Tetra-μ-6-methyl­pyridin-2-olato-ditungsten toluene sesquisolvate

The red title compound, [W₂(C₆H₆NO)₄]·1.5C₇H₈, contains isolated W₂(hmp)₄ molecules (hmp is 6-methyl­pyridin-2-olate) in which the W—W separation of 2.1617 (5) Å is consistent with the expected tungsten–tungsten quadruple bond. The complex molecule cocrystallizes with 1.5 mol­ecules of toluene. One toluene mol­ecule is disordered about a crystallographic inversion center, and the other, in a general position, is also disordered.

Key indicators

• Single-crystal X-ray study
• T = 200 K
• Mean [sigma](C-C) = 0.010 Å
• Disorder in solvent or counterion
• R factor = 0.034
• wR factor = 0.080
• Data-to-parameter ratio = 12.5

checkCIF/PLATON results

No syntax errors found



Alert level B
PLAT331_ALERT_2_B Small Average Phenyl C-C Dist.   C61A   -C66A          1.36 Ang.

Alert level C
PLAT041_ALERT_1_C Calc. and Rep. SumFormula Strings    Differ ....          ?
PLAT042_ALERT_1_C Calc. and Rep. MoietyFormula Strings Differ ....          ?
PLAT045_ALERT_1_C Calculated and Reported Z Differ by ............       0.50 Ratio
PLAT243_ALERT_4_C High  'Solvent' Ueq as Compared to Neighbors for       C64A
PLAT244_ALERT_4_C Low   'Solvent' Ueq as Compared to Neighbors for       C51A
PLAT244_ALERT_4_C Low   'Solvent' Ueq as Compared to Neighbors for       C62A
PLAT302_ALERT_4_C Anion/Solvent Disorder .........................      50.00 Perc.
PLAT331_ALERT_2_C Small Average Phenyl C-C Dist.   C51A   -C56A          1.36 Ang.
PLAT331_ALERT_2_C Small Average Phenyl C-C Dist.   C51B   -C56B          1.37 Ang.
PLAT342_ALERT_3_C Low Bond Precision on C-C bonds (x 1000) Ang ...         10
PLAT380_ALERT_4_C Check Incorrectly? Oriented X(sp2)-Methyl Moiety       C57A
PLAT380_ALERT_4_C Check Incorrectly? Oriented X(sp2)-Methyl Moiety       C67A

   0 ALERT level A = In general: serious problem
   1 ALERT level B = Potentially serious problem
  12 ALERT level C = Check and explain
   0 ALERT level G = General alerts; check

   3 ALERT type 1 CIF construction/syntax error, inconsistent or missing data
   3 ALERT type 2 Indicator that the structure model may be wrong or deficient
   1 ALERT type 3 Indicator that the structure quality may be low
   6 ALERT type 4 Improvement, methodology, query or suggestion

---

Computing details

Data collection: Please provide; cell refinement: Please provide; data reduction: Please provide; program(s) used to solve structure: SHELXS97 (Sheldrick, 1997); program(s) used to refine structure: SHELXL97 (Sheldrick, 1997); molecular graphics: ORTEP-3 for Windows (Farrugia, 1997); software used to prepare material for publication: WinGX (Farrugia, 1999).

Tetra-µ-6-methylpyridin-2-olato-ditungsten toluene sesquisolvate

Crystal data

[W2(C6H6NO)4]·1.5C7H8	F(000) = 1804
Mr = 938.37	Dx = 1.884 Mg m^−3
Monoclinic, P21/c	Mo Kα radiation, λ = 0.71073 Å
Hall symbol: -P 2ybc	Cell parameters from 6111 reflections
a = 15.563 (2) Å	θ = 2.0–25.0°
b = 12.975 (2) Å	µ = 6.99 mm^−1
c = 16.486 (3) Å	T = 200 K
β = 96.48 (1)°	Plate, red
V = 3307.8 (9) Å^3	0.19 × 0.08 × 0.04 mm
Z = 4

Data collection

Nonius KappaCCD diffractometer	4480 reflections with I > 2σ(I)
Graphite monochromator	Rint = 0.082
φ and ω scans	θmax = 25.0°, θmin = 2.1°
Absorption correction: multi-scan (SCALEPACK; Otwinowski & Minor, 1997)	h = −18→18
Tmin = 0.553, Tmax = 0.756	k = −15→15
51699 measured reflections	l = −19→19
5840 independent reflections

Refinement

Refinement on F^2	Primary atom site location: heavy-atom method
Least-squares matrix: full	Secondary atom site location: difference Fourier map
R[F^2 > 2σ(F^2)] = 0.034	Hydrogen site location: inferred from neighbouring sites
wR(F^2) = 0.081	H-atom parameters constrained
S = 1.04	w = 1/[σ^2(Fo^2) + (0.0387P)^2 + 6.3721P] where P = (Fo^2 + 2Fc^2)/3
5840 reflections	(Δ/σ)max = 0.028
466 parameters	Δρmax = 1.43 e Å^−3
334 restraints	Δρmin = −1.30 e Å^−3

Special details

Experimental. All work was done at 200 K using an Oxford Cryosystems Cryostream Cooler. The data collection strategy was set up to measure a quadrant of reciprocal space with a redundancy factor of 4.1, which means that 90% of the reflections were measured 4.1 times. A combination of phi and omega scans with a frame width of 1.0 degree was used. Data integration was done with DENZO. Scaling and merging of the data was done with SCALEPACK.

