.2491 | 0.0921 | 0.1845 | 0.115* | |
C5 | 0.3004 (3) | 0.4548 (5) | 0.0597 (2) | 0.0308 (15) | |
H5A | 0.2558 | 0.4763 | 0.0541 | 0.037* | |
H5B | 0.3000 | 0.3725 | 0.0502 | 0.037* | |
C6 | 0.3182 (3) | 0.5198 (5) | 0.0089 (3) | 0.0342 (16) | |
H6A | 0.2777 | 0.5435 | −0.0266 | 0.041* | |
H6B | 0.3418 | 0.5897 | 0.0294 | 0.041* | |
C7 | 0.3593 (3) | 0.4544 (6) | −0.0207 (3) | 0.0440 (19) | |
H7A | 0.4031 | 0.4429 | 0.0129 | 0.053* | |
H7B | 0.3399 | 0.3785 | −0.0348 | 0.053* | |
C8 | 0.3649 (3) | 0.5150 (6) | −0.0775 (3) | 0.061 (2) | |
H8A | 0.3916 | 0.4700 | −0.0947 | 0.092* | |
H8B | 0.3849 | 0.5896 | −0.0636 | 0.092* | |
H8C | 0.3218 | 0.5251 | −0.1113 | 0.092* | |
C9 | 0.3488 (2) | 0.5979 (5) | 0.1488 (2) | 0.0237 (14) | |
H9A | 0.3763 | 0.6044 | 0.1954 | 0.028* | |
H9B | 0.3711 | 0.6383 | 0.1243 | 0.028* | |
C10 | 0.2854 (3) | 0.6578 (5) | 0.1369 (3) | 0.0340 (16) | |
H10A | 0.2649 | 0.6246 | 0.1652 | 0.041* | |
H10B | 0.2557 | 0.6464 | 0.0913 | 0.041* | |
C11 | 0.2962 (3) | 0.7850 (5) | 0.1507 (3) | 0.0383 (17) | |
H11A | 0.2556 | 0.8191 | 0.1504 | 0.046* | |
H11B | 0.3296 | 0.7952 | 0.1947 | 0.046* | |
C12 | 0.3168 (3) | 0.8480 (6) | 0.1033 (3) | 0.055 (2) | |
H12A | 0.3231 | 0.9285 | 0.1154 | 0.083* | |
H12B | 0.2833 | 0.8408 | 0.0597 | 0.083* | |
H12C | 0.3574 | 0.8159 | 0.1038 | 0.083* | |
C13 | 0.4105 (2) | 0.4298 (5) | 0.1412 (2) | 0.0318 (15) | |
H13A | 0.4322 | 0.4860 | 0.1233 | 0.048* | 0.555 (11) |
H13B | 0.4064 | 0.3582 | 0.1166 | 0.048* | 0.555 (11) |
H13C | 0.4247 | 0.4639 | 0.1082 | 0.048* | 0.445 (11) |
H13D | 0.4084 | 0.3464 | 0.1346 | 0.048* | 0.445 (11) |
C14 | 0.4544 (6) | 0.4072 (13) | 0.2131 (6) | 0.035 (4) | 0.555 (11) |
H14A | 0.4622 | 0.4795 | 0.2376 | 0.041* | 0.555 (11) |
H14B | 0.4323 | 0.3544 | 0.2325 | 0.041* | 0.555 (11) |
C15 | 0.5189 (7) | 0.3559 (16) | 0.2183 (13) | 0.037 (5) | 0.555 (11) |
H15A | 0.5437 | 0.3341 | 0.2639 | 0.044* | 0.555 (11) |
H15B | 0.5106 | 0.2858 | 0.1917 | 0.044* | 0.555 (11) |
C16 | 0.5591 (5) | 0.4353 (11) | 0.1964 (6) | 0.063 (5) | 0.555 (11) |
H16A | 0.5990 | 0.3970 | 0.1994 | 0.094* | 0.555 (11) |
H16B | 0.5698 | 0.5030 | 0.2241 | 0.094* | 0.555 (11) |
H16C | 0.5347 | 0.4580 | 0.1514 | 0.094* | 0.555 (11) |
C14A | 0.4620 (8) | 0.4559 (16) | 0.2091 (7) | 0.043 (5) | 0.445 (11) |
H14C | 0.4753 | 0.5366 | 0.2117 | 0.052* | 0.445 (11) |
H14D | 0.4440 | 0.4420 | 0.2427 | 0.052* | 0.445 (11) |
C15A | 0.5203 (9) | 0.378 (2) | 0.2205 (18) | 0.054 (7) | 0.445 (11) |
H15C | 0.5340 | 0.3857 | 0.1834 | 0.064* | 0.445 (11) |
H15D | 0.5566 | 0.4041 | 0.2599 | 0.064* | 0.445 (11) |
C16A | 0.5064 (9) | 0.2560 (14) | 0.2284 (8) | 0.073 (6) | 0.445 (11) |
H16D | 0.5452 | 0.2105 | 0.2356 | 0.109* | 0.445 (11) |
H16E | 0.4712 | 0.2295 | 0.1892 | 0.109* | 0.445 (11) |
H16F | 0.4937 | 0.2480 | 0.2657 | 0.109* | 0.445 (11) |
N2 | 0.1419 (2) | 0.5124 (4) | 0.3572 (2) | 0.0241 (11) | |
C17 | 0.1525 (3) | 0.3975 (5) | 0.3331 (3) | 0.0309 (15) | |
H17A | 0.1364 | 0.4005 | 0.2852 | 0.037* | |
H17B | 0.1258 | 0.3414 | 0.3447 | 0.037* | |
C18 | 0.2211 (3) | 0.3546 (5) | 0.3580 (3) | 0.0346 (16) | |
H18A | 0.2409 | 0.3635 | 0.4056 | 0.041* | |
H18B | 0.2468 | 0.3997 | 0.3388 | 0.041* | |
C19 | 0.2219 (3) | 0.2286 (5) | 0.3400 (3) | 0.0366 (17) | |
H19A | 0.1983 | 0.2200 | 0.2927 | 0.044* | |
H19B | 0.2672 | 0.2050 | 0.3504 | 0.044* | |
C20 | 0.1918 (3) | 0.1497 (6) | 0.3747 (3) | 0.049 (2) | |
H20A | 0.1937 | 0.0713 | 0.3607 | 0.073* | |
H20B | 0.1467 | 0.1715 | 0.3641 | 0.073* | |
H20C | 0.2158 | 0.1556 | 0.4216 | 0.073* | |
C21 | 0.1640 (3) | 0.5136 (5) | 0.4299 (2) | 0.0301 (15) | |
H21A | 0.1532 | 0.5888 | 0.4430 | 0.036* | |
H21B | 0.2117 | 0.5065 | 0.4484 | 0.036* | |
C22 | 0.1363 (3) | 0.4224 (6) | 0.4605 (3) | 0.0450 (19) | |
H22A | 0.1490 | 0.3464 | 0.4502 | 0.054* | |
H22B | 0.0886 | 0.4269 | 0.4418 | 0.054* | |
C23 | 0.1604 (3) | 0.4363 (6) | 0.5339 (3) | 0.0391 (17) | |
H23A | 0.1496 | 0.3667 | 0.5527 | 0.047* | |
H23B | 0.2080 | 0.4438 | 0.5515 | 0.047* | |
C24 | 0.1322 (4) | 0.5374 (6) | 0.5550 (3) | 0.057 (2) | |
H24A | 0.1499 | 0.5418 | 0.6024 | 0.086* | |
H24B | 0.0851 | 0.5295 | 0.5391 | 0.086* | |
H24C | 0.1431 | 0.6069 | 0.5372 | 0.086* | |
C25 | 0.0688 (3) | 0.5328 (5) | 0.3244 (3) | 0.0324 (16) | |
H25A | 0.0563 | 0.5248 | 0.2771 | 0.039* | |
H25B | 0.0465 | 0.4718 | 0.3385 | 0.039* | |
C26 | 0.0437 (3) | 0.6457 (5) | 0.3371 (3) | 0.0404 (17) | |
H26A | 0.0675 | 0.7084 | 0.3265 | 0.048* | |
H26B | 0.0504 | 0.6517 | 0.3835 | 0.048* | |
C27 | −0.0285 (3) | 0.6554 (6) | 0.2953 (3) | 0.0470 (19) | |
H27A | −0.0434 | 0.7331 | 0.2998 | 0.056* | |
H27B | −0.0349 | 0.6442 | 0.2493 | 0.056* | |
C28 | −0.0691 (3) | 0.5708 (6) | 0.3132 (4) | 0.071 (3) | |
H28A | −0.1146 | 0.5807 | 0.2848 | 0.107* | |
H28B | −0.0641 | 0.5827 | 0.3584 | 0.107* | |
H28C | −0.0552 | 0.4935 | 0.3082 | 0.107* | |
C29 | 0.1799 (3) | 0.6055 (5) | 0.3419 (3) | 0.0323 (16) | |
H29A | 0.2264 | 0.5863 | 0.3626 | 0.039* | |
H29B | 0.1730 | 0.6766 | 0.3621 | 0.039* | |
C30 | 0.1643 (3) | 0.6291 (6) | 0.2702 (3) | 0.0403 (17) | |
H30A | 0.1172 | 0.6416 | 0.2477 | 0.048* | |
H30B | 0.1765 | 0.5624 | 0.2502 | 0.048* | |
C31 | 0.2013 (3) | 0.7347 (6) | 0.2623 (3) | 0.0434 (18) | |
H31A | 0.2481 | 0.7215 | 0.2863 | 0.052* | |
H31B | 0.1941 | 0.7427 | 0.2159 | 0.052* | |
C32 | 0.1839 (4) | 0.8414 (6) | 0.2845 (4) | 0.081 (3) | |
H32A | 0.2101 | 0.9031 | 0.2777 | 0.121* | |
H32B | 0.1918 | 0.8357 | 0.3307 | 0.121* | |
H32C | 0.1380 | 0.8573 | 0.2599 | 0.121* |
U11 | U22 | U33 | U12 | U13 | U23 | |
W1 | 0.01714 (12) | 0.02436 (14) | 0.01831 (12) | 0.00064 (11) | 0.00554 (10) | 0.00179 (10) |
W2 | 0.01866 (13) | 0.02461 (15) | 0.01960 (12) | 0.00046 (11) | 0.00745 (10) | −0.00325 (10) |
W3 | 0.01668 (12) | 0.02333 (14) | 0.01932 (12) | −0.00061 (11) | 0.00678 (10) | 0.00118 (10) |
Cl1 | 0.0265 (8) | 0.0449 (11) | 0.0303 (8) | 0.0060 (8) | 0.0043 (7) | 0.0122 (8) |
Cl2 | 0.0381 (10) | 0.0380 (10) | 0.0342 (8) | 0.0058 (8) | 0.0092 (7) | −0.0147 (8) |
Cl3 | 0.0247 (8) | 0.0392 (10) | 0.0361 (8) | −0.0026 (7) | 0.0140 (7) | 0.0081 (8) |
Cl4 | 0.0303 (8) | 0.0378 (10) | 0.0192 (7) | −0.0012 (7) | 0.0113 (6) | 0.0020 (7) |
Cl5 | 0.0211 (7) | 0.0312 (9) | 0.0221 (7) | −0.0052 (7) | 0.0042 (6) | −0.0048 (7) |
Cl6 | 0.0260 (8) | 0.0225 (8) | 0.0334 (8) | 0.0009 (7) | 0.0094 (7) | 0.0037 (7) |
Cl7 | 0.0202 (7) | 0.0283 (9) | 0.0263 (7) | 0.0042 (6) | 0.0085 (6) | −0.0007 (7) |
W4 | 0.02044 (13) | 0.02468 (14) | 0.01888 (12) | −0.00077 (11) | 0.00879 (10) | 0.00346 (11) |
