Penta­carbon­yl{N,N-dimethyl-N′-[4-(pyridin-4-ylethynyl-κN)benzyl­idene]benzene-1,4-diamine}tungsten(0)

The asymmetric unit of the title compound, [W(C₂₂H₁₉N₃)(CO)₅], contains two mol­ecules. The geometry at the W atom is approximately octa­hedral, with the cis bond angles in the range 86.11 (13)–92.75 (11)°. The axial carbonyl bonds [W—C = 1.960 (4) and 1.967 (4) Å] are shorter than the equatorial carbonyl bonds, which lie in the range 2.014 (4)–2.047 (4) Å.

Key indicators

• Single-crystal X-ray study
• T = 100 K
• Mean [sigma](C-C) = 0.005 Å
• R factor = 0.022
• wR factor = 0.049
• Data-to-parameter ratio = 13.9

checkCIF/PLATON results

No syntax errors found



Alert level C
ABSTM02_ALERT_3_C  The ratio of expected to reported Tmax/Tmin(RR) is > 1.10
            Tmin and Tmax reported:      0.493     0.986
            Tmin and Tmax expected:      0.268     0.695
            RR =      1.297
            Please check that your absorption correction is appropriate.
PLAT060_ALERT_3_C Ratio Tmax/Tmin (Exp-to-Rep) (too) Large .......       1.31
PLAT062_ALERT_4_C Rescale T(min) & T(max) by .....................       0.70
PLAT154_ALERT_1_C The su's on the Cell Angles are Equal (x 10000)         100 Deg.
PLAT180_ALERT_3_C Check Cell Rounding: # of Values Ending with 0 =          3
PLAT230_ALERT_2_C Hirshfeld Test Diff for    O3     -   C3      ..       5.61 su
PLAT230_ALERT_2_C Hirshfeld Test Diff for    O5     -   C5      ..       5.79 su
PLAT230_ALERT_2_C Hirshfeld Test Diff for    O10    -   C10     ..       5.56 su
PLAT232_ALERT_2_C Hirshfeld Test Diff (M-X)  W1     -   C3      ..       7.63 su
PLAT232_ALERT_2_C Hirshfeld Test Diff (M-X)  W1     -   C4      ..       5.59 su
PLAT232_ALERT_2_C Hirshfeld Test Diff (M-X)  W1     -   C5      ..       7.07 su
PLAT232_ALERT_2_C Hirshfeld Test Diff (M-X)  W2     -   C6      ..       5.70 su
PLAT232_ALERT_2_C Hirshfeld Test Diff (M-X)  W2     -   C7      ..       8.71 su
PLAT232_ALERT_2_C Hirshfeld Test Diff (M-X)  W2     -   C8      ..       5.49 su
PLAT232_ALERT_2_C Hirshfeld Test Diff (M-X)  W2     -   C10     ..       7.19 su
PLAT242_ALERT_2_C Check Low       Ueq as Compared to Neighbors for        N43
PLAT371_ALERT_2_C Long   C(sp2)-C(sp1) Bond  C14    -   C17    ...       1.42 Ang.
PLAT371_ALERT_2_C Long   C(sp2)-C(sp1) Bond  C18    -   C19    ...       1.44 Ang.
PLAT371_ALERT_2_C Long   C(sp2)-C(sp1) Bond  C44    -   C47    ...       1.43 Ang.
PLAT371_ALERT_2_C Long   C(sp2)-C(sp1) Bond  C48    -   C49    ...       1.43 Ang.
PLAT790_ALERT_4_C Centre of Gravity not Within Unit Cell: Resd.  #          1
              C27 H19 N3 O5 W

Alert level G
ABSTM02_ALERT_3_G  When printed, the submitted absorption T values will be
            replaced by the scaled T values. Since the ratio of scaled T's
            is identical to the ratio of reported T values, the scaling
            does not imply a change to the absorption corrections used in
            the study.
            Ratio of Tmax expected/reported      0.705
            Tmax scaled      0.695 Tmin scaled      0.348

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

   1 ALERT type 1 CIF construction/syntax error, inconsistent or missing data
  15 ALERT type 2 Indicator that the structure model may be wrong or deficient
   4 ALERT type 3 Indicator that the structure quality may be low
   2 ALERT type 4 Improvement, methodology, query or suggestion
   0 ALERT type 5 Informative message, check

---

Computing details

Data collection: SMART (Bruker, 2001); cell refinement: SMART; data reduction: SAINT (Bruker, 2001); 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).