Geometry. All e.s.d.'s (except the e.s.d. in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell e.s.d.'s are taken into account individually in the estimation of e.s.d.'s in distances, angles and torsion angles; correlations between e.s.d.'s in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell e.s.d.'s is used for estimating e.s.d.'s involving l.s. planes.

Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Ų)

	x	y	z	Uiso*/Ueq	Occ. (<1)
W1	0.240278 (18)	0.11123 (2)	0.171820 (15)	0.02990 (10)
W2	0.373034 (18)	0.14165 (2)	0.152580 (15)	0.02943 (10)
O1	0.4188 (3)	0.1231 (3)	0.2737 (2)	0.0331 (11)
O2	0.2513 (3)	−0.0450 (3)	0.1560 (3)	0.0361 (11)
O3	0.2118 (3)	0.2637 (3)	0.1922 (2)	0.0327 (10)
O4	0.3442 (3)	0.1643 (3)	0.0289 (2)	0.0292 (10)
N1	0.2796 (4)	0.0906 (4)	0.2999 (3)	0.0329 (13)
N2	0.3926 (4)	−0.0195 (4)	0.1331 (3)	0.0314 (13)
N3	0.3527 (4)	0.3023 (4)	0.1746 (3)	0.0297 (13)
N4	0.2025 (3)	0.1341 (4)	0.0450 (3)	0.0294 (12)
C11	0.3649 (5)	0.1002 (5)	0.3271 (4)	0.0344 (16)
C12	0.3950 (5)	0.0854 (5)	0.4100 (4)	0.0413 (18)
H12	0.455	0.0909	0.4282	0.05*
C13	0.3372 (6)	0.0632 (6)	0.4638 (4)	0.054 (2)
H13	0.3568	0.0527	0.5199	0.065*
C14	0.2498 (6)	0.0558 (6)	0.4365 (4)	0.053 (2)
H14	0.2092	0.0417	0.474	0.064*
C15	0.2223 (5)	0.0690 (5)	0.3562 (4)	0.0389 (17)
C16	0.1313 (5)	0.0613 (7)	0.3226 (5)	0.058 (2)
H16A	0.1244	0.0051	0.2827	0.087*
H16B	0.1128	0.1263	0.2958	0.087*
H16C	0.0958	0.0473	0.3668	0.087*
C21	0.3256 (5)	−0.0851 (5)	0.1422 (4)	0.0330 (16)
C22	0.3352 (5)	−0.1921 (5)	0.1344 (4)	0.0437 (18)
H22	0.2881	−0.2369	0.1407	0.052*
C23	0.4122 (6)	−0.2311 (6)	0.1177 (5)	0.056 (2)
H23	0.4196	−0.3035	0.1134	0.068*
C24	0.4806 (5)	−0.1646 (6)	0.1067 (4)	0.0463 (19)
H24	0.5341	−0.1916	0.0935	0.056*
C25	0.4704 (5)	−0.0605 (5)	0.1151 (4)	0.0364 (16)
C26	0.5391 (5)	0.0152 (5)	0.1028 (4)	0.0406 (17)
H26A	0.5553	0.0528	0.1538	0.061*
H26B	0.5176	0.0638	0.0598	0.061*
H26C	0.5898	−0.0211	0.0868	0.061*
C31	0.2723 (4)	0.3339 (5)	0.1905 (4)	0.0294 (15)
C32	0.2544 (5)	0.4371 (5)	0.2059 (4)	0.0388 (17)
H32	0.198	0.4577	0.2161	0.047*
C33	0.3198 (5)	0.5085 (5)	0.2061 (4)	0.0426 (18)
H33	0.3091	0.5789	0.2169	0.051*
C34	0.4017 (5)	0.4769 (5)	0.1903 (4)	0.0410 (18)
H34	0.447	0.5259	0.1901	0.049*
C35	0.4171 (5)	0.3751 (5)	0.1751 (4)	0.0341 (17)
C36	0.5031 (5)	0.3360 (6)	0.1592 (5)	0.0453 (19)
H36A	0.5256	0.2895	0.2034	0.068*
H36B	0.543	0.3941	0.1565	0.068*
H36C	0.4977	0.2987	0.1072	0.068*
C41	0.2647 (4)	0.1577 (5)	−0.0050 (4)	0.0284 (15)
C42	0.2423 (5)	0.1757 (5)	−0.0887 (4)	0.0370 (17)
H42	0.2863	0.1912	−0.1223	0.044*
C43	0.1584 (5)	0.1713 (6)	−0.1225 (4)	0.0418 (18)