W5 | 0.02025 (13) | 0.03016 (16) | 0.01508 (11) | −0.00390 (11) | 0.00609 (10) | −0.00129 (11) |
W6 | 0.01891 (12) | 0.02552 (15) | 0.01830 (12) | −0.00058 (11) | 0.00859 (10) | 0.00120 (11) |
Cl8 | 0.0431 (10) | 0.0356 (10) | 0.0545 (10) | 0.0012 (8) | 0.0260 (9) | 0.0178 (9) |
Cl9 | 0.0441 (10) | 0.0721 (14) | 0.0198 (8) | −0.0226 (10) | 0.0029 (7) | −0.0096 (9) |
Cl10 | 0.0320 (9) | 0.0382 (10) | 0.0400 (9) | 0.0054 (8) | 0.0213 (7) | −0.0007 (8) |
Cl11 | 0.0358 (9) | 0.0246 (9) | 0.0345 (8) | −0.0054 (7) | 0.0182 (7) | −0.0076 (7) |
Cl12 | 0.0241 (8) | 0.0386 (10) | 0.0263 (7) | 0.0052 (7) | 0.0075 (6) | 0.0132 (7) |
Cl13 | 0.0221 (8) | 0.0335 (9) | 0.0258 (7) | −0.0069 (7) | 0.0105 (6) | −0.0020 (7) |
Cl14 | 0.0297 (8) | 0.0406 (10) | 0.0168 (7) | −0.0040 (7) | 0.0108 (6) | −0.0004 (7) |
N1 | 0.021 (3) | 0.037 (3) | 0.025 (3) | −0.002 (2) | 0.014 (2) | −0.005 (2) |
C1 | 0.036 (4) | 0.046 (5) | 0.030 (3) | −0.011 (3) | 0.021 (3) | −0.006 (3) |
C2 | 0.055 (5) | 0.049 (5) | 0.039 (4) | −0.006 (4) | 0.031 (4) | −0.002 (4) |
C3 | 0.051 (5) | 0.052 (5) | 0.037 (4) | 0.001 (4) | 0.025 (3) | 0.004 (4) |
C4 | 0.139 (9) | 0.046 (6) | 0.058 (5) | −0.002 (6) | 0.051 (6) | 0.000 (4) |
C5 | 0.024 (3) | 0.042 (4) | 0.023 (3) | −0.005 (3) | 0.006 (3) | −0.010 (3) |
C6 | 0.026 (4) | 0.046 (5) | 0.025 (3) | −0.001 (3) | 0.004 (3) | 0.001 (3) |
C7 | 0.049 (4) | 0.061 (5) | 0.028 (3) | 0.003 (4) | 0.021 (3) | −0.002 (4) |
C8 | 0.073 (6) | 0.080 (7) | 0.036 (4) | −0.008 (5) | 0.028 (4) | −0.002 (4) |
C9 | 0.023 (3) | 0.030 (4) | 0.020 (3) | −0.002 (3) | 0.010 (3) | −0.008 (3) |
C10 | 0.028 (4) | 0.045 (5) | 0.032 (3) | −0.005 (3) | 0.014 (3) | −0.003 (3) |
C11 | 0.038 (4) | 0.039 (4) | 0.047 (4) | −0.001 (3) | 0.027 (3) | 0.005 (3) |
C12 | 0.062 (5) | 0.048 (5) | 0.071 (5) | 0.007 (4) | 0.044 (4) | 0.003 (4) |
C13 | 0.025 (3) | 0.044 (4) | 0.026 (3) | 0.005 (3) | 0.009 (3) | −0.005 (3) |
C14 | 0.034 (7) | 0.041 (10) | 0.027 (6) | 0.008 (7) | 0.010 (5) | 0.003 (6) |
C15 | 0.038 (7) | 0.051 (11) | 0.022 (8) | 0.011 (7) | 0.013 (6) | −0.002 (8) |
C16 | 0.024 (7) | 0.090 (12) | 0.063 (9) | 0.011 (7) | 0.004 (6) | 0.038 (8) |
C14A | 0.035 (9) | 0.057 (12) | 0.034 (8) | 0.008 (8) | 0.010 (6) | −0.001 (9) |
C15A | 0.044 (11) | 0.079 (13) | 0.036 (13) | 0.021 (10) | 0.012 (9) | 0.005 (12) |
C16A | 0.083 (15) | 0.069 (11) | 0.049 (10) | 0.041 (11) | 0.005 (10) | 0.009 (11) |
N2 | 0.024 (3) | 0.029 (3) | 0.018 (2) | −0.001 (2) | 0.007 (2) | −0.002 (2) |
C17 | 0.028 (4) | 0.034 (4) | 0.028 (3) | 0.001 (3) | 0.007 (3) | −0.002 (3) |
C18 | 0.024 (3) | 0.035 (4) | 0.039 (4) | 0.005 (3) | 0.005 (3) | −0.001 (3) |
C19 | 0.037 (4) | 0.041 (5) | 0.032 (3) | 0.010 (3) | 0.013 (3) | 0.004 (3) |
C20 | 0.052 (5) | 0.042 (5) | 0.056 (4) | 0.007 (4) | 0.025 (4) | 0.012 (4) |
C21 | 0.037 (4) | 0.030 (4) | 0.016 (3) | −0.006 (3) | 0.002 (3) | −0.001 (3) |
C22 | 0.068 (5) | 0.043 (5) | 0.027 (3) | −0.010 (4) | 0.021 (3) | 0.005 (3) |
C23 | 0.043 (4) | 0.042 (5) | 0.036 (4) | 0.001 (4) | 0.019 (3) | 0.011 (3) |
C24 | 0.079 (6) | 0.058 (6) | 0.045 (4) | 0.011 (5) | 0.035 (4) | 0.006 (4) |
C25 | 0.033 (4) | 0.036 (4) | 0.031 (3) | 0.005 (3) | 0.015 (3) | 0.001 (3) |
C26 | 0.045 (4) | 0.039 (4) | 0.041 (4) | 0.004 (4) | 0.021 (3) | −0.001 (3) |
C27 | 0.042 (4) | 0.036 (5) | 0.061 (5) | 0.014 (4) | 0.018 (4) | 0.005 (4) |
C28 | 0.042 (5) | 0.059 (6) | 0.106 (7) | −0.001 (4) | 0.020 (5) | −0.003 (5) |
C29 | 0.031 (4) | 0.037 (4) | 0.026 (3) | −0.006 (3) | 0.008 (3) | −0.002 (3) |
C30 | 0.049 (4) | 0.044 (5) | 0.033 (4) | −0.003 (4) | 0.021 (3) | 0.000 (3) |
C31 | 0.047 (4) | 0.053 (5) | 0.036 (4) | −0.010 (4) | 0.022 (3) | 0.006 (4) |
C32 | 0.122 (9) | 0.044 (6) | 0.102 (7) | −0.003 (6) | 0.071 (6) | 0.003 (5) |
W1—W2 | 2.6056 (3) | C12—H12B | 0.9800 |
W1—W2i | 2.6228 (3) | C12—H12C | 0.9800 |
W1—W3 | 2.6191 (3) | C13—N1 | 1.511 (6) |
W1—W3i | 2.6101 (3) | C13—C14 | 1.553 (11) |
W2—W3 | 2.6131 (3) | C13—C14A | 1.547 (12) |
W2—W3i | 2.6239 (3) | C13—H13A | 0.9900 |
W1—Cl1 | 2.4177 (14) | C13—H13B | 0.9900 |
W2—Cl2 | 2.4289 (14) | C13—H13C | 0.9900 |
W3—Cl3 | 2.4285 (14) | C13—H13D | 0.9900 |
W1—Cl4 | 2.5012 (14) | C14—C15 | 1.528 (12) |
W1—Cl5 | 2.4961 (14) | C14—H14A | 0.9900 |
W1—Cl6 | 2.4980 (15) | C14—H14B | 0.9900 |
W1—Cl7 | 2.4962 (14) | C14A—C15A | 1.531 (13) |
W2—Cl4 | 2.5067 (14) | C14A—H14C | 0.9900 |
W2—Cl5 | 2.4905 (14) | C14A—H14D | 0.9900 |
W2—Cl6i | 2.4864 (14) | C15—C16 | 1.500 (14) |
W2—Cl7i | 2.4967 (13) | C15—H15A | 0.9900 |
W3—Cl4 | 2.4965 (13) | C15—H15B | 0.9900 |
W3—Cl5i | 2.4888 (13) | C15A—C16A | 1.497 (16) |
W3—Cl6 | 2.5088 (15) | C15A—H15C | 0.9900 |
W3—Cl7i | 2.5020 (14) | C15A—H15D | 0.9900 |
W4—W5 | 2.6113 (3) | C16—H16A | 0.9800 |
W4—W5ii | 2.6157 (3) | C16—H16B | 0.9800 |
W4—W6 | 2.6169 (3) | C16—H16C | 0.9800 |
W4—W6ii | 2.6170 (3) | C16A—H16D | 0.9800 |
W5—W6 | 2.6186 (3) | C16A—H16E | 0.9800 |
W5—W6ii | 2.6096 (3) | C16A—H16F | 0.9800 |
W4—Cl8 | 2.4187 (16) | C17—N2 | 1.505 (7) |
W5—Cl9 | 2.4173 (14) | C17—C18 | 1.507 (7) |
W6—Cl10 | 2.4297 (15) | C17—H17A | 0.9900 |
W4—Cl11 | 2.4928 (14) | C17—H17B | 0.9900 |
W4—Cl12 | 2.4903 (14) | C18—C19 | 1.537 (8) |
W4—Cl13 | 2.5029 (14) | C18—H18A | 0.9900 |
W4—Cl14 | 2.4965 (14) | C18—H18B | 0.9900 |
W5—Cl11ii | 2.5003 (16) | C19—C20 | 1.518 (8) |
W5—Cl12 | 2.5033 (15) | C19—H19A | 0.9900 |
W5—Cl13ii | 2.4932 (14) | C19—H19B | 0.9900 |
W5—Cl14 | 2.4967 (14) | C20—H20A | 0.9800 |
W6—Cl11ii | 2.4964 (15) | C20—H20B | 0.9800 |
W6—Cl12ii | 2.4936 (13) | C20—H20C | 0.9800 |
W6—Cl13 | 2.5046 (14) | C21—N2 | 1.506 (6) |
W6—Cl14 | 2.4836 (13) | C21—C22 | 1.525 (8) |
C1—N1 | 1.518 (6) | C21—H21A | 0.9900 |
C1—C2 | 1.533 (7) | C21—H21B | 0.9900 |
C1—H1A | 0.9900 | C22—C23 | 1.526 (7) |
C1—H1B | 0.9900 | C22—H22A | 0.9900 |
C2—C3 | 1.514 (7) | C22—H22B | 0.9900 |
C2—H2A | 0.9900 | C23—C24 | 1.503 (8) |
C2—H2B | 0.9900 | C23—H23A | 0.9900 |
C3—C4 | 1.493 (8) | C23—H23B | 0.9900 |
C3—H3A | 0.9900 | C24—H24A | 0.9800 |
C3—H3B | 0.9900 | C24—H24B | 0.9800 |
C4—H4A | 0.9800 | C24—H24C | 0.9800 |
C4—H4B | 0.9800 | C25—N2 | 1.537 (7) |
C4—H4C | 0.9800 | C25—C26 | 1.509 (8) |
C5—N1 | 1.514 (6) | C25—H25A | 0.9900 |
C5—C6 | 1.539 (7) | C25—H25B | 0.9900 |
C5—H5A | 0.9900 | C26—C27 | 1.531 (8) |
C5—H5B | 0.9900 | C26—H26A | 0.9900 |
C6—C7 | 1.528 (7) | C26—H26B | 0.9900 |
C6—H6A | 0.9900 | C27—C28 | 1.500 (9) |
C6—H6B | 0.9900 | C27—H27A | 0.9900 |
C7—C8 | 1.501 (7) | C27—H27B | 0.9900 |
C7—H7A | 0.9900 | C28—H28A | 0.9800 |
C7—H7B | 0.9900 | C28—H28B | 0.9800 |
C8—H8A | 0.9800 | C28—H28C | 0.9800 |
C8—H8B | 0.9800 | C29—N2 | 1.503 (7) |
