Supporting information
Crystallographic Information File (CIF) https://doi.org/10.1107/S205322961901101X/qf3033sup1.cif | |
Structure factor file (CIF format) https://doi.org/10.1107/S205322961901101X/qf30331sup2.hkl | |
Structure factor file (CIF format) https://doi.org/10.1107/S205322961901101X/qf30332sup3.hkl | |
Structure factor file (CIF format) https://doi.org/10.1107/S205322961901101X/qf30333sup4.hkl | |
Portable Document Format (PDF) file https://doi.org/10.1107/S205322961901101X/qf3033sup5.pdf |
CCDC references: 1945886; 1945885; 1945884
Data collection: SMART (Bruker, 2003) for (1), (2); APEX2 (Bruker, 2013) for (3). Cell refinement: SAINT (Bruker, 2003) for (1), (2); SAINT (Bruker, 2013) for (3). Data reduction: SAINT (Bruker, 2003) for (1), (2); SAINT (Bruker, 2013) for (3). For all structures, program(s) used to solve structure: SHELXS97 (Sheldrick, 2008); program(s) used to refine structure: SHELXL2018 (Sheldrick, 2015); molecular graphics: SHELXTL (Sheldrick, 2008); software used to prepare material for publication: SHELXTL (Sheldrick, 2008).
[Nb2(C9H9N)10(C36H36N4)] | F(000) = 4248 |
Mr = 2022.22 | Dx = 1.076 Mg m−3 |
Monoclinic, C2/c | Mo Kα radiation, λ = 0.71073 Å |
a = 32.077 (5) Å | Cell parameters from 3690 reflections |
b = 15.830 (2) Å | θ = 2.3–23.5° |
c = 24.815 (4) Å | µ = 0.23 mm−1 |
β = 97.655 (2)° | T = 173 K |
V = 12488 (3) Å3 | Plate, green-black |
Z = 4 | 0.50 × 0.50 × 0.20 mm |
Bruker SMART CCD platform diffractometer | 6478 reflections with I > 2σ(I) |
Radiation source: normal-focus sealed tube | Rint = 0.051 |
ω scans | θmax = 25.1°, θmin = 1.4° |
Absorption correction: multi-scan (SADABS; Sheldrick, 1996) | h = −24→38 |
Tmin = 0.893, Tmax = 0.955 | k = −17→18 |
22038 measured reflections | l = −17→29 |
10394 independent 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)] = 0.055 | Hydrogen site location: inferred from neighbouring sites |
wR(F2) = 0.144 | H-atom parameters constrained |
S = 1.00 | w = 1/[σ2(Fo2) + (0.0754P)2] where P = (Fo2 + 2Fc2)/3 |
10394 reflections | (Δ/σ)max = 0.001 |
773 parameters | Δρmax = 0.38 e Å−3 |
462 restraints | Δρmin = −0.25 e Å−3 |
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. Reflection contributions from highly disordered solvent were fixed and added to the calculated structure factors using the SQUEEZE routine of program Platon (Spek, 2015), which determined there to be 408 electrons in 1634 Å3 treated this way per unit cell. Because the exact identity and amount of solvent were unknown, no solvent was included in the atom list or molecular formula. Thus all calculated quantities that derive from the molecular formula (e.g., F(000), density, molecular weight, etc.) are known to be incorrect. 2,6-dimethylphenyl group C8-C15 is modeled as disordered over two positions (0.570 (7):0.430 (7)). Isocyanide ligand C7/N7/C57-C63 is modeled as disordered over four positions as an approximation for what appears to be a frozen dynamic disorder (0.417 (3):0.331 (3):0.185 (3):0.067 (3)). For each site of disorder, analogous bond lengths and angles were restrained to be similar. Anisotropic displacement parameters for proximal and related atoms were restrained to be similar and/or constrained to be equivalent. |
x | y | z | Uiso*/Ueq | Occ. (<1) | |
Nb1 | 0.11101 (2) | 0.48958 (2) | 0.98057 (2) | 0.03672 (13) | |
N1 | 0.04468 (9) | 0.4410 (2) | 0.94357 (13) | 0.0428 (8) | |
N2 | 0.06582 (9) | 0.55025 (19) | 1.03720 (12) | 0.0369 (7) | |
N3 | 0.19727 (12) | 0.5470 (2) | 0.93368 (16) | 0.0600 (10) | |
N4 | 0.18134 (10) | 0.5429 (2) | 1.08353 (14) | 0.0499 (9) | |
N5 | 0.14160 (10) | 0.3377 (2) | 0.90392 (15) | 0.0499 (9) | |
N6 | 0.13805 (10) | 0.3208 (2) | 1.05731 (15) | 0.0480 (9) | |
C1 | 0.01683 (11) | 0.4716 (2) | 0.97262 (15) | 0.0360 (9) | |
C2 | 0.02745 (11) | 0.5256 (2) | 1.01901 (15) | 0.0353 (9) | |
C3 | 0.16549 (13) | 0.5279 (2) | 0.95014 (17) | 0.0436 (10) | |
C4 | 0.15651 (11) | 0.5265 (2) | 1.04569 (16) | 0.0392 (9) | |
C5 | 0.13066 (11) | 0.3942 (3) | 0.92927 (17) | 0.0412 (10) | |
C6 | 0.12637 (11) | 0.3801 (3) | 1.03103 (16) | 0.0394 (9) | |
C8 | 0.0355 (10) | 0.3598 (7) | 0.9174 (5) | 0.041 (2) | 0.430 (7) |
C9 | 0.0264 (9) | 0.2836 (10) | 0.9428 (6) | 0.049 (3) | 0.430 (7) |
C10 | 0.0192 (8) | 0.2101 (10) | 0.9109 (6) | 0.079 (4) | 0.430 (7) |
H10 | 0.012406 | 0.158791 | 0.927615 | 0.094* | 0.430 (7) |
C11 | 0.0218 (6) | 0.2110 (9) | 0.8548 (6) | 0.084 (4) | 0.430 (7) |
H11 | 0.017064 | 0.160482 | 0.834290 | 0.100* | 0.430 (7) |
C12 | 0.0313 (8) | 0.2860 (10) | 0.8290 (6) | 0.083 (4) | 0.430 (7) |
H12 | 0.033698 | 0.287014 | 0.791227 | 0.100* | 0.430 (7) |
C13 | 0.0372 (6) | 0.3595 (8) | 0.8606 (5) | 0.046 (3) | 0.430 (7) |
C14 | 0.0222 (12) | 0.282 (2) | 1.0021 (7) | 0.063 (4) | 0.430 (7) |
H14A | 0.047974 | 0.304354 | 1.022962 | 0.094* | 0.430 (7) |
H14B | 0.017459 | 0.224223 | 1.013488 | 0.094* | 0.430 (7) |
H14C | −0.001732 | 0.317658 | 1.008756 | 0.094* | 0.430 (7) |
C15 | 0.0452 (7) | 0.4396 (11) | 0.8316 (8) | 0.063 (3) | 0.430 (7) |
H15A | 0.022617 | 0.480050 | 0.835061 | 0.094* | 0.430 (7) |
H15B | 0.046218 | 0.427519 | 0.793060 | 0.094* | 0.430 (7) |
H15C | 0.072192 | 0.463735 | 0.847712 | 0.094* | 0.430 (7) |
C8' | 0.0339 (7) | 0.3790 (5) | 0.9015 (3) | 0.041 (2) | 0.570 (7) |
C9' | 0.0261 (6) | 0.2992 (7) | 0.9210 (4) | 0.049 (3) | 0.570 (7) |
C10' | 0.0197 (5) | 0.2332 (8) | 0.8825 (5) | 0.079 (4) | 0.570 (7) |
H10' | 0.014203 | 0.177333 | 0.893628 | 0.094* | 0.570 (7) |
C11' | 0.0215 (4) | 0.2511 (7) | 0.8279 (5) | 0.084 (4) | 0.570 (7) |
H11' | 0.016482 | 0.206766 | 0.802081 | 0.100* | 0.570 (7) |
C12' | 0.0302 (5) | 0.3314 (7) | 0.8099 (5) | 0.083 (4) | 0.570 (7) |
H12' | 0.031684 | 0.340935 | 0.772420 | 0.100* | 0.570 (7) |
C13' | 0.0369 (4) | 0.3979 (6) | 0.8469 (4) | 0.046 (3) | 0.570 (7) |
C14' | 0.0263 (9) | 0.2789 (16) | 0.9802 (5) | 0.063 (4) | 0.570 (7) |
H14D | 0.052469 | 0.299260 | 1.000912 | 0.094* | 0.570 (7) |
H14E | 0.024130 | 0.217617 | 0.984690 | 0.094* | 0.570 (7) |
H14F | 0.002269 | 0.306539 | 0.993459 | 0.094* | 0.570 (7) |
C15' | 0.0452 (5) | 0.4856 (7) | 0.8286 (6) | 0.063 (3) | 0.570 (7) |
H15D | 0.030193 | 0.526137 | 0.848859 | 0.094* | 0.570 (7) |
H15E | 0.035325 | 0.490989 | 0.789634 | 0.094* | 0.570 (7) |
H15F | 0.075446 | 0.497160 | 0.835292 | 0.094* | 0.570 (7) |
C16 | 0.07426 (11) | 0.5846 (3) | 1.09123 (16) | 0.0420 (10) | |
C17 | 0.07078 (13) | 0.5331 (3) | 1.13580 (18) | 0.0549 (12) | |
C18 | 0.08118 (16) | 0.5678 (4) | 1.1880 (2) | 0.0786 (16) | |
H18 | 0.078891 | 0.534016 | 1.219111 | 0.094* | |
C19 | 0.09474 (16) | 0.6509 (4) | 1.1946 (2) | 0.0847 (18) | |
H19 | 0.101076 | 0.674062 | 1.230109 | 0.102* | |
C20 | 0.09887 (14) | 0.6983 (4) | 1.1511 (2) | 0.0727 (15) | |
H20 | 0.108911 | 0.754551 | 1.156327 | 0.087* | |
C21 | 0.08891 (13) | 0.6678 (3) | 1.0982 (2) | 0.0564 (12) | |
C22 | 0.05723 (16) | 0.4428 (3) | 1.1288 (2) | 0.0740 (15) | |
H22A | 0.028016 | 0.440492 | 1.111220 | 0.111* | |
H22B | 0.059411 | 0.415370 | 1.164422 | 0.111* | |
H22C | 0.075398 | 0.413516 | 1.106035 | 0.111* | |
C23 | 0.09445 (16) | 0.7228 (3) | 1.0511 (2) | 0.0769 (16) | |
H23A | 0.106432 | 0.777092 | 1.064364 | 0.115* | |
H23B | 0.067100 | 0.732299 | 1.029247 | 0.115* | |
H23C | 0.113478 | 0.695305 | 1.028760 | 0.115* | |
C24 | 0.23068 (13) | 0.5715 (3) | 0.9067 (2) | 0.0522 (11) | |
C25 | 0.22221 (15) | 0.6082 (3) | 0.8558 (2) | 0.0617 (13) | |
C26 | 0.25588 (19) | 0.6324 (3) | 0.8300 (2) | 0.0801 (16) | |
H26 | 0.250920 | 0.657956 | 0.795068 | 0.096* | |
C27 | 0.2964 (2) | 0.6198 (4) | 0.8541 (3) | 0.0875 (19) | |
H27 | 0.319088 | 0.636749 | 0.835677 | 0.105* | |
C28 | 0.30469 (15) | 0.5831 (3) | 0.9045 (3) | 0.0777 (17) | |
H28 | 0.332990 | 0.575502 | 0.920724 | 0.093* | |
C29 | 0.27134 (15) | 0.5566 (3) | 0.9325 (2) | 0.0632 (13) | |
C30 | 0.17781 (16) | 0.6246 (3) | 0.8284 (2) | 0.0800 (16) | |
H30A | 0.163339 | 0.662148 | 0.851231 | 0.120* | |
H30B | 0.162537 | 0.570936 | 0.823299 | 0.120* | |
H30C | 0.178880 | 0.651206 | 0.792966 | 0.120* | |
C31 | 0.27966 (17) | 0.5121 (3) | 0.9868 (3) | 0.0856 (17) | |
H31A | 0.264747 | 0.541501 | 1.013302 | 0.128* | |
H31B | 0.309925 | 0.512470 | 0.999493 | 0.128* | |
H31C | 0.269685 | 0.453670 | 0.982848 | 0.128* | |
C32 | 0.21258 (11) | 0.5657 (3) | 1.12518 (17) | 0.0435 (10) | |
C33 | 0.23594 (14) | 0.6372 (3) | 1.11786 (18) | 0.0562 (12) | |
C34 | 0.26788 (16) | 0.6569 (3) | 1.1595 (2) | 0.0782 (16) | |
H34 | 0.284997 | 0.705037 | 1.155943 | 0.094* | |
C35 | 0.27522 (16) | 0.6085 (3) | 1.2055 (2) | 0.0752 (15) | |
H35 | 0.297612 | 0.622822 | 1.233018 | 0.090* | |
C36 | 0.25077 (14) | 0.5400 (3) | 1.21227 (18) | 0.0598 (12) | |
H36 | 0.255600 | 0.508396 | 1.245067 | 0.072* | |
C37 | 0.21904 (13) | 0.5158 (3) | 1.17208 (17) | 0.0517 (11) | |
C38 | 0.22611 (16) | 0.6916 (3) | 1.0681 (2) | 0.0761 (15) | |
H38A | 0.196733 | 0.710177 | 1.064873 | 0.114* | |
H38B | 0.230562 | 0.659100 | 1.035783 | 0.114* | |
H38C | 0.244634 | 0.741124 | 1.071316 | 0.114* | |
C39 | 0.19141 (16) | 0.4412 (3) | 1.1790 (2) | 0.0798 (16) | |
H39A | 0.192979 | 0.427466 | 1.217751 | 0.120* | |
H39B | 0.200909 | 0.392608 | 1.159440 | 0.120* | |
H39C | 0.162282 | 0.454815 | 1.164423 | 0.120* | |
C40 | 0.15562 (12) | 0.2774 (3) | 0.86965 (18) | 0.0478 (11) | |
C41 | 0.15487 (14) | 0.1917 (3) | 0.8852 (2) | 0.0605 (13) | |
C42 | 0.17149 (17) | 0.1336 (3) | 0.8512 (3) | 0.0813 (16) | |
H42 | 0.172977 | 0.075478 | 0.860733 | 0.098* | |
C43 | 0.18571 (19) | 0.1603 (4) | 0.8040 (3) | 0.0940 (19) | |
H43 | 0.195791 | 0.119527 | 0.780774 | 0.113* | |
C44 | 0.18570 (16) | 0.2437 (4) | 0.7897 (2) | 0.0753 (15) | |
H44 | 0.196412 | 0.260102 | 0.757344 | 0.090* | |
C45 | 0.17022 (13) | 0.3044 (3) | 0.82190 (19) | 0.0573 (12) | |
C46 | 0.13898 (16) | 0.1665 (3) | 0.9369 (2) | 0.0768 (15) | |
H46A | 0.137305 | 0.104734 | 0.938756 | 0.115* | |
H46B | 0.110978 | 0.190715 | 0.937850 | 0.115* | |
H46C | 0.158262 | 0.187394 | 0.968012 | 0.115* | |
C47 | 0.17069 (15) | 0.3965 (3) | 0.8075 (2) | 0.0734 (14) | |
H47A | 0.142717 | 0.420719 | 0.808821 | 0.110* | |
H47B | 0.178310 | 0.402952 | 0.770777 | 0.110* | |
H47C | 0.191338 | 0.426044 | 0.833546 | 0.110* | |
