Supporting information
Crystallographic Information File (CIF) https://doi.org/10.1107/S1600536807002152/ww2078sup1.cif | |
Structure factor file (CIF format) https://doi.org/10.1107/S1600536807002152/ww2078Isup2.hkl |
CCDC reference: 636838
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).
[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) Å3 |
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 on F2 | Secondary atom site location: difference Fourier map |
Least-squares matrix: full | Hydrogen site location: inferred from neighbouring sites |
R[F2 > 2σ(F2)] = 0.022 | H-atom parameters constrained |
wR(F2) = 0.049 | w = 1/[σ2(Fo2) + (0.0204P)2] where P = (Fo2 + 2Fc2)/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+0.001xFc2λ3/sin(2θ)]-1/4 |
Primary atom site location: structure-invariant direct methods | Extinction coefficient: 0.00043 (5) |
Geometry. All e.s.d.'s (except the e.s.d. in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell e.s.d.'s are taken into account individually in the estimation of e.s.d.'s in distances, angles and torsion angles; correlations between e.s.d.'s in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell e.s.d.'s is used for estimating e.s.d.'s involving l.s. planes. |
Refinement. Refinement of F2 against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F2, conventional R-factors R are based on F, with F set to zero for negative F2. The threshold expression of F2 > σ(F2) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F2 are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. |
x | y | z | Uiso*/Ueq | ||
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* |
U11 | U22 | U33 | U12 | U13 | U23 | |
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) |
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 |