C8—H8C | 0.9800 | C29—C30 | 1.527 (7) |
C9—N1 | 1.521 (6) | C29—H29A | 0.9900 |
C9—C10 | 1.515 (7) | C29—H29B | 0.9900 |
C9—H9A | 0.9900 | C30—C31 | 1.540 (8) |
C9—H9B | 0.9900 | C30—H30A | 0.9900 |
C10—C11 | 1.528 (7) | C30—H30B | 0.9900 |
C10—H10A | 0.9900 | C31—C32 | 1.455 (9) |
C10—H10B | 0.9900 | C31—H31A | 0.9900 |
C11—C12 | 1.500 (7) | C31—H31B | 0.9900 |
C11—H11A | 0.9900 | C32—H32A | 0.9800 |
C11—H11B | 0.9900 | C32—H32B | 0.9800 |
C12—H12A | 0.9800 | C32—H32C | 0.9800 |
Cl1—W1—Cl5 | 90.05 (5) | W6—Cl14—W4 | 63.40 (3) |
Cl1—W1—Cl7 | 91.89 (5) | W6—Cl14—W5 | 63.44 (3) |
Cl5—W1—Cl7 | 90.22 (5) | W4—Cl14—W5 | 63.06 (3) |
Cl1—W1—Cl6 | 94.07 (5) | C13—N1—C5 | 109.0 (4) |
Cl5—W1—Cl6 | 175.82 (5) | C13—N1—C1 | 111.4 (4) |
Cl7—W1—Cl6 | 88.96 (5) | C5—N1—C1 | 108.9 (4) |
Cl1—W1—Cl4 | 91.53 (5) | C13—N1—C9 | 108.1 (4) |
Cl5—W1—Cl4 | 90.58 (5) | C5—N1—C9 | 111.9 (4) |
Cl7—W1—Cl4 | 176.49 (4) | C1—N1—C9 | 107.5 (4) |
Cl6—W1—Cl4 | 90.00 (5) | N1—C1—C2 | 116.1 (5) |
Cl1—W1—W2 | 133.27 (4) | N1—C1—H1A | 108.3 |
Cl5—W1—W2 | 58.39 (3) | C2—C1—H1A | 108.3 |
Cl7—W1—W2 | 119.02 (3) | N1—C1—H1B | 108.3 |
Cl6—W1—W2 | 118.65 (3) | C2—C1—H1B | 108.3 |
Cl4—W1—W2 | 58.75 (3) | H1A—C1—H1B | 107.4 |
Cl1—W1—W3i | 133.53 (4) | C3—C2—C1 | 110.7 (5) |
Cl5—W1—W3i | 58.29 (3) | C3—C2—H2A | 109.5 |
Cl7—W1—W3i | 58.63 (3) | C1—C2—H2A | 109.5 |
Cl6—W1—W3i | 117.95 (3) | C3—C2—H2B | 109.5 |
Cl4—W1—W3i | 119.14 (4) | C1—C2—H2B | 109.5 |
W2—W1—W3i | 60.406 (9) | H2A—C2—H2B | 108.1 |
Cl1—W1—W3 | 136.25 (4) | C4—C3—C2 | 114.2 (5) |
Cl5—W1—W3 | 118.39 (3) | C4—C3—H3A | 108.7 |
Cl7—W1—W3 | 118.39 (3) | C2—C3—H3A | 108.7 |
Cl6—W1—W3 | 58.66 (3) | C4—C3—H3B | 108.7 |
Cl4—W1—W3 | 58.31 (3) | C2—C3—H3B | 108.7 |
W2—W1—W3 | 60.018 (9) | H3A—C3—H3B | 107.6 |
W3i—W1—W3 | 90.186 (10) | C3—C4—H4A | 109.5 |
Cl1—W1—W2i | 136.53 (4) | C3—C4—H4B | 109.5 |
Cl5—W1—W2i | 118.19 (3) | H4A—C4—H4B | 109.5 |
Cl7—W1—W2i | 58.32 (3) | C3—C4—H4C | 109.5 |
Cl6—W1—W2i | 58.04 (3) | H4A—C4—H4C | 109.5 |
Cl4—W1—W2i | 118.38 (3) | H4B—C4—H4C | 109.5 |
W2—W1—W2i | 90.170 (10) | N1—C5—C6 | 116.9 (4) |
W3i—W1—W2i | 59.914 (9) | N1—C5—H5A | 108.1 |
W3—W1—W2i | 60.073 (8) | C6—C5—H5A | 108.1 |
Cl2—W2—Cl6i | 94.38 (5) | N1—C5—H5B | 108.1 |
Cl2—W2—Cl5 | 90.48 (5) | C6—C5—H5B | 108.1 |
Cl6i—W2—Cl5 | 89.77 (5) | H5A—C5—H5B | 107.3 |
Cl2—W2—Cl7i | 93.37 (5) | C7—C6—C5 | 115.8 (5) |
Cl6i—W2—Cl7i | 89.20 (5) | C7—C6—H6A | 108.3 |
Cl5—W2—Cl7i | 176.08 (5) | C5—C6—H6A | 108.3 |
Cl2—W2—Cl4 | 89.48 (5) | C7—C6—H6B | 108.3 |
Cl6i—W2—Cl4 | 176.12 (5) | C5—C6—H6B | 108.3 |
Cl5—W2—Cl4 | 90.58 (5) | H6A—C6—H6B | 107.4 |
Cl7i—W2—Cl4 | 90.19 (5) | C8—C7—C6 | 112.5 (6) |
Cl2—W2—W1 | 132.14 (4) | C8—C7—H7A | 109.1 |
Cl6i—W2—W1 | 118.60 (4) | C6—C7—H7A | 109.1 |
Cl5—W2—W1 | 58.60 (3) | C8—C7—H7B | 109.1 |
Cl7i—W2—W1 | 118.81 (3) | C6—C7—H7B | 109.1 |
Cl4—W2—W1 | 58.54 (3) | H7A—C7—H7B | 107.8 |
Cl2—W2—W3 | 134.11 (4) | C7—C8—H8A | 109.5 |
Cl6i—W2—W3 | 118.27 (3) | C7—C8—H8B | 109.5 |
Cl5—W2—W3 | 118.83 (4) | H8A—C8—H8B | 109.5 |
Cl7i—W2—W3 | 58.58 (3) | C7—C8—H8C | 109.5 |
Cl4—W2—W3 | 58.32 (3) | H8A—C8—H8C | 109.5 |
W1—W2—W3 | 60.247 (9) | H8B—C8—H8C | 109.5 |
Cl2—W2—W1i | 138.02 (4) | C10—C9—N1 | 115.6 (4) |
Cl6i—W2—W1i | 58.47 (3) | C10—C9—H9A | 108.4 |
Cl5—W2—W1i | 118.05 (3) | N1—C9—H9A | 108.4 |
Cl7i—W2—W1i | 58.30 (3) | C10—C9—H9B | 108.4 |
Cl4—W2—W1i | 118.11 (3) | N1—C9—H9B | 108.4 |
W1—W2—W1i | 89.829 (10) | H9A—C9—H9B | 107.5 |
W3—W2—W1i | 59.802 (9) | C9—C10—C11 | 110.7 (5) |
Cl2—W2—W3i | 135.74 (4) | C9—C10—H10A | 109.5 |
Cl6i—W2—W3i | 58.73 (3) | C11—C10—H10A | 109.5 |
Cl5—W2—W3i | 58.17 (3) | C9—C10—H10B | 109.5 |
Cl7i—W2—W3i | 118.19 (3) | C11—C10—H10B | 109.5 |
Cl4—W2—W3i | 118.40 (3) | H10A—C10—H10B | 108.1 |
W1—W2—W3i | 59.881 (9) | C12—C11—C10 | 114.1 (5) |
W3—W2—W3i | 90.016 (10) | C12—C11—H11A | 108.7 |
W1i—W2—W3i | 59.891 (8) | C10—C11—H11A | 108.7 |
Cl3—W3—Cl5i | 91.46 (5) | C12—C11—H11B | 108.7 |
Cl3—W3—Cl4 | 92.07 (5) | C10—C11—H11B | 108.7 |
Cl5i—W3—Cl4 | 176.43 (5) | H11A—C11—H11B | 107.6 |
Cl3—W3—Cl7i | 90.05 (5) | C11—C12—H12A | 109.5 |
Cl5i—W3—Cl7i | 90.25 (5) | C11—C12—H12B | 109.5 |
Cl4—W3—Cl7i | 90.31 (5) | H12A—C12—H12B | 109.5 |
Cl3—W3—Cl6 | 94.62 (5) | C11—C12—H12C | 109.5 |
Cl5i—W3—Cl6 | 89.29 (5) | H12A—C12—H12C | 109.5 |
Cl4—W3—Cl6 | 89.86 (5) | H12B—C12—H12C | 109.5 |
Cl7i—W3—Cl6 | 175.31 (5) | N1—C13—C14A | 114.7 (8) |
Cl3—W3—W1i | 133.26 (4) | N1—C13—C14 | 115.2 (7) |
Cl5i—W3—W1i | 58.56 (3) | N1—C13—H13A | 108.5 |
Cl4—W3—W1i | 118.97 (4) | C14A—C13—H13A | 88.1 |
Cl7i—W3—W1i | 58.41 (3) | C14—C13—H13A | 108.5 |
Cl6—W3—W1i | 117.60 (3) | N1—C13—H13B | 108.5 |
Cl3—W3—W2 | 133.75 (4) | C14A—C13—H13B | 126.2 |
Cl5i—W3—W2 | 118.83 (3) | C14—C13—H13B | 108.5 |
Cl4—W3—W2 | 58.71 (3) | H13A—C13—H13B | 107.5 |
Cl7i—W3—W2 | 58.39 (3) | N1—C13—H13C | 108.6 |
Cl6—W3—W2 | 117.97 (3) | C14A—C13—H13C | 108.6 |
W1i—W3—W2 | 60.284 (9) | C14—C13—H13C | 125.6 |
Cl3—W3—W1 | 136.91 (4) | H13B—C13—H13C | 85.4 |
Cl5i—W3—W1 | 118.26 (3) | N1—C13—H13D | 108.6 |
Cl4—W3—W1 | 58.48 (3) | C14A—C13—H13D | 108.6 |
Cl7i—W3—W1 | 118.10 (3) | C14—C13—H13D | 87.7 |
Cl6—W3—W1 | 58.26 (3) | H13A—C13—H13D | 127.2 |
W1i—W3—W1 | 89.812 (10) | H13C—C13—H13D | 107.6 |
W2—W3—W1 | 59.736 (9) | C15—C14—C13 | 110.7 (12) |
Cl3—W3—W2i | 136.21 (4) | C15—C14—H14A | 109.5 |
Cl5i—W3—W2i | 58.23 (3) | C13—C14—H14A | 109.5 |
Cl4—W3—W2i | 118.51 (3) | C15—C14—H14B | 109.5 |
Cl7i—W3—W2i | 118.10 (3) | C13—C14—H14B | 109.5 |
Cl6—W3—W2i | 57.90 (3) | H14A—C14—H14B | 108.1 |
W1i—W3—W2i | 59.711 (9) | C16—C15—C14 | 113.2 (12) |
W2—W3—W2i | 89.984 (10) | C16—C15—H15A | 108.9 |
W1—W3—W2i | 60.033 (8) | C14—C15—H15A | 108.9 |
W3—Cl4—W1 | 63.21 (3) | C16—C15—H15B | 108.9 |
W3—Cl4—W2 | 62.97 (3) | C14—C15—H15B | 108.9 |
W1—Cl4—W2 | 62.70 (3) | H15A—C15—H15B | 107.8 |
W3i—Cl5—W2 | 63.60 (3) | C15—C16—H16A | 109.5 |
W3i—Cl5—W1 | 63.15 (3) | C15—C16—H16B | 109.5 |
W2—Cl5—W1 | 63.00 (3) | H16A—C16—H16B | 109.5 |
W2i—Cl6—W1 | 63.50 (4) | C15—C16—H16C | 109.5 |
W2i—Cl6—W3 | 63.37 (4) | H16A—C16—H16C | 109.5 |
W1—Cl6—W3 | 63.08 (4) | H16B—C16—H16C | 109.5 |
W1—Cl7—W2i | 63.37 (3) | C15A—C14A—C13 | 108.3 (15) |
W1—Cl7—W3i | 62.96 (3) | C15A—C14A—H14C | 110.0 |
W2i—Cl7—W3i | 63.03 (3) | C13—C14A—H14C | 110.0 |
Cl8—W4—Cl12 | 90.62 (5) | C15A—C14A—H14D | 110.0 |
Cl8—W4—Cl11 | 92.35 (5) | C13—C14A—H14D | 110.0 |
Cl12—W4—Cl11 | 89.63 (5) | H14C—C14A—H14D | 108.4 |
Cl8—W4—Cl14 | 91.82 (5) | C16A—C15A—C14A | 113.0 (15) |
Cl12—W4—Cl14 | 90.54 (5) | C16A—C15A—H15C | 109.0 |
Cl11—W4—Cl14 | 175.82 (5) | C14A—C15A—H15C | 109.0 |