C48 | 0.16300 (13) | 0.2566 (3) | 1.08325 (17) | 0.0483 (11) | |
C49 | 0.20542 (13) | 0.2554 (3) | 1.07676 (18) | 0.0510 (11) | |
C50 | 0.22961 (14) | 0.1910 (3) | 1.1029 (2) | 0.0629 (13) | |
H50 | 0.258806 | 0.188371 | 1.099967 | 0.075* | |
C51 | 0.21204 (16) | 0.1307 (3) | 1.1332 (2) | 0.0678 (14) | |
H51 | 0.229002 | 0.086266 | 1.149847 | 0.081* | |
C52 | 0.17053 (16) | 0.1346 (3) | 1.1393 (2) | 0.0693 (14) | |
H52 | 0.159028 | 0.093438 | 1.160954 | 0.083* | |
C53 | 0.14477 (14) | 0.1976 (3) | 1.1144 (2) | 0.0647 (13) | |
C54 | 0.22421 (13) | 0.3223 (3) | 1.0446 (2) | 0.0665 (14) | |
H54A | 0.210272 | 0.321568 | 1.007004 | 0.100* | |
H54B | 0.254325 | 0.311321 | 1.045103 | 0.100* | |
H54C | 0.220316 | 0.377787 | 1.060765 | 0.100* | |
C55 | 0.09883 (17) | 0.2029 (4) | 1.1206 (3) | 0.121 (3) | |
H55A | 0.092441 | 0.259468 | 1.133293 | 0.182* | |
H55B | 0.092204 | 0.160743 | 1.147139 | 0.182* | |
H55C | 0.081906 | 0.191894 | 1.085449 | 0.182* | |
C7 | 0.099 (8) | 0.609 (3) | 0.933 (3) | 0.046 (3) | 0.067 (3) |
N7 | 0.097 (2) | 0.6814 (17) | 0.9198 (19) | 0.049 (3) | 0.067 (3) |
C56 | 0.0849 (14) | 0.7695 (17) | 0.9243 (13) | 0.082 (3) | 0.067 (3) |
C57 | 0.1154 (13) | 0.826 (3) | 0.9496 (16) | 0.084 (4) | 0.067 (3) |
C58 | 0.1033 (19) | 0.912 (3) | 0.954 (2) | 0.130 (6) | 0.067 (3) |
H58 | 0.123482 | 0.950674 | 0.970656 | 0.156* | 0.067 (3) |
C59 | 0.063 (2) | 0.941 (3) | 0.934 (3) | 0.149 (6) | 0.067 (3) |
H59 | 0.055810 | 0.998920 | 0.937324 | 0.179* | 0.067 (3) |
C60 | 0.0345 (16) | 0.882 (3) | 0.909 (3) | 0.142 (6) | 0.067 (3) |
H60 | 0.007037 | 0.901199 | 0.895707 | 0.170* | 0.067 (3) |
C61 | 0.0441 (14) | 0.795 (3) | 0.904 (2) | 0.114 (5) | 0.067 (3) |
C62 | 0.1607 (14) | 0.812 (5) | 0.975 (2) | 0.068 (4) | 0.067 (3) |
H62A | 0.172595 | 0.866370 | 0.988740 | 0.102* | 0.067 (3) |
H62B | 0.161653 | 0.771646 | 1.004501 | 0.102* | 0.067 (3) |
H62C | 0.177001 | 0.790896 | 0.946965 | 0.102* | 0.067 (3) |
C63 | 0.011 (4) | 0.735 (8) | 0.876 (3) | 0.136 (7) | 0.067 (3) |
H63A | −0.014840 | 0.765533 | 0.864907 | 0.204* | 0.067 (3) |
H63B | 0.021528 | 0.709341 | 0.844650 | 0.204* | 0.067 (3) |
H63C | 0.006177 | 0.690375 | 0.902222 | 0.204* | 0.067 (3) |
C7' | 0.092 (2) | 0.607 (3) | 0.933 (3) | 0.046 (3) | 0.331 (3) |
N7' | 0.0917 (10) | 0.6715 (9) | 0.9090 (9) | 0.049 (3) | 0.331 (3) |
C56' | 0.0871 (7) | 0.7626 (10) | 0.9009 (6) | 0.082 (3) | 0.331 (3) |
C57' | 0.1218 (7) | 0.8145 (13) | 0.9185 (7) | 0.084 (4) | 0.331 (3) |
C58' | 0.1159 (7) | 0.9025 (13) | 0.9097 (8) | 0.130 (6) | 0.331 (3) |
H58' | 0.138934 | 0.938998 | 0.920918 | 0.156* | 0.331 (3) |
C59' | 0.0785 (6) | 0.9387 (12) | 0.8855 (8) | 0.149 (6) | 0.331 (3) |
H59' | 0.075713 | 0.998074 | 0.880839 | 0.179* | 0.331 (3) |
C60' | 0.0451 (6) | 0.8839 (12) | 0.8685 (8) | 0.142 (6) | 0.331 (3) |
H60' | 0.019317 | 0.906784 | 0.851430 | 0.170* | 0.331 (3) |
C61' | 0.0487 (7) | 0.7951 (11) | 0.8761 (7) | 0.114 (5) | 0.331 (3) |
C62' | 0.1600 (9) | 0.765 (2) | 0.9445 (11) | 0.068 (4) | 0.331 (3) |
H62D | 0.183107 | 0.804264 | 0.956016 | 0.102* | 0.331 (3) |
H62E | 0.152729 | 0.734218 | 0.976238 | 0.102* | 0.331 (3) |
H62F | 0.168647 | 0.724951 | 0.918085 | 0.102* | 0.331 (3) |
C63' | 0.0133 (12) | 0.735 (3) | 0.8587 (11) | 0.136 (7) | 0.331 (3) |
H63D | −0.011387 | 0.766297 | 0.842090 | 0.204* | 0.331 (3) |
H63E | 0.021991 | 0.694750 | 0.832107 | 0.204* | 0.331 (3) |
H63F | 0.006288 | 0.703668 | 0.890411 | 0.204* | 0.331 (3) |
C7" | 0.096 (2) | 0.6074 (19) | 0.932 (2) | 0.046 (3) | 0.417 (3) |
N7" | 0.0852 (8) | 0.6754 (7) | 0.9164 (7) | 0.049 (3) | 0.417 (3) |
C56" | 0.0869 (5) | 0.7569 (8) | 0.8900 (5) | 0.082 (3) | 0.417 (3) |
C57" | 0.1227 (5) | 0.8071 (9) | 0.9051 (6) | 0.084 (4) | 0.417 (3) |
C58" | 0.1236 (5) | 0.8856 (10) | 0.8787 (6) | 0.130 (6) | 0.417 (3) |
H58" | 0.147419 | 0.921210 | 0.887541 | 0.156* | 0.417 (3) |
C59" | 0.0907 (5) | 0.9130 (10) | 0.8399 (6) | 0.149 (6) | 0.417 (3) |
H59" | 0.091979 | 0.966713 | 0.823100 | 0.179* | 0.417 (3) |
C60" | 0.0560 (5) | 0.8608 (10) | 0.8263 (6) | 0.142 (6) | 0.417 (3) |
H60" | 0.033831 | 0.879280 | 0.799691 | 0.170* | 0.417 (3) |
C61" | 0.0529 (5) | 0.7805 (9) | 0.8511 (6) | 0.114 (5) | 0.417 (3) |
C62" | 0.1614 (7) | 0.7890 (16) | 0.9466 (9) | 0.068 (4) | 0.417 (3) |
H62G | 0.180962 | 0.836760 | 0.947746 | 0.102* | 0.417 (3) |
H62H | 0.152729 | 0.780870 | 0.982629 | 0.102* | 0.417 (3) |
H62I | 0.175419 | 0.737718 | 0.935976 | 0.102* | 0.417 (3) |
C63" | 0.0150 (8) | 0.724 (2) | 0.8363 (10) | 0.136 (7) | 0.417 (3) |
H63G | −0.004897 | 0.752473 | 0.808647 | 0.204* | 0.417 (3) |
H63H | 0.023975 | 0.670710 | 0.822012 | 0.204* | 0.417 (3) |
H63I | 0.001420 | 0.713867 | 0.868785 | 0.204* | 0.417 (3) |
C7Z | 0.088 (2) | 0.603 (4) | 0.932 (3) | 0.046 (3) | 0.185 (3) |
N7Z | 0.0840 (8) | 0.6559 (11) | 0.8977 (9) | 0.049 (3) | 0.185 (3) |
C56Z | 0.0915 (5) | 0.7233 (10) | 0.8621 (7) | 0.082 (3) | 0.185 (3) |
C57Z | 0.1208 (7) | 0.7867 (13) | 0.8794 (9) | 0.084 (4) | 0.185 (3) |
C58Z | 0.1249 (8) | 0.8498 (15) | 0.8395 (11) | 0.130 (6) | 0.185 (3) |
H58Z | 0.144201 | 0.894692 | 0.848705 | 0.156* | 0.185 (3) |
C59Z | 0.1019 (8) | 0.8493 (16) | 0.7873 (11) | 0.149 (6) | 0.185 (3) |
H59Z | 0.105583 | 0.892851 | 0.762022 | 0.179* | 0.185 (3) |
C60Z | 0.0736 (7) | 0.7834 (16) | 0.7731 (10) | 0.142 (6) | 0.185 (3) |
H60Z | 0.058082 | 0.782070 | 0.737704 | 0.170* | 0.185 (3) |
C61Z | 0.0677 (6) | 0.7188 (13) | 0.8106 (8) | 0.114 (5) | 0.185 (3) |
C62Z | 0.1454 (11) | 0.786 (3) | 0.9363 (12) | 0.068 (4) | 0.185 (3) |
H62J | 0.164119 | 0.835414 | 0.940657 | 0.102* | 0.185 (3) |
H62K | 0.125727 | 0.788780 | 0.963285 | 0.102* | 0.185 (3) |
H62L | 0.162091 | 0.734416 | 0.941510 | 0.102* | 0.185 (3) |
C63Z | 0.0363 (7) | 0.6489 (17) | 0.7950 (14) | 0.136 (7) | 0.185 (3) |
H63J | 0.023055 | 0.657286 | 0.757486 | 0.204* | 0.185 (3) |
H63K | 0.050857 | 0.594270 | 0.797973 | 0.204* | 0.185 (3) |
H63L | 0.014728 | 0.649661 | 0.819467 | 0.204* | 0.185 (3) |
U11 | U22 | U33 | U12 | U13 | U23 | |
Nb1 | 0.02807 (18) | 0.0448 (2) | 0.0384 (2) | 0.00011 (16) | 0.00866 (14) | −0.00220 (18) |
N1 | 0.0296 (18) | 0.060 (2) | 0.0391 (19) | −0.0040 (15) | 0.0063 (15) | −0.0181 (17) |
N2 | 0.0259 (16) | 0.0480 (19) | 0.0372 (19) | −0.0011 (14) | 0.0062 (14) | −0.0073 (15) |
N3 | 0.054 (2) | 0.061 (2) | 0.072 (3) | −0.0142 (19) | 0.031 (2) | −0.010 (2) |
N4 | 0.0311 (18) | 0.068 (2) | 0.050 (2) | 0.0029 (16) | 0.0065 (17) | −0.0074 (19) |
N5 | 0.0361 (19) | 0.055 (2) | 0.060 (2) | 0.0042 (17) | 0.0107 (17) | −0.0124 (19) |
N6 | 0.0341 (19) | 0.047 (2) | 0.063 (2) | −0.0007 (16) | 0.0087 (17) | 0.0086 (19) |
C1 | 0.029 (2) | 0.041 (2) | 0.038 (2) | 0.0023 (17) | 0.0061 (18) | −0.0022 (17) |
C2 | 0.029 (2) | 0.041 (2) | 0.037 (2) | −0.0015 (16) | 0.0059 (16) | −0.0051 (17) |
C3 | 0.039 (2) | 0.043 (2) | 0.050 (3) | −0.0028 (19) | 0.009 (2) | −0.0064 (19) |
C4 | 0.030 (2) | 0.046 (2) | 0.044 (2) | 0.0052 (17) | 0.0131 (19) | 0.0015 (19) |
C5 | 0.028 (2) | 0.048 (3) | 0.048 (3) | −0.0010 (18) | 0.0073 (18) | 0.002 (2) |
C6 | 0.027 (2) | 0.045 (2) | 0.047 (3) | −0.0026 (17) | 0.0099 (18) | −0.003 (2) |
C8 | 0.027 (3) | 0.066 (5) | 0.029 (6) | 0.012 (5) | 0.000 (7) | 0.000 (5) |
C9 | 0.041 (3) | 0.057 (6) | 0.048 (8) | 0.005 (4) | 0.000 (8) | −0.009 (6) |
C10 | 0.066 (4) | 0.069 (8) | 0.095 (11) | 0.002 (6) | −0.011 (10) | −0.033 (7) |
C11 | 0.081 (5) | 0.077 (9) | 0.087 (10) | 0.004 (7) | −0.010 (8) | −0.041 (7) |
C12 | 0.078 (5) | 0.114 (11) | 0.061 (8) | −0.018 (10) | 0.021 (7) | −0.037 (7) |
C13 | 0.036 (3) | 0.062 (8) | 0.038 (6) | −0.001 (7) | 0.007 (4) | −0.004 (5) |
C14 | 0.056 (6) | 0.054 (4) | 0.082 (12) | −0.008 (4) | 0.022 (11) | −0.001 (11) |
C15 | 0.062 (4) | 0.090 (10) | 0.037 (3) | −0.003 (9) | 0.009 (3) | 0.000 (8) |
C8' | 0.027 (3) | 0.066 (5) | 0.029 (6) | 0.012 (5) | 0.000 (7) | 0.000 (5) |
C9' | 0.041 (3) | 0.057 (6) | 0.048 (8) | 0.005 (4) | 0.000 (8) | −0.009 (6) |
C10' | 0.066 (4) | 0.069 (8) | 0.095 (11) | 0.002 (6) | −0.011 (10) | −0.033 (7) |
C11' | 0.081 (5) | 0.077 (9) | 0.087 (10) | 0.004 (7) | −0.010 (8) | −0.041 (7) |
C12' | 0.078 (5) | 0.114 (11) | 0.061 (8) | −0.018 (10) | 0.021 (7) | −0.037 (7) |
C13' | 0.036 (3) | 0.062 (8) | 0.038 (6) | −0.001 (7) | 0.007 (4) | −0.004 (5) |
C14' | 0.056 (6) | 0.054 (4) | 0.082 (12) | −0.008 (4) | 0.022 (11) | −0.001 (11) |
C15' | 0.062 (4) | 0.090 (10) | 0.037 (3) | −0.003 (9) | 0.009 (3) | 0.000 (8) |
C16 | 0.025 (2) | 0.061 (3) | 0.041 (2) | 0.0010 (18) | 0.0073 (18) | −0.015 (2) |
C17 | 0.047 (3) | 0.078 (4) | 0.040 (3) | 0.009 (2) | 0.010 (2) | −0.005 (2) |
C18 | 0.073 (4) | 0.122 (5) | 0.041 (3) | 0.017 (3) | 0.010 (3) | −0.005 (3) |
C19 | 0.070 (4) | 0.122 (5) | 0.058 (4) | 0.006 (3) | −0.006 (3) | −0.048 (4) |
C20 | 0.055 (3) | 0.091 (4) | 0.070 (4) | −0.002 (3) | 0.002 (3) | −0.041 (3) |
C21 | 0.040 (2) | 0.068 (3) | 0.060 (3) | 0.003 (2) | 0.006 (2) | −0.022 (3) |
C22 | 0.086 (4) | 0.085 (4) | 0.056 (3) | 0.010 (3) | 0.030 (3) | 0.015 (3) |
C23 | 0.078 (4) | 0.055 (3) | 0.099 (4) | −0.014 (3) | 0.018 (3) | −0.020 (3) |
C24 | 0.044 (3) | 0.048 (3) | 0.070 (3) | −0.016 (2) | 0.025 (2) | −0.015 (2) |
C25 | 0.069 (3) | 0.062 (3) | 0.060 (3) | −0.018 (2) | 0.029 (3) | −0.010 (3) |
C26 | 0.087 (4) | 0.086 (4) | 0.075 (4) | −0.019 (3) | 0.041 (4) | −0.009 (3) |
C27 | 0.090 (5) | 0.071 (4) | 0.116 (6) | −0.022 (3) | 0.067 (4) | −0.009 (4) |
C28 | 0.049 (3) | 0.060 (3) | 0.130 (6) | −0.011 (2) | 0.036 (3) | −0.015 (3) |
C29 | 0.058 (3) | 0.052 (3) | 0.085 (4) | −0.011 (2) | 0.030 (3) | −0.016 (3) |
C30 | 0.091 (4) | 0.085 (4) | 0.063 (4) | −0.022 (3) | 0.008 (3) | −0.006 (3) |
C31 | 0.075 (4) | 0.068 (4) | 0.115 (5) | 0.008 (3) | 0.017 (3) | 0.001 (3) |
C32 | 0.035 (2) | 0.046 (3) | 0.049 (3) | 0.0054 (18) | 0.0016 (19) | −0.014 (2) |
C33 | 0.060 (3) | 0.047 (3) | 0.058 (3) | 0.002 (2) | −0.008 (2) | −0.005 (2) |
C34 | 0.093 (4) | 0.063 (3) | 0.072 (4) | −0.027 (3) | −0.016 (3) | −0.002 (3) |
C35 | 0.077 (4) | 0.078 (4) | 0.062 (4) | −0.014 (3) | −0.024 (3) | −0.005 (3) |
C36 | 0.070 (3) | 0.065 (3) | 0.042 (3) | 0.005 (2) | 0.001 (2) | −0.003 (2) |
C37 | 0.053 (3) | 0.061 (3) | 0.043 (2) | 0.004 (2) | 0.011 (2) | −0.005 (2) |
C38 | 0.093 (4) | 0.058 (3) | 0.071 (4) | −0.011 (3) | −0.010 (3) | 0.003 (3) |