Pentacarbonyl{N,N-dimethyl-N'-[4-(pyridin-4-ylethynyl-κN)benzylidene]benzene- 1,4-diamine}tungsten(0)

Crystal data

[W(C22H19N3)(CO)5]	Z = 4
Mr = 649.30	F(000) = 1264
Triclinic, P1	Dx = 1.682 Mg m^−3 Dm = 1.682 Mg m^−3 Dm measured by not measured
Hall symbol: -P 1	Mo Kα radiation, λ = 0.71073 Å
a = 12.2258 (2) Å	Cell parameters from 9811 reflections
b = 12.5046 (2) Å	θ = 2.4–29.3°
c = 17.3157 (3) Å	µ = 4.55 mm^−1
α = 102.595 (1)°	T = 100 K
β = 95.362 (1)°	Plate, red
γ = 93.249 (1)°	0.3 × 0.25 × 0.08 mm
V = 2564.09 (7) Å^3

Data collection

Bruker SMART CCD area-detector diffractometer	9009 independent reflections
Radiation source: fine-focus sealed tube	7221 reflections with I > 2σ(I)
Graphite monochromator	Rint = 0.060
φ and ω scans	θmax = 25.0°, θmin = 1.2°
Absorption correction: multi-scan (SADABS; Bruker, 2001)	h = −14→14
Tmin = 0.493, Tmax = 0.986	k = −14→14
39209 measured reflections	l = −20→20

Refinement

Refinement on F^2	Secondary atom site location: difference Fourier map
Least-squares matrix: full	Hydrogen site location: inferred from neighbouring sites
R[F^2 > 2σ(F^2)] = 0.022	H-atom parameters constrained
wR(F^2) = 0.049	w = 1/[σ^2(Fo^2) + (0.0204P)^2] where P = (Fo^2 + 2Fc^2)/3
S = 0.99	(Δ/σ)max = 0.002
9009 reflections	Δρmax = 0.54 e Å^−3
650 parameters	Δρmin = −0.94 e Å^−3
0 restraints	Extinction correction: SHELXL97, Fc^*=kFc[1+0.001xFc^2λ^3/sin(2θ)]^-1/4
Primary atom site location: structure-invariant direct methods	Extinction coefficient: 0.00043 (5)

Special details

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

Refinement. Refinement of F² against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F², conventional R-factors R are based on F, with F set to zero for negative F². The threshold expression of F² > σ(F²) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F² are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger.