Cl8—W4—Cl13 | 93.04 (5) | C16A—C15A—H15D | 109.0 |
Cl12—W4—Cl13 | 176.30 (5) | C14A—C15A—H15D | 109.0 |
Cl11—W4—Cl13 | 89.69 (5) | H15C—C15A—H15D | 107.8 |
Cl14—W4—Cl13 | 89.88 (5) | C15A—C16A—H16D | 109.5 |
Cl8—W4—W5 | 133.96 (4) | C15A—C16A—H16E | 109.5 |
Cl12—W4—W5 | 58.71 (4) | H16D—C16A—H16E | 109.5 |
Cl11—W4—W5 | 118.30 (4) | C15A—C16A—H16F | 109.5 |
Cl14—W4—W5 | 58.47 (3) | H16D—C16A—H16F | 109.5 |
Cl13—W4—W5 | 118.62 (4) | H16E—C16A—H16F | 109.5 |
Cl8—W4—W5ii | 136.16 (4) | C29—N2—C17 | 113.2 (4) |
Cl12—W4—W5ii | 118.44 (3) | C29—N2—C21 | 104.8 (4) |
Cl11—W4—W5ii | 58.55 (4) | C17—N2—C21 | 111.2 (4) |
Cl14—W4—W5ii | 117.88 (3) | C29—N2—C25 | 111.7 (4) |
Cl13—W4—W5ii | 58.25 (3) | C17—N2—C25 | 104.7 (4) |
W5—W4—W5ii | 89.878 (10) | C21—N2—C25 | 111.4 (4) |
Cl8—W4—W6 | 135.48 (4) | N2—C17—C18 | 116.4 (5) |
Cl12—W4—W6 | 118.81 (4) | N2—C17—H17A | 108.2 |
Cl11—W4—W6 | 118.37 (4) | C18—C17—H17A | 108.2 |
Cl14—W4—W6 | 58.06 (3) | N2—C17—H17B | 108.2 |
Cl13—W4—W6 | 58.52 (4) | C18—C17—H17B | 108.2 |
W5—W4—W6 | 60.115 (9) | H17A—C17—H17B | 107.3 |
W5ii—W4—W6 | 59.833 (9) | C17—C18—C19 | 109.7 (5) |
Cl8—W4—W6ii | 134.48 (4) | C17—C18—H18A | 109.7 |
Cl12—W4—W6ii | 58.39 (3) | C19—C18—H18A | 109.7 |
Cl11—W4—W6ii | 58.43 (3) | C17—C18—H18B | 109.7 |
Cl14—W4—W6ii | 118.33 (3) | C19—C18—H18B | 109.7 |
Cl13—W4—W6ii | 118.30 (3) | H18A—C18—H18B | 108.2 |
W5—W4—W6ii | 59.885 (9) | C20—C19—C18 | 113.9 (5) |
W5ii—W4—W6ii | 60.059 (8) | C20—C19—H19A | 108.8 |
W6—W4—W6ii | 90.028 (10) | C18—C19—H19A | 108.8 |
Cl9—W5—Cl13ii | 90.88 (5) | C20—C19—H19B | 108.8 |
Cl9—W5—Cl14 | 92.82 (5) | C18—C19—H19B | 108.8 |
Cl13ii—W5—Cl14 | 176.26 (4) | H19A—C19—H19B | 107.7 |
Cl9—W5—Cl11ii | 93.40 (6) | C19—C20—H20A | 109.5 |
Cl13ii—W5—Cl11ii | 89.73 (5) | C19—C20—H20B | 109.5 |
Cl14—W5—Cl11ii | 89.52 (5) | H20A—C20—H20B | 109.5 |
Cl9—W5—Cl12 | 90.72 (6) | C19—C20—H20C | 109.5 |
Cl13ii—W5—Cl12 | 90.25 (5) | H20A—C20—H20C | 109.5 |
Cl14—W5—Cl12 | 90.23 (5) | H20B—C20—H20C | 109.5 |
Cl11ii—W5—Cl12 | 175.88 (5) | N2—C21—C22 | 117.0 (5) |
Cl9—W5—W6ii | 133.42 (5) | N2—C21—H21A | 108.1 |
Cl13ii—W5—W6ii | 58.73 (3) | C22—C21—H21A | 108.1 |
Cl14—W5—W6ii | 118.61 (3) | N2—C21—H21B | 108.1 |
Cl11ii—W5—W6ii | 118.36 (3) | C22—C21—H21B | 108.1 |
Cl12—W5—W6ii | 58.33 (3) | H21A—C21—H21B | 107.3 |
Cl9—W5—W4 | 134.44 (4) | C21—C22—C23 | 111.6 (5) |
Cl13ii—W5—W4 | 118.89 (3) | C21—C22—H22A | 109.3 |
Cl14—W5—W4 | 58.46 (3) | C23—C22—H22A | 109.3 |
Cl11ii—W5—W4 | 118.35 (3) | C21—C22—H22B | 109.3 |
Cl12—W5—W4 | 58.23 (3) | C23—C22—H22B | 109.3 |
W6ii—W5—W4 | 60.165 (9) | H22A—C22—H22B | 108.0 |
Cl9—W5—W4ii | 135.40 (4) | C24—C23—C22 | 113.7 (6) |
Cl13ii—W5—W4ii | 58.61 (3) | C24—C23—H23A | 108.8 |
Cl14—W5—W4ii | 118.02 (3) | C22—C23—H23A | 108.8 |
Cl11ii—W5—W4ii | 58.27 (3) | C24—C23—H23B | 108.8 |
Cl12—W5—W4ii | 118.42 (3) | C22—C23—H23B | 108.8 |
W6ii—W5—W4ii | 60.107 (9) | H23A—C23—H23B | 107.7 |
W4—W5—W4ii | 90.121 (10) | C23—C24—H24A | 109.5 |
Cl9—W5—W6 | 136.42 (5) | C23—C24—H24B | 109.5 |
Cl13ii—W5—W6 | 118.60 (3) | H24A—C24—H24B | 109.5 |
Cl14—W5—W6 | 58.03 (3) | C23—C24—H24C | 109.5 |
Cl11ii—W5—W6 | 58.32 (3) | H24A—C24—H24C | 109.5 |
Cl12—W5—W6 | 118.26 (3) | H24B—C24—H24C | 109.5 |
W6ii—W5—W6 | 90.151 (10) | C26—C25—N2 | 117.0 (5) |
W4—W5—W6 | 60.048 (9) | C26—C25—H25A | 108.1 |
W4ii—W5—W6 | 59.994 (8) | N2—C25—H25A | 108.1 |
Cl10—W6—Cl14 | 91.72 (5) | C26—C25—H25B | 108.1 |
Cl10—W6—Cl12ii | 91.95 (5) | N2—C25—H25B | 108.1 |
Cl14—W6—Cl12ii | 176.30 (5) | H25A—C25—H25B | 107.3 |
Cl10—W6—Cl11ii | 93.03 (5) | C25—C26—C27 | 109.5 (5) |
Cl14—W6—Cl11ii | 89.91 (5) | C25—C26—H26A | 109.8 |
Cl12ii—W6—Cl11ii | 89.47 (5) | C27—C26—H26A | 109.8 |
Cl10—W6—Cl13 | 91.07 (5) | C25—C26—H26B | 109.8 |
Cl14—W6—Cl13 | 90.14 (5) | C27—C26—H26B | 109.8 |
Cl12ii—W6—Cl13 | 90.21 (5) | H26A—C26—H26B | 108.2 |
Cl11ii—W6—Cl13 | 175.89 (5) | C28—C27—C26 | 113.2 (6) |
Cl10—W6—W5ii | 134.39 (4) | C28—C27—H27A | 108.9 |
Cl14—W6—W5ii | 118.59 (4) | C26—C27—H27A | 108.9 |
Cl12ii—W6—W5ii | 58.70 (4) | C28—C27—H27B | 108.9 |
Cl11ii—W6—W5ii | 118.23 (3) | C26—C27—H27B | 108.9 |
Cl13—W6—W5ii | 58.31 (3) | H27A—C27—H27B | 107.8 |
Cl10—W6—W4 | 134.26 (4) | C27—C28—H28A | 109.5 |
Cl14—W6—W4 | 58.54 (4) | C27—C28—H28B | 109.5 |
Cl12ii—W6—W4 | 118.74 (4) | H28A—C28—H28B | 109.5 |
Cl11ii—W6—W4 | 118.29 (4) | C27—C28—H28C | 109.5 |
Cl13—W6—W4 | 58.46 (3) | H28A—C28—H28C | 109.5 |
W5ii—W6—W4 | 60.061 (9) | H28B—C28—H28C | 109.5 |
Cl10—W6—W4ii | 135.76 (4) | N2—C29—C30 | 116.4 (5) |
Cl14—W6—W4ii | 118.46 (3) | N2—C29—H29A | 108.2 |
Cl12ii—W6—W4ii | 58.26 (3) | C30—C29—H29A | 108.2 |
Cl11ii—W6—W4ii | 58.30 (3) | N2—C29—H29B | 108.2 |
Cl13—W6—W4ii | 118.25 (3) | C30—C29—H29B | 108.2 |
W5ii—W6—W4ii | 59.949 (9) | H29A—C29—H29B | 107.3 |
W4—W6—W4ii | 89.971 (10) | C29—C30—C31 | 110.3 (5) |
Cl10—W6—W5 | 135.75 (4) | C29—C30—H30A | 109.6 |
Cl14—W6—W5 | 58.52 (3) | C31—C30—H30A | 109.6 |
Cl12ii—W6—W5 | 118.20 (3) | C29—C30—H30B | 109.6 |
Cl11ii—W6—W5 | 58.47 (4) | C31—C30—H30B | 109.6 |
Cl13—W6—W5 | 118.28 (3) | H30A—C30—H30B | 108.1 |
W5ii—W6—W5 | 89.849 (10) | C32—C31—C30 | 115.6 (6) |
W4—W6—W5 | 59.837 (9) | C32—C31—H31A | 108.4 |
W4ii—W6—W5 | 59.945 (8) | C30—C31—H31A | 108.4 |
W4—Cl11—W6ii | 63.27 (3) | C32—C31—H31B | 108.4 |
W4—Cl11—W5ii | 63.18 (4) | C30—C31—H31B | 108.4 |
W6ii—Cl11—W5ii | 63.21 (4) | H31A—C31—H31B | 107.4 |
W4—Cl12—W6ii | 63.35 (3) | C31—C32—H32A | 109.5 |
W4—Cl12—W5 | 63.06 (3) | C31—C32—H32B | 109.5 |
W6ii—Cl12—W5 | 62.97 (3) | H32A—C32—H32B | 109.5 |
W5ii—Cl13—W4 | 63.14 (3) | C31—C32—H32C | 109.5 |
W5ii—Cl13—W6 | 62.95 (3) | H32A—C32—H32C | 109.5 |
W4—Cl13—W6 | 63.01 (3) | H32B—C32—H32C | 109.5 |
Cl1—W1—W2—Cl2 | −2.69 (8) | Cl12—W4—W5—Cl11ii | 177.34 (5) |
Cl5—W1—W2—Cl2 | −57.39 (7) | Cl11—W4—W5—Cl11ii | 106.96 (5) |
Cl7—W1—W2—Cl2 | −127.74 (7) | Cl14—W4—W5—Cl11ii | −69.98 (5) |
Cl6—W1—W2—Cl2 | 126.03 (7) | Cl13—W4—W5—Cl11ii | 0.30 (5) |
Cl4—W1—W2—Cl2 | 55.40 (7) | W5ii—W4—W5—Cl11ii | 53.38 (4) |
W3i—W1—W2—Cl2 | −126.28 (6) | W6—W4—W5—Cl11ii | −1.28 (4) |
W3—W1—W2—Cl2 | 124.34 (6) | W6ii—W4—W5—Cl11ii | 108.23 (4) |
W2i—W1—W2—Cl2 | 179.05 (6) | Cl8—W4—W5—Cl12 | 55.36 (7) |
Cl1—W1—W2—Cl6i | 124.93 (6) | Cl11—W4—W5—Cl12 | −70.38 (5) |
Cl5—W1—W2—Cl6i | 70.24 (5) | Cl14—W4—W5—Cl12 | 112.68 (5) |
Cl7—W1—W2—Cl6i | −0.11 (5) | Cl13—W4—W5—Cl12 | −177.04 (5) |
Cl6—W1—W2—Cl6i | −106.34 (5) | W5ii—W4—W5—Cl12 | −123.95 (4) |
Cl4—W1—W2—Cl6i | −176.97 (5) | W6—W4—W5—Cl12 | −178.62 (4) |
W3i—W1—W2—Cl6i | 1.35 (4) | W6ii—W4—W5—Cl12 | −69.11 (4) |
W3—W1—W2—Cl6i | −108.04 (4) | Cl8—W4—W5—W6ii | 124.46 (6) |