C39 | 0.089 (4) | 0.099 (4) | 0.054 (3) | −0.024 (3) | 0.018 (3) | 0.001 (3) |
C40 | 0.033 (2) | 0.053 (3) | 0.058 (3) | 0.0035 (19) | 0.004 (2) | −0.015 (2) |
C41 | 0.049 (3) | 0.063 (3) | 0.069 (3) | 0.002 (2) | 0.006 (2) | −0.005 (3) |
C42 | 0.092 (4) | 0.056 (3) | 0.096 (5) | 0.012 (3) | 0.011 (4) | −0.017 (3) |
C43 | 0.114 (5) | 0.091 (5) | 0.082 (5) | 0.033 (4) | 0.029 (4) | −0.026 (4) |
C44 | 0.085 (4) | 0.081 (4) | 0.064 (4) | 0.020 (3) | 0.025 (3) | −0.011 (3) |
C45 | 0.045 (3) | 0.069 (3) | 0.059 (3) | 0.006 (2) | 0.009 (2) | −0.012 (3) |
C46 | 0.076 (4) | 0.064 (3) | 0.091 (4) | −0.004 (3) | 0.014 (3) | 0.005 (3) |
C47 | 0.076 (3) | 0.067 (3) | 0.080 (4) | −0.007 (3) | 0.017 (3) | −0.008 (3) |
C48 | 0.042 (2) | 0.047 (3) | 0.056 (3) | 0.004 (2) | 0.005 (2) | 0.004 (2) |
C49 | 0.042 (2) | 0.057 (3) | 0.054 (3) | 0.005 (2) | 0.005 (2) | 0.001 (2) |
C50 | 0.045 (3) | 0.075 (3) | 0.068 (3) | 0.012 (2) | 0.003 (2) | 0.002 (3) |
C51 | 0.067 (4) | 0.068 (3) | 0.066 (3) | 0.016 (3) | −0.002 (3) | 0.011 (3) |
C52 | 0.075 (4) | 0.054 (3) | 0.079 (4) | 0.002 (3) | 0.008 (3) | 0.023 (3) |
C53 | 0.055 (3) | 0.057 (3) | 0.081 (4) | 0.005 (2) | 0.004 (3) | 0.019 (3) |
C54 | 0.041 (3) | 0.087 (4) | 0.073 (4) | 0.008 (2) | 0.014 (2) | 0.015 (3) |
C55 | 0.066 (4) | 0.119 (5) | 0.183 (7) | 0.000 (3) | 0.035 (4) | 0.087 (5) |
C7 | 0.031 (7) | 0.057 (3) | 0.050 (3) | −0.001 (3) | 0.007 (5) | 0.008 (2) |
N7 | 0.034 (6) | 0.061 (3) | 0.054 (4) | −0.003 (3) | 0.005 (4) | 0.015 (3) |
C56 | 0.078 (4) | 0.084 (5) | 0.082 (8) | 0.000 (4) | 0.000 (5) | 0.043 (5) |
C57 | 0.087 (5) | 0.072 (6) | 0.090 (10) | −0.013 (4) | 0.000 (7) | 0.037 (7) |
C58 | 0.153 (9) | 0.101 (9) | 0.127 (15) | −0.052 (7) | −0.012 (11) | 0.071 (10) |
C59 | 0.144 (10) | 0.104 (9) | 0.186 (14) | −0.021 (8) | −0.025 (11) | 0.102 (10) |
C60 | 0.117 (9) | 0.121 (9) | 0.177 (14) | 0.004 (7) | −0.023 (10) | 0.109 (10) |
C61 | 0.092 (7) | 0.102 (7) | 0.138 (13) | −0.012 (5) | −0.017 (9) | 0.073 (8) |
C62 | 0.061 (6) | 0.046 (11) | 0.092 (6) | −0.016 (8) | −0.006 (4) | −0.007 (6) |
C63 | 0.083 (6) | 0.155 (10) | 0.16 (2) | −0.009 (6) | −0.037 (11) | 0.092 (12) |
C7' | 0.031 (7) | 0.057 (3) | 0.050 (3) | −0.001 (3) | 0.007 (5) | 0.008 (2) |
N7' | 0.034 (6) | 0.061 (3) | 0.054 (4) | −0.003 (3) | 0.005 (4) | 0.015 (3) |
C56' | 0.078 (4) | 0.084 (5) | 0.082 (8) | 0.000 (4) | 0.000 (5) | 0.043 (5) |
C57' | 0.087 (5) | 0.072 (6) | 0.090 (10) | −0.013 (4) | 0.000 (7) | 0.037 (7) |
C58' | 0.153 (9) | 0.101 (9) | 0.127 (15) | −0.052 (7) | −0.012 (11) | 0.071 (10) |
C59' | 0.144 (10) | 0.104 (9) | 0.186 (14) | −0.021 (8) | −0.025 (11) | 0.102 (10) |
C60' | 0.117 (9) | 0.121 (9) | 0.177 (14) | 0.004 (7) | −0.023 (10) | 0.109 (10) |
C61' | 0.092 (7) | 0.102 (7) | 0.138 (13) | −0.012 (5) | −0.017 (9) | 0.073 (8) |
C62' | 0.061 (6) | 0.046 (11) | 0.092 (6) | −0.016 (8) | −0.006 (4) | −0.007 (6) |
C63' | 0.083 (6) | 0.155 (10) | 0.16 (2) | −0.009 (6) | −0.037 (11) | 0.092 (12) |
C7" | 0.031 (7) | 0.057 (3) | 0.050 (3) | −0.001 (3) | 0.007 (5) | 0.008 (2) |
N7" | 0.034 (6) | 0.061 (3) | 0.054 (4) | −0.003 (3) | 0.005 (4) | 0.015 (3) |
C56" | 0.078 (4) | 0.084 (5) | 0.082 (8) | 0.000 (4) | 0.000 (5) | 0.043 (5) |
C57" | 0.087 (5) | 0.072 (6) | 0.090 (10) | −0.013 (4) | 0.000 (7) | 0.037 (7) |
C58" | 0.153 (9) | 0.101 (9) | 0.127 (15) | −0.052 (7) | −0.012 (11) | 0.071 (10) |
C59" | 0.144 (10) | 0.104 (9) | 0.186 (14) | −0.021 (8) | −0.025 (11) | 0.102 (10) |
C60" | 0.117 (9) | 0.121 (9) | 0.177 (14) | 0.004 (7) | −0.023 (10) | 0.109 (10) |
C61" | 0.092 (7) | 0.102 (7) | 0.138 (13) | −0.012 (5) | −0.017 (9) | 0.073 (8) |
C62" | 0.061 (6) | 0.046 (11) | 0.092 (6) | −0.016 (8) | −0.006 (4) | −0.007 (6) |
C63" | 0.083 (6) | 0.155 (10) | 0.16 (2) | −0.009 (6) | −0.037 (11) | 0.092 (12) |
C7Z | 0.031 (7) | 0.057 (3) | 0.050 (3) | −0.001 (3) | 0.007 (5) | 0.008 (2) |
N7Z | 0.034 (6) | 0.061 (3) | 0.054 (4) | −0.003 (3) | 0.005 (4) | 0.015 (3) |
C56Z | 0.078 (4) | 0.084 (5) | 0.082 (8) | 0.000 (4) | 0.000 (5) | 0.043 (5) |
C57Z | 0.087 (5) | 0.072 (6) | 0.090 (10) | −0.013 (4) | 0.000 (7) | 0.037 (7) |
C58Z | 0.153 (9) | 0.101 (9) | 0.127 (15) | −0.052 (7) | −0.012 (11) | 0.071 (10) |
C59Z | 0.144 (10) | 0.104 (9) | 0.186 (14) | −0.021 (8) | −0.025 (11) | 0.102 (10) |
C60Z | 0.117 (9) | 0.121 (9) | 0.177 (14) | 0.004 (7) | −0.023 (10) | 0.109 (10) |
C61Z | 0.092 (7) | 0.102 (7) | 0.138 (13) | −0.012 (5) | −0.017 (9) | 0.073 (8) |
C62Z | 0.061 (6) | 0.046 (11) | 0.092 (6) | −0.016 (8) | −0.006 (4) | −0.007 (6) |
C63Z | 0.083 (6) | 0.155 (10) | 0.16 (2) | −0.009 (6) | −0.037 (11) | 0.092 (12) |
Nb1—C3 | 2.084 (4) | C40—C45 | 1.398 (6) |
Nb1—C4 | 2.110 (4) | C40—C41 | 1.412 (6) |
Nb1—C5 | 2.124 (4) | C41—C42 | 1.401 (7) |
Nb1—C6 | 2.157 (4) | C41—C46 | 1.497 (7) |
Nb1—C7Z | 2.233 (6) | C42—C43 | 1.378 (7) |
Nb1—C7" | 2.234 (5) | C42—H42 | 0.9500 |
Nb1—C7' | 2.234 (6) | C43—C44 | 1.368 (7) |
Nb1—C7 | 2.234 (6) | C43—H43 | 0.9500 |
Nb1—N1 | 2.333 (3) | C44—C45 | 1.384 (6) |
Nb1—N2 | 2.354 (3) | C44—H44 | 0.9500 |
N1—C1 | 1.312 (4) | C45—C47 | 1.502 (6) |
N1—C8' | 1.441 (7) | C46—H46A | 0.9800 |
N1—C8 | 1.454 (8) | C46—H46B | 0.9800 |
N2—C2 | 1.312 (4) | C46—H46C | 0.9800 |
N2—C16 | 1.439 (5) | C47—H47A | 0.9800 |
N3—C3 | 1.187 (5) | C47—H47B | 0.9800 |
N3—C24 | 1.393 (5) | C47—H47C | 0.9800 |
N4—C4 | 1.177 (5) | C48—C53 | 1.391 (6) |
N4—C32 | 1.388 (5) | C48—C49 | 1.392 (5) |
N5—C5 | 1.174 (5) | C49—C50 | 1.389 (6) |
N5—C40 | 1.391 (5) | C49—C54 | 1.500 (6) |
N6—C6 | 1.174 (5) | C50—C51 | 1.380 (6) |
N6—C48 | 1.396 (5) | C50—H50 | 0.9500 |
C1—C2 | 1.438 (5) | C51—C52 | 1.361 (6) |
C1—C2i | 1.463 (5) | C51—H51 | 0.9500 |
C8—C9 | 1.409 (12) | C52—C53 | 1.386 (6) |
C8—C13 | 1.417 (11) | C52—H52 | 0.9500 |
C9—C10 | 1.410 (12) | C53—C55 | 1.504 (7) |
C9—C14 | 1.497 (9) | C54—H54A | 0.9800 |
C10—C11 | 1.404 (12) | C54—H54B | 0.9800 |
C10—H10 | 0.9500 | C54—H54C | 0.9800 |
C11—C12 | 1.403 (13) | C55—H55A | 0.9800 |
C11—H11 | 0.9500 | C55—H55B | 0.9800 |
C12—C13 | 1.402 (12) | C55—H55C | 0.9800 |
C12—H12 | 0.9500 | C7—N7 | 1.19 (2) |
C13—C15 | 1.498 (9) | N7—C56 | 1.454 (16) |
C14—H14A | 0.9800 | C56—C61 | 1.402 (15) |
C14—H14B | 0.9800 | C56—C57 | 1.406 (15) |
C14—H14C | 0.9800 | C57—C58 | 1.422 (16) |
C15—H15A | 0.9800 | C57—C62 | 1.516 (17) |
C15—H15B | 0.9800 | C58—C59 | 1.395 (17) |
C15—H15C | 0.9800 | C58—H58 | 0.9500 |
C8'—C9' | 1.387 (10) | C59—C60 | 1.394 (17) |
C8'—C13' | 1.405 (10) | C59—H59 | 0.9500 |
C9'—C10' | 1.414 (10) | C60—C61 | 1.420 (16) |
C9'—C14' | 1.501 (8) | C60—H60 | 0.9500 |
C10'—C11' | 1.391 (11) | C61—C63 | 1.513 (18) |
C10'—H10' | 0.9500 | C62—H62A | 0.9800 |
C11'—C12' | 1.388 (11) | C62—H62B | 0.9800 |
C11'—H11' | 0.9500 | C62—H62C | 0.9800 |
C12'—C13' | 1.395 (10) | C63—H63A | 0.9800 |
C12'—H12' | 0.9500 | C63—H63B | 0.9800 |
C13'—C15' | 1.495 (8) | C63—H63C | 0.9800 |
C14'—H14D | 0.9800 | C7'—N7' | 1.19 (2) |
C14'—H14E | 0.9800 | N7'—C56' | 1.461 (12) |
C14'—H14F | 0.9800 | C56'—C61' | 1.402 (13) |
C15'—H15D | 0.9800 | C56'—C57' | 1.404 (13) |
C15'—H15E | 0.9800 | C57'—C58' | 1.418 (14) |
C15'—H15F | 0.9800 | C57'—C62' | 1.524 (15) |
C16—C17 | 1.390 (6) | C58'—C59' | 1.391 (14) |
C16—C21 | 1.401 (6) | C58'—H58' | 0.9500 |
C17—C18 | 1.406 (6) | C59'—C60' | 1.398 (14) |
C17—C22 | 1.498 (6) | C59'—H59' | 0.9500 |
C18—C19 | 1.388 (7) | C60'—C61' | 1.421 (14) |
C18—H18 | 0.9500 | C60'—H60' | 0.9500 |
C19—C20 | 1.336 (7) | C61'—C63' | 1.502 (15) |
C19—H19 | 0.9500 | C62'—H62D | 0.9800 |
C20—C21 | 1.396 (6) | C62'—H62E | 0.9800 |
C20—H20 | 0.9500 | C62'—H62F | 0.9800 |
C21—C23 | 1.487 (7) | C63'—H63D | 0.9800 |
C22—H22A | 0.9800 | C63'—H63E | 0.9800 |
C22—H22B | 0.9800 | C63'—H63F | 0.9800 |
C22—H22C | 0.9800 | C7"—N7" | 1.18 (2) |
C23—H23A | 0.9800 | N7"—C56" | 1.450 (11) |
C23—H23B | 0.9800 | C56"—C57" | 1.404 (11) |
C23—H23C | 0.9800 | C56"—C61" | 1.409 (12) |
C24—C25 | 1.382 (6) | C57"—C58" | 1.407 (12) |
C24—C29 | 1.395 (6) | C57"—C62" | 1.533 (13) |
C25—C26 | 1.382 (6) | C58"—C59" | 1.401 (13) |
C25—C30 | 1.516 (7) | C58"—H58" | 0.9500 |
C26—C27 | 1.371 (8) | C59"—C60" | 1.391 (13) |
C26—H26 | 0.9500 | C59"—H59" | 0.9500 |
C27—C28 | 1.372 (8) | C60"—C61" | 1.422 (13) |
C27—H27 | 0.9500 | C60"—H60" | 0.9500 |
C28—C29 | 1.414 (7) | C61"—C63" | 1.508 (14) |
C28—H28 | 0.9500 | C62"—H62G | 0.9800 |
C29—C31 | 1.512 (7) | C62"—H62H | 0.9800 |
C30—H30A | 0.9800 | C62"—H62I | 0.9800 |
C30—H30B | 0.9800 | C63"—H63G | 0.9800 |
C30—H30C | 0.9800 | C63"—H63H | 0.9800 |
C31—H31A | 0.9800 | C63"—H63I | 0.9800 |
C31—H31B | 0.9800 | C7Z—N7Z | 1.18 (2) |
C31—H31C | 0.9800 | N7Z—C56Z | 1.428 (14) |
C32—C33 | 1.382 (6) | C56Z—C61Z | 1.401 (14) |
C32—C37 | 1.399 (6) | C56Z—C57Z | 1.402 (14) |
C33—C34 | 1.390 (6) | C57Z—C58Z | 1.425 (15) |
C33—C38 | 1.504 (6) | C57Z—C62Z | 1.522 (16) |
C34—C35 | 1.370 (7) | C58Z—C59Z | 1.402 (16) |
C34—H34 | 0.9500 | C58Z—H58Z | 0.9500 |
C35—C36 | 1.362 (6) | C59Z—C60Z | 1.397 (16) |
C35—H35 | 0.9500 | C59Z—H59Z | 0.9500 |
C36—C37 | 1.381 (6) | C60Z—C61Z | 1.412 (15) |
C36—H36 | 0.9500 | C60Z—H60Z | 0.9500 |
C37—C39 | 1.500 (6) | C61Z—C63Z | 1.511 (16) |
C38—H38A | 0.9800 | C62Z—H62J | 0.9800 |
C38—H38B | 0.9800 | C62Z—H62K | 0.9800 |
C38—H38C | 0.9800 | C62Z—H62L | 0.9800 |
C39—H39A | 0.9800 | C63Z—H63J | 0.9800 |
C39—H39B | 0.9800 | C63Z—H63K | 0.9800 |
C39—H39C | 0.9800 | C63Z—H63L | 0.9800 |
C3—Nb1—C4 | 70.68 (15) | C33—C38—H38B | 109.5 |
C3—Nb1—C5 | 70.12 (14) | H38A—C38—H38B | 109.5 |
C4—Nb1—C5 | 115.18 (14) | C33—C38—H38C | 109.5 |
C3—Nb1—C6 | 107.88 (14) | H38A—C38—H38C | 109.5 |
C4—Nb1—C6 | 72.34 (14) | H38B—C38—H38C | 109.5 |
C5—Nb1—C6 | 73.36 (15) | C37—C39—H39A | 109.5 |
C3—Nb1—C7Z | 78.3 (15) | C37—C39—H39B | 109.5 |
C4—Nb1—C7Z | 109 (3) | H39A—C39—H39B | 109.5 |
C5—Nb1—C7Z | 111 (2) | C37—C39—H39C | 109.5 |
C6—Nb1—C7Z | 173.7 (15) | H39A—C39—H39C | 109.5 |
C3—Nb1—C7" | 72 (2) | H39B—C39—H39C | 109.5 |
C4—Nb1—C7" | 104.9 (14) | N5—C40—C45 | 118.7 (4) |
C5—Nb1—C7" | 109.4 (19) | N5—C40—C41 | 118.2 (4) |
C6—Nb1—C7" | 176.9 (14) | C45—C40—C41 | 123.0 (4) |
C3—Nb1—C7' | 75 (2) | C42—C41—C40 | 116.4 (5) |
C4—Nb1—C7' | 106.5 (18) | C42—C41—C46 | 122.8 (5) |
C5—Nb1—C7' | 111 (2) | C40—C41—C46 | 120.8 (4) |