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

	x	y	z	Uiso*/Ueq
W1	0.313430 (9)	0.065464 (10)	0.581730 (8)	0.04472 (6)
W2	0.197581 (10)	0.435429 (10)	0.434860 (8)	0.04733 (6)
O1	0.5483 (2)	0.0570 (2)	0.67523 (17)	0.0807 (8)
O2	0.2822 (2)	0.3026 (2)	0.68455 (17)	0.0843 (8)
O3	0.0996 (2)	0.0827 (2)	0.46951 (18)	0.0943 (9)
O4	0.3294 (3)	−0.1655 (2)	0.46542 (19)	0.1044 (10)
O5	0.4319 (2)	0.1786 (2)	0.46525 (18)	0.0947 (9)
O6	−0.0325 (2)	0.4438 (2)	0.33517 (15)	0.0718 (7)
O7	0.1721 (3)	0.6669 (2)	0.54753 (18)	0.1022 (10)
O8	0.4163 (3)	0.4261 (3)	0.5458 (2)	0.1201 (12)
O9	0.2271 (2)	0.1980 (2)	0.33270 (16)	0.0731 (7)
O10	0.0686 (2)	0.3270 (2)	0.54908 (17)	0.0883 (9)
N11	0.22107 (19)	−0.02356 (19)	0.66027 (15)	0.0419 (6)
N12	−0.2356 (2)	−0.5262 (2)	1.05873 (16)	0.0519 (7)
N13	−0.4645 (3)	−0.7601 (3)	1.24377 (19)	0.0770 (9)
N41	0.2915 (2)	0.5192 (2)	0.35461 (14)	0.0462 (6)
N42	0.7365 (2)	1.0359 (2)	−0.03675 (17)	0.0635 (8)
N43	0.9494 (2)	1.2434 (2)	−0.24533 (18)	0.0677 (8)
C1	0.4624 (3)	0.0585 (2)	0.6437 (2)	0.0536 (8)
C2	0.2925 (2)	0.2155 (3)	0.6508 (2)	0.0512 (8)
C3	0.1738 (3)	0.0766 (3)	0.5133 (2)	0.0581 (9)
C4	0.3271 (3)	−0.0828 (3)	0.5083 (2)	0.0594 (9)
C5	0.3895 (3)	0.1377 (3)	0.5099 (2)	0.0619 (9)
C6	0.0508 (3)	0.4420 (2)	0.36930 (19)	0.0492 (8)
C7	0.1795 (3)	0.5843 (3)	0.5063 (2)	0.0637 (10)
C8	0.3392 (3)	0.4287 (3)	0.5040 (2)	0.0720 (11)
C9	0.2184 (2)	0.2842 (3)	0.36754 (19)	0.0478 (8)
C10	0.1174 (3)	0.3662 (3)	0.5069 (2)	0.0631 (10)
C12	0.2539 (3)	−0.0220 (3)	0.73593 (19)	0.0607 (9)
H12	0.3180	0.0210	0.7593	0.073*
C13	0.1995 (3)	−0.0799 (3)	0.78199 (19)	0.0632 (9)
H13	0.2282	−0.0773	0.8341	0.076*
C14	0.1018 (3)	−0.1419 (2)	0.75006 (19)	0.0468 (8)
C15	0.0677 (2)	−0.1443 (2)	0.67202 (18)	0.0529 (8)
H15	0.0032	−0.1857	0.6475	0.063*
C16	0.1278 (2)	−0.0865 (2)	0.63020 (18)	0.0523 (8)
H16	0.1025	−0.0909	0.5772	0.063*
C17	0.0406 (3)	−0.2011 (3)	0.79510 (19)	0.0537 (8)
C18	−0.0154 (3)	−0.2538 (3)	0.82876 (18)	0.0509 (8)
C19	−0.0812 (3)	−0.3173 (2)	0.86992 (18)	0.0476 (8)
C20	−0.1922 (3)	−0.3451 (3)	0.84620 (18)	0.0604 (9)
H20	−0.2253	−0.3225	0.8025	0.072*
C21	−0.2543 (3)	−0.4056 (3)	0.88602 (18)	0.0600 (9)
H21	−0.3287	−0.4236	0.8687	0.072*
C22	−0.2080 (3)	−0.4399 (2)	0.95134 (18)	0.0470 (8)
C23	−0.0978 (3)	−0.4115 (3)	0.97504 (19)	0.0592 (9)
H23	−0.0650	−0.4336	1.0190	0.071*
C24	−0.0351 (3)	−0.3514 (3)	0.93554 (19)	0.0608 (9)
H24	0.0393	−0.3334	0.9531	0.073*
C25	−0.2752 (3)	−0.5011 (2)	0.99520 (19)	0.0530 (8)
H25	−0.3487	−0.5222	0.9761	0.064*