W2i—W1—W2—Cl6i | −53.33 (4) | Cl12—W4—W5—W6ii | 69.11 (4) |
Cl1—W1—W2—Cl5 | 54.70 (6) | Cl11—W4—W5—W6ii | −1.27 (4) |
Cl7—W1—W2—Cl5 | −70.35 (5) | Cl14—W4—W5—W6ii | −178.21 (4) |
Cl6—W1—W2—Cl5 | −176.57 (5) | Cl13—W4—W5—W6ii | −107.93 (4) |
Cl4—W1—W2—Cl5 | 112.79 (5) | W5ii—W4—W5—W6ii | −54.847 (8) |
W3i—W1—W2—Cl5 | −68.89 (4) | W6—W4—W5—W6ii | −109.511 (9) |
W3—W1—W2—Cl5 | −178.27 (4) | Cl8—W4—W5—W4ii | 179.31 (6) |
W2i—W1—W2—Cl5 | −123.56 (4) | Cl12—W4—W5—W4ii | 123.96 (4) |
Cl1—W1—W2—Cl7i | −128.71 (6) | Cl11—W4—W5—W4ii | 53.58 (4) |
Cl5—W1—W2—Cl7i | 176.60 (5) | Cl14—W4—W5—W4ii | −123.36 (4) |
Cl7—W1—W2—Cl7i | 106.25 (5) | Cl13—W4—W5—W4ii | −53.08 (4) |
Cl6—W1—W2—Cl7i | 0.02 (5) | W5ii—W4—W5—W4ii | 0.0 |
Cl4—W1—W2—Cl7i | −70.62 (5) | W6—W4—W5—W4ii | −54.662 (8) |
W3i—W1—W2—Cl7i | 107.71 (4) | W6ii—W4—W5—W4ii | 54.849 (8) |
W3—W1—W2—Cl7i | −1.68 (4) | Cl8—W4—W5—W6 | −126.03 (6) |
W2i—W1—W2—Cl7i | 53.03 (4) | Cl12—W4—W5—W6 | 178.62 (4) |
Cl1—W1—W2—Cl4 | −58.09 (7) | Cl11—W4—W5—W6 | 108.24 (4) |
Cl5—W1—W2—Cl4 | −112.79 (5) | Cl14—W4—W5—W6 | −68.70 (4) |
Cl7—W1—W2—Cl4 | 176.86 (5) | Cl13—W4—W5—W6 | 1.58 (4) |
Cl6—W1—W2—Cl4 | 70.64 (5) | W5ii—W4—W5—W6 | 54.664 (8) |
W3i—W1—W2—Cl4 | 178.33 (4) | W6ii—W4—W5—W6 | 109.511 (9) |
W3—W1—W2—Cl4 | 68.94 (4) | Cl8—W4—W6—Cl10 | −2.32 (8) |
W2i—W1—W2—Cl4 | 123.65 (4) | Cl12—W4—W6—Cl10 | −127.54 (6) |
Cl1—W1—W2—W3 | −127.03 (5) | Cl11—W4—W6—Cl10 | 125.68 (6) |
Cl5—W1—W2—W3 | 178.27 (4) | Cl14—W4—W6—Cl10 | −56.84 (6) |
Cl7—W1—W2—W3 | 107.92 (4) | Cl13—W4—W6—Cl10 | 55.43 (6) |
Cl6—W1—W2—W3 | 1.70 (4) | W5—W4—W6—Cl10 | −126.20 (5) |
Cl4—W1—W2—W3 | −68.94 (4) | W5ii—W4—W6—Cl10 | 124.46 (5) |
W3i—W1—W2—W3 | 109.389 (9) | W6ii—W4—W6—Cl10 | 179.18 (5) |
W2i—W1—W2—W3 | 54.712 (8) | Cl8—W4—W6—Cl14 | 54.52 (7) |
Cl1—W1—W2—W1i | 178.26 (5) | Cl12—W4—W6—Cl14 | −70.71 (5) |
Cl5—W1—W2—W1i | 123.56 (4) | Cl11—W4—W6—Cl14 | −177.49 (6) |
Cl7—W1—W2—W1i | 53.21 (4) | Cl13—W4—W6—Cl14 | 112.26 (5) |
Cl6—W1—W2—W1i | −53.01 (4) | W5—W4—W6—Cl14 | −69.36 (4) |
Cl4—W1—W2—W1i | −123.65 (4) | W5ii—W4—W6—Cl14 | −178.70 (4) |
W3i—W1—W2—W1i | 54.675 (8) | W6ii—W4—W6—Cl14 | −123.98 (4) |
W3—W1—W2—W1i | −54.714 (8) | Cl8—W4—W6—Cl12ii | −128.38 (7) |
W2i—W1—W2—W1i | 0.0 | Cl12—W4—W6—Cl12ii | 106.39 (5) |
Cl1—W1—W2—W3i | 123.58 (5) | Cl11—W4—W6—Cl12ii | −0.39 (6) |
Cl5—W1—W2—W3i | 68.89 (4) | Cl14—W4—W6—Cl12ii | 177.10 (6) |
Cl7—W1—W2—W3i | −1.46 (4) | Cl13—W4—W6—Cl12ii | −70.64 (5) |
Cl6—W1—W2—W3i | −107.69 (4) | W5—W4—W6—Cl12ii | 107.74 (4) |
Cl4—W1—W2—W3i | −178.33 (4) | W5ii—W4—W6—Cl12ii | −1.60 (4) |
W3—W1—W2—W3i | −109.389 (9) | W6ii—W4—W6—Cl12ii | 53.12 (4) |
W2i—W1—W2—W3i | −54.677 (8) | Cl8—W4—W6—Cl11ii | 125.16 (7) |
Cl2—W2—W3—Cl3 | 6.24 (7) | Cl12—W4—W6—Cl11ii | −0.06 (5) |
Cl6i—W2—W3—Cl3 | −123.70 (6) | Cl11—W4—W6—Cl11ii | −106.84 (4) |
Cl5—W2—W3—Cl3 | 129.40 (6) | Cl14—W4—W6—Cl11ii | 70.65 (5) |
Cl7i—W2—W3—Cl3 | −54.00 (6) | Cl13—W4—W6—Cl11ii | −177.09 (5) |
Cl4—W2—W3—Cl3 | 58.43 (6) | W5—W4—W6—Cl11ii | 1.28 (4) |
W1—W2—W3—Cl3 | 127.72 (5) | W5ii—W4—W6—Cl11ii | −108.06 (4) |
W1i—W2—W3—Cl3 | −123.09 (5) | W6ii—W4—W6—Cl11ii | −53.34 (4) |
W3i—W2—W3—Cl3 | −177.60 (5) | Cl8—W4—W6—Cl13 | −57.75 (7) |
Cl2—W2—W3—Cl5i | 130.79 (6) | Cl12—W4—W6—Cl13 | 177.03 (5) |
Cl6i—W2—W3—Cl5i | 0.85 (6) | Cl11—W4—W6—Cl13 | 70.25 (5) |
Cl5—W2—W3—Cl5i | −106.04 (4) | Cl14—W4—W6—Cl13 | −112.26 (5) |
Cl7i—W2—W3—Cl5i | 70.55 (5) | W5—W4—W6—Cl13 | 178.38 (4) |
Cl4—W2—W3—Cl5i | −177.02 (6) | W5ii—W4—W6—Cl13 | 69.04 (4) |
W1—W2—W3—Cl5i | −107.73 (4) | W6ii—W4—W6—Cl13 | 123.75 (4) |
W1i—W2—W3—Cl5i | 1.46 (4) | Cl8—W4—W6—W5ii | −126.78 (6) |
W3i—W2—W3—Cl5i | −53.05 (4) | Cl12—W4—W6—W5ii | 107.99 (4) |
Cl2—W2—W3—Cl4 | −52.19 (7) | Cl11—W4—W6—W5ii | 1.21 (4) |
Cl6i—W2—W3—Cl4 | 177.87 (6) | Cl14—W4—W6—W5ii | 178.70 (4) |
Cl5—W2—W3—Cl4 | 70.98 (5) | Cl13—W4—W6—W5ii | −69.04 (4) |
Cl7i—W2—W3—Cl4 | −112.43 (5) | W5—W4—W6—W5ii | 109.341 (9) |
W1—W2—W3—Cl4 | 69.29 (4) | W6ii—W4—W6—W5ii | 54.719 (8) |
W1i—W2—W3—Cl4 | 178.48 (4) | Cl8—W4—W6—W4ii | 178.50 (6) |
W3i—W2—W3—Cl4 | 123.97 (4) | Cl12—W4—W6—W4ii | 53.27 (4) |
Cl2—W2—W3—Cl7i | 60.24 (6) | Cl11—W4—W6—W4ii | −53.50 (4) |
Cl6i—W2—W3—Cl7i | −69.70 (5) | Cl14—W4—W6—W4ii | 123.98 (4) |
Cl5—W2—W3—Cl7i | −176.59 (5) | Cl13—W4—W6—W4ii | −123.75 (4) |
Cl4—W2—W3—Cl7i | 112.43 (5) | W5—W4—W6—W4ii | 54.622 (8) |
W1—W2—W3—Cl7i | −178.28 (4) | W5ii—W4—W6—W4ii | −54.718 (8) |
W1i—W2—W3—Cl7i | −69.09 (4) | W6ii—W4—W6—W4ii | 0.0 |
W3i—W2—W3—Cl7i | −123.60 (4) | Cl8—W4—W6—W5 | 123.88 (6) |
Cl2—W2—W3—Cl6 | −123.16 (6) | Cl12—W4—W6—W5 | −1.35 (4) |
Cl6i—W2—W3—Cl6 | 106.90 (4) | Cl11—W4—W6—W5 | −108.13 (4) |
Cl5—W2—W3—Cl6 | 0.00 (5) | Cl14—W4—W6—W5 | 69.36 (4) |
Cl7i—W2—W3—Cl6 | 176.59 (5) | Cl13—W4—W6—W5 | −178.38 (4) |
Cl4—W2—W3—Cl6 | −70.97 (5) | W5ii—W4—W6—W5 | −109.341 (9) |
W1—W2—W3—Cl6 | −1.68 (4) | W6ii—W4—W6—W5 | −54.621 (8) |
W1i—W2—W3—Cl6 | 107.51 (4) | Cl9—W5—W6—Cl10 | −0.45 (9) |
W3i—W2—W3—Cl6 | 53.00 (4) | Cl13ii—W5—W6—Cl10 | −127.21 (7) |
Cl2—W2—W3—W1i | 129.33 (5) | Cl14—W5—W6—Cl10 | 54.68 (7) |
Cl6i—W2—W3—W1i | −0.61 (4) | Cl11ii—W5—W6—Cl10 | −57.25 (7) |
Cl5—W2—W3—W1i | −107.51 (4) | Cl12—W5—W6—Cl10 | 125.41 (7) |
Cl7i—W2—W3—W1i | 69.09 (4) | W6ii—W5—W6—Cl10 | 178.93 (6) |
Cl4—W2—W3—W1i | −178.48 (4) | W4—W5—W6—Cl10 | 124.08 (6) |
W1—W2—W3—W1i | −109.189 (9) | W4ii—W5—W6—Cl10 | −126.31 (6) |
W3i—W2—W3—W1i | −54.509 (8) | Cl9—W5—W6—Cl14 | −55.13 (8) |
Cl2—W2—W3—W1 | −121.48 (5) | Cl13ii—W5—W6—Cl14 | 178.11 (6) |
Cl6i—W2—W3—W1 | 108.58 (4) | Cl11ii—W5—W6—Cl14 | −111.93 (6) |
Cl5—W2—W3—W1 | 1.68 (4) | Cl12—W5—W6—Cl14 | 70.73 (6) |
Cl7i—W2—W3—W1 | 178.28 (4) | W6ii—W5—W6—Cl14 | 124.24 (4) |
Cl4—W2—W3—W1 | −69.29 (4) | W4—W5—W6—Cl14 | 69.39 (4) |
W1i—W2—W3—W1 | 109.189 (9) | W4ii—W5—W6—Cl14 | 179.00 (4) |
W3i—W2—W3—W1 | 54.679 (8) | Cl9—W5—W6—Cl12ii | 126.85 (8) |
Cl2—W2—W3—W2i | −176.16 (5) | Cl13ii—W5—W6—Cl12ii | 0.09 (6) |
Cl6i—W2—W3—W2i | 53.90 (4) | Cl14—W5—W6—Cl12ii | −178.02 (6) |
Cl5—W2—W3—W2i | −53.00 (4) | Cl11ii—W5—W6—Cl12ii | 70.05 (6) |
Cl7i—W2—W3—W2i | 123.60 (4) | Cl12—W5—W6—Cl12ii | −107.29 (5) |
Cl4—W2—W3—W2i | −123.97 (4) | W6ii—W5—W6—Cl12ii | −53.78 (4) |
W1—W2—W3—W2i | −54.679 (8) | W4—W5—W6—Cl12ii | −108.63 (4) |
W1i—W2—W3—W2i | 54.509 (8) | W4ii—W5—W6—Cl12ii | 0.98 (4) |
W3i—W2—W3—W2i | 0.0 | Cl9—W5—W6—Cl11ii | 56.80 (7) |
Cl1—W1—W3—Cl3 | −0.44 (8) | Cl13ii—W5—W6—Cl11ii | −69.96 (5) |
Cl5—W1—W3—Cl3 | −124.92 (7) | Cl14—W5—W6—Cl11ii | 111.93 (6) |
Cl7—W1—W3—Cl3 | 127.80 (7) | Cl12—W5—W6—Cl11ii | −177.34 (5) |
Cl6—W1—W3—Cl3 | 58.50 (7) | W6ii—W5—W6—Cl11ii | −123.82 (4) |