C6—Nb1—C7' | 176 (2) | C43—C42—C41 | 120.4 (5) |
C3—Nb1—C7 | 70 (6) | C43—C42—H42 | 119.8 |
C4—Nb1—C7 | 103 (4) | C41—C42—H42 | 119.8 |
C5—Nb1—C7 | 109 (3) | C44—C43—C42 | 121.9 (5) |
C6—Nb1—C7 | 175 (4) | C44—C43—H43 | 119.1 |
C3—Nb1—N1 | 135.91 (13) | C42—C43—H43 | 119.1 |
C4—Nb1—N1 | 153.39 (13) | C43—C44—C45 | 120.5 (5) |
C5—Nb1—N1 | 81.83 (12) | C43—C44—H44 | 119.7 |
C6—Nb1—N1 | 95.14 (13) | C45—C44—H44 | 119.7 |
C7Z—Nb1—N1 | 81 (2) | C44—C45—C40 | 117.7 (5) |
C7"—Nb1—N1 | 86.8 (17) | C44—C45—C47 | 121.4 (5) |
C7'—Nb1—N1 | 84.2 (19) | C40—C45—C47 | 120.9 (4) |
C7—Nb1—N1 | 89 (6) | C41—C46—H46A | 109.5 |
C3—Nb1—N2 | 135.25 (13) | C41—C46—H46B | 109.5 |
C4—Nb1—N2 | 81.27 (12) | H46A—C46—H46B | 109.5 |
C5—Nb1—N2 | 154.60 (13) | C41—C46—H46C | 109.5 |
C6—Nb1—N2 | 95.30 (13) | H46A—C46—H46C | 109.5 |
C7Z—Nb1—N2 | 79.1 (18) | H46B—C46—H46C | 109.5 |
C7"—Nb1—N2 | 83 (2) | C45—C47—H47A | 109.5 |
C7'—Nb1—N2 | 80 (2) | C45—C47—H47B | 109.5 |
C7—Nb1—N2 | 84 (5) | H47A—C47—H47B | 109.5 |
N1—Nb1—N2 | 76.54 (10) | C45—C47—H47C | 109.5 |
C1—N1—C8' | 122.2 (9) | H47A—C47—H47C | 109.5 |
C1—N1—C8 | 117.3 (12) | H47B—C47—H47C | 109.5 |
C1—N1—Nb1 | 108.3 (2) | C53—C48—C49 | 123.0 (4) |
C8'—N1—Nb1 | 128.9 (9) | C53—C48—N6 | 119.2 (4) |
C8—N1—Nb1 | 126.0 (13) | C49—C48—N6 | 117.8 (4) |
C2—N2—C16 | 119.0 (3) | C50—C49—C48 | 116.8 (4) |
C2—N2—Nb1 | 107.3 (2) | C50—C49—C54 | 121.9 (4) |
C16—N2—Nb1 | 131.0 (2) | C48—C49—C54 | 121.3 (4) |
C3—N3—C24 | 171.1 (5) | C51—C50—C49 | 121.2 (4) |
C4—N4—C32 | 175.2 (4) | C51—C50—H50 | 119.4 |
C5—N5—C40 | 173.6 (4) | C49—C50—H50 | 119.4 |
C6—N6—C48 | 163.3 (4) | C52—C51—C50 | 120.4 (4) |
N1—C1—C2 | 123.6 (3) | C52—C51—H51 | 119.8 |
N1—C1—C2i | 146.5 (3) | C50—C51—H51 | 119.8 |
C2—C1—C2i | 90.0 (3) | C51—C52—C53 | 121.1 (5) |
N2—C2—C1 | 124.3 (3) | C51—C52—H52 | 119.4 |
N2—C2—C1i | 145.7 (3) | C53—C52—H52 | 119.4 |
C1—C2—C1i | 90.0 (3) | C52—C53—C48 | 117.5 (4) |
N3—C3—Nb1 | 177.4 (4) | C52—C53—C55 | 121.9 (5) |
N4—C4—Nb1 | 176.2 (3) | C48—C53—C55 | 120.6 (4) |
N5—C5—Nb1 | 175.3 (4) | C49—C54—H54A | 109.5 |
N6—C6—Nb1 | 174.4 (3) | C49—C54—H54B | 109.5 |
C9—C8—C13 | 118.7 (9) | H54A—C54—H54B | 109.5 |
C9—C8—N1 | 126.8 (11) | C49—C54—H54C | 109.5 |
C13—C8—N1 | 114.5 (11) | H54A—C54—H54C | 109.5 |
C8—C9—C10 | 118.9 (12) | H54B—C54—H54C | 109.5 |
C8—C9—C14 | 120 (2) | C53—C55—H55A | 109.5 |
C10—C9—C14 | 120.8 (19) | C53—C55—H55B | 109.5 |
C11—C10—C9 | 121.3 (12) | H55A—C55—H55B | 109.5 |
C11—C10—H10 | 119.3 | C53—C55—H55C | 109.5 |
C9—C10—H10 | 119.3 | H55A—C55—H55C | 109.5 |
C12—C11—C10 | 120.5 (12) | H55B—C55—H55C | 109.5 |
C12—C11—H11 | 119.7 | N7—C7—Nb1 | 164 (6) |
C10—C11—H11 | 119.7 | C7—N7—C56 | 155 (7) |
C13—C12—C11 | 117.9 (12) | C61—C56—C57 | 122.5 (19) |
C13—C12—H12 | 121.1 | C61—C56—N7 | 120 (2) |
C11—C12—H12 | 121.1 | C57—C56—N7 | 117.9 (19) |
C12—C13—C8 | 122.6 (10) | C56—C57—C58 | 117.3 (19) |
C12—C13—C15 | 116.9 (14) | C56—C57—C62 | 132 (4) |
C8—C13—C15 | 120.5 (14) | C58—C57—C62 | 111 (4) |
C9—C14—H14A | 109.5 | C59—C58—C57 | 123 (2) |
C9—C14—H14B | 109.5 | C59—C58—H58 | 118.6 |
H14A—C14—H14B | 109.5 | C57—C58—H58 | 118.6 |
C9—C14—H14C | 109.5 | C60—C59—C58 | 117 (2) |
H14A—C14—H14C | 109.5 | C60—C59—H59 | 121.5 |
H14B—C14—H14C | 109.5 | C58—C59—H59 | 121.5 |
C13—C15—H15A | 109.5 | C59—C60—C61 | 124 (2) |
C13—C15—H15B | 109.5 | C59—C60—H60 | 118.2 |
H15A—C15—H15B | 109.5 | C61—C60—H60 | 118.2 |
C13—C15—H15C | 109.5 | C56—C61—C60 | 116.8 (19) |
H15A—C15—H15C | 109.5 | C56—C61—C63 | 122 (7) |
H15B—C15—H15C | 109.5 | C60—C61—C63 | 121 (7) |
C9'—C8'—C13' | 124.8 (7) | C57—C62—H62A | 109.5 |
C9'—C8'—N1 | 113.9 (7) | C57—C62—H62B | 109.5 |
C13'—C8'—N1 | 120.8 (8) | H62A—C62—H62B | 109.5 |
C8'—C9'—C10' | 117.0 (8) | C57—C62—H62C | 109.5 |
C8'—C9'—C14' | 124.0 (13) | H62A—C62—H62C | 109.5 |
C10'—C9'—C14' | 118.9 (12) | H62B—C62—H62C | 109.5 |
C11'—C10'—C9' | 119.1 (10) | C61—C63—H63A | 109.5 |
C11'—C10'—H10' | 120.4 | C61—C63—H63B | 109.5 |
C9'—C10'—H10' | 120.4 | H63A—C63—H63B | 109.5 |
C12'—C11'—C10' | 122.4 (10) | C61—C63—H63C | 109.5 |
C12'—C11'—H11' | 118.8 | H63A—C63—H63C | 109.5 |
C10'—C11'—H11' | 118.8 | H63B—C63—H63C | 109.5 |
C11'—C12'—C13' | 120.0 (9) | N7'—C7'—Nb1 | 165 (6) |
C11'—C12'—H12' | 120.0 | C7'—N7'—C56' | 157 (4) |
C13'—C12'—H12' | 120.0 | C61'—C56'—C57' | 122.4 (13) |
C12'—C13'—C8' | 116.7 (8) | C61'—C56'—N7' | 119.3 (14) |
C12'—C13'—C15' | 121.3 (9) | C57'—C56'—N7' | 118.3 (14) |
C8'—C13'—C15' | 121.9 (9) | C56'—C57'—C58' | 116.4 (14) |
C9'—C14'—H14D | 109.5 | C56'—C57'—C62' | 112.9 (19) |
C9'—C14'—H14E | 109.5 | C58'—C57'—C62' | 131 (2) |
H14D—C14'—H14E | 109.5 | C59'—C58'—C57' | 124.0 (15) |
C9'—C14'—H14F | 109.5 | C59'—C58'—H58' | 118.0 |
H14D—C14'—H14F | 109.5 | C57'—C58'—H58' | 118.0 |
H14E—C14'—H14F | 109.5 | C58'—C59'—C60' | 117.2 (15) |
C13'—C15'—H15D | 109.5 | C58'—C59'—H59' | 121.4 |
C13'—C15'—H15E | 109.5 | C60'—C59'—H59' | 121.4 |
H15D—C15'—H15E | 109.5 | C59'—C60'—C61' | 121.9 (14) |
C13'—C15'—H15F | 109.5 | C59'—C60'—H60' | 119.0 |
H15D—C15'—H15F | 109.5 | C61'—C60'—H60' | 119.0 |
H15E—C15'—H15F | 109.5 | C56'—C61'—C60' | 118.1 (13) |
C17—C16—C21 | 120.9 (4) | C56'—C61'—C63' | 119 (2) |
C17—C16—N2 | 119.7 (4) | C60'—C61'—C63' | 123 (2) |
C21—C16—N2 | 119.2 (4) | C57'—C62'—H62D | 109.5 |
C16—C17—C18 | 118.0 (5) | C57'—C62'—H62E | 109.5 |
C16—C17—C22 | 121.3 (4) | H62D—C62'—H62E | 109.5 |
C18—C17—C22 | 120.7 (5) | C57'—C62'—H62F | 109.5 |
C19—C18—C17 | 120.8 (5) | H62D—C62'—H62F | 109.5 |
C19—C18—H18 | 119.6 | H62E—C62'—H62F | 109.5 |
C17—C18—H18 | 119.6 | C61'—C63'—H63D | 109.5 |
C20—C19—C18 | 119.9 (5) | C61'—C63'—H63E | 109.5 |
C20—C19—H19 | 120.0 | H63D—C63'—H63E | 109.5 |
C18—C19—H19 | 120.0 | C61'—C63'—H63F | 109.5 |
C19—C20—C21 | 122.1 (5) | H63D—C63'—H63F | 109.5 |
C19—C20—H20 | 119.0 | H63E—C63'—H63F | 109.5 |
C21—C20—H20 | 119.0 | N7"—C7"—Nb1 | 166 (6) |
C20—C21—C16 | 118.2 (5) | C7"—N7"—C56" | 159 (5) |
C20—C21—C23 | 120.0 (5) | C57"—C56"—C61" | 124.3 (10) |
C16—C21—C23 | 121.8 (4) | C57"—C56"—N7" | 117.6 (11) |
C17—C22—H22A | 109.5 | C61"—C56"—N7" | 118.1 (11) |
C17—C22—H22B | 109.5 | C56"—C57"—C58" | 116.4 (11) |
H22A—C22—H22B | 109.5 | C56"—C57"—C62" | 129.3 (15) |
C17—C22—H22C | 109.5 | C58"—C57"—C62" | 114.3 (16) |
H22A—C22—H22C | 109.5 | C59"—C58"—C57" | 122.1 (12) |
H22B—C22—H22C | 109.5 | C59"—C58"—H58" | 118.9 |
C21—C23—H23A | 109.5 | C57"—C58"—H58" | 118.9 |
C21—C23—H23B | 109.5 | C60"—C59"—C58" | 119.3 (12) |
H23A—C23—H23B | 109.5 | C60"—C59"—H59" | 120.4 |
C21—C23—H23C | 109.5 | C58"—C59"—H59" | 120.4 |
H23A—C23—H23C | 109.5 | C59"—C60"—C61" | 121.8 (12) |
H23B—C23—H23C | 109.5 | C59"—C60"—H60" | 119.1 |
C25—C24—N3 | 119.1 (4) | C61"—C60"—H60" | 119.1 |
C25—C24—C29 | 123.3 (4) | C56"—C61"—C60" | 116.1 (11) |
N3—C24—C29 | 117.6 (5) | C56"—C61"—C63" | 122.4 (16) |
C26—C25—C24 | 118.0 (5) | C60"—C61"—C63" | 121.4 (17) |
C26—C25—C30 | 119.3 (5) | C57"—C62"—H62G | 109.5 |
C24—C25—C30 | 122.7 (4) | C57"—C62"—H62H | 109.5 |
C27—C26—C25 | 120.7 (6) | H62G—C62"—H62H | 109.5 |
C27—C26—H26 | 119.7 | C57"—C62"—H62I | 109.5 |
C25—C26—H26 | 119.7 | H62G—C62"—H62I | 109.5 |
C26—C27—C28 | 121.2 (5) | H62H—C62"—H62I | 109.5 |
C26—C27—H27 | 119.4 | C61"—C63"—H63G | 109.5 |
C28—C27—H27 | 119.4 | C61"—C63"—H63H | 109.5 |
C27—C28—C29 | 120.3 (5) | H63G—C63"—H63H | 109.5 |
C27—C28—H28 | 119.8 | C61"—C63"—H63I | 109.5 |
C29—C28—H28 | 119.8 | H63G—C63"—H63I | 109.5 |
C24—C29—C28 | 116.5 (5) | H63H—C63"—H63I | 109.5 |
C24—C29—C31 | 122.1 (4) | N7Z—C7Z—Nb1 | 162 (5) |
C28—C29—C31 | 121.4 (5) | C7Z—N7Z—C56Z | 163 (4) |
C25—C30—H30A | 109.5 | C61Z—C56Z—C57Z | 125.3 (15) |
C25—C30—H30B | 109.5 | C61Z—C56Z—N7Z | 114.2 (15) |
H30A—C30—H30B | 109.5 | C57Z—C56Z—N7Z | 120.5 (16) |
C25—C30—H30C | 109.5 | C56Z—C57Z—C58Z | 114.1 (15) |
H30A—C30—H30C | 109.5 | C56Z—C57Z—C62Z | 122 (2) |
H30B—C30—H30C | 109.5 | C58Z—C57Z—C62Z | 124 (3) |
C29—C31—H31A | 109.5 | C59Z—C58Z—C57Z | 123.5 (18) |
C29—C31—H31B | 109.5 | C59Z—C58Z—H58Z | 118.3 |
H31A—C31—H31B | 109.5 | C57Z—C58Z—H58Z | 118.3 |
C29—C31—H31C | 109.5 | C60Z—C59Z—C58Z | 118.8 (19) |
H31A—C31—H31C | 109.5 | C60Z—C59Z—H59Z | 120.6 |
H31B—C31—H31C | 109.5 | C58Z—C59Z—H59Z | 120.6 |
C33—C32—N4 | 117.7 (4) | C59Z—C60Z—C61Z | 120.9 (17) |
C33—C32—C37 | 123.3 (4) | C59Z—C60Z—H60Z | 119.5 |
N4—C32—C37 | 119.0 (4) | C61Z—C60Z—H60Z | 119.5 |
C32—C33—C34 | 116.4 (4) | C56Z—C61Z—C60Z | 117.3 (16) |
C32—C33—C38 | 121.3 (4) | C56Z—C61Z—C63Z | 122.3 (19) |
C34—C33—C38 | 122.3 (4) | C60Z—C61Z—C63Z | 120 (2) |
C35—C34—C33 | 121.4 (5) | C57Z—C62Z—H62J | 109.5 |
C35—C34—H34 | 119.3 | C57Z—C62Z—H62K | 109.5 |
C33—C34—H34 | 119.3 | H62J—C62Z—H62K | 109.5 |
C36—C35—C34 | 120.7 (4) | C57Z—C62Z—H62L | 109.5 |
C36—C35—H35 | 119.7 | H62J—C62Z—H62L | 109.5 |
C34—C35—H35 | 119.7 | H62K—C62Z—H62L | 109.5 |
C35—C36—C37 | 120.9 (4) | C61Z—C63Z—H63J | 109.5 |
C35—C36—H36 | 119.6 | C61Z—C63Z—H63K | 109.5 |
C37—C36—H36 | 119.6 | H63J—C63Z—H63K | 109.5 |
C36—C37—C32 | 117.2 (4) | C61Z—C63Z—H63L | 109.5 |
C36—C37—C39 | 121.7 (4) | H63J—C63Z—H63L | 109.5 |
C32—C37—C39 | 121.0 (4) | H63K—C63Z—H63L | 109.5 |
C33—C38—H38A | 109.5 | ||
C8'—N1—C1—C2 | 172.2 (6) | C45—C40—C41—C42 | 2.8 (6) |
C8—N1—C1—C2 | 150.3 (9) | N5—C40—C41—C46 | 0.6 (6) |
Nb1—N1—C1—C2 | 0.1 (5) | C45—C40—C41—C46 | 179.8 (4) |
C8'—N1—C1—C2i | −5.5 (9) | C40—C41—C42—C43 | −3.0 (7) |
C8—N1—C1—C2i | −27.5 (11) | C46—C41—C42—C43 | −180.0 (5) |
Nb1—N1—C1—C2i | −177.7 (5) | C41—C42—C43—C44 | 2.6 (9) |
C16—N2—C2—C1 | −163.4 (4) | C42—C43—C44—C45 | −1.7 (9) |
Nb1—N2—C2—C1 | −0.2 (4) | C43—C44—C45—C40 | 1.3 (7) |
C16—N2—C2—C1i | 14.5 (8) | C43—C44—C45—C47 | 178.8 (5) |
Nb1—N2—C2—C1i | 177.8 (5) | N5—C40—C45—C44 | 177.2 (4) |
N1—C1—C2—N2 | 0.1 (6) | C41—C40—C45—C44 | −2.0 (6) |
C2i—C1—C2—N2 | 178.8 (5) | N5—C40—C45—C47 | −0.3 (6) |
N1—C1—C2—C1i | −178.8 (5) | C41—C40—C45—C47 | −179.5 (4) |
C2i—C1—C2—C1i | −0.001 (1) | C6—N6—C48—C49 | 1.5 (16) |
C1—N1—C8—C9 | −56 (3) | C53—C48—C49—C50 | 0.4 (7) |
Nb1—N1—C8—C9 | 89 (3) | N6—C48—C49—C50 | 180.0 (4) |
C1—N1—C8—C13 | 126.1 (19) | C53—C48—C49—C54 | −177.5 (4) |
Nb1—N1—C8—C13 | −90 (2) | N6—C48—C49—C54 | 2.1 (6) |
C13—C8—C9—C10 | 0 (4) | C48—C49—C50—C51 | 0.9 (7) |
N1—C8—C9—C10 | −178 (2) | C54—C49—C50—C51 | 178.8 (4) |
C13—C8—C9—C14 | −177 (3) | C49—C50—C51—C52 | −1.9 (8) |