H43	0.1437	0.1836	−0.1791	0.05*
C44	0.0940 (5)	0.1480 (6)	−0.0718 (4)	0.0446 (19)
H44	0.0348	0.146	−0.0936	0.054*
C45	0.1176 (5)	0.1279 (5)	0.0106 (4)	0.0341 (16)
C46	0.0539 (4)	0.1004 (6)	0.0685 (4)	0.0425 (18)
H46A	−0.0042	0.0967	0.0388	0.064*
H46B	0.055	0.1531	0.1112	0.064*
H46C	0.0692	0.0334	0.0935	0.064*
C51A	0.8478 (7)	0.2303 (9)	0.2109 (7)	0.060 (3)	0.698 (8)
C52A	0.7789 (8)	0.2904 (10)	0.1821 (7)	0.061 (3)	0.698 (8)
H52A	0.7691	0.3547	0.207	0.073*	0.698 (8)
C53A	0.7248 (9)	0.2567 (10)	0.1175 (8)	0.072 (3)	0.698 (8)
H53A	0.6769	0.2984	0.0974	0.086*	0.698 (8)
C54A	0.7370 (9)	0.1630 (10)	0.0794 (8)	0.071 (3)	0.698 (8)
H54A	0.6988	0.14	0.034	0.085*	0.698 (8)
C55A	0.8057 (8)	0.1063 (10)	0.1099 (8)	0.068 (3)	0.698 (8)
H55A	0.8168	0.0426	0.0845	0.081*	0.698 (8)
C56A	0.8598 (10)	0.1373 (10)	0.1759 (8)	0.066 (3)	0.698 (8)
H56A	0.9059	0.0939	0.1977	0.08*	0.698 (8)
C57A	0.9103 (11)	0.2675 (15)	0.2827 (10)	0.104 (5)	0.698 (8)
H57A	0.892	0.3355	0.3002	0.156*	0.698 (8)
H57B	0.9686	0.2724	0.2661	0.156*	0.698 (8)
H57C	0.9103	0.2186	0.328	0.156*	0.698 (8)
C51B	0.7889 (14)	0.2105 (17)	0.1457 (13)	0.065 (4)	0.302 (8)
C52B	0.8404 (16)	0.1248 (18)	0.1477 (16)	0.063 (5)	0.302 (8)
H52B	0.8315	0.0752	0.1052	0.075*	0.302 (8)
C53B	0.9051 (16)	0.1101 (18)	0.2107 (15)	0.066 (5)	0.302 (8)
H53B	0.9399	0.0498	0.2115	0.08*	0.302 (8)
C54B	0.9199 (16)	0.1805 (19)	0.2717 (15)	0.066 (5)	0.302 (8)
H54B	0.9659	0.1718	0.3141	0.079*	0.302 (8)
C55B	0.8659 (18)	0.265 (2)	0.2699 (17)	0.067 (5)	0.302 (8)
H55B	0.8736	0.3132	0.3132	0.08*	0.302 (8)
C56B	0.802 (2)	0.281 (2)	0.2077 (16)	0.061 (5)	0.302 (8)
H56B	0.7662	0.3402	0.2075	0.074*	0.302 (8)
C57B	0.717 (2)	0.230 (3)	0.0785 (18)	0.080 (8)	0.302 (8)
H57D	0.7145	0.1742	0.0385	0.12*	0.302 (8)
H57E	0.7268	0.2958	0.0516	0.12*	0.302 (8)
H57F	0.6614	0.2337	0.1018	0.12*	0.302 (8)
C61A	0.0255 (10)	0.5557 (11)	−0.0013 (9)	0.076 (5)*	0.5
C62A	0.0654 (10)	0.4944 (11)	0.0577 (9)	0.056 (5)*	0.5
H62A	0.1169	0.5157	0.0898	0.068*	0.5
C63A	0.0288 (11)	0.4007 (12)	0.0693 (10)	0.082 (6)*	0.5
H63A	0.0557	0.3566	0.1106	0.099*	0.5
C64A	−0.0443 (15)	0.3683 (15)	0.0244 (15)	0.105 (9)*	0.5
H64A	−0.0687	0.3028	0.0337	0.126*	0.5
C65A	−0.0822 (11)	0.4335 (13)	−0.0353 (11)	0.092 (6)*	0.5
H65A	−0.1337	0.4129	−0.0678	0.11*	0.5
C66A	−0.0462 (11)	0.5277 (13)	−0.0482 (11)	0.069 (6)*	0.5
H66A	−0.0719	0.5723	−0.0898	0.083*	0.5
C67A	0.0690 (16)	0.6539 (19)	−0.0168 (14)	0.092 (8)*	0.5
H67A	0.1201	0.6624	0.0231	0.138*	0.5
H67B	0.029	0.7113	−0.0119	0.138*	0.5
H67C	0.0867	0.653	−0.072	0.138*	0.5

Atomic displacement parameters (Ų)