C26	−0.2988 (2)	−0.5862 (2)	1.10217 (19)	0.0486 (8)
C27	−0.3969 (3)	−0.6506 (3)	1.07185 (19)	0.0594 (9)
H27	−0.4269	−0.6541	1.0199	0.071*
C28	−0.4496 (3)	−0.7090 (3)	1.1182 (2)	0.0633 (9)
H28	−0.5144	−0.7520	1.0966	0.076*
C29	−0.4087 (3)	−0.7056 (3)	1.1966 (2)	0.0549 (8)
C30	−0.3092 (3)	−0.6428 (3)	1.2252 (2)	0.0623 (9)
H30	−0.2780	−0.6396	1.2768	0.075*
C31	−0.2573 (3)	−0.5861 (3)	1.17828 (19)	0.0585 (9)
H31	−0.1909	−0.5456	1.1990	0.070*
C32	−0.4230 (3)	−0.7540 (3)	1.3242 (2)	0.0838 (12)
H32A	−0.4726	−0.7964	1.3479	0.126*
H32B	−0.4165	−0.6787	1.3532	0.126*
H32C	−0.3519	−0.7828	1.3259	0.126*
C33	−0.5566 (3)	−0.8394 (3)	1.2085 (2)	0.0890 (13)
H33A	−0.5862	−0.8698	1.2493	0.134*
H33B	−0.5319	−0.8973	1.1695	0.134*
H33C	−0.6127	−0.8036	1.1835	0.134*
C42	0.3854 (2)	0.4820 (2)	0.32692 (18)	0.0509 (8)
H42	0.4105	0.4190	0.3405	0.061*
C43	0.4455 (2)	0.5320 (3)	0.28000 (18)	0.0521 (8)
H43	0.5097	0.5033	0.2628	0.063*
C44	0.4104 (3)	0.6250 (3)	0.25842 (18)	0.0486 (8)
C45	0.3137 (3)	0.6640 (2)	0.28605 (18)	0.0559 (9)
H45	0.2868	0.7264	0.2727	0.067*
C46	0.2587 (3)	0.6097 (3)	0.33323 (19)	0.0547 (8)
H46	0.1945	0.6374	0.3515	0.066*
C47	0.4702 (3)	0.6786 (3)	0.20825 (19)	0.0566 (9)
C48	0.5226 (3)	0.7247 (3)	0.16878 (19)	0.0571 (9)
C49	0.5866 (3)	0.7831 (3)	0.12359 (18)	0.0537 (9)
C50	0.5437 (3)	0.8695 (3)	0.09530 (19)	0.0590 (9)
H50	0.4733	0.8892	0.1054	0.071*
C51	0.6052 (3)	0.9256 (3)	0.05241 (19)	0.0584 (9)
H51	0.5765	0.9843	0.0346	0.070*
C52	0.7093 (3)	0.8964 (3)	0.03514 (19)	0.0553 (9)
C53	0.7520 (3)	0.8130 (3)	0.0652 (2)	0.0692 (10)
H53	0.8229	0.7945	0.0560	0.083*
C54	0.6921 (3)	0.7565 (3)	0.1085 (2)	0.0660 (10)
H54	0.7226	0.6998	0.1280	0.079*
C55	0.7717 (3)	0.9545 (3)	−0.0136 (2)	0.0638 (10)
H55	0.8391	0.9305	−0.0278	0.077*
C56	0.7950 (3)	1.0851 (3)	−0.0890 (2)	0.0589 (9)
C57	0.8431 (3)	1.0270 (3)	−0.1520 (2)	0.0839 (13)
H57	0.8410	0.9508	−0.1604	0.101*
C58	0.8942 (3)	1.0781 (3)	−0.2030 (2)	0.0845 (13)
H58	0.9242	1.0356	−0.2457	0.101*
C59	0.9024 (3)	1.1920 (3)	−0.1923 (2)	0.0596 (9)
C60	0.8524 (3)	1.2506 (3)	−0.1284 (2)	0.0647 (9)
H60	0.8556	1.3269	−0.1190	0.078*
C61	0.7986 (3)	1.1981 (3)	−0.07916 (19)	0.0631 (9)
H61	0.7640	1.2393	−0.0384	0.076*
C62	1.0026 (4)	1.1790 (3)	−0.3077 (3)	0.1128 (17)
H62A	1.0310	1.2257	−0.3397	0.169*
H62B	0.9504	1.1234	−0.3403	0.169*
H62C	1.0621	1.1449	−0.2849	0.169*
C63	0.9974 (3)	1.3559 (3)	−0.2158 (2)	0.0896 (13)
H63A	1.0277	1.3816	−0.2583	0.134*
H63B	1.0546	1.3581	−0.1735	0.134*
H63C	0.9413	1.4022	−0.1963	0.134*