N1—C8—C9—C14 | 5 (5) | C50—C51—C52—C53 | 1.5 (8) |
C8—C9—C10—C11 | 1 (4) | C51—C52—C53—C48 | −0.2 (8) |
C14—C9—C10—C11 | 178 (3) | C51—C52—C53—C55 | 179.9 (5) |
C9—C10—C11—C12 | −1 (4) | C49—C48—C53—C52 | −0.8 (7) |
C10—C11—C12—C13 | −1 (4) | N6—C48—C53—C52 | 179.7 (4) |
C11—C12—C13—C8 | 3 (4) | C49—C48—C53—C55 | 179.1 (5) |
C11—C12—C13—C15 | −177 (2) | N6—C48—C53—C55 | −0.4 (7) |
C9—C8—C13—C12 | −2 (4) | Nb1—C7—N7—C56 | −50 (80) |
N1—C8—C13—C12 | 177 (2) | C7—N7—C56—C61 | −84 (23) |
C9—C8—C13—C15 | 178 (2) | C7—N7—C56—C57 | 96 (23) |
N1—C8—C13—C15 | −4 (3) | C61—C56—C57—C58 | 0.1 (8) |
C1—N1—C8'—C9' | −72.0 (18) | N7—C56—C57—C58 | 180.0 (5) |
Nb1—N1—C8'—C9' | 98.5 (17) | C61—C56—C57—C62 | −180.0 (8) |
C1—N1—C8'—C13' | 116.0 (15) | N7—C56—C57—C62 | −0.1 (6) |
Nb1—N1—C8'—C13' | −73.6 (17) | C56—C57—C58—C59 | 0.1 (12) |
C13'—C8'—C9'—C10' | −2 (3) | C62—C57—C58—C59 | −179.8 (10) |
N1—C8'—C9'—C10' | −173.6 (15) | C57—C58—C59—C60 | −0.2 (16) |
C13'—C8'—C9'—C14' | 175 (2) | C58—C59—C60—C61 | 0.0 (17) |
N1—C8'—C9'—C14' | 3 (3) | C57—C56—C61—C60 | −0.2 (12) |
C8'—C9'—C10'—C11' | 0 (3) | N7—C56—C61—C60 | 179.9 (7) |
C14'—C9'—C10'—C11' | −177.1 (18) | C57—C56—C61—C63 | −179.9 (7) |
C9'—C10'—C11'—C12' | 1 (2) | N7—C56—C61—C63 | 0.2 (12) |
C10'—C11'—C12'—C13' | −1 (2) | C59—C60—C61—C56 | 0.2 (16) |
C11'—C12'—C13'—C8' | −1 (2) | C59—C60—C61—C63 | 179.8 (11) |
C11'—C12'—C13'—C15' | −178.2 (13) | Nb1—C7'—N7'—C56' | −100 (26) |
C9'—C8'—C13'—C12' | 2 (3) | C7'—N7'—C56'—C61' | −97 (11) |
N1—C8'—C13'—C12' | 173.3 (14) | C7'—N7'—C56'—C57' | 83 (11) |
C9'—C8'—C13'—C15' | 179.7 (18) | C61'—C56'—C57'—C58' | −0.2 (7) |
N1—C8'—C13'—C15' | −9 (3) | N7'—C56'—C57'—C58' | 179.8 (5) |
C2—N2—C16—C17 | 65.8 (5) | C61'—C56'—C57'—C62' | 179.6 (7) |
Nb1—N2—C16—C17 | −92.8 (4) | N7'—C56'—C57'—C62' | −0.3 (5) |
C2—N2—C16—C21 | −118.9 (4) | C56'—C57'—C58'—C59' | 0.6 (12) |
Nb1—N2—C16—C21 | 82.5 (4) | C62'—C57'—C58'—C59' | −179.3 (9) |
C21—C16—C17—C18 | 1.9 (6) | C57'—C58'—C59'—C60' | −0.9 (15) |
N2—C16—C17—C18 | 177.1 (4) | C58'—C59'—C60'—C61' | 0.9 (16) |
C21—C16—C17—C22 | −176.9 (4) | C57'—C56'—C61'—C60' | 0.3 (11) |
N2—C16—C17—C22 | −1.7 (6) | N7'—C56'—C61'—C60' | −179.8 (7) |
C16—C17—C18—C19 | −0.4 (7) | C57'—C56'—C61'—C63' | −179.9 (6) |
C22—C17—C18—C19 | 178.4 (4) | N7'—C56'—C61'—C63' | 0.1 (11) |
C17—C18—C19—C20 | −1.4 (8) | C59'—C60'—C61'—C56' | −0.7 (15) |
C18—C19—C20—C21 | 1.7 (8) | C59'—C60'—C61'—C63' | 179.5 (10) |
C19—C20—C21—C16 | −0.2 (7) | Nb1—C7"—N7"—C56" | 134 (21) |
C19—C20—C21—C23 | −179.4 (5) | C7"—N7"—C56"—C57" | −52 (8) |
C17—C16—C21—C20 | −1.7 (6) | C7"—N7"—C56"—C61" | 128 (8) |
N2—C16—C21—C20 | −176.9 (4) | C61"—C56"—C57"—C58" | −0.2 (7) |
C17—C16—C21—C23 | 177.6 (4) | N7"—C56"—C57"—C58" | 179.8 (5) |
N2—C16—C21—C23 | 2.4 (6) | C61"—C56"—C57"—C62" | 179.8 (7) |
N3—C24—C25—C26 | 179.7 (4) | N7"—C56"—C57"—C62" | −0.3 (5) |
C29—C24—C25—C26 | −1.2 (7) | C56"—C57"—C58"—C59" | 0.6 (11) |
N3—C24—C25—C30 | 1.3 (7) | C62"—C57"—C58"—C59" | −179.4 (9) |
C29—C24—C25—C30 | −179.6 (4) | C57"—C58"—C59"—C60" | −0.8 (15) |
C24—C25—C26—C27 | 0.3 (7) | C58"—C59"—C60"—C61" | 0.7 (16) |
C30—C25—C26—C27 | 178.8 (5) | C57"—C56"—C61"—C60" | 0.0 (11) |
C25—C26—C27—C28 | −0.1 (8) | N7"—C56"—C61"—C60" | −179.9 (7) |
C26—C27—C28—C29 | 0.6 (8) | C57"—C56"—C61"—C63" | −179.8 (7) |
C25—C24—C29—C28 | 1.7 (7) | N7"—C56"—C61"—C63" | 0.2 (11) |
N3—C24—C29—C28 | −179.2 (4) | C59"—C60"—C61"—C56" | −0.2 (14) |
C25—C24—C29—C31 | −176.7 (4) | C59"—C60"—C61"—C63" | 179.6 (10) |
N3—C24—C29—C31 | 2.5 (6) | Nb1—C7Z—N7Z—C56Z | −61 (36) |
C27—C28—C29—C24 | −1.4 (7) | C7Z—N7Z—C56Z—C61Z | 148 (15) |
C27—C28—C29—C31 | 177.0 (5) | C7Z—N7Z—C56Z—C57Z | −32 (15) |
N4—C32—C33—C34 | −178.0 (4) | C61Z—C56Z—C57Z—C58Z | 0.3 (8) |
C37—C32—C33—C34 | 1.8 (7) | N7Z—C56Z—C57Z—C58Z | −179.9 (5) |
N4—C32—C33—C38 | 3.8 (6) | C61Z—C56Z—C57Z—C62Z | −179.9 (8) |
C37—C32—C33—C38 | −176.3 (4) | N7Z—C56Z—C57Z—C62Z | −0.1 (5) |
C32—C33—C34—C35 | −0.9 (8) | C56Z—C57Z—C58Z—C59Z | −0.1 (13) |
C38—C33—C34—C35 | 177.2 (5) | C62Z—C57Z—C58Z—C59Z | −179.9 (10) |
C33—C34—C35—C36 | −1.2 (9) | C57Z—C58Z—C59Z—C60Z | −0.3 (17) |
C34—C35—C36—C37 | 2.5 (8) | C58Z—C59Z—C60Z—C61Z | 0.6 (17) |
C35—C36—C37—C32 | −1.6 (7) | C57Z—C56Z—C61Z—C60Z | 0.0 (12) |
C35—C36—C37—C39 | −179.2 (5) | N7Z—C56Z—C61Z—C60Z | −179.8 (8) |
C33—C32—C37—C36 | −0.6 (6) | C57Z—C56Z—C61Z—C63Z | −179.3 (7) |
N4—C32—C37—C36 | 179.2 (4) | N7Z—C56Z—C61Z—C63Z | 0.8 (12) |
C33—C32—C37—C39 | 177.0 (4) | C59Z—C60Z—C61Z—C56Z | −0.5 (16) |
N4—C32—C37—C39 | −3.1 (6) | C59Z—C60Z—C61Z—C63Z | 178.9 (11) |
N5—C40—C41—C42 | −176.4 (4) |
Symmetry code: (i) −x, −y+1, −z+2. |
[Nb2(C9H9N)8(C36H36N4)]·3C4H8O | Z = 1 |
Mr = 1976.19 | F(000) = 1042 |
Triclinic, P1 | Dx = 1.231 Mg m−3 |
a = 12.2029 (13) Å | Mo Kα radiation, λ = 0.71073 Å |
b = 12.5921 (14) Å | Cell parameters from 2821 reflections |
c = 19.676 (2) Å | θ = 1.1–25.1° |
α = 95.620 (2)° | µ = 0.27 mm−1 |
β = 101.807 (2)° | T = 173 K |
γ = 113.236 (2)° | Rod, black |
V = 2665.2 (5) Å3 | 0.40 × 0.20 × 0.10 mm |
Bruker SMART CCD platform diffractometer | 6686 reflections with I > 2σ(I) |
Radiation source: normal-focus sealed tube | Rint = 0.040 |
ω scans | θmax = 25.1°, θmin = 1.8° |
Absorption correction: multi-scan (SADABS; Sheldrick, 1996) | h = −14→14 |
Tmin = 0.899, Tmax = 0.973 | k = −14→15 |
18395 measured reflections | l = −18→23 |
9307 independent 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)] = 0.048 | Hydrogen site location: inferred from neighbouring sites |
wR(F2) = 0.107 | H-atom parameters constrained |
S = 1.02 | w = 1/[σ2(Fo2) + (0.0421P)2 + 1.0933P] where P = (Fo2 + 2Fc2)/3 |
9307 reflections | (Δ/σ)max = 0.001 |
680 parameters | Δρmax = 0.39 e Å−3 |
58 restraints | Δρmin = −0.36 e Å−3 |
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. THF solvent molecule O1/C55-C58 is modeled as disordered over two positions, 0.536 (8):0.464 (8). THF solvent molecule O2/C59-C62 was modeled as disordered over a crystallographic inversion center (0.50:0.50). Analogous bond lengths and angles were restrained to be similar and anisotropic displacement parameters for pairs of proximal and symmetry-related atoms were restrained to be similar or constrained to be equivalent. O–C andC–C bond lengths for THF molecule O1/C55-C58 were restrained toward ideal values. |
x | y | z | Uiso*/Ueq | Occ. (<1) | |
Nb1 | 0.57320 (3) | 0.50730 (3) | 0.68770 (2) | 0.02883 (10) | |
N1 | 0.6605 (2) | 0.5876 (2) | 0.60352 (13) | 0.0295 (6) | |
N2 | 0.4103 (2) | 0.4358 (2) | 0.59059 (13) | 0.0297 (6) | |
N3 | 0.5491 (3) | 0.6757 (3) | 0.81385 (16) | 0.0446 (8) | |
N4 | 0.3673 (3) | 0.3418 (3) | 0.76245 (15) | 0.0444 (8) | |
N5 | 0.6764 (3) | 0.3225 (3) | 0.74646 (16) | 0.0510 (8) | |
N6 | 0.8486 (3) | 0.6647 (3) | 0.79647 (15) | 0.0456 (8) | |
C1 | 0.5776 (3) | 0.5429 (3) | 0.54152 (15) | 0.0254 (7) | |
C2 | 0.4498 (3) | 0.4657 (3) | 0.53506 (15) | 0.0268 (7) | |
C3 | 0.5587 (3) | 0.6129 (3) | 0.76794 (17) | 0.0352 (8) | |
C4 | 0.4421 (3) | 0.4001 (3) | 0.73619 (17) | 0.0347 (8) | |
C5 | 0.6378 (3) | 0.3903 (3) | 0.72580 (17) | 0.0385 (8) | |
C6 | 0.7515 (3) | 0.6063 (3) | 0.75656 (18) | 0.0363 (8) | |
C7 | 0.7869 (3) | 0.6632 (3) | 0.60681 (16) | 0.0378 (9) | |
C8 | 0.8335 (4) | 0.7828 (3) | 0.6365 (2) | 0.0569 (11) | |
C9 | 0.9574 (5) | 0.8546 (4) | 0.6403 (3) | 0.0862 (17) | |
H9 | 0.992079 | 0.936200 | 0.660757 | 0.103* | |
C10 | 1.0280 (5) | 0.8088 (7) | 0.6151 (3) | 0.104 (2) | |
H10 | 1.110985 | 0.859478 | 0.617251 | 0.124* | |
C11 | 0.9830 (4) | 0.6921 (6) | 0.5868 (2) | 0.0812 (16) | |
H11 | 1.034877 | 0.662390 | 0.569676 | 0.097* | |
C12 | 0.8608 (3) | 0.6153 (4) | 0.58274 (19) | 0.0525 (10) | |
C13 | 0.7558 (5) | 0.8335 (4) | 0.6645 (2) | 0.0789 (15) | |
H13A | 0.677088 | 0.809232 | 0.628751 | 0.118* | |
H13B | 0.799542 | 0.919718 | 0.675498 | 0.118* | |
H13C | 0.739811 | 0.804739 | 0.707593 | 0.118* | |
C14 | 0.8127 (4) | 0.4862 (4) | 0.5568 (2) | 0.0665 (12) | |
H14A | 0.879166 | 0.468004 | 0.546244 | 0.100* | |
H14B | 0.744613 | 0.461262 | 0.513806 | 0.100* | |
H14C | 0.782681 | 0.444310 | 0.593417 | 0.100* | |
C15 | 0.2847 (3) | 0.3561 (3) | 0.58493 (16) | 0.0371 (8) | |
C16 | 0.2457 (4) | 0.2356 (3) | 0.56130 (19) | 0.0510 (10) | |
C17 | 0.1253 (4) | 0.1590 (4) | 0.5613 (2) | 0.0770 (15) | |
H17 | 0.095909 | 0.076589 | 0.545053 | 0.092* | |
C18 | 0.0497 (5) | 0.2031 (6) | 0.5847 (3) | 0.0944 (19) | |
H18 | −0.031676 | 0.150535 | 0.584435 | 0.113* | |
C19 | 0.0897 (4) | 0.3201 (6) | 0.6079 (2) | 0.0805 (16) | |
H19 | 0.035380 | 0.348061 | 0.623455 | 0.097* | |
C20 | 0.2085 (3) | 0.4009 (4) | 0.60979 (19) | 0.0517 (10) | |
C21 | 0.3304 (4) | 0.1897 (3) | 0.5385 (2) | 0.0661 (12) | |
H21A | 0.407339 | 0.217894 | 0.576354 | 0.099* | |
H21B | 0.349144 | 0.217600 | 0.495652 | 0.099* | |
H21C | 0.290640 | 0.103257 | 0.528514 | 0.099* | |
C22 | 0.2527 (4) | 0.5295 (4) | 0.6381 (2) | 0.0660 (12) | |
H22A | 0.181794 | 0.546322 | 0.641083 | 0.099* | |
H22B | 0.295503 | 0.575251 | 0.606402 | 0.099* | |
H22C | 0.309790 | 0.551119 | 0.685381 | 0.099* | |
C23 | 0.5571 (3) | 0.7353 (3) | 0.87918 (17) | 0.0339 (8) | |
C24 | 0.5339 (3) | 0.8360 (3) | 0.88106 (18) | 0.0387 (8) | |
C25 | 0.5452 (3) | 0.8954 (3) | 0.94660 (19) | 0.0442 (9) | |
H25 | 0.531794 | 0.964881 | 0.949650 | 0.053* | |
C26 | 0.5754 (3) | 0.8568 (3) | 1.00783 (19) | 0.0453 (9) | |
H26 | 0.581791 | 0.898897 | 1.052332 | 0.054* | |
C27 | 0.5965 (3) | 0.7565 (3) | 1.00420 (18) | 0.0411 (9) | |
H27 | 0.617162 | 0.730250 | 1.046584 | 0.049* | |
C28 | 0.5881 (3) | 0.6940 (3) | 0.94047 (18) | 0.0369 (8) | |
C29 | 0.4988 (4) | 0.8756 (3) | 0.8135 (2) | 0.0577 (11) | |
H29A | 0.483485 | 0.945308 | 0.824362 | 0.087* | |
H29B | 0.423626 | 0.811968 | 0.781776 | 0.087* | |
H29C | 0.566268 | 0.895164 | 0.790449 | 0.087* | |
C30 | 0.6127 (4) | 0.5858 (3) | 0.9361 (2) | 0.0534 (10) | |
H30A | 0.642479 | 0.575237 | 0.983976 | 0.080* | |
H30B | 0.675618 | 0.595058 | 0.910257 | 0.080* | |
H30C | 0.536159 | 0.516501 | 0.911080 | 0.080* | |
C31 | 0.2795 (3) | 0.2697 (3) | 0.79359 (18) | 0.0405 (9) | |
C32 | 0.2535 (3) | 0.1503 (3) | 0.78455 (19) | 0.0459 (9) | |
C33 | 0.1692 (4) | 0.0819 (4) | 0.8173 (2) | 0.0577 (11) | |