Cl4—W1—W3—Cl3 | −53.59 (7) | W4—W5—W6—Cl11ii | −178.67 (4) |
W2—W1—W3—Cl3 | −123.25 (6) | W4ii—W5—W6—Cl11ii | −69.07 (4) |
W3i—W1—W3—Cl3 | −178.36 (6) | Cl9—W5—W6—Cl13 | −126.10 (7) |
W2i—W1—W3—Cl3 | 127.12 (6) | Cl13ii—W5—W6—Cl13 | 107.14 (5) |
Cl1—W1—W3—Cl5i | −128.52 (7) | Cl14—W5—W6—Cl13 | −70.97 (5) |
Cl5—W1—W3—Cl5i | 107.01 (4) | Cl11ii—W5—W6—Cl13 | 177.10 (5) |
Cl7—W1—W3—Cl5i | −0.27 (6) | Cl12—W5—W6—Cl13 | −0.24 (5) |
Cl6—W1—W3—Cl5i | −69.58 (5) | W6ii—W5—W6—Cl13 | 53.28 (4) |
Cl4—W1—W3—Cl5i | 178.33 (6) | W4—W5—W6—Cl13 | −1.57 (4) |
W2—W1—W3—Cl5i | 108.68 (4) | W4ii—W5—W6—Cl13 | 108.04 (4) |
W3i—W1—W3—Cl5i | 53.57 (4) | Cl9—W5—W6—W5ii | −179.38 (7) |
W2i—W1—W3—Cl5i | −0.96 (4) | Cl13ii—W5—W6—W5ii | 53.86 (4) |
Cl1—W1—W3—Cl4 | 53.15 (7) | Cl14—W5—W6—W5ii | −124.24 (4) |
Cl5—W1—W3—Cl4 | −71.33 (5) | Cl11ii—W5—W6—W5ii | 123.82 (4) |
Cl7—W1—W3—Cl4 | −178.61 (6) | Cl12—W5—W6—W5ii | −53.52 (4) |
Cl6—W1—W3—Cl4 | 112.09 (6) | W6ii—W5—W6—W5ii | 0.0 |
W2—W1—W3—Cl4 | −69.66 (4) | W4—W5—W6—W5ii | −54.851 (8) |
W3i—W1—W3—Cl4 | −124.77 (4) | W4ii—W5—W6—W5ii | 54.758 (8) |
W2i—W1—W3—Cl4 | −179.29 (4) | Cl9—W5—W6—W4 | −124.53 (7) |
Cl1—W1—W3—Cl7i | 124.47 (7) | Cl13ii—W5—W6—W4 | 108.71 (4) |
Cl5—W1—W3—Cl7i | −0.01 (5) | Cl14—W5—W6—W4 | −69.39 (4) |
Cl7—W1—W3—Cl7i | −107.29 (4) | Cl11ii—W5—W6—W4 | 178.67 (4) |
Cl6—W1—W3—Cl7i | −176.59 (5) | Cl12—W5—W6—W4 | 1.33 (4) |
Cl4—W1—W3—Cl7i | 71.32 (5) | W6ii—W5—W6—W4 | 54.850 (8) |
W2—W1—W3—Cl7i | 1.66 (4) | W4ii—W5—W6—W4 | 109.608 (10) |
W3i—W1—W3—Cl7i | −53.44 (4) | Cl9—W5—W6—W4ii | 125.87 (7) |
W2i—W1—W3—Cl7i | −107.97 (4) | Cl13ii—W5—W6—W4ii | −0.89 (4) |
Cl1—W1—W3—Cl6 | −58.94 (7) | Cl14—W5—W6—W4ii | −179.00 (4) |
Cl5—W1—W3—Cl6 | 176.58 (5) | Cl11ii—W5—W6—W4ii | 69.07 (4) |
Cl7—W1—W3—Cl6 | 69.30 (5) | Cl12—W5—W6—W4ii | −108.27 (4) |
Cl4—W1—W3—Cl6 | −112.09 (6) | W6ii—W5—W6—W4ii | −54.758 (8) |
W2—W1—W3—Cl6 | 178.25 (4) | W4—W5—W6—W4ii | −109.608 (10) |
W3i—W1—W3—Cl6 | 123.15 (4) | Cl8—W4—Cl11—W6ii | −142.92 (5) |
W2i—W1—W3—Cl6 | 68.62 (4) | Cl12—W4—Cl11—W6ii | −52.32 (4) |
Cl1—W1—W3—W1i | 177.91 (6) | Cl14—W4—Cl11—W6ii | 39.9 (7) |
Cl5—W1—W3—W1i | 53.44 (4) | Cl13—W4—Cl11—W6ii | 124.05 (4) |
Cl7—W1—W3—W1i | −53.84 (4) | W5—W4—Cl11—W6ii | 1.29 (4) |
Cl6—W1—W3—W1i | −123.14 (4) | W5ii—W4—Cl11—W6ii | 71.89 (3) |
Cl4—W1—W3—W1i | 124.77 (4) | W6—W4—Cl11—W6ii | 70.66 (3) |
W2—W1—W3—W1i | 55.110 (8) | Cl8—W4—Cl11—W5ii | 145.19 (5) |
W3i—W1—W3—W1i | 0.0 | Cl12—W4—Cl11—W5ii | −124.21 (4) |
W2i—W1—W3—W1i | −54.528 (8) | Cl14—W4—Cl11—W5ii | −31.9 (7) |
Cl1—W1—W3—W2 | 122.80 (6) | Cl13—W4—Cl11—W5ii | 52.16 (4) |
Cl5—W1—W3—W2 | −1.67 (4) | W5—W4—Cl11—W5ii | −70.60 (3) |
Cl7—W1—W3—W2 | −108.95 (4) | W6—W4—Cl11—W5ii | −1.23 (4) |
Cl6—W1—W3—W2 | −178.25 (4) | W6ii—W4—Cl11—W5ii | −71.89 (3) |
Cl4—W1—W3—W2 | 69.66 (4) | Cl8—W4—Cl12—W6ii | 144.70 (5) |
W3i—W1—W3—W2 | −55.109 (8) | Cl11—W4—Cl12—W6ii | 52.35 (4) |
W2i—W1—W3—W2 | −109.637 (9) | Cl14—W4—Cl12—W6ii | −123.47 (4) |
Cl1—W1—W3—W2i | −127.56 (6) | Cl13—W4—Cl12—W6ii | −27.0 (8) |
Cl5—W1—W3—W2i | 107.97 (4) | W5—W4—Cl12—W6ii | −71.62 (3) |
Cl7—W1—W3—W2i | 0.69 (4) | W5ii—W4—Cl12—W6ii | −1.00 (4) |
Cl6—W1—W3—W2i | −68.62 (4) | W6—W4—Cl12—W6ii | −70.25 (3) |
Cl4—W1—W3—W2i | 179.29 (4) | Cl8—W4—Cl12—W5 | −143.68 (5) |
W2—W1—W3—W2i | 109.637 (9) | Cl11—W4—Cl12—W5 | 123.97 (4) |
W3i—W1—W3—W2i | 54.528 (8) | Cl14—W4—Cl12—W5 | −51.86 (4) |
Cl3—W3—Cl4—W1 | 146.62 (4) | Cl13—W4—Cl12—W5 | 44.6 (8) |
Cl5i—W3—Cl4—W1 | −24.3 (8) | W5ii—W4—Cl12—W5 | 70.61 (3) |
Cl7i—W3—Cl4—W1 | −123.31 (4) | W6—W4—Cl12—W5 | 1.37 (4) |
Cl6—W3—Cl4—W1 | 52.00 (4) | W6ii—W4—Cl12—W5 | 71.62 (3) |
W1i—W3—Cl4—W1 | −69.88 (4) | Cl9—W5—Cl12—W4 | 144.67 (5) |
W2—W3—Cl4—W1 | −71.39 (3) | Cl13ii—W5—Cl12—W4 | −124.44 (4) |
W2i—W3—Cl4—W1 | −0.70 (4) | Cl14—W5—Cl12—W4 | 51.85 (4) |
Cl3—W3—Cl4—W2 | −141.99 (4) | Cl11ii—W5—Cl12—W4 | −34.7 (7) |
Cl5i—W3—Cl4—W2 | 47.1 (8) | W6ii—W5—Cl12—W4 | −72.21 (2) |
Cl7i—W3—Cl4—W2 | −51.92 (4) | W4ii—W5—Cl12—W4 | −70.59 (3) |
Cl6—W3—Cl4—W2 | 123.39 (4) | W6—W5—Cl12—W4 | −1.36 (4) |
W1i—W3—Cl4—W2 | 1.51 (4) | Cl9—W5—Cl12—W6ii | −143.12 (5) |
W1—W3—Cl4—W2 | 71.39 (3) | Cl13ii—W5—Cl12—W6ii | −52.23 (4) |
W2i—W3—Cl4—W2 | 70.70 (4) | Cl14—W5—Cl12—W6ii | 124.06 (4) |
Cl1—W1—Cl4—W3 | −146.39 (5) | Cl11ii—W5—Cl12—W6ii | 37.5 (7) |
Cl5—W1—Cl4—W3 | 123.54 (4) | W4—W5—Cl12—W6ii | 72.21 (2) |
Cl7—W1—Cl4—W3 | 20.4 (8) | W4ii—W5—Cl12—W6ii | 1.62 (4) |
Cl6—W1—Cl4—W3 | −52.32 (4) | W6—W5—Cl12—W6ii | 70.85 (3) |
W2—W1—Cl4—W3 | 71.80 (2) | Cl8—W4—Cl13—W5ii | −144.74 (5) |
W3i—W1—Cl4—W3 | 70.13 (4) | Cl12—W4—Cl13—W5ii | 26.9 (8) |
W2i—W1—Cl4—W3 | 0.69 (4) | Cl11—W4—Cl13—W5ii | −52.40 (4) |
Cl1—W1—Cl4—W2 | 141.81 (5) | Cl14—W4—Cl13—W5ii | 123.45 (4) |
Cl5—W1—Cl4—W2 | 51.74 (4) | W5—W4—Cl13—W5ii | 70.09 (3) |
Cl7—W1—Cl4—W2 | −51.4 (8) | W6—W4—Cl13—W5ii | 71.70 (3) |
Cl6—W1—Cl4—W2 | −124.12 (4) | W6ii—W4—Cl13—W5ii | 0.91 (4) |
W3i—W1—Cl4—W2 | −1.67 (4) | Cl8—W4—Cl13—W6 | 143.57 (4) |
W3—W1—Cl4—W2 | −71.80 (2) | Cl12—W4—Cl13—W6 | −44.8 (8) |
W2i—W1—Cl4—W2 | −71.11 (3) | Cl11—W4—Cl13—W6 | −124.09 (4) |
Cl2—W2—Cl4—W3 | 145.44 (4) | Cl14—W4—Cl13—W6 | 51.75 (4) |
Cl6i—W2—Cl4—W3 | −28.9 (7) | W5—W4—Cl13—W6 | −1.60 (4) |
Cl5—W2—Cl4—W3 | −124.08 (4) | W5ii—W4—Cl13—W6 | −71.70 (3) |
Cl7i—W2—Cl4—W3 | 52.07 (4) | W6ii—W4—Cl13—W6 | −70.79 (3) |
W1—W2—Cl4—W3 | −72.17 (3) | Cl10—W6—Cl13—W5ii | 144.16 (4) |
W1i—W2—Cl4—W3 | −1.49 (4) | Cl14—W6—Cl13—W5ii | −124.11 (4) |
W3i—W2—Cl4—W3 | −70.53 (3) | Cl12ii—W6—Cl13—W5ii | 52.20 (4) |
Cl2—W2—Cl4—W1 | −142.38 (4) | Cl11ii—W6—Cl13—W5ii | −33.4 (7) |
Cl6i—W2—Cl4—W1 | 43.3 (7) | W4—W6—Cl13—W5ii | −71.98 (3) |
Cl5—W2—Cl4—W1 | −51.91 (4) | W4ii—W6—Cl13—W5ii | −1.27 (4) |
Cl7i—W2—Cl4—W1 | 124.25 (4) | W5—W6—Cl13—W5ii | −70.39 (3) |
W3—W2—Cl4—W1 | 72.17 (3) | Cl10—W6—Cl13—W4 | −143.86 (4) |
W1i—W2—Cl4—W1 | 70.69 (3) | Cl14—W6—Cl13—W4 | −52.13 (4) |
W3i—W2—Cl4—W1 | 1.65 (4) | Cl12ii—W6—Cl13—W4 | 124.18 (4) |
Cl2—W2—Cl5—W3i | −146.90 (5) | Cl11ii—W6—Cl13—W4 | 38.6 (7) |
Cl6i—W2—Cl5—W3i | −52.52 (4) | W5ii—W6—Cl13—W4 | 71.98 (3) |
Cl7i—W2—Cl5—W3i | 22.2 (7) | W4ii—W6—Cl13—W4 | 70.71 (3) |
Cl4—W2—Cl5—W3i | 123.61 (4) | W5—W6—Cl13—W4 | 1.59 (4) |
W1—W2—Cl5—W3i | 71.75 (2) | Cl10—W6—Cl14—W4 | 143.15 (4) |
W3—W2—Cl5—W3i | 70.04 (3) | Cl12ii—W6—Cl14—W4 | −43.4 (8) |
W1i—W2—Cl5—W3i | 0.98 (4) | Cl11ii—W6—Cl14—W4 | −123.82 (4) |
Cl2—W2—Cl5—W1 | 141.34 (4) | Cl13—W6—Cl14—W4 | 52.07 (4) |
Cl6i—W2—Cl5—W1 | −124.28 (4) | W5ii—W6—Cl14—W4 | −1.28 (4) |
Cl7i—W2—Cl5—W1 | −49.5 (7) | W4ii—W6—Cl14—W4 | −70.59 (3) |
Cl4—W2—Cl5—W1 | 51.86 (4) | W5—W6—Cl14—W4 | −71.57 (3) |