	U^11	U^22	U^33	U^12	U^13	U^23
W1	0.03606 (17)	0.02863 (16)	0.02599 (16)	−0.00196 (12)	0.00780 (12)	0.00131 (11)
W2	0.03441 (17)	0.02764 (16)	0.02676 (16)	−0.00080 (12)	0.00573 (12)	0.00136 (11)
O1	0.039 (3)	0.036 (3)	0.024 (2)	0.000 (2)	0.000 (2)	0.0027 (19)
O2	0.041 (3)	0.030 (3)	0.039 (3)	−0.002 (2)	0.008 (2)	0.003 (2)
O3	0.043 (3)	0.024 (2)	0.030 (2)	0.000 (2)	0.005 (2)	−0.0006 (19)
O4	0.034 (3)	0.030 (3)	0.024 (2)	−0.001 (2)	0.006 (2)	0.0032 (18)
N1	0.041 (4)	0.030 (3)	0.028 (3)	−0.003 (3)	0.006 (3)	0.002 (2)
N2	0.046 (4)	0.022 (3)	0.025 (3)	0.003 (3)	0.002 (3)	0.000 (2)
N3	0.040 (4)	0.023 (3)	0.026 (3)	−0.002 (3)	0.004 (2)	0.005 (2)
N4	0.030 (3)	0.027 (3)	0.031 (3)	−0.005 (2)	0.004 (2)	0.000 (2)
C11	0.053 (5)	0.021 (4)	0.029 (4)	−0.002 (3)	0.005 (3)	0.001 (3)
C12	0.053 (5)	0.038 (4)	0.030 (4)	−0.001 (4)	−0.004 (3)	0.000 (3)
C13	0.086 (7)	0.050 (5)	0.026 (4)	−0.002 (5)	0.009 (4)	0.003 (3)
C14	0.063 (6)	0.062 (5)	0.038 (5)	−0.013 (4)	0.018 (4)	0.004 (4)
C15	0.056 (5)	0.031 (4)	0.030 (4)	−0.005 (3)	0.005 (3)	0.002 (3)
C16	0.079 (7)	0.054 (5)	0.045 (5)	−0.009 (5)	0.023 (4)	0.009 (4)
C21	0.043 (5)	0.027 (4)	0.029 (4)	−0.005 (3)	0.005 (3)	0.004 (3)
C22	0.051 (5)	0.027 (4)	0.052 (5)	0.001 (4)	0.002 (4)	0.007 (3)
C23	0.073 (6)	0.030 (4)	0.065 (5)	0.009 (4)	0.005 (5)	0.007 (4)
C24	0.052 (5)	0.036 (5)	0.052 (5)	0.013 (4)	0.016 (4)	0.003 (3)
C25	0.040 (4)	0.040 (4)	0.030 (4)	0.004 (3)	0.006 (3)	0.005 (3)
C26	0.043 (4)	0.043 (4)	0.036 (4)	0.004 (3)	0.004 (3)	0.001 (3)
C31	0.038 (4)	0.028 (4)	0.021 (3)	0.003 (3)	−0.002 (3)	−0.002 (3)
C32	0.046 (5)	0.037 (4)	0.032 (4)	0.004 (4)	0.000 (3)	0.000 (3)
C33	0.064 (6)	0.028 (4)	0.035 (4)	0.003 (4)	0.003 (4)	−0.002 (3)
C34	0.064 (5)	0.029 (4)	0.029 (4)	−0.013 (4)	0.001 (3)	0.000 (3)
C35	0.051 (5)	0.029 (4)	0.020 (3)	−0.004 (3)	−0.005 (3)	0.004 (3)
C36	0.040 (5)	0.039 (4)	0.057 (5)	−0.012 (3)	0.003 (4)	0.005 (4)
C41	0.036 (4)	0.020 (3)	0.027 (3)	0.000 (3)	−0.001 (3)	−0.002 (3)
C42	0.049 (5)	0.035 (4)	0.030 (4)	−0.008 (3)	0.015 (3)	0.001 (3)
C43	0.051 (5)	0.046 (5)	0.027 (4)	−0.003 (4)	0.001 (3)	0.001 (3)
C44	0.049 (5)	0.050 (5)	0.032 (4)	0.004 (4)	−0.007 (3)	0.000 (3)
C45	0.044 (4)	0.029 (4)	0.031 (4)	−0.004 (3)	0.008 (3)	−0.001 (3)
C46	0.034 (4)	0.057 (5)	0.036 (4)	−0.005 (4)	0.003 (3)	0.001 (3)
C51A	0.061 (6)	0.066 (6)	0.054 (6)	−0.010 (5)	0.011 (5)	0.005 (4)
C52A	0.074 (7)	0.051 (6)	0.062 (7)	0.001 (5)	0.020 (5)	−0.009 (5)
C53A	0.063 (7)	0.082 (7)	0.071 (8)	0.010 (6)	0.006 (5)	0.006 (6)
C54A	0.087 (8)	0.082 (8)	0.044 (6)	−0.027 (6)	0.007 (5)	−0.006 (5)
C55A	0.088 (8)	0.057 (6)	0.067 (7)	−0.012 (5)	0.044 (5)	−0.012 (5)
C56A	0.073 (7)	0.057 (6)	0.071 (7)	0.008 (5)	0.020 (5)	0.017 (5)
C57A	0.094 (11)	0.124 (12)	0.088 (10)	−0.033 (10)	−0.014 (7)	0.000 (8)
C51B	0.074 (8)	0.062 (7)	0.062 (7)	−0.002 (6)	0.017 (6)	0.002 (6)
C52B	0.074 (10)	0.054 (8)	0.064 (11)	−0.006 (8)	0.022 (8)	−0.002 (8)
C53B	0.068 (11)	0.058 (10)	0.076 (11)	−0.004 (8)	0.022 (8)	0.008 (8)
C54B	0.060 (10)	0.065 (10)	0.072 (10)	−0.007 (8)	0.009 (8)	0.008 (8)
C55B	0.068 (11)	0.063 (10)	0.071 (10)	−0.006 (9)	0.012 (8)	0.000 (8)
C56B	0.068 (10)	0.054 (9)	0.065 (9)	0.002 (8)	0.017 (8)	0.000 (7)
C57B	0.093 (16)	0.085 (18)	0.062 (15)	0.007 (13)	0.008 (11)	−0.002 (14)