H33 | 0.149698 | 0.000160 | 0.812551 | 0.069* | |
C34 | 0.1128 (4) | 0.1295 (4) | 0.8568 (2) | 0.0677 (13) | |
H34 | 0.055126 | 0.080655 | 0.878964 | 0.081* | |
C35 | 0.1394 (4) | 0.2475 (4) | 0.8643 (2) | 0.0615 (12) | |
H35 | 0.099488 | 0.278958 | 0.891688 | 0.074* | |
C36 | 0.2233 (3) | 0.3216 (3) | 0.8327 (2) | 0.0471 (10) | |
C37 | 0.3150 (4) | 0.0995 (4) | 0.7403 (2) | 0.0697 (13) | |
H37A | 0.287121 | 0.015235 | 0.740820 | 0.105* | |
H37B | 0.404951 | 0.140129 | 0.759837 | 0.105* | |
H37C | 0.292885 | 0.110045 | 0.691488 | 0.105* | |
C38 | 0.2527 (4) | 0.4504 (4) | 0.8404 (2) | 0.0670 (12) | |
H38A | 0.207802 | 0.470317 | 0.871784 | 0.101* | |
H38B | 0.227621 | 0.467811 | 0.793821 | 0.101* | |
H38C | 0.341847 | 0.497096 | 0.860745 | 0.101* | |
C39 | 0.7154 (3) | 0.2535 (3) | 0.78667 (18) | 0.0377 (8) | |
C40 | 0.7757 (3) | 0.1925 (3) | 0.7587 (2) | 0.0449 (9) | |
C41 | 0.8139 (4) | 0.1244 (4) | 0.7999 (3) | 0.0641 (12) | |
H41 | 0.854156 | 0.081246 | 0.782141 | 0.077* | |
C42 | 0.7945 (4) | 0.1179 (4) | 0.8662 (3) | 0.0712 (13) | |
H42 | 0.821010 | 0.070162 | 0.893685 | 0.085* | |
C43 | 0.7372 (4) | 0.1800 (3) | 0.8927 (2) | 0.0592 (11) | |
H43 | 0.725586 | 0.175906 | 0.938814 | 0.071* | |
C44 | 0.6959 (3) | 0.2484 (3) | 0.85364 (19) | 0.0403 (8) | |
C45 | 0.7996 (4) | 0.2033 (4) | 0.6872 (2) | 0.0760 (14) | |
H45A | 0.847295 | 0.159249 | 0.677853 | 0.114* | |
H45B | 0.846412 | 0.286588 | 0.686422 | 0.114* | |
H45C | 0.720541 | 0.171195 | 0.650770 | 0.114* | |
C46 | 0.6334 (4) | 0.3174 (4) | 0.8829 (2) | 0.0591 (11) | |
H46A | 0.677247 | 0.400748 | 0.881206 | 0.089* | |
H46B | 0.634751 | 0.309350 | 0.932048 | 0.089* | |
H46C | 0.547463 | 0.286856 | 0.854383 | 0.089* | |
C47 | 0.9716 (3) | 0.7229 (3) | 0.83431 (18) | 0.0414 (9) | |
C48 | 1.0572 (4) | 0.6863 (3) | 0.8150 (2) | 0.0514 (10) | |
C49 | 1.1787 (4) | 0.7456 (4) | 0.8541 (2) | 0.0604 (11) | |
H49 | 1.238967 | 0.722581 | 0.842372 | 0.073* | |
C50 | 1.2141 (4) | 0.8368 (4) | 0.9095 (2) | 0.0651 (13) | |
H50 | 1.298684 | 0.876936 | 0.935310 | 0.078* | |
C51 | 1.1287 (4) | 0.8712 (3) | 0.9283 (2) | 0.0571 (11) | |
H51 | 1.154751 | 0.934430 | 0.967231 | 0.069* | |
C52 | 1.0049 (3) | 0.8143 (3) | 0.89102 (19) | 0.0433 (9) | |
C53 | 1.0141 (4) | 0.5833 (4) | 0.7552 (2) | 0.0775 (14) | |
H53A | 1.085560 | 0.571737 | 0.747093 | 0.116* | |
H53B | 0.971343 | 0.598819 | 0.712114 | 0.116* | |
H53C | 0.957228 | 0.512211 | 0.767356 | 0.116* | |
C54 | 0.9087 (4) | 0.8479 (4) | 0.9110 (2) | 0.0665 (12) | |
H54A | 0.857036 | 0.856341 | 0.868500 | 0.100* | |
H54B | 0.949472 | 0.922961 | 0.945171 | 0.100* | |
H54C | 0.856728 | 0.786471 | 0.932214 | 0.100* | |
O1 | 0.3329 (10) | 0.9262 (12) | 0.5822 (9) | 0.159 (5) | 0.459 (8) |
C55 | 0.3266 (13) | 0.8267 (15) | 0.5316 (8) | 0.162 (4) | 0.459 (8) |
H55A | 0.342531 | 0.850229 | 0.486755 | 0.194* | 0.459 (8) |
H55B | 0.245591 | 0.757554 | 0.521116 | 0.194* | 0.459 (8) |
C56 | 0.4316 (14) | 0.8018 (12) | 0.5741 (12) | 0.155 (6) | 0.459 (8) |
H56A | 0.412392 | 0.768764 | 0.616060 | 0.186* | 0.459 (8) |
H56B | 0.454665 | 0.749933 | 0.544519 | 0.186* | 0.459 (8) |
C57 | 0.5240 (11) | 0.9230 (13) | 0.5928 (11) | 0.150 (6) | 0.459 (8) |
H57A | 0.542704 | 0.955029 | 0.550451 | 0.180* | 0.459 (8) |
H57B | 0.601498 | 0.931819 | 0.625854 | 0.180* | 0.459 (8) |
C58 | 0.4565 (12) | 0.9799 (13) | 0.6282 (7) | 0.115 (5) | 0.459 (8) |
H58A | 0.457011 | 0.962861 | 0.676347 | 0.137* | 0.459 (8) |
H58B | 0.494215 | 1.066343 | 0.631626 | 0.137* | 0.459 (8) |
O1' | 0.3511 (11) | 0.8622 (14) | 0.6171 (6) | 0.188 (5) | 0.541 (8) |
C55' | 0.3033 (10) | 0.8369 (14) | 0.5386 (7) | 0.162 (4) | 0.541 (8) |
H55C | 0.285441 | 0.901496 | 0.521908 | 0.194* | 0.541 (8) |
H55D | 0.227843 | 0.761747 | 0.521509 | 0.194* | 0.541 (8) |
C56' | 0.4131 (12) | 0.8288 (12) | 0.5153 (7) | 0.117 (4) | 0.541 (8) |
H56C | 0.424924 | 0.758185 | 0.525858 | 0.140* | 0.541 (8) |
H56D | 0.406617 | 0.831734 | 0.464606 | 0.140* | 0.541 (8) |
C57' | 0.5075 (11) | 0.9368 (13) | 0.5618 (7) | 0.169 (6) | 0.541 (8) |
H57C | 0.494687 | 1.006793 | 0.551022 | 0.203* | 0.541 (8) |
H57D | 0.591769 | 0.947914 | 0.559954 | 0.203* | 0.541 (8) |
C58' | 0.4838 (12) | 0.9103 (16) | 0.6321 (6) | 0.153 (6) | 0.541 (8) |
H58C | 0.514679 | 0.852267 | 0.647430 | 0.184* | 0.541 (8) |
H58D | 0.523654 | 0.982869 | 0.669219 | 0.184* | 0.541 (8) |
O2 | −0.1056 (8) | 0.5221 (7) | 1.0162 (4) | 0.096 (2) | 0.5 |
C59 | −0.057 (3) | 0.562 (3) | 0.9627 (16) | 0.097 (5) | 0.5 |
H59A | −0.001643 | 0.646856 | 0.976764 | 0.116* | 0.5 |
H59B | −0.124060 | 0.548958 | 0.920132 | 0.116* | 0.5 |
C60 | 0.012 (4) | 0.492 (4) | 0.9481 (16) | 0.094 (6) | 0.5 |
H60A | 0.094461 | 0.544259 | 0.942770 | 0.113* | 0.5 |
H60B | −0.033760 | 0.431414 | 0.904173 | 0.113* | 0.5 |
C61 | 0.026 (3) | 0.436 (3) | 1.0113 (15) | 0.097 (5) | 0.5 |
H61A | −0.016561 | 0.348712 | 0.997454 | 0.116* | 0.5 |
H61B | 0.114778 | 0.459092 | 1.034645 | 0.116* | 0.5 |
C62 | −0.032 (4) | 0.482 (4) | 1.0587 (16) | 0.094 (6) | 0.5 |
H62A | −0.082858 | 0.418872 | 1.080275 | 0.113* | 0.5 |
H62B | 0.031351 | 0.547073 | 1.096976 | 0.113* | 0.5 |
U11 | U22 | U33 | U12 | U13 | U23 | |
Nb1 | 0.02715 (17) | 0.03660 (18) | 0.02138 (16) | 0.01177 (13) | 0.00716 (12) | 0.00606 (12) |
N1 | 0.0242 (15) | 0.0362 (15) | 0.0222 (15) | 0.0084 (13) | 0.0040 (12) | 0.0043 (12) |
N2 | 0.0245 (14) | 0.0384 (15) | 0.0249 (15) | 0.0103 (13) | 0.0093 (12) | 0.0081 (12) |
N3 | 0.0491 (19) | 0.0476 (19) | 0.0368 (18) | 0.0191 (16) | 0.0159 (15) | 0.0037 (15) |
N4 | 0.0361 (18) | 0.060 (2) | 0.0347 (18) | 0.0146 (16) | 0.0127 (15) | 0.0195 (16) |
N5 | 0.064 (2) | 0.057 (2) | 0.049 (2) | 0.0371 (19) | 0.0206 (17) | 0.0187 (16) |
N6 | 0.0362 (19) | 0.0517 (19) | 0.0357 (18) | 0.0103 (16) | −0.0012 (15) | 0.0102 (15) |
C1 | 0.0258 (17) | 0.0289 (17) | 0.0223 (17) | 0.0113 (14) | 0.0087 (14) | 0.0056 (13) |
C2 | 0.0263 (17) | 0.0308 (17) | 0.0250 (18) | 0.0132 (15) | 0.0079 (14) | 0.0058 (14) |
C3 | 0.0312 (19) | 0.041 (2) | 0.030 (2) | 0.0126 (17) | 0.0054 (16) | 0.0093 (16) |
C4 | 0.037 (2) | 0.043 (2) | 0.0255 (19) | 0.0195 (18) | 0.0058 (16) | 0.0082 (16) |
C5 | 0.039 (2) | 0.044 (2) | 0.031 (2) | 0.0163 (18) | 0.0136 (16) | 0.0043 (16) |
C6 | 0.043 (2) | 0.043 (2) | 0.0292 (19) | 0.0215 (19) | 0.0151 (17) | 0.0114 (16) |
C7 | 0.0286 (19) | 0.049 (2) | 0.0218 (18) | 0.0041 (17) | 0.0006 (15) | 0.0120 (16) |
C8 | 0.059 (3) | 0.048 (2) | 0.034 (2) | −0.002 (2) | −0.001 (2) | 0.0081 (19) |
C9 | 0.071 (4) | 0.066 (3) | 0.057 (3) | −0.024 (3) | −0.009 (3) | 0.010 (2) |
C10 | 0.042 (3) | 0.140 (6) | 0.076 (4) | −0.012 (4) | 0.005 (3) | 0.034 (4) |
C11 | 0.032 (3) | 0.140 (5) | 0.062 (3) | 0.024 (3) | 0.013 (2) | 0.033 (3) |
C12 | 0.029 (2) | 0.090 (3) | 0.037 (2) | 0.022 (2) | 0.0102 (17) | 0.022 (2) |
C13 | 0.120 (4) | 0.042 (2) | 0.055 (3) | 0.021 (3) | 0.009 (3) | 0.003 (2) |
C14 | 0.064 (3) | 0.103 (4) | 0.056 (3) | 0.055 (3) | 0.023 (2) | 0.013 (3) |
C15 | 0.0268 (19) | 0.054 (2) | 0.0220 (18) | 0.0073 (17) | 0.0074 (15) | 0.0128 (16) |
C16 | 0.046 (2) | 0.055 (3) | 0.034 (2) | 0.003 (2) | 0.0076 (18) | 0.0136 (19) |
C17 | 0.064 (3) | 0.069 (3) | 0.052 (3) | −0.014 (3) | 0.005 (2) | 0.013 (2) |
C18 | 0.040 (3) | 0.136 (5) | 0.066 (4) | −0.008 (3) | 0.017 (3) | 0.024 (4) |
C19 | 0.036 (3) | 0.142 (5) | 0.055 (3) | 0.026 (3) | 0.018 (2) | 0.024 (3) |
C20 | 0.033 (2) | 0.094 (3) | 0.034 (2) | 0.028 (2) | 0.0151 (17) | 0.022 (2) |
C21 | 0.085 (3) | 0.042 (2) | 0.058 (3) | 0.019 (2) | 0.010 (2) | 0.005 (2) |
C22 | 0.060 (3) | 0.108 (4) | 0.056 (3) | 0.058 (3) | 0.026 (2) | 0.015 (3) |
C23 | 0.0287 (18) | 0.0378 (19) | 0.032 (2) | 0.0108 (16) | 0.0115 (15) | −0.0009 (16) |
C24 | 0.032 (2) | 0.044 (2) | 0.040 (2) | 0.0156 (17) | 0.0099 (16) | 0.0070 (17) |
C25 | 0.046 (2) | 0.043 (2) | 0.050 (2) | 0.0246 (19) | 0.0153 (19) | 0.0029 (18) |
C26 | 0.049 (2) | 0.046 (2) | 0.038 (2) | 0.0174 (19) | 0.0146 (18) | −0.0019 (17) |
C27 | 0.040 (2) | 0.048 (2) | 0.034 (2) | 0.0174 (18) | 0.0100 (17) | 0.0080 (17) |
C28 | 0.0305 (19) | 0.041 (2) | 0.040 (2) | 0.0155 (16) | 0.0116 (16) | 0.0038 (17) |
C29 | 0.067 (3) | 0.059 (3) | 0.049 (3) | 0.031 (2) | 0.010 (2) | 0.013 (2) |
C30 | 0.064 (3) | 0.050 (2) | 0.056 (3) | 0.034 (2) | 0.015 (2) | 0.0103 (19) |
C31 | 0.033 (2) | 0.054 (2) | 0.034 (2) | 0.0147 (18) | 0.0105 (16) | 0.0217 (18) |
C32 | 0.041 (2) | 0.055 (2) | 0.037 (2) | 0.0157 (19) | 0.0067 (18) | 0.0144 (18) |
C33 | 0.053 (3) | 0.052 (2) | 0.059 (3) | 0.012 (2) | 0.011 (2) | 0.024 (2) |
C34 | 0.049 (3) | 0.080 (3) | 0.080 (3) | 0.019 (2) | 0.035 (2) | 0.044 (3) |
C35 | 0.048 (3) | 0.082 (3) | 0.074 (3) | 0.033 (2) | 0.037 (2) | 0.038 (3) |
C36 | 0.037 (2) | 0.061 (3) | 0.052 (2) | 0.023 (2) | 0.0176 (19) | 0.027 (2) |
C37 | 0.082 (3) | 0.066 (3) | 0.055 (3) | 0.026 (3) | 0.020 (2) | 0.004 (2) |
C38 | 0.062 (3) | 0.068 (3) | 0.095 (4) | 0.038 (2) | 0.040 (3) | 0.034 (3) |
C39 | 0.032 (2) | 0.0359 (19) | 0.043 (2) | 0.0132 (17) | 0.0082 (17) | 0.0081 (16) |
C40 | 0.040 (2) | 0.044 (2) | 0.051 (2) | 0.0190 (19) | 0.0148 (19) | 0.0062 (18) |
C41 | 0.063 (3) | 0.062 (3) | 0.080 (3) | 0.042 (2) | 0.016 (3) | 0.008 (2) |
C42 | 0.083 (3) | 0.066 (3) | 0.076 (3) | 0.046 (3) | 0.011 (3) | 0.028 (3) |
C43 | 0.067 (3) | 0.063 (3) | 0.053 (3) | 0.030 (2) | 0.017 (2) | 0.023 (2) |
C44 | 0.036 (2) | 0.043 (2) | 0.040 (2) | 0.0161 (17) | 0.0085 (17) | 0.0089 (17) |
C45 | 0.086 (4) | 0.083 (3) | 0.075 (3) | 0.045 (3) | 0.040 (3) | 0.010 (3) |
C46 | 0.069 (3) | 0.078 (3) | 0.045 (2) | 0.044 (3) | 0.023 (2) | 0.012 (2) |
C47 | 0.030 (2) | 0.048 (2) | 0.037 (2) | 0.0082 (18) | 0.0029 (17) | 0.0163 (18) |
C48 | 0.047 (2) | 0.064 (3) | 0.042 (2) | 0.024 (2) | 0.0072 (19) | 0.017 (2) |
C49 | 0.036 (2) | 0.073 (3) | 0.071 (3) | 0.021 (2) | 0.010 (2) | 0.029 (3) |
C50 | 0.033 (2) | 0.061 (3) | 0.077 (3) | 0.003 (2) | −0.008 (2) | 0.030 (3) |
C51 | 0.048 (3) | 0.046 (2) | 0.056 (3) | 0.004 (2) | 0.000 (2) | 0.016 (2) |
C52 | 0.031 (2) | 0.044 (2) | 0.045 (2) | 0.0063 (18) | 0.0050 (18) | 0.0152 (18) |
C53 | 0.080 (3) | 0.112 (4) | 0.054 (3) | 0.058 (3) | 0.013 (3) | 0.007 (3) |
C54 | 0.059 (3) | 0.054 (3) | 0.073 (3) | 0.011 (2) | 0.017 (2) | 0.005 (2) |
O1 | 0.116 (7) | 0.180 (11) | 0.213 (13) | 0.089 (7) | 0.060 (8) | 0.038 (8) |