W3—W2—Cl5—W1 | −1.71 (4) | Cl10—W6—Cl14—W5 | −145.28 (5) |
W1i—W2—Cl5—W1 | −70.78 (3) | Cl12ii—W6—Cl14—W5 | 28.2 (8) |
W3i—W2—Cl5—W1 | −71.75 (2) | Cl11ii—W6—Cl14—W5 | −52.25 (4) |
Cl1—W1—Cl5—W3i | 144.00 (4) | Cl13—W6—Cl14—W5 | 123.65 (4) |
Cl7—W1—Cl5—W3i | 52.10 (4) | W5ii—W6—Cl14—W5 | 70.29 (4) |
Cl6—W1—Cl5—W3i | −26.5 (7) | W4—W6—Cl14—W5 | 71.57 (3) |
Cl4—W1—Cl5—W3i | −124.48 (4) | W4ii—W6—Cl14—W5 | 0.98 (4) |
W2—W1—Cl5—W3i | −72.46 (2) | Cl8—W4—Cl14—W6 | −145.16 (5) |
W3—W1—Cl5—W3i | −70.76 (3) | Cl12—W4—Cl14—W6 | 124.21 (4) |
W2i—W1—Cl5—W3i | −1.48 (4) | Cl11—W4—Cl14—W6 | 32.0 (7) |
Cl1—W1—Cl5—W2 | −143.55 (4) | Cl13—W4—Cl14—W6 | −52.12 (4) |
Cl7—W1—Cl5—W2 | 124.56 (4) | W5—W4—Cl14—W6 | 72.16 (3) |
Cl6—W1—Cl5—W2 | 46.0 (7) | W5ii—W4—Cl14—W6 | 1.27 (4) |
Cl4—W1—Cl5—W2 | −52.02 (4) | W6ii—W4—Cl14—W6 | 70.40 (3) |
W3i—W1—Cl5—W2 | 72.46 (2) | Cl8—W4—Cl14—W5 | 142.68 (4) |
W3—W1—Cl5—W2 | 1.70 (4) | Cl12—W4—Cl14—W5 | 52.05 (4) |
W2i—W1—Cl5—W2 | 70.98 (3) | Cl11—W4—Cl14—W5 | −40.2 (7) |
Cl1—W1—Cl6—W2i | −144.40 (4) | Cl13—W4—Cl14—W5 | −124.28 (4) |
Cl5—W1—Cl6—W2i | 26.1 (7) | W5ii—W4—Cl14—W5 | −70.89 (3) |
Cl7—W1—Cl6—W2i | −52.58 (4) | W6—W4—Cl14—W5 | −72.16 (3) |
Cl4—W1—Cl6—W2i | 124.07 (4) | W6ii—W4—Cl14—W5 | −1.76 (4) |
W2—W1—Cl6—W2i | 70.31 (3) | Cl9—W5—Cl14—W6 | 145.51 (5) |
W3i—W1—Cl6—W2i | 0.62 (4) | Cl13ii—W5—Cl14—W6 | −26.4 (8) |
W3—W1—Cl6—W2i | 72.03 (2) | Cl11ii—W5—Cl14—W6 | 52.13 (4) |
Cl1—W1—Cl6—W3 | 143.57 (4) | Cl12—W5—Cl14—W6 | −123.75 (4) |
Cl5—W1—Cl6—W3 | −46.0 (7) | W6ii—W5—Cl14—W6 | −70.32 (4) |
Cl7—W1—Cl6—W3 | −124.61 (4) | W4—W5—Cl14—W6 | −72.09 (2) |
Cl4—W1—Cl6—W3 | 52.04 (4) | W4ii—W5—Cl14—W6 | −0.98 (4) |
W2—W1—Cl6—W3 | −1.72 (4) | Cl9—W5—Cl14—W4 | −142.40 (5) |
W3i—W1—Cl6—W3 | −71.41 (3) | Cl13ii—W5—Cl14—W4 | 45.7 (8) |
W2i—W1—Cl6—W3 | −72.03 (2) | Cl11ii—W5—Cl14—W4 | 124.22 (4) |
Cl3—W3—Cl6—W2i | 143.54 (4) | Cl12—W5—Cl14—W4 | −51.66 (4) |
Cl5i—W3—Cl6—W2i | 52.13 (4) | W6ii—W5—Cl14—W4 | 1.77 (4) |
Cl4—W3—Cl6—W2i | −124.40 (4) | W4ii—W5—Cl14—W4 | 71.11 (4) |
Cl7i—W3—Cl6—W2i | −32.3 (6) | W6—W5—Cl14—W4 | 72.09 (2) |
W1i—W3—Cl6—W2i | −1.35 (4) | C13—N1—C1—C2 | −56.5 (7) |
W2—W3—Cl6—W2i | −70.52 (3) | C5—N1—C1—C2 | 63.7 (7) |
W1—W3—Cl6—W2i | −72.22 (3) | C9—N1—C1—C2 | −174.8 (5) |
Cl3—W3—Cl6—W1 | −144.24 (4) | N1—C1—C2—C3 | 156.8 (5) |
Cl5i—W3—Cl6—W1 | 124.36 (4) | C1—C2—C3—C4 | 169.2 (6) |
Cl4—W3—Cl6—W1 | −52.18 (4) | C13—N1—C5—C6 | −63.4 (7) |
Cl7i—W3—Cl6—W1 | 39.9 (6) | C1—N1—C5—C6 | 174.9 (5) |
W1i—W3—Cl6—W1 | 70.87 (3) | C9—N1—C5—C6 | 56.1 (6) |
W2—W3—Cl6—W1 | 1.71 (4) | N1—C5—C6—C7 | 95.1 (6) |
W2i—W3—Cl6—W1 | 72.22 (3) | C5—C6—C7—C8 | 170.0 (5) |
Cl1—W1—Cl7—W2i | 146.39 (5) | C13—N1—C9—C10 | 176.4 (4) |
Cl5—W1—Cl7—W2i | −123.55 (4) | C5—N1—C9—C10 | 56.4 (6) |
Cl6—W1—Cl7—W2i | 52.35 (4) | C1—N1—C9—C10 | −63.2 (6) |
Cl4—W1—Cl7—W2i | −20.4 (8) | N1—C9—C10—C11 | −174.0 (4) |
W2—W1—Cl7—W2i | −70.23 (3) | C9—C10—C11—C12 | 68.7 (7) |
W3i—W1—Cl7—W2i | −71.72 (2) | C5—N1—C13—C14A | 173.0 (9) |
W3—W1—Cl7—W2i | −0.70 (4) | C1—N1—C13—C14A | −66.8 (10) |
Cl1—W1—Cl7—W3i | −141.90 (4) | C9—N1—C13—C14A | 51.1 (10) |
Cl5—W1—Cl7—W3i | −51.84 (4) | C5—N1—C13—C14 | −161.8 (8) |
Cl6—W1—Cl7—W3i | 124.06 (4) | C1—N1—C13—C14 | −41.6 (9) |
Cl4—W1—Cl7—W3i | 51.3 (8) | C9—N1—C13—C14 | 76.3 (8) |
W2—W1—Cl7—W3i | 1.49 (4) | N1—C13—C14—C15 | 175.9 (10) |
W3—W1—Cl7—W3i | 71.02 (3) | C14A—C13—C14—C15 | −90 (3) |
W2i—W1—Cl7—W3i | 71.72 (2) | C13—C14—C15—C16 | 65 (2) |
Cl8—W4—W5—Cl9 | 1.27 (9) | N1—C13—C14A—C15A | 163.0 (13) |
Cl12—W4—W5—Cl9 | −54.08 (7) | C14—C13—C14A—C15A | 66 (3) |
Cl11—W4—W5—Cl9 | −124.46 (8) | C13—C14A—C15A—C16A | −69 (3) |
Cl14—W4—W5—Cl9 | 58.60 (7) | C29—N2—C17—C18 | 58.4 (6) |
Cl13—W4—W5—Cl9 | 128.88 (7) | C21—N2—C17—C18 | −59.3 (6) |
W5ii—W4—W5—Cl9 | −178.04 (7) | C25—N2—C17—C18 | −179.7 (5) |
W6—W4—W5—Cl9 | 127.30 (6) | N2—C17—C18—C19 | 168.8 (5) |
W6ii—W4—W5—Cl9 | −123.19 (6) | C17—C18—C19—C20 | −67.5 (7) |
Cl8—W4—W5—Cl13ii | 125.73 (7) | C29—N2—C21—C22 | −176.5 (5) |
Cl12—W4—W5—Cl13ii | 70.37 (5) | C17—N2—C21—C22 | −53.9 (7) |
Cl11—W4—W5—Cl13ii | 0.00 (6) | C25—N2—C21—C22 | 62.5 (7) |
Cl14—W4—W5—Cl13ii | −176.94 (5) | N2—C21—C22—C23 | −177.6 (5) |
Cl13—W4—W5—Cl13ii | −106.67 (5) | C21—C22—C23—C24 | 71.2 (8) |
W5ii—W4—W5—Cl13ii | −53.58 (4) | C29—N2—C25—C26 | −54.3 (6) |
W6—W4—W5—Cl13ii | −108.24 (4) | C17—N2—C25—C26 | −177.1 (5) |
W6ii—W4—W5—Cl13ii | 1.27 (4) | C21—N2—C25—C26 | 62.6 (7) |
Cl8—W4—W5—Cl14 | −57.33 (7) | N2—C25—C26—C27 | 174.2 (5) |
Cl12—W4—W5—Cl14 | −112.68 (5) | C25—C26—C27—C28 | 65.6 (8) |
Cl11—W4—W5—Cl14 | 176.94 (6) | C17—N2—C29—C30 | 62.3 (7) |
Cl13—W4—W5—Cl14 | 70.28 (5) | C21—N2—C29—C30 | −176.4 (5) |
W5ii—W4—W5—Cl14 | 123.36 (4) | C25—N2—C29—C30 | −55.6 (7) |
W6—W4—W5—Cl14 | 68.70 (4) | N2—C29—C30—C31 | 173.6 (5) |
W6ii—W4—W5—Cl14 | 178.21 (4) | C29—C30—C31—C32 | −64.4 (8) |
Cl8—W4—W5—Cl11ii | −127.31 (7) |
Symmetry codes: (i) −x, −y+1, −z; (ii) −x+1, −y+2, −z. |
Experimental details
(I_150K) | (I_200K) | |
Crystal data | ||
Chemical formula | (C16H36N)2[W6Cl14] | (C16H36N)2[W6Cl14] |
Mr | 2084.32 | 2084.32 |
Crystal system, space group | Monoclinic, P21/c | Monoclinic, P21/c |
Temperature (K) | 150 | 200 |
a, b, c (Å) | 22.3152 (2), 11.7220 (1), 22.2786 (1) | 22.3689 (2), 11.7596 (1), 22.3108 (2) |
β (°) | 112.415 (1) | 112.320 (1) |
V (Å3) | 5387.31 (7) | 5429.13 (8) |
Z | 4 | 4 |
Radiation type | Mo Kα | Mo Kα |
µ (mm−1) | 13.48 | 13.38 |
Crystal size (mm) | 0.31 × 0.27 × 0.23 | 0.27 × 0.19 × 0.19 |
Data collection | ||
Diffractometer | Nonius KappaCCD diffractometer | Nonius KappaCCD diffractometer |
Absorption correction | Multi-scan (SADABS; Bruker, 2008) | Multi-scan (HKL SCALEPACK; Otwinowski & Minor, 1997) |
Tmin, Tmax | 0.484, 0.746 | 0.055, 0.079 |
No. of measured, independent and observed [I > 2σ(I)] reflections | 137050, 12352, 9499 | 101212, 12422, 9227 |
Rint | 0.086 | 0.063 |
(sin θ/λ)max (Å−1) | 0.650 | 0.649 |
Refinement | ||
R[F2 > 2σ(F2)], wR(F2), S | 0.031, 0.054, 1.07 | 0.031, 0.064, 1.03 |
No. of reflections | 12352 | 12422 |
No. of parameters | 515 | 515 |
No. of restraints | 148 | 148 |
H-atom treatment | H-atom parameters constrained | H-atom parameters constrained |
Δρmax, Δρmin (e Å−3) | 1.20, −1.69 | 2.36, −2.11 |
Computer programs: COLLECT (Nonius, 2000), HKL SCALEPACK (Otwinowski & Minor, 1997), HKL DENZO and SCALEPACK (Otwinowski & Minor, 1997), SHELXS97 (Sheldrick, 2008), SHELXL97 (Sheldrick, 2008), ORTEP-3 for Windows (Farrugia, 1997), Mercury (Macrae et al., 2008), POV-RAY (Cason, 2004), WinGX publication routines (Farrugia, 1999).