Atomic displacement parameters (Ų)

	U^11	U^22	U^33	U^12	U^13	U^23
W1	0.03965 (8)	0.04785 (9)	0.04712 (10)	−0.00122 (6)	0.00423 (6)	0.01306 (7)
W2	0.05498 (9)	0.04632 (10)	0.03995 (9)	−0.00594 (6)	0.00240 (6)	0.01181 (6)
O1	0.0511 (15)	0.0865 (19)	0.101 (2)	0.0048 (13)	−0.0110 (15)	0.0218 (16)
O2	0.089 (2)	0.0609 (18)	0.092 (2)	0.0118 (15)	−0.0071 (16)	−0.0004 (15)
O3	0.0728 (19)	0.110 (2)	0.102 (2)	−0.0090 (16)	−0.0348 (17)	0.0496 (19)
O4	0.104 (2)	0.083 (2)	0.105 (3)	−0.0024 (18)	0.0271 (19)	−0.0268 (19)
O5	0.090 (2)	0.114 (2)	0.105 (2)	0.0101 (17)	0.0442 (17)	0.0647 (19)
O6	0.0614 (16)	0.0793 (18)	0.0717 (18)	0.0041 (14)	−0.0034 (14)	0.0155 (14)
O7	0.131 (3)	0.071 (2)	0.091 (2)	−0.0078 (18)	0.0313 (19)	−0.0169 (17)
O8	0.108 (2)	0.128 (3)	0.114 (3)	−0.022 (2)	−0.058 (2)	0.044 (2)
O9	0.0825 (18)	0.0561 (17)	0.0771 (19)	0.0088 (14)	0.0095 (14)	0.0060 (14)
O10	0.113 (2)	0.087 (2)	0.084 (2)	0.0078 (16)	0.0421 (18)	0.0480 (17)
N11	0.0419 (14)	0.0407 (15)	0.0412 (16)	−0.0001 (11)	−0.0024 (12)	0.0084 (12)
N12	0.0550 (16)	0.0523 (17)	0.0520 (18)	0.0029 (13)	0.0100 (14)	0.0180 (14)
N13	0.077 (2)	0.095 (3)	0.069 (2)	−0.0108 (18)	0.0214 (18)	0.0373 (19)
N41	0.0497 (16)	0.0410 (16)	0.0461 (16)	−0.0036 (12)	−0.0010 (13)	0.0103 (13)
N42	0.0717 (19)	0.0565 (19)	0.065 (2)	−0.0039 (15)	0.0248 (16)	0.0140 (16)
N43	0.074 (2)	0.062 (2)	0.082 (2)	0.0125 (16)	0.0379 (18)	0.0337 (17)
C1	0.050 (2)	0.046 (2)	0.063 (2)	−0.0001 (16)	0.0009 (18)	0.0111 (17)
C2	0.0431 (18)	0.056 (2)	0.051 (2)	−0.0026 (16)	−0.0064 (16)	0.0123 (18)
C3	0.055 (2)	0.059 (2)	0.060 (2)	−0.0106 (17)	0.0026 (19)	0.0185 (18)
C4	0.051 (2)	0.068 (3)	0.057 (2)	−0.0025 (18)	0.0072 (18)	0.0097 (19)
C5	0.051 (2)	0.069 (2)	0.069 (3)	0.0027 (17)	0.0056 (19)	0.023 (2)
C6	0.060 (2)	0.0437 (19)	0.043 (2)	−0.0033 (16)	0.0112 (18)	0.0073 (15)
C7	0.071 (2)	0.072 (3)	0.045 (2)	−0.014 (2)	0.0069 (18)	0.011 (2)
C8	0.085 (3)	0.065 (2)	0.060 (3)	−0.015 (2)	−0.014 (2)	0.014 (2)
C9	0.0480 (19)	0.051 (2)	0.045 (2)	0.0004 (16)	0.0009 (16)	0.0157 (17)
C10	0.081 (3)	0.057 (2)	0.053 (2)	0.0000 (19)	0.004 (2)	0.0173 (18)
C12	0.065 (2)	0.064 (2)	0.044 (2)	−0.0206 (17)	−0.0046 (18)	0.0028 (17)
C13	0.079 (2)	0.071 (2)	0.0349 (19)	−0.0173 (19)	−0.0007 (18)	0.0108 (17)
C14	0.055 (2)	0.0418 (18)	0.044 (2)	0.0047 (15)	0.0103 (16)	0.0098 (15)
C15	0.0459 (18)	0.063 (2)	0.050 (2)	−0.0122 (15)	−0.0013 (16)	0.0218 (17)
C16	0.0463 (18)	0.063 (2)	0.045 (2)	−0.0092 (16)	−0.0060 (16)	0.0162 (17)
C17	0.064 (2)	0.051 (2)	0.046 (2)	0.0008 (17)	0.0076 (17)	0.0102 (16)
C18	0.062 (2)	0.051 (2)	0.043 (2)	0.0101 (16)	0.0135 (17)	0.0126 (16)