Geometric parameters (Å, º)

W1—W2	2.1617 (5)	C42—C43	1.360 (10)
W2—O1	2.056 (4)	C42—H42	0.95
W1—O2	2.054 (4)	C43—C44	1.409 (10)
W1—O3	2.063 (4)	C43—H43	0.95
W2—O4	2.060 (4)	C44—C45	1.390 (9)
W1—N1	2.147 (5)	C44—H44	0.95
W2—N2	2.142 (5)	C45—C46	1.495 (9)
W2—N3	2.146 (5)	C46—H46A	0.98
W1—N4	2.129 (5)	C46—H46B	0.98
O1—C11	1.317 (8)	C46—H46C	0.98
O2—C21	1.311 (8)	C51A—C56A	1.359 (11)
O3—C31	1.313 (8)	C51A—C52A	1.368 (11)
O4—C41	1.301 (7)	C51A—C57A	1.522 (17)
N1—C11	1.359 (9)	C52A—C53A	1.354 (12)
N1—C15	1.386 (9)	C52A—H52A	0.95
N2—C21	1.368 (8)	C53A—C54A	1.391 (12)
N2—C25	1.386 (9)	C53A—H53A	0.95
N3—C31	1.369 (8)	C54A—C55A	1.348 (12)
N3—C35	1.376 (8)	C54A—H54A	0.95
N4—C41	1.374 (8)	C55A—C56A	1.359 (12)
N4—C45	1.380 (9)	C55A—H55A	0.95
C11—C12	1.406 (9)	C56A—H56A	0.95
C12—C13	1.364 (10)	C57A—H57A	0.98
C12—H12	0.95	C57A—H57B	0.98
C13—C14	1.387 (11)	C57A—H57C	0.98
C13—H13	0.95	C51B—C56B	1.366 (14)
C14—C15	1.355 (9)	C51B—C52B	1.369 (14)
C14—H14	0.95	C51B—C57B	1.51 (2)
C15—C16	1.465 (11)	C52B—C53B	1.375 (14)
C16—H16A	0.98	C52B—H52B	0.95
C16—H16B	0.98	C53B—C54B	1.359 (14)
C16—H16C	0.98	C53B—H53B	0.95
C21—C22	1.404 (10)	C54B—C55B	1.377 (14)
C22—C23	1.358 (11)	C54B—H54B	0.95
C22—H22	0.95	C55B—C56B	1.363 (14)
C23—C24	1.398 (11)	C55B—H55B	0.95
C23—H23	0.95	C56B—H56B	0.95
C24—C25	1.368 (10)	C57B—H57D	0.98
C24—H24	0.95	C57B—H57E	0.98
C25—C26	1.482 (10)	C57B—H57F	0.98
C26—H26A	0.98	C61A—C66A	1.335 (13)
C26—H26B	0.98	C61A—C62A	1.352 (13)
C26—H26C	0.98	C61A—C67A	1.48 (3)
C31—C32	1.397 (9)	C62A—C63A	1.365 (15)
C32—C33	1.376 (10)	C62A—H62A	0.95
C32—H32	0.95	C63A—C64A	1.353 (15)
C33—C34	1.390 (10)	C63A—H63A	0.95
C33—H33	0.95	C64A—C65A	1.379 (15)
C34—C35	1.370 (9)	C64A—H64A	0.95
C34—H34	0.95	C65A—C66A	1.371 (15)
C35—C36	1.483 (10)	C65A—H65A	0.95
C36—H36A	0.98	C66A—H66A	0.95
C36—H36B	0.98	C67A—H67A	0.98
C36—H36C	0.98	C67A—H67B	0.98
C41—C42	1.405 (9)	C67A—H67C	0.98
O2—W1—O3	171.82 (18)	C35—C36—H36C	109.5
O1—W2—O4	172.31 (17)	H36A—C36—H36C	109.5
N4—W1—N1	179.0 (2)	H36B—C36—H36C	109.5
N2—W2—N3	178.80 (19)	O4—C41—N4	117.2 (5)
O2—W1—N4	91.76 (18)	O4—C41—C42	121.9 (6)
O3—W1—N4	89.20 (17)	N4—C41—C42	120.8 (6)
O2—W1—N1	89.02 (18)	C43—C42—C41	121.0 (6)
O3—W1—N1	90.10 (18)	C43—C42—H42	119.5
O2—W1—W2	93.83 (13)	C41—C42—H42	119.5
O3—W1—W2	94.31 (13)	C42—C43—C44	118.7 (6)
N1—W1—W2	89.79 (15)	C42—C43—H43	120.6