W1—W2 | 2.6048 (3) | W4—W5 | 2.6092 (3) |
W1—W2i | 2.6212 (3) | W4—W5ii | 2.6127 (3) |
W1—W3 | 2.6163 (3) | W4—W6 | 2.6133 (3) |
W1—W3i | 2.6091 (3) | W4—W6ii | 2.6143 (3) |
W2—W3 | 2.6120 (3) | W5—W6 | 2.6152 (3) |
W2—W3i | 2.6207 (3) | W5—W6ii | 2.6071 (3) |
W1—Cl1 | 2.4181 (13) | W4—Cl8 | 2.4243 (14) |
W2—Cl2 | 2.4292 (13) | W5—Cl9 | 2.4187 (13) |
W3—Cl3 | 2.4310 (13) | W6—Cl10 | 2.4328 (13) |
W1—Cl4 | 2.5037 (12) | W4—Cl11 | 2.4941 (13) |
W1—Cl5 | 2.5028 (13) | W4—Cl12 | 2.4926 (13) |
W1—Cl6 | 2.4968 (13) | W4—Cl13 | 2.5034 (12) |
W1—Cl7 | 2.4934 (12) | W4—Cl14 | 2.4979 (13) |
W2—Cl4 | 2.5044 (13) | W5—Cl11ii | 2.4969 (14) |
W2—Cl5 | 2.4927 (12) | W5—Cl12 | 2.5044 (14) |
W2—Cl6i | 2.4919 (13) | W5—Cl13ii | 2.4954 (13) |
W2—Cl7i | 2.4987 (12) | W5—Cl14 | 2.4974 (13) |
W3—Cl4 | 2.4977 (13) | W6—Cl11ii | 2.4972 (13) |
W3—Cl5i | 2.4856 (12) | W6—Cl12ii | 2.4978 (13) |
W3—Cl6 | 2.5090 (13) | W6—Cl13 | 2.5062 (14) |
W3—Cl7i | 2.5055 (13) | W6—Cl14 | 2.4844 (13) |
Symmetry codes: (i) −x, −y+1, −z; (ii) −x+1, −y+2, −z. |
W1—W2 | 2.6056 (3) | W4—W5 | 2.6113 (3) |
W1—W2i | 2.6228 (3) | W4—W5ii | 2.6157 (3) |
W1—W3 | 2.6191 (3) | W4—W6 | 2.6169 (3) |
W1—W3i | 2.6101 (3) | W4—W6ii | 2.6170 (3) |
W2—W3 | 2.6131 (3) | W5—W6 | 2.6186 (3) |
W2—W3i | 2.6239 (3) | W5—W6ii | 2.6096 (3) |
W1—Cl1 | 2.4177 (14) | W4—Cl8 | 2.4187 (16) |
W2—Cl2 | 2.4289 (14) | W5—Cl9 | 2.4173 (14) |
W3—Cl3 | 2.4285 (14) | W6—Cl10 | 2.4297 (15) |
W1—Cl4 | 2.5012 (14) | W4—Cl11 | 2.4928 (14) |
W1—Cl5 | 2.4961 (14) | W4—Cl12 | 2.4903 (14) |
W1—Cl6 | 2.4980 (15) | W4—Cl13 | 2.5029 (14) |
W1—Cl7 | 2.4962 (14) | W4—Cl14 | 2.4965 (14) |
W2—Cl4 | 2.5067 (14) | W5—Cl11ii | 2.5003 (16) |
W2—Cl5 | 2.4905 (14) | W5—Cl12 | 2.5033 (15) |
W2—Cl6i | 2.4864 (14) | W5—Cl13ii | 2.4932 (14) |
W2—Cl7i | 2.4967 (13) | W5—Cl14 | 2.4967 (14) |
W3—Cl4 | 2.4965 (13) | W6—Cl11ii | 2.4964 (15) |
W3—Cl5i | 2.4888 (13) | W6—Cl12ii | 2.4936 (13) |
W3—Cl6 | 2.5088 (15) | W6—Cl13 | 2.5046 (14) |
W3—Cl7i | 2.5020 (14) | W6—Cl14 | 2.4836 (13) |
Symmetry codes: (i) −x, −y+1, −z; (ii) −x+1, −y+2, −z. |
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The lower halides of tungsten, including tungsten(II)chloride, have been known for over 100 years (Kepert & Vrieze, 1967; Prokopuk & Shriver, 1999) and numerous methods for their synthesis have been developed (Hogue & McCarley, 1970; Dorman & McCarley, 1974; Kolesnichenko & Messerle, 1998; Ströbele et al., 2009). The structure of the [(W6Cl8)Cl6]2- anion was first determined by Zietlow, Schaefer et al. (1986) at room temperature. A subsequent structure determination of the same form was published by Venkataraman et al. (1999). The tungsten(II) halide clusters have been intensely studied because of their fascinating photochemical and electrochemical properties (Maverick et al., 1983; Nocera & Gray, 1984; Zietlow et al., 1985; Zietlow, Nocera et al., 1986; Jackson et al., 1990; Mussell & Nocera, 1990; Arratia-Pérez & Hernández-Acevedo, 1997; Gray, 2009).
At low temperaure, the two independent [(W6Cl8)Cl6]2- cluster units (Fig. 1) sit on crystallographic inversion centers and have bond lengths and bond angles comparable to previously determined structures (Zietlow, Schaefer et al., 1986; Venkataraman et al., 1999). One hydrocarbon chain of one of the two tetrabutylammonium cations (Fig. 1) is disordered and was modeled with two sites each for three different carbon atoms. A packing diagram is shown in Fig. 2.
There is a close relationship between the unit cell of the herein reported low-temperature (200 K and 150 K) structures and the unit cell of the previously determined room-temperature structures. The cell dimensions of the room-temperature unit cell are a = 18.512, b = 11.661, c = 12.789 Å, α = 90.00, β = 90.17, γ = 90.00° (Zietlow, Schaefer et al., 1986), while at 150 K the unit cell is a = 22.3152 (2), b = 11.7220 (1), c = 22.2786 (1) Å, α = 90.00, β = 112.451 (1), γ = 90.00°. Application of the transformation matrix [0.5 0 -0.5 / 0 1 0 / 0.5 0 0.5] to the unit cell of the low-temperature form produces the following unit cell, which is approximately identical to the room-temperature cell: a = 18.534, b = 11.722, c = 12.395 Å, α = 90.00, β = 89.90, γ = 90.00°. An overlay of the two unit cells is shown in Fig. 3 (r.m.s. overlay = 0.177 Å for 122 non-H atoms). This transformation is possible because the low-temperature unit cell shows higher metric symmetry, namely the a and c axes are approximately equal. This allows for a pseudo-orthorhombic C-centered cell to be generated using the transformation matrix [1 0 1 / 1 0 -1 / 0 1 0]. The room-temperature cell can be generated from this pseudo-orthorhombic cell by dividing the a and b axes by two, followed by a rearrangement of the axes.
The relationship between the unit cells was not noticed until after the data collection when the crystal had already been removed from the diffractometer. At a later point, a new crystal of the same sample was mounted on the diffractometer at 150 K and a preliminary unit-cell determination agreed with the cell at 200 K from the data-collection crystal. Then the temperature was raised to 200 K and the unit cell was determined again and it was essentially the same cell. Finally, the temperature was increased to room temperature (293 K) and the unit cell changed to become the room-temperature cell reported in the literature.
A further study was undertaken to determine the phase-transition temperature. A new crystal of the title compound was mounted on a Rigaku SCXmini small-molecule X-ray crystallography system equipped with a Rigaku TEC-50 low-temperature device. The temperature at the sample was verified using a calibrated thermocouple. The previously determined unit cells were confirmed at room temperature and 223 K. Repeated indexing of the crystal at successively higher temperatures demonstrated that the crystal undergoes a reversible phase transition between 267 and 269 K. This result was reproduced using a different crystal of the same compound.
A search of the Cambridge Structure Database (CSD; Allen, 2002) revealed that the smaller P21/n unit cell observed for the room-temperature structure is common to a range of tetrabutylammonium salts of metal–halide and metal–chalcogenide cluster dianions. Examples include molybdenum halide clusters (Preetz et al., 1992, 1994; Kirakci, et al., 2005), molybdenum chalcogenide/halide clusters (Ebihara et al., 1992), tungsten halide clusters (Zietlow, Schaefer et al., 1986; Venkataraman et al., 1999) and rhenium chalcogenide/halide clusters (Gabriel et al., 1993; Uriel et al., 1995, 1996, 2001). Only two examples were found with the same larger P21/c unit cell as the low-temperature phase of the title compound: the [(Os2Re4Se8)Cl6]2- dianion structure determined at 153 K by Tulsky & Long (2001) and the [(Re6Se5Cl2N-TMS)Cl6]2- anion structure determined at room temperature by Uriel et al. (1996).
Among these examples, only one structure was found that potentially undergoes a similar phase change. The [(Re6Se6Cl2)Cl6]2- dianion structure was determined in a tetragonal setting (space group I4/mmm; Yaghi et al., 1992) at 198 K, while two other structure determinations of the same compound at room temperature (Uriel et al., 1995, 2001) display the P21/n unit cell found for the room-temperature structure of the title compound and many other structures. The analogous [(Mo6Br8)Br6]2- dianion structure, however, has been determined at 100 K and room temperature (Kirakci et al., 2005) and in both cases the P21/n unit cell was found.