C19	0.065 (2)	0.0447 (19)	0.0356 (19)	0.0085 (16)	0.0131 (16)	0.0100 (15)
C20	0.068 (2)	0.071 (2)	0.042 (2)	−0.0080 (18)	−0.0060 (18)	0.0226 (18)
C21	0.061 (2)	0.073 (2)	0.043 (2)	−0.0142 (17)	−0.0044 (17)	0.0157 (18)
C22	0.059 (2)	0.0447 (19)	0.0379 (19)	0.0050 (15)	0.0096 (16)	0.0095 (15)
C23	0.057 (2)	0.078 (2)	0.054 (2)	0.0155 (18)	0.0093 (18)	0.0352 (19)
C24	0.0489 (19)	0.085 (3)	0.059 (2)	0.0124 (18)	0.0115 (17)	0.036 (2)
C25	0.059 (2)	0.050 (2)	0.049 (2)	0.0004 (16)	0.0091 (17)	0.0099 (17)
C26	0.0535 (19)	0.048 (2)	0.047 (2)	0.0042 (16)	0.0124 (17)	0.0142 (16)
C27	0.064 (2)	0.064 (2)	0.048 (2)	−0.0039 (18)	0.0066 (18)	0.0115 (17)
C28	0.060 (2)	0.067 (2)	0.060 (2)	−0.0139 (17)	0.0118 (19)	0.0093 (19)
C29	0.063 (2)	0.054 (2)	0.054 (2)	0.0104 (17)	0.0200 (18)	0.0201 (18)
C30	0.066 (2)	0.072 (2)	0.055 (2)	−0.0030 (19)	0.0032 (19)	0.0292 (19)
C31	0.052 (2)	0.071 (2)	0.056 (2)	−0.0060 (17)	0.0003 (17)	0.0262 (19)
C32	0.098 (3)	0.092 (3)	0.078 (3)	0.020 (2)	0.039 (3)	0.041 (2)
C33	0.081 (3)	0.084 (3)	0.113 (4)	−0.007 (2)	0.037 (3)	0.038 (3)
C42	0.0481 (19)	0.051 (2)	0.054 (2)	0.0019 (16)	−0.0024 (16)	0.0163 (16)
C43	0.0429 (18)	0.060 (2)	0.054 (2)	0.0017 (16)	0.0075 (16)	0.0145 (17)
C44	0.0524 (19)	0.050 (2)	0.0394 (19)	−0.0104 (16)	−0.0007 (16)	0.0082 (16)
C45	0.064 (2)	0.049 (2)	0.060 (2)	0.0013 (17)	0.0118 (18)	0.0214 (17)
C46	0.056 (2)	0.049 (2)	0.060 (2)	0.0040 (16)	0.0141 (17)	0.0125 (18)
C47	0.061 (2)	0.057 (2)	0.045 (2)	−0.0129 (17)	0.0014 (17)	0.0057 (17)
C48	0.066 (2)	0.057 (2)	0.043 (2)	−0.0108 (17)	0.0049 (18)	0.0042 (17)
C49	0.068 (2)	0.047 (2)	0.042 (2)	−0.0128 (17)	0.0088 (17)	0.0038 (16)
C50	0.050 (2)	0.072 (2)	0.055 (2)	−0.0057 (17)	0.0041 (17)	0.0174 (19)
C51	0.058 (2)	0.063 (2)	0.056 (2)	−0.0065 (17)	0.0010 (18)	0.0222 (18)
C52	0.065 (2)	0.051 (2)	0.049 (2)	−0.0041 (17)	0.0169 (18)	0.0056 (17)
C53	0.078 (2)	0.055 (2)	0.081 (3)	0.0083 (19)	0.041 (2)	0.014 (2)
C54	0.085 (3)	0.048 (2)	0.071 (3)	0.0128 (19)	0.033 (2)	0.0133 (18)
C55	0.073 (2)	0.053 (2)	0.067 (3)	0.0002 (19)	0.032 (2)	0.0087 (19)
C56	0.064 (2)	0.049 (2)	0.067 (2)	0.0012 (17)	0.0284 (19)	0.0144 (18)
C57	0.127 (3)	0.041 (2)	0.097 (3)	0.015 (2)	0.064 (3)	0.018 (2)
C58	0.121 (3)	0.056 (3)	0.091 (3)	0.021 (2)	0.069 (3)	0.021 (2)
C59	0.065 (2)	0.054 (2)	0.066 (2)	0.0111 (17)	0.0232 (19)	0.0197 (19)
C60	0.080 (2)	0.045 (2)	0.074 (3)	0.0035 (18)	0.024 (2)	0.0160 (18)
C61	0.076 (2)	0.050 (2)	0.064 (2)	0.0054 (17)	0.029 (2)	0.0054 (18)
C62	0.147 (4)	0.098 (3)	0.121 (4)	0.026 (3)	0.089 (4)	0.047 (3)
C63	0.096 (3)	0.085 (3)	0.093 (3)	−0.023 (2)	0.016 (3)	0.037 (2)