C55 | 0.106 (7) | 0.208 (9) | 0.150 (8) | 0.091 (7) | −0.003 (6) | −0.086 (7) |
C56 | 0.111 (9) | 0.147 (11) | 0.182 (14) | 0.037 (9) | 0.033 (12) | 0.011 (11) |
C57 | 0.100 (9) | 0.197 (11) | 0.173 (17) | 0.064 (9) | 0.046 (10) | 0.103 (12) |
C58 | 0.106 (9) | 0.179 (15) | 0.086 (7) | 0.091 (9) | 0.025 (7) | 0.020 (9) |
O1' | 0.117 (7) | 0.243 (12) | 0.191 (12) | 0.063 (8) | 0.054 (8) | 0.019 (8) |
C55' | 0.106 (7) | 0.208 (9) | 0.150 (8) | 0.091 (7) | −0.003 (6) | −0.086 (7) |
C56' | 0.087 (8) | 0.140 (9) | 0.122 (11) | 0.043 (7) | 0.044 (9) | 0.004 (9) |
C57' | 0.121 (9) | 0.220 (11) | 0.155 (15) | 0.031 (9) | 0.065 (10) | 0.104 (11) |
C58' | 0.125 (10) | 0.231 (17) | 0.080 (7) | 0.052 (10) | 0.031 (7) | 0.024 (10) |
O2 | 0.121 (7) | 0.115 (6) | 0.073 (5) | 0.063 (6) | 0.033 (5) | 0.039 (4) |
C59 | 0.076 (13) | 0.102 (5) | 0.14 (2) | 0.050 (8) | 0.047 (12) | 0.080 (12) |
C60 | 0.085 (12) | 0.130 (16) | 0.085 (6) | 0.045 (13) | 0.040 (5) | 0.062 (5) |
C61 | 0.076 (13) | 0.102 (5) | 0.14 (2) | 0.050 (8) | 0.047 (12) | 0.080 (12) |
C62 | 0.085 (12) | 0.130 (16) | 0.085 (6) | 0.045 (13) | 0.040 (5) | 0.062 (5) |
Nb1—C3 | 2.045 (4) | C36—C38 | 1.501 (5) |
Nb1—C5 | 2.061 (4) | C37—H37A | 0.9800 |
Nb1—C6 | 2.109 (4) | C37—H37B | 0.9800 |
Nb1—C4 | 2.112 (4) | C37—H37C | 0.9800 |
Nb1—N1 | 2.259 (2) | C38—H38A | 0.9800 |
Nb1—N2 | 2.261 (2) | C38—H38B | 0.9800 |
N1—C1 | 1.319 (4) | C38—H38C | 0.9800 |
N1—C7 | 1.441 (4) | C39—C44 | 1.389 (5) |
N2—C2 | 1.312 (4) | C39—C40 | 1.402 (5) |
N2—C15 | 1.436 (4) | C40—C41 | 1.380 (5) |
N3—C3 | 1.196 (4) | C40—C45 | 1.502 (5) |
N3—C23 | 1.388 (4) | C41—C42 | 1.378 (6) |
N4—C4 | 1.174 (4) | C41—H41 | 0.9500 |
N4—C31 | 1.399 (4) | C42—C43 | 1.369 (6) |
N5—C5 | 1.193 (4) | C42—H42 | 0.9500 |
N5—C39 | 1.383 (4) | C43—C44 | 1.378 (5) |
N6—C6 | 1.175 (4) | C43—H43 | 0.9500 |
N6—C47 | 1.382 (4) | C44—C46 | 1.507 (5) |
C1—C2 | 1.446 (4) | C45—H45A | 0.9800 |
C1—C2i | 1.458 (4) | C45—H45B | 0.9800 |
C7—C8 | 1.396 (5) | C45—H45C | 0.9800 |
C7—C12 | 1.396 (5) | C46—H46A | 0.9800 |
C8—C9 | 1.405 (6) | C46—H46B | 0.9800 |
C8—C13 | 1.494 (6) | C46—H46C | 0.9800 |
C9—C10 | 1.352 (8) | C47—C52 | 1.389 (5) |
C9—H9 | 0.9500 | C47—C48 | 1.398 (5) |
C10—C11 | 1.361 (8) | C48—C49 | 1.377 (5) |
C10—H10 | 0.9500 | C48—C53 | 1.501 (5) |
C11—C12 | 1.402 (6) | C49—C50 | 1.365 (6) |
C11—H11 | 0.9500 | C49—H49 | 0.9500 |
C12—C14 | 1.486 (6) | C50—C51 | 1.377 (6) |
C13—H13A | 0.9800 | C50—H50 | 0.9500 |
C13—H13B | 0.9800 | C51—C52 | 1.387 (5) |
C13—H13C | 0.9800 | C51—H51 | 0.9500 |
C14—H14A | 0.9800 | C52—C54 | 1.504 (5) |
C14—H14B | 0.9800 | C53—H53A | 0.9800 |
C14—H14C | 0.9800 | C53—H53B | 0.9800 |
C15—C16 | 1.396 (5) | C53—H53C | 0.9800 |
C15—C20 | 1.403 (5) | C54—H54A | 0.9800 |
C16—C17 | 1.403 (6) | C54—H54B | 0.9800 |
C16—C21 | 1.489 (6) | C54—H54C | 0.9800 |
C17—C18 | 1.379 (7) | O1—C58 | 1.439 (8) |
C17—H17 | 0.9500 | O1—C55 | 1.489 (8) |
C18—C19 | 1.352 (7) | C55—C56 | 1.539 (8) |
C18—H18 | 0.9500 | C55—H55A | 0.9900 |
C19—C20 | 1.395 (6) | C55—H55B | 0.9900 |
C19—H19 | 0.9500 | C56—C57 | 1.449 (9) |
C20—C22 | 1.494 (6) | C56—H56A | 0.9900 |
C21—H21A | 0.9800 | C56—H56B | 0.9900 |
C21—H21B | 0.9800 | C57—C58 | 1.510 (8) |
C21—H21C | 0.9800 | C57—H57A | 0.9900 |
C22—H22A | 0.9800 | C57—H57B | 0.9900 |
C22—H22B | 0.9800 | C58—H58A | 0.9900 |
C22—H22C | 0.9800 | C58—H58B | 0.9900 |
C23—C28 | 1.400 (4) | O1'—C58' | 1.439 (8) |
C23—C24 | 1.403 (4) | O1'—C55' | 1.489 (8) |
C24—C25 | 1.378 (5) | C55'—C56' | 1.539 (8) |
C24—C29 | 1.504 (5) | C55'—H55C | 0.9900 |
C25—C26 | 1.378 (5) | C55'—H55D | 0.9900 |
C25—H25 | 0.9500 | C56'—C57' | 1.450 (9) |
C26—C27 | 1.383 (5) | C56'—H56C | 0.9900 |
C26—H26 | 0.9500 | C56'—H56D | 0.9900 |
C27—C28 | 1.376 (4) | C57'—C58' | 1.510 (8) |
C27—H27 | 0.9500 | C57'—H57C | 0.9900 |
C28—C30 | 1.505 (4) | C57'—H57D | 0.9900 |
C29—H29A | 0.9800 | C58'—H58C | 0.9900 |
C29—H29B | 0.9800 | C58'—H58D | 0.9900 |
C29—H29C | 0.9800 | O2—C59 | 1.35 (2) |
C30—H30A | 0.9800 | O2—C62 | 1.37 (2) |
C30—H30B | 0.9800 | C59—C60 | 1.488 (12) |
C30—H30C | 0.9800 | C59—H59A | 0.9900 |
C31—C32 | 1.393 (5) | C59—H59B | 0.9900 |
C31—C36 | 1.400 (5) | C60—C61 | 1.505 (15) |
C32—C33 | 1.377 (5) | C60—H60A | 0.9900 |
C32—C37 | 1.506 (5) | C60—H60B | 0.9900 |
C33—C34 | 1.375 (6) | C61—C62 | 1.491 (12) |
C33—H33 | 0.9500 | C61—H61A | 0.9900 |
C34—C35 | 1.375 (6) | C61—H61B | 0.9900 |
C34—H34 | 0.9500 | C62—H62A | 0.9900 |
C35—C36 | 1.388 (5) | C62—H62B | 0.9900 |
C35—H35 | 0.9500 | ||
C3—Nb1—C5 | 111.28 (12) | H37A—C37—H37B | 109.5 |
C3—Nb1—C6 | 71.98 (12) | C32—C37—H37C | 109.5 |
C5—Nb1—C6 | 72.25 (13) | H37A—C37—H37C | 109.5 |
C3—Nb1—C4 | 71.43 (13) | H37B—C37—H37C | 109.5 |
C5—Nb1—C4 | 73.17 (13) | C36—C38—H38A | 109.5 |
C6—Nb1—C4 | 114.44 (12) | C36—C38—H38B | 109.5 |
C3—Nb1—N1 | 119.74 (11) | H38A—C38—H38B | 109.5 |
C5—Nb1—N1 | 112.71 (11) | C36—C38—H38C | 109.5 |
C6—Nb1—N1 | 84.55 (11) | H38A—C38—H38C | 109.5 |
C4—Nb1—N1 | 160.83 (10) | H38B—C38—H38C | 109.5 |
C3—Nb1—N2 | 114.55 (11) | N5—C39—C44 | 119.4 (3) |
C5—Nb1—N2 | 117.44 (11) | N5—C39—C40 | 118.5 (3) |
C6—Nb1—N2 | 161.93 (10) | C44—C39—C40 | 122.0 (3) |
C4—Nb1—N2 | 83.52 (11) | C41—C40—C39 | 117.5 (4) |
N1—Nb1—N2 | 77.62 (9) | C41—C40—C45 | 121.7 (4) |
C1—N1—C7 | 119.5 (3) | C39—C40—C45 | 120.8 (3) |
C1—N1—Nb1 | 108.92 (19) | C42—C41—C40 | 121.1 (4) |
C7—N1—Nb1 | 131.08 (19) | C42—C41—H41 | 119.4 |
C2—N2—C15 | 122.5 (3) | C40—C41—H41 | 119.4 |
C2—N2—Nb1 | 109.19 (19) | C43—C42—C41 | 120.1 (4) |
C15—N2—Nb1 | 127.79 (19) | C43—C42—H42 | 119.9 |
C3—N3—C23 | 163.7 (3) | C41—C42—H42 | 119.9 |
C4—N4—C31 | 178.3 (4) | C42—C43—C44 | 121.2 (4) |
C5—N5—C39 | 165.0 (3) | C42—C43—H43 | 119.4 |
C6—N6—C47 | 168.6 (4) | C44—C43—H43 | 119.4 |
N1—C1—C2 | 121.9 (3) | C43—C44—C39 | 118.0 (3) |
N1—C1—C2i | 147.8 (3) | C43—C44—C46 | 121.3 (3) |
C2—C1—C2i | 90.3 (2) | C39—C44—C46 | 120.7 (3) |
N2—C2—C1 | 121.7 (3) | C40—C45—H45A | 109.5 |
N2—C2—C1i | 148.6 (3) | C40—C45—H45B | 109.5 |
C1—C2—C1i | 89.7 (2) | H45A—C45—H45B | 109.5 |
N3—C3—Nb1 | 178.6 (3) | C40—C45—H45C | 109.5 |
N4—C4—Nb1 | 178.3 (3) | H45A—C45—H45C | 109.5 |
N5—C5—Nb1 | 178.4 (3) | H45B—C45—H45C | 109.5 |
N6—C6—Nb1 | 176.8 (3) | C44—C46—H46A | 109.5 |
C8—C7—C12 | 121.6 (4) | C44—C46—H46B | 109.5 |
C8—C7—N1 | 118.6 (3) | H46A—C46—H46B | 109.5 |
C12—C7—N1 | 119.8 (3) | C44—C46—H46C | 109.5 |
C7—C8—C9 | 117.7 (5) | H46A—C46—H46C | 109.5 |
C7—C8—C13 | 121.7 (4) | H46B—C46—H46C | 109.5 |
C9—C8—C13 | 120.6 (4) | N6—C47—C52 | 118.5 (3) |
C10—C9—C8 | 120.6 (5) | N6—C47—C48 | 118.9 (3) |
C10—C9—H9 | 119.7 | C52—C47—C48 | 122.5 (3) |
C8—C9—H9 | 119.7 | C49—C48—C47 | 117.5 (4) |
C9—C10—C11 | 121.7 (5) | C49—C48—C53 | 122.7 (4) |
C9—C10—H10 | 119.2 | C47—C48—C53 | 119.8 (4) |
C11—C10—H10 | 119.2 | C50—C49—C48 | 121.2 (4) |
C10—C11—C12 | 120.4 (5) | C50—C49—H49 | 119.4 |
C10—C11—H11 | 119.8 | C48—C49—H49 | 119.4 |
C12—C11—H11 | 119.8 | C49—C50—C51 | 120.8 (4) |
C7—C12—C11 | 117.9 (4) | C49—C50—H50 | 119.6 |
C7—C12—C14 | 120.8 (3) | C51—C50—H50 | 119.6 |
C11—C12—C14 | 121.2 (4) | C50—C51—C52 | 120.6 (4) |
C8—C13—H13A | 109.5 | C50—C51—H51 | 119.7 |
C8—C13—H13B | 109.5 | C52—C51—H51 | 119.7 |
H13A—C13—H13B | 109.5 | C51—C52—C47 | 117.5 (4) |
C8—C13—H13C | 109.5 | C51—C52—C54 | 122.0 (4) |
H13A—C13—H13C | 109.5 | C47—C52—C54 | 120.5 (3) |
H13B—C13—H13C | 109.5 | C48—C53—H53A | 109.5 |
C12—C14—H14A | 109.5 | C48—C53—H53B | 109.5 |
C12—C14—H14B | 109.5 | H53A—C53—H53B | 109.5 |
H14A—C14—H14B | 109.5 | C48—C53—H53C | 109.5 |
C12—C14—H14C | 109.5 | H53A—C53—H53C | 109.5 |
H14A—C14—H14C | 109.5 | H53B—C53—H53C | 109.5 |
H14B—C14—H14C | 109.5 | C52—C54—H54A | 109.5 |
C16—C15—C20 | 121.9 (3) | C52—C54—H54B | 109.5 |
C16—C15—N2 | 119.2 (3) | H54A—C54—H54B | 109.5 |
C20—C15—N2 | 118.6 (3) | C52—C54—H54C | 109.5 |
C15—C16—C17 | 118.0 (4) | H54A—C54—H54C | 109.5 |
C15—C16—C21 | 120.9 (3) | H54B—C54—H54C | 109.5 |
C17—C16—C21 | 121.1 (4) | C58—O1—C55 | 106.2 (6) |
C18—C17—C16 | 120.2 (5) | O1—C55—C56 | 100.9 (7) |
C18—C17—H17 | 119.9 | O1—C55—H55A | 111.6 |
C16—C17—H17 | 119.9 | C56—C55—H55A | 111.6 |
C19—C18—C17 | 120.9 (5) | O1—C55—H55B | 111.6 |
C19—C18—H18 | 119.6 | C56—C55—H55B | 111.6 |
C17—C18—H18 | 119.6 | H55A—C55—H55B | 109.4 |
C18—C19—C20 | 121.9 (5) | C57—C56—C55 | 96.1 (7) |
C18—C19—H19 | 119.1 | C57—C56—H56A | 112.5 |
C20—C19—H19 | 119.1 | C55—C56—H56A | 112.5 |
C19—C20—C15 | 117.2 (4) | C57—C56—H56B | 112.5 |
C19—C20—C22 | 121.1 (4) | C55—C56—H56B | 112.5 |
C15—C20—C22 | 121.7 (3) | H56A—C56—H56B | 110.0 |
C16—C21—H21A | 109.5 | C56—C57—C58 | 99.7 (8) |
C16—C21—H21B | 109.5 | C56—C57—H57A | 111.8 |
H21A—C21—H21B | 109.5 | C58—C57—H57A | 111.8 |
C16—C21—H21C | 109.5 | C56—C57—H57B | 111.8 |
H21A—C21—H21C | 109.5 | C58—C57—H57B | 111.8 |
H21B—C21—H21C | 109.5 | H57A—C57—H57B | 109.5 |
C20—C22—H22A | 109.5 | O1—C58—C57 | 103.5 (7) |
C20—C22—H22B | 109.5 | O1—C58—H58A | 111.1 |
H22A—C22—H22B | 109.5 | C57—C58—H58A | 111.1 |
C20—C22—H22C | 109.5 | O1—C58—H58B | 111.1 |
H22A—C22—H22C | 109.5 | C57—C58—H58B | 111.1 |
H22B—C22—H22C | 109.5 | H58A—C58—H58B | 109.0 |
N3—C23—C28 | 119.5 (3) | C58'—O1'—C55' | 106.3 (6) |
N3—C23—C24 | 118.1 (3) | O1'—C55'—C56' | 101.2 (7) |
C28—C23—C24 | 122.4 (3) | O1'—C55'—H55C | 111.5 |
C25—C24—C23 | 117.2 (3) | C56'—C55'—H55C | 111.5 |
C25—C24—C29 | 122.6 (3) | O1'—C55'—H55D | 111.5 |
C23—C24—C29 | 120.3 (3) | C56'—C55'—H55D | 111.5 |
C26—C25—C24 | 121.8 (3) | H55C—C55'—H55D | 109.4 |
C26—C25—H25 | 119.1 | C57'—C56'—C55' | 96.2 (7) |
C24—C25—H25 | 119.1 | C57'—C56'—H56C | 112.5 |
C25—C26—C27 | 119.7 (3) | C55'—C56'—H56C | 112.5 |
C25—C26—H26 | 120.2 | C57'—C56'—H56D | 112.5 |
C27—C26—H26 | 120.2 | C55'—C56'—H56D | 112.5 |
C28—C27—C26 | 121.4 (3) | H56C—C56'—H56D | 110.0 |
C28—C27—H27 | 119.3 | C56'—C57'—C58' | 99.4 (8) |
C26—C27—H27 | 119.3 | C56'—C57'—H57C | 111.9 |
C27—C28—C23 | 117.6 (3) | C58'—C57'—H57C | 111.9 |
C27—C28—C30 | 121.8 (3) | C56'—C57'—H57D | 111.9 |
C23—C28—C30 | 120.6 (3) | C58'—C57'—H57D | 111.9 |
C24—C29—H29A | 109.5 | H57C—C57'—H57D | 109.6 |
C24—C29—H29B | 109.5 | O1'—C58'—C57' | 103.2 (7) |
H29A—C29—H29B | 109.5 | O1'—C58'—H58C | 111.1 |
C24—C29—H29C | 109.5 | C57'—C58'—H58C | 111.1 |
H29A—C29—H29C | 109.5 | O1'—C58'—H58D | 111.1 |