N4—W1—W2	89.61 (14)	C44—C43—H43	120.6
O1—W2—N2	89.55 (17)	C45—C44—C43	119.4 (7)
O4—W2—N2	90.54 (17)	C45—C44—H44	120.3
O1—W2—N3	89.47 (17)	C43—C44—H44	120.3
O4—W2—N3	90.52 (17)	N4—C45—C44	121.7 (6)
O1—W2—W1	93.90 (13)	N4—C45—C46	115.1 (6)
O4—W2—W1	93.79 (12)	C44—C45—C46	123.2 (7)
N2—W2—W1	89.90 (15)	C45—C46—H46A	109.5
N3—W2—W1	89.48 (15)	C45—C46—H46B	109.5
C11—O1—W2	120.0 (4)	H46A—C46—H46B	109.5
C21—O2—W1	120.1 (4)	C45—C46—H46C	109.5
C31—O3—W1	119.7 (4)	H46A—C46—H46C	109.5
C41—O4—W2	120.4 (4)	H46B—C46—H46C	109.5
C11—N1—C15	118.4 (6)	C56A—C51A—C52A	119.9 (11)
C11—N1—W1	118.2 (4)	C56A—C51A—C57A	120.4 (12)
C15—N1—W1	123.4 (5)	C52A—C51A—C57A	119.8 (11)
C21—N2—C25	118.7 (6)	C53A—C52A—C51A	118.9 (11)
C21—N2—W2	117.9 (4)	C53A—C52A—H52A	120.6
C25—N2—W2	123.4 (4)	C51A—C52A—H52A	120.6
C31—N3—C35	118.3 (5)	C52A—C53A—C54A	122.2 (12)
C31—N3—W2	118.6 (4)	C52A—C53A—H53A	118.9
C35—N3—W2	123.1 (5)	C54A—C53A—H53A	118.9
C41—N4—C45	118.2 (5)	C55A—C54A—C53A	116.9 (11)
C41—N4—W1	119.0 (4)	C55A—C54A—H54A	121.6
C45—N4—W1	122.8 (4)	C53A—C54A—H54A	121.6
O1—C11—N1	118.1 (6)	C54A—C55A—C56A	122.0 (12)
O1—C11—C12	120.9 (7)	C54A—C55A—H55A	119
N1—C11—C12	121.0 (6)	C56A—C55A—H55A	119
C13—C12—C11	119.3 (7)	C51A—C56A—C55A	120.1 (12)
C13—C12—H12	120.4	C51A—C56A—H56A	120
C11—C12—H12	120.4	C55A—C56A—H56A	120
C12—C13—C14	119.9 (7)	C51A—C57A—H57A	109.5
C12—C13—H13	120.1	C51A—C57A—H57B	109.5
C14—C13—H13	120.1	H57A—C57A—H57B	109.5
C15—C14—C13	119.9 (7)	C51A—C57A—H57C	109.5
C15—C14—H14	120.1	H57A—C57A—H57C	109.5
C13—C14—H14	120.1	H57B—C57A—H57C	109.5
C14—C15—N1	121.6 (7)	C56B—C51B—C52B	119.2 (17)
C14—C15—C16	123.1 (7)	C56B—C51B—C57B	118.1 (19)
N1—C15—C16	115.3 (6)	C52B—C51B—C57B	122.8 (19)
C15—C16—H16A	109.5	C51B—C52B—C53B	120.5 (19)
C15—C16—H16B	109.5	C51B—C52B—H52B	119.8
H16A—C16—H16B	109.5	C53B—C52B—H52B	119.8
C15—C16—H16C	109.5	C54B—C53B—C52B	121 (2)
H16A—C16—H16C	109.5	C54B—C53B—H53B	119.5
H16B—C16—H16C	109.5	C52B—C53B—H53B	119.5
O2—C21—N2	118.1 (6)	C53B—C54B—C55B	117.7 (18)
O2—C21—C22	120.9 (6)	C53B—C54B—H54B	121.1
N2—C21—C22	121.0 (6)	C55B—C54B—H54B	121.1
C23—C22—C21	119.5 (7)	C56B—C55B—C54B	122 (2)
C23—C22—H22	120.2	C56B—C55B—H55B	119
C21—C22—H22	120.2	C54B—C55B—H55B	119
C22—C23—C24	119.9 (7)	C55B—C56B—C51B	120 (2)
C22—C23—H23	120.1	C55B—C56B—H56B	120.2
C24—C23—H23	120.1	C51B—C56B—H56B	120.2
C25—C24—C23	119.9 (7)	C51B—C57B—H57D	109.5