Geometric parameters (Å, º)

W1—C5	1.960 (4)	C24—H24	0.9300
W1—C3	2.014 (4)	C25—H25	0.9300
W1—C4	2.032 (4)	C26—C31	1.367 (4)
W1—C2	2.037 (4)	C26—C27	1.397 (4)
W1—C1	2.042 (3)	C27—C28	1.375 (4)
W1—N11	2.273 (2)	C27—H27	0.9300
W2—C10	1.967 (4)	C28—C29	1.393 (4)
W2—C8	2.028 (4)	C28—H28	0.9300
W2—C7	2.035 (4)	C29—C30	1.397 (4)
W2—C9	2.037 (4)	C30—C31	1.365 (4)
W2—C6	2.047 (4)	C30—H30	0.9300
W2—N41	2.267 (2)	C31—H31	0.9300
O1—C1	1.140 (4)	C32—H32A	0.9600
O2—C2	1.138 (4)	C32—H32B	0.9600
O3—C3	1.144 (4)	C32—H32C	0.9600
O4—C4	1.137 (4)	C33—H33A	0.9600
O5—C5	1.159 (4)	C33—H33B	0.9600
O6—C6	1.133 (4)	C33—H33C	0.9600
O7—C7	1.133 (4)	C42—C43	1.368 (4)
O8—C8	1.139 (4)	C42—H42	0.9300
O9—C9	1.130 (4)	C43—C44	1.375 (4)
O10—C10	1.156 (4)	C43—H43	0.9300
N11—C12	1.330 (4)	C44—C45	1.390 (4)
N11—C16	1.341 (4)	C44—C47	1.435 (4)
N12—C25	1.269 (4)	C45—C46	1.370 (4)
N12—C26	1.419 (4)	C45—H45	0.9300
N13—C29	1.374 (4)	C46—H46	0.9300
N13—C32	1.421 (4)	C47—C48	1.192 (4)
N13—C33	1.452 (4)	C48—C49	1.434 (4)
N41—C46	1.336 (4)	C49—C54	1.385 (4)
N41—C42	1.353 (4)	C49—C50	1.389 (4)
N42—C55	1.256 (4)	C50—C51	1.372 (4)
N42—C56	1.422 (4)	C50—H50	0.9300
N43—C59	1.378 (4)	C51—C52	1.385 (4)
N43—C62	1.431 (4)	C51—H51	0.9300
N43—C63	1.457 (4)	C52—C53	1.371 (4)
C12—C13	1.378 (4)	C52—C55	1.465 (4)
C12—H12	0.9300	C53—C54	1.368 (4)
C13—C14	1.385 (4)	C53—H53	0.9300
C13—H13	0.9300	C54—H54	0.9300
C14—C15	1.370 (4)	C55—H55	0.9300
C14—C17	1.420 (4)	C56—C57	1.374 (4)
C15—C16	1.362 (4)	C56—C61	1.383 (4)
C15—H15	0.9300	C57—C58	1.372 (4)
C16—H16	0.9300	C57—H57	0.9300
C17—C18	1.197 (4)	C58—C59	1.393 (4)
C18—C19	1.438 (4)	C58—H58	0.9300
C19—C24	1.382 (4)	C59—C60	1.400 (4)
C19—C20	1.382 (4)	C60—C61	1.375 (4)
C20—C21	1.372 (4)	C60—H60	0.9300
C20—H20	0.9300	C61—H61	0.9300
C21—C22	1.380 (4)	C62—H62A	0.9600
C21—H21	0.9300	C62—H62B	0.9600
C22—C23	1.375 (4)	C62—H62C	0.9600
C22—C25	1.462 (4)	C63—H63A	0.9600
C23—C24	1.370 (4)	C63—H63B	0.9600
C23—H23	0.9300	C63—H63C	0.9600
C5—W1—C3	86.11 (13)	C28—C27—C26	120.5 (3)
C5—W1—C4	89.60 (14)	C28—C27—H27	119.7
C3—W1—C4	87.78 (14)	C26—C27—H27	119.7
C5—W1—C2	89.67 (14)	C27—C28—C29	121.9 (3)
C3—W1—C2	88.97 (13)	C27—C28—H28	119.1
C4—W1—C2	176.70 (12)	C29—C28—H28	119.1
C5—W1—C1	88.92 (13)	N13—C29—C28	121.6 (3)
C3—W1—C1	174.96 (12)	N13—C29—C30	121.7 (3)
C4—W1—C1	91.34 (13)	C28—C29—C30	116.7 (3)
C2—W1—C1	91.86 (12)	C31—C30—C29	120.7 (3)
C5—W1—N11	177.46 (11)	C31—C30—H30	119.6
C3—W1—N11	92.18 (11)	C29—C30—H30	119.6
C4—W1—N11	88.46 (11)	C30—C31—C26	122.9 (3)
C2—W1—N11	92.18 (11)	C30—C31—H31	118.6
C1—W1—N11	92.75 (11)	C26—C31—H31	118.6
C10—W2—C8	88.52 (15)	N13—C32—H32A	109.5
C10—W2—C7	88.47 (14)	N13—C32—H32B	109.5
C8—W2—C7	88.35 (15)	H32A—C32—H32B	109.5
C10—W2—C9	90.01 (13)	N13—C32—H32C	109.5
C8—W2—C9	89.68 (14)	H32A—C32—H32C	109.5
C7—W2—C9	177.54 (13)	H32B—C32—H32C	109.5
C10—W2—C6	89.17 (13)	N13—C33—H33A	109.5
C8—W2—C6	177.47 (13)	N13—C33—H33B	109.5
C7—W2—C6	90.57 (13)	H33A—C33—H33B	109.5