C25—C24—H24	120.1	C51B—C57B—H57E	109.5
C23—C24—H24	120.1	H57D—C57B—H57E	109.5
C24—C25—N2	121.0 (7)	C51B—C57B—H57F	109.5
C24—C25—C26	123.2 (7)	H57D—C57B—H57F	109.5
N2—C25—C26	115.8 (6)	H57E—C57B—H57F	109.5
C25—C26—H26A	109.5	C66A—C61A—C62A	122.9 (12)
C25—C26—H26B	109.5	C66A—C61A—C67A	120.2 (11)
H26A—C26—H26B	109.5	C62A—C61A—C67A	116.7 (11)
C25—C26—H26C	109.5	C61A—C62A—C63A	117.4 (10)
H26A—C26—H26C	109.5	C61A—C62A—H62A	121.3
H26B—C26—H26C	109.5	C63A—C62A—H62A	121.3
O3—C31—N3	118.0 (5)	C64A—C63A—C62A	122.6 (10)
O3—C31—C32	120.2 (6)	C64A—C63A—H63A	118.7
N3—C31—C32	121.8 (6)	C62A—C63A—H63A	118.7
C33—C32—C31	118.8 (7)	C63A—C64A—C65A	117.7 (12)
C33—C32—H32	120.6	C63A—C64A—H64A	121.1
C31—C32—H32	120.6	C65A—C64A—H64A	121.1
C32—C33—C34	119.7 (7)	C66A—C65A—C64A	120.6 (10)
C32—C33—H33	120.2	C66A—C65A—H65A	119.7
C34—C33—H33	120.2	C64A—C65A—H65A	119.7
C35—C34—C33	120.1 (7)	C61A—C66A—C65A	118.8 (10)
C35—C34—H34	120	C61A—C66A—H66A	120.6
C33—C34—H34	120	C65A—C66A—H66A	120.6
C34—C35—N3	121.3 (7)	C61A—C67A—H67A	109.5
C34—C35—C36	122.8 (7)	C61A—C67A—H67B	109.5
N3—C35—C36	115.8 (6)	H67A—C67A—H67B	109.5
C35—C36—H36A	109.5	C61A—C67A—H67C	109.5
C35—C36—H36B	109.5	H67A—C67A—H67C	109.5
H36A—C36—H36B	109.5	H67B—C67A—H67C	109.5
O2—W1—W2—O1	−88.78 (16)	C25—N2—C21—O2	−177.3 (5)
O3—W1—W2—O1	90.32 (16)	W2—N2—C21—O2	5.3 (7)
N4—W1—W2—O1	179.49 (18)	C25—N2—C21—C22	0.6 (9)
N1—W1—W2—O1	0.23 (18)	W2—N2—C21—C22	−176.8 (5)
O2—W1—W2—O4	91.30 (16)	O2—C21—C22—C23	178.0 (6)
O3—W1—W2—O4	−89.60 (16)	N2—C21—C22—C23	0.2 (10)
N4—W1—W2—O4	−0.43 (17)	C21—C22—C23—C24	−1.3 (11)
N1—W1—W2—O4	−179.69 (18)	C22—C23—C24—C25	1.8 (11)
O2—W1—W2—N2	0.77 (17)	C23—C24—C25—N2	−1.0 (10)
O3—W1—W2—N2	179.87 (17)	C23—C24—C25—C26	−178.7 (7)
N4—W1—W2—N2	−90.97 (19)	C21—N2—C25—C24	−0.2 (9)
N1—W1—W2—N2	89.78 (19)	W2—N2—C25—C24	177.1 (5)
O2—W1—W2—N3	−178.21 (17)	C21—N2—C25—C26	177.7 (5)
O3—W1—W2—N3	0.89 (16)	W2—N2—C25—C26	−5.1 (7)
N4—W1—W2—N3	90.06 (19)	W1—O3—C31—N3	0.3 (7)
N1—W1—W2—N3	−89.20 (19)	W1—O3—C31—C32	−178.7 (4)
N2—W2—O1—C11	−89.7 (4)	C35—N3—C31—O3	−178.1 (5)
N3—W2—O1—C11	89.6 (4)	W2—N3—C31—O3	0.6 (7)
W1—W2—O1—C11	0.2 (4)	C35—N3—C31—C32	0.9 (8)
N4—W1—O2—C21	91.4 (4)	W2—N3—C31—C32	179.6 (4)
N1—W1—O2—C21	−88.1 (5)	O3—C31—C32—C33	178.1 (6)
W2—W1—O2—C21	1.7 (4)	N3—C31—C32—C33	−0.9 (9)
N4—W1—O3—C31	−90.5 (4)	C31—C32—C33—C34	0.6 (10)
N1—W1—O3—C31	88.8 (4)	C32—C33—C34—C35	−0.3 (10)
W2—W1—O3—C31	−1.0 (4)	C33—C34—C35—N3	0.3 (10)
N2—W2—O4—C41	90.7 (4)	C33—C34—C35—C36	−179.0 (6)
N3—W2—O4—C41	−88.7 (4)	C31—N3—C35—C34	−0.6 (9)
W1—W2—O4—C41	0.8 (4)	W2—N3—C35—C34	−179.3 (5)
O2—W1—N1—C11	93.1 (5)	C31—N3—C35—C36	178.8 (5)
O3—W1—N1—C11	−95.0 (5)	W2—N3—C35—C36	0.1 (7)
W2—W1—N1—C11	−0.7 (5)	W2—O4—C41—N4	−0.7 (7)
O2—W1—N1—C15	−87.5 (5)	W2—O4—C41—C42	178.0 (5)
O3—W1—N1—C15	84.3 (5)	C45—N4—C41—O4	179.2 (5)
W2—W1—N1—C15	178.6 (5)	W1—N4—C41—O4	0.2 (7)
O1—W2—N2—C21	90.6 (4)	C45—N4—C41—C42	0.5 (9)
O4—W2—N2—C21	−97.1 (4)	W1—N4—C41—C42	−178.5 (5)
W1—W2—N2—C21	−3.3 (4)	O4—C41—C42—C43	−178.1 (6)
O1—W2—N2—C25	−86.7 (5)	N4—C41—C42—C43	0.6 (10)
O4—W2—N2—C25	85.6 (5)	C41—C42—C43—C44	−0.1 (11)
W1—W2—N2—C25	179.4 (4)	C42—C43—C44—C45	−1.5 (11)
O1—W2—N3—C31	−95.0 (4)	C41—N4—C45—C44	−2.1 (9)
O4—W2—N3—C31	92.7 (4)	W1—N4—C45—C44	176.9 (5)
W1—W2—N3—C31	−1.1 (4)	C41—N4—C45—C46	179.1 (6)
O1—W2—N3—C35	83.7 (4)	W1—N4—C45—C46	−1.9 (8)
O4—W2—N3—C35	−88.7 (4)	C43—C44—C45—N4	2.6 (10)
W1—W2—N3—C35	177.6 (4)	C43—C44—C45—C46	−178.7 (7)
O2—W1—N4—C41	−93.5 (4)	C56A—C51A—C52A—C53A	−1.6 (14)
O3—W1—N4—C41	94.6 (4)	C57A—C51A—C52A—C53A	179.1 (12)
W2—W1—N4—C41	0.3 (4)	C51A—C52A—C53A—C54A	0.0 (15)
O2—W1—N4—C45	87.5 (5)	C52A—C53A—C54A—C55A	0.1 (19)
O3—W1—N4—C45	−84.4 (5)	C53A—C54A—C55A—C56A	1 (2)
W2—W1—N4—C45	−178.7 (5)	C52A—C51A—C56A—C55A	3.2 (19)
W2—O1—C11—N1	−0.7 (7)	C57A—C51A—C56A—C55A	−177.5 (13)
W2—O1—C11—C12	178.9 (5)	C54A—C55A—C56A—C51A	−3 (2)
C15—N1—C11—O1	−178.4 (5)	C56B—C51B—C52B—C53B	−1 (2)
W1—N1—C11—O1	0.9 (8)	C57B—C51B—C52B—C53B	−180 (2)
C15—N1—C11—C12	2.0 (9)	C51B—C52B—C53B—C54B	−1 (2)
W1—N1—C11—C12	−178.6 (5)	C52B—C53B—C54B—C55B	2 (3)
O1—C11—C12—C13	179.1 (6)	C53B—C54B—C55B—C56B	−3 (5)
N1—C11—C12—C13	−1.3 (10)	C54B—C55B—C56B—C51B	1 (5)
C11—C12—C13—C14	−0.3 (11)	C52B—C51B—C56B—C55B	1 (4)
C12—C13—C14—C15	1.2 (12)	C57B—C51B—C56B—C55B	179 (3)
C13—C14—C15—N1	−0.5 (11)	C66A—C61A—C62A—C63A	−1 (2)
C13—C14—C15—C16	179.3 (7)	C67A—C61A—C62A—C63A	−176.1 (16)
C11—N1—C15—C14	−1.1 (10)	C61A—C62A—C63A—C64A	0 (2)
W1—N1—C15—C14	179.6 (5)	C62A—C63A—C64A—C65A	0 (3)
C11—N1—C15—C16	179.1 (6)	C63A—C64A—C65A—C66A	0 (4)
W1—N1—C15—C16	−0.2 (8)	C62A—C61A—C66A—C65A	1 (3)
W1—O2—C21—N2	−4.5 (7)	C67A—C61A—C66A—C65A	176 (2)
W1—O2—C21—C22	177.5 (5)	C64A—C65A—C66A—C61A	−1 (3)