C9—W2—C6	91.34 (12)	N13—C33—H33C	109.5
C10—W2—N41	178.46 (11)	H33A—C33—H33C	109.5
C8—W2—N41	90.78 (12)	H33B—C33—H33C	109.5
C7—W2—N41	90.14 (11)	N41—C42—C43	123.5 (3)
C9—W2—N41	91.36 (10)	N41—C42—H42	118.2
C6—W2—N41	91.51 (10)	C43—C42—H42	118.2
C12—N11—C16	114.9 (3)	C42—C43—C44	119.7 (3)
C12—N11—W1	125.0 (2)	C42—C43—H43	120.1
C16—N11—W1	120.1 (2)	C44—C43—H43	120.1
C25—N12—C26	122.7 (3)	C43—C44—C45	117.5 (3)
C29—N13—C32	121.0 (3)	C43—C44—C47	121.3 (3)
C29—N13—C33	119.9 (3)	C45—C44—C47	121.2 (3)
C32—N13—C33	118.3 (3)	C46—C45—C44	119.3 (3)
C46—N41—C42	116.0 (3)	C46—C45—H45	120.4
C46—N41—W2	122.0 (2)	C44—C45—H45	120.4
C42—N41—W2	122.1 (2)	N41—C46—C45	124.0 (3)
C55—N42—C56	120.2 (3)	N41—C46—H46	118.0
C59—N43—C62	118.9 (3)	C45—C46—H46	118.0
C59—N43—C63	117.9 (3)	C48—C47—C44	177.7 (3)
C62—N43—C63	114.9 (3)	C47—C48—C49	178.1 (3)
O1—C1—W1	176.2 (3)	C54—C49—C50	118.8 (3)
O2—C2—W1	174.8 (3)	C54—C49—C48	121.2 (3)
O3—C3—W1	174.5 (3)	C50—C49—C48	120.0 (3)
O4—C4—W1	176.5 (3)	C51—C50—C49	119.9 (3)
O5—C5—W1	177.6 (3)	C51—C50—H50	120.0
O6—C6—W2	177.2 (3)	C49—C50—H50	120.0
O7—C7—W2	177.9 (4)	C50—C51—C52	121.2 (3)
O8—C8—W2	176.9 (4)	C50—C51—H51	119.4
O9—C9—W2	176.6 (3)	C52—C51—H51	119.4
O10—C10—W2	178.6 (3)	C53—C52—C51	118.3 (3)
N11—C12—C13	124.4 (3)	C53—C52—C55	121.4 (3)
N11—C12—H12	117.8	C51—C52—C55	120.3 (3)
C13—C12—H12	117.8	C54—C53—C52	121.3 (3)
C12—C13—C14	119.5 (3)	C54—C53—H53	119.3
C12—C13—H13	120.3	C52—C53—H53	119.3
C14—C13—H13	120.3	C53—C54—C49	120.4 (3)
C15—C14—C13	116.4 (3)	C53—C54—H54	119.8
C15—C14—C17	121.4 (3)	C49—C54—H54	119.8
C13—C14—C17	122.1 (3)	N42—C55—C52	121.8 (3)
C16—C15—C14	120.3 (3)	N42—C55—H55	119.1
C16—C15—H15	119.9	C52—C55—H55	119.1
C14—C15—H15	119.9	C57—C56—C61	117.3 (3)
N11—C16—C15	124.5 (3)	C57—C56—N42	124.1 (3)
N11—C16—H16	117.8	C61—C56—N42	118.4 (3)
C15—C16—H16	117.8	C58—C57—C56	121.9 (3)
C18—C17—C14	175.8 (4)	C58—C57—H57	119.1
C17—C18—C19	179.1 (4)	C56—C57—H57	119.1
C24—C19—C20	117.8 (3)	C57—C58—C59	121.6 (3)
C24—C19—C18	120.6 (3)	C57—C58—H58	119.2
C20—C19—C18	121.6 (3)	C59—C58—H58	119.2
C21—C20—C19	121.1 (3)	N43—C59—C58	121.8 (3)
C21—C20—H20	119.5	N43—C59—C60	121.9 (3)
C19—C20—H20	119.5	C58—C59—C60	116.2 (3)
C20—C21—C22	121.0 (3)	C61—C60—C59	121.6 (3)
C20—C21—H21	119.5	C61—C60—H60	119.2
C22—C21—H21	119.5	C59—C60—H60	119.2
C23—C22—C21	117.7 (3)	C60—C61—C56	121.4 (3)
C23—C22—C25	121.4 (3)	C60—C61—H61	119.3
C21—C22—C25	120.9 (3)	C56—C61—H61	119.3
C24—C23—C22	121.7 (3)	N43—C62—H62A	109.5
C24—C23—H23	119.1	N43—C62—H62B	109.5
C22—C23—H23	119.1	H62A—C62—H62B	109.5
C23—C24—C19	120.7 (3)	N43—C62—H62C	109.5
C23—C24—H24	119.7	H62A—C62—H62C	109.5
C19—C24—H24	119.7	H62B—C62—H62C	109.5
N12—C25—C22	121.5 (3)	N43—C63—H63A	109.5
N12—C25—H25	119.3	N43—C63—H63B	109.5
C22—C25—H25	119.3	H63A—C63—H63B	109.5
C31—C26—C27	117.2 (3)	N43—C63—H63C	109.5
C31—C26—N12	117.5 (3)	H63A—C63—H63C	109.5
C27—C26—N12	125.2 (3)	H63B—C63—H63C	109.5