H29B—C29—H29C | 109.5 | C57'—C58'—H58D | 111.1 |
C28—C30—H30A | 109.5 | H58C—C58'—H58D | 109.1 |
C28—C30—H30B | 109.5 | C59—O2—C62 | 111 (2) |
H30A—C30—H30B | 109.5 | O2—C59—C60 | 105.8 (18) |
C28—C30—H30C | 109.5 | O2—C59—H59A | 110.6 |
H30A—C30—H30C | 109.5 | C60—C59—H59A | 110.6 |
H30B—C30—H30C | 109.5 | O2—C59—H59B | 110.6 |
C32—C31—N4 | 118.2 (3) | C60—C59—H59B | 110.6 |
C32—C31—C36 | 123.5 (3) | H59A—C59—H59B | 108.7 |
N4—C31—C36 | 118.3 (3) | C59—C60—C61 | 105.2 (10) |
C33—C32—C31 | 117.1 (4) | C59—C60—H60A | 110.7 |
C33—C32—C37 | 122.0 (4) | C61—C60—H60A | 110.7 |
C31—C32—C37 | 120.8 (3) | C59—C60—H60B | 110.7 |
C34—C33—C32 | 121.2 (4) | C61—C60—H60B | 110.7 |
C34—C33—H33 | 119.4 | H60A—C60—H60B | 108.8 |
C32—C33—H33 | 119.4 | C62—C61—C60 | 103.6 (9) |
C33—C34—C35 | 120.5 (4) | C62—C61—H61A | 111.0 |
C33—C34—H34 | 119.8 | C60—C61—H61A | 111.0 |
C35—C34—H34 | 119.8 | C62—C61—H61B | 111.0 |
C34—C35—C36 | 121.3 (4) | C60—C61—H61B | 111.0 |
C34—C35—H35 | 119.3 | H61A—C61—H61B | 109.0 |
C36—C35—H35 | 119.3 | O2—C62—C61 | 105.7 (17) |
C35—C36—C31 | 116.3 (4) | O2—C62—H62A | 110.6 |
C35—C36—C38 | 121.7 (4) | C61—C62—H62A | 110.6 |
C31—C36—C38 | 121.9 (3) | O2—C62—H62B | 110.6 |
C32—C37—H37A | 109.5 | C61—C62—H62B | 110.6 |
C32—C37—H37B | 109.5 | H62A—C62—H62B | 108.7 |
C7—N1—C1—C2 | 179.4 (3) | C24—C23—C28—C30 | −179.7 (3) |
Nb1—N1—C1—C2 | 6.3 (3) | N4—C31—C32—C33 | 178.3 (3) |
C7—N1—C1—C2i | −1.4 (6) | C36—C31—C32—C33 | −1.2 (5) |
Nb1—N1—C1—C2i | −174.5 (4) | N4—C31—C32—C37 | −2.1 (5) |
C15—N2—C2—C1 | −177.9 (3) | C36—C31—C32—C37 | 178.5 (3) |
Nb1—N2—C2—C1 | −5.7 (3) | C31—C32—C33—C34 | 0.5 (6) |
C15—N2—C2—C1i | 2.1 (7) | C37—C32—C33—C34 | −179.2 (4) |
Nb1—N2—C2—C1i | 174.2 (4) | C32—C33—C34—C35 | 0.1 (6) |
N1—C1—C2—N2 | −0.5 (4) | C33—C34—C35—C36 | −0.1 (7) |
C2i—C1—C2—N2 | 180.0 (4) | C34—C35—C36—C31 | −0.5 (6) |
N1—C1—C2—C1i | 179.6 (3) | C34—C35—C36—C38 | 179.9 (4) |
C2i—C1—C2—C1i | 0.004 (1) | C32—C31—C36—C35 | 1.2 (5) |
C1—N1—C7—C8 | 110.8 (3) | N4—C31—C36—C35 | −178.3 (3) |
Nb1—N1—C7—C8 | −77.9 (4) | C32—C31—C36—C38 | −179.2 (3) |
C1—N1—C7—C12 | −71.3 (4) | N4—C31—C36—C38 | 1.3 (5) |
Nb1—N1—C7—C12 | 99.9 (3) | C5—N5—C39—C44 | 8.1 (16) |
C12—C7—C8—C9 | 1.1 (5) | C5—N5—C39—C40 | −170.7 (13) |
N1—C7—C8—C9 | 179.0 (3) | N5—C39—C40—C41 | 179.9 (3) |
C12—C7—C8—C13 | −177.9 (3) | C44—C39—C40—C41 | 1.1 (5) |
N1—C7—C8—C13 | −0.1 (5) | N5—C39—C40—C45 | 1.0 (5) |
C7—C8—C9—C10 | 0.8 (7) | C44—C39—C40—C45 | −177.7 (4) |
C13—C8—C9—C10 | 179.8 (5) | C39—C40—C41—C42 | −0.7 (6) |
C8—C9—C10—C11 | −1.5 (8) | C45—C40—C41—C42 | 178.1 (4) |
C9—C10—C11—C12 | 0.2 (8) | C40—C41—C42—C43 | −0.3 (7) |
C8—C7—C12—C11 | −2.3 (5) | C41—C42—C43—C44 | 1.1 (7) |
N1—C7—C12—C11 | 179.9 (3) | C42—C43—C44—C39 | −0.7 (6) |
C8—C7—C12—C14 | 174.9 (3) | C42—C43—C44—C46 | −179.7 (4) |
N1—C7—C12—C14 | −3.0 (5) | N5—C39—C44—C43 | −179.2 (3) |
C10—C11—C12—C7 | 1.7 (6) | C40—C39—C44—C43 | −0.5 (5) |
C10—C11—C12—C14 | −175.5 (4) | N5—C39—C44—C46 | −0.2 (5) |
C2—N2—C15—C16 | 75.4 (4) | C40—C39—C44—C46 | 178.5 (3) |
Nb1—N2—C15—C16 | −95.2 (3) | C6—N6—C47—C52 | 171.4 (16) |
C2—N2—C15—C20 | −110.6 (4) | C6—N6—C47—C48 | −9.8 (19) |
Nb1—N2—C15—C20 | 78.8 (4) | N6—C47—C48—C49 | −179.5 (3) |
C20—C15—C16—C17 | 1.6 (5) | C52—C47—C48—C49 | −0.7 (5) |
N2—C15—C16—C17 | 175.4 (3) | N6—C47—C48—C53 | −1.6 (5) |
C20—C15—C16—C21 | −176.9 (3) | C52—C47—C48—C53 | 177.2 (4) |
N2—C15—C16—C21 | −3.2 (5) | C47—C48—C49—C50 | −0.2 (6) |
C15—C16—C17—C18 | −0.6 (6) | C53—C48—C49—C50 | −178.1 (4) |
C21—C16—C17—C18 | 178.0 (4) | C48—C49—C50—C51 | 0.8 (6) |
C16—C17—C18—C19 | 0.0 (8) | C49—C50—C51—C52 | −0.5 (6) |
C17—C18—C19—C20 | −0.4 (8) | C50—C51—C52—C47 | −0.4 (5) |
C18—C19—C20—C15 | 1.4 (6) | C50—C51—C52—C54 | 178.8 (4) |
C18—C19—C20—C22 | −177.8 (4) | N6—C47—C52—C51 | 179.8 (3) |
C16—C15—C20—C19 | −2.0 (5) | C48—C47—C52—C51 | 1.0 (5) |
N2—C15—C20—C19 | −175.8 (3) | N6—C47—C52—C54 | 0.6 (5) |
C16—C15—C20—C22 | 177.2 (3) | C48—C47—C52—C54 | −178.2 (3) |
N2—C15—C20—C22 | 3.4 (5) | C58—O1—C55—C56 | 23.2 (14) |
C3—N3—C23—C28 | −17.5 (13) | O1—C55—C56—C57 | −49.1 (13) |
C3—N3—C23—C24 | 162.2 (11) | C55—C56—C57—C58 | 55.7 (14) |
N3—C23—C24—C25 | −178.5 (3) | C55—O1—C58—C57 | 10.8 (16) |
C28—C23—C24—C25 | 1.2 (5) | C56—C57—C58—O1 | −43.2 (15) |
N3—C23—C24—C29 | 1.3 (5) | C58'—O1'—C55'—C56' | 21.5 (14) |
C28—C23—C24—C29 | −179.0 (3) | O1'—C55'—C56'—C57' | −48.3 (13) |
C23—C24—C25—C26 | −1.3 (5) | C55'—C56'—C57'—C58' | 56.1 (14) |
C29—C24—C25—C26 | 178.9 (4) | C55'—O1'—C58'—C57' | 12.8 (16) |
C24—C25—C26—C27 | 0.7 (6) | C56'—C57'—C58'—O1' | −44.7 (15) |
C25—C26—C27—C28 | 0.1 (5) | C62—O2—C59—C60 | 29 (3) |
C26—C27—C28—C23 | −0.2 (5) | O2—C59—C60—C61 | −15 (4) |
C26—C27—C28—C30 | 179.1 (3) | C59—C60—C61—C62 | −2 (6) |
N3—C23—C28—C27 | 179.2 (3) | C59—O2—C62—C61 | −31 (4) |
C24—C23—C28—C27 | −0.5 (5) | C60—C61—C62—O2 | 19 (5) |
N3—C23—C28—C30 | −0.1 (5) |
Symmetry code: (i) −x+1, −y+1, −z+1. |
[Nb(C13H17N)6] | Dx = 1.124 Mg m−3 |
Mr = 1216.56 | Mo Kα radiation, λ = 0.71073 Å |
Trigonal, R3:H | Cell parameters from 2975 reflections |
a = 15.2582 (10) Å | θ = 2.2–21.4° |
c = 26.7313 (17) Å | µ = 0.21 mm−1 |
V = 5389.6 (8) Å3 | T = 173 K |
Z = 3 | Block, red |
F(000) = 1959 | 0.20 × 0.20 × 0.20 mm |
Bruker APEXII CCD platform diffractometer | 2752 independent reflections |
Radiation source: normal-focus sealed tube | 2606 reflections with I > 2σ(I) |
Graphite monochromator | Rint = 0.046 |
area detector, ω scans | θmax = 27.5°, θmin = 1.7° |
Absorption correction: multi-scan (SADABS; Sheldrick, 2012) | h = −19→19 |
Tmin = 0.691, Tmax = 0.746 | k = −19→19 |
21272 measured reflections | l = −34→34 |
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)] = 0.035 | Hydrogen site location: mixed |
wR(F2) = 0.085 | H-atom parameters constrained |
S = 1.04 | w = 1/[σ2(Fo2) + (0.0354P)2 + 7.2006P] where P = (Fo2 + 2Fc2)/3 |
2752 reflections | (Δ/σ)max < 0.001 |
193 parameters | Δρmax = 0.26 e Å−3 |
341 restraints | Δρmin = −0.36 e Å−3 |
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. The Nb atom is on a crystallographic -3 position, and thus one-sixth of the molecule is unique. The isocyanide ligand is modeled as disordered over two positions, anchored at carbon atom C1 (0.547 (3):0.453 (3)). Analogous bond lengths and angles between the two positions were restrained to be similar. Anisotropic displacement parameters for proximal atoms were constrained to be equivalent. Additionally, anisotropic displacement parameters over the entire asymmetric unit were heavily restrained to be similar. |
x | y | z | Uiso*/Ueq | Occ. (<1) | |
Nb1 | 0.000000 | 0.000000 | 0.000000 | 0.02289 (11) | |
C1 | 0.07125 (12) | 0.13928 (12) | 0.04187 (6) | 0.0309 (3) | 0.547 (3) |
N1 | 0.1230 (4) | 0.2219 (3) | 0.0583 (2) | 0.0326 (10) | 0.547 (3) |
C2 | 0.1871 (4) | 0.31814 (19) | 0.07710 (18) | 0.0282 (11) | 0.547 (3) |
C3 | 0.2023 (3) | 0.4013 (3) | 0.04831 (12) | 0.0327 (8) | 0.547 (3) |
C4 | 0.2706 (3) | 0.4964 (3) | 0.0667 (2) | 0.0377 (11) | 0.547 (3) |
H4A | 0.282894 | 0.554679 | 0.048242 | 0.045* | 0.547 (3) |
C5 | 0.3209 (7) | 0.5084 (4) | 0.1110 (3) | 0.0410 (13) | 0.547 (3) |
H5A | 0.368891 | 0.574376 | 0.122173 | 0.049* | 0.547 (3) |
C6 | 0.3024 (8) | 0.4257 (5) | 0.1391 (3) | 0.0400 (5) | 0.547 (3) |
H6A | 0.336129 | 0.435568 | 0.170258 | 0.048* | 0.547 (3) |
C7 | 0.2355 (6) | 0.3280 (4) | 0.1231 (2) | 0.0338 (4) | 0.547 (3) |
C8 | 0.2141 (9) | 0.2355 (7) | 0.1536 (3) | 0.0476 (7) | 0.547 (3) |
H8A | 0.207461 | 0.182248 | 0.129546 | 0.057* | 0.547 (3) |
C9 | 0.1143 (16) | 0.1934 (19) | 0.1814 (12) | 0.077 (2) | 0.547 (3) |
H9A | 0.060535 | 0.182215 | 0.157833 | 0.115* | 0.547 (3) |
H9B | 0.119972 | 0.241694 | 0.207151 | 0.115* | 0.547 (3) |
H9C | 0.098070 | 0.129056 | 0.197256 | 0.115* | 0.547 (3) |
C10 | 0.2996 (17) | 0.2557 (16) | 0.1895 (12) | 0.0835 (19) | 0.547 (3) |
H10A | 0.364386 | 0.290804 | 0.171794 | 0.125* | 0.547 (3) |
H10B | 0.289363 | 0.191306 | 0.202727 | 0.125* | 0.547 (3) |
H10C | 0.299969 | 0.297948 | 0.217242 | 0.125* | 0.547 (3) |
C11 | 0.1481 (3) | 0.3869 (3) | −0.00123 (13) | 0.0481 (10) | 0.547 (3) |
H11A | 0.143270 | 0.326138 | −0.018029 | 0.058* | 0.547 (3) |
C12 | 0.0409 (3) | 0.3659 (4) | 0.00837 (17) | 0.0732 (15) | 0.547 (3) |
H12A | 0.005078 | 0.305903 | 0.029689 | 0.110* | 0.547 (3) |
H12B | 0.004998 | 0.353874 | −0.023538 | 0.110* | 0.547 (3) |
H12C | 0.043520 | 0.424264 | 0.025142 | 0.110* | 0.547 (3) |
C13 | 0.2024 (4) | 0.4762 (3) | −0.03649 (15) | 0.0735 (14) | 0.547 (3) |
H13A | 0.273258 | 0.493620 | −0.039798 | 0.110* | 0.547 (3) |
H13B | 0.199289 | 0.534343 | −0.023075 | 0.110* | 0.547 (3) |
H13C | 0.169688 | 0.458219 | −0.069386 | 0.110* | 0.547 (3) |
C1' | 0.07125 (12) | 0.13928 (12) | 0.04187 (6) | 0.0309 (3) | 0.453 (3) |
N1' | 0.1008 (6) | 0.2137 (3) | 0.0665 (3) | 0.0326 (10) | 0.453 (3) |
C2' | 0.1663 (6) | 0.3122 (2) | 0.0824 (2) | 0.0282 (11) | 0.453 (3) |
C3' | 0.1688 (3) | 0.3924 (3) | 0.05563 (15) | 0.0327 (8) | 0.453 (3) |
C4' | 0.2395 (4) | 0.4894 (3) | 0.0708 (3) | 0.0377 (11) | 0.453 (3) |
H4B | 0.244304 | 0.545772 | 0.053187 | 0.045* | 0.453 (3) |
C5' | 0.3025 (9) | 0.5060 (5) | 0.1107 (4) | 0.0410 (13) | 0.453 (3) |
H5B | 0.349890 | 0.573267 | 0.120430 | 0.049* | 0.453 (3) |
C6' | 0.2978 (10) | 0.4261 (6) | 0.1366 (4) | 0.0400 (5) | 0.453 (3) |
H6B | 0.341772 | 0.438921 | 0.164207 | 0.048* | 0.453 (3) |
C7' | 0.2300 (7) | 0.3269 (5) | 0.1232 (2) | 0.0338 (4) | 0.453 (3) |
C8' | 0.2209 (11) | 0.2366 (8) | 0.1517 (4) | 0.0476 (7) | 0.453 (3) |
H8B | 0.219543 | 0.187515 | 0.126478 | 0.057* | 0.453 (3) |
C9' | 0.1219 (19) | 0.184 (2) | 0.1806 (15) | 0.077 (2) | 0.453 (3) |
H9D | 0.063325 | 0.158504 | 0.157916 | 0.115* | 0.453 (3) |
H9E | 0.122258 | 0.235233 | 0.202910 | 0.115* | 0.453 (3) |
H9F | 0.116611 | 0.126501 | 0.200274 | 0.115* | 0.453 (3) |
C10' | 0.310 (2) | 0.265 (2) | 0.1863 (15) | 0.0835 (19) | 0.453 (3) |
H10D | 0.374915 | 0.300197 | 0.167868 | 0.125* | 0.453 (3) |
H10E | 0.303073 | 0.202279 | 0.201305 | 0.125* | 0.453 (3) |
H10F | 0.310046 | 0.309804 | 0.212562 | 0.125* | 0.453 (3) |
C11' | 0.0987 (4) | 0.3722 (3) | 0.01170 (14) | 0.0406 (11) | 0.453 (3) |
H11B | 0.037378 | 0.304934 | 0.018218 | 0.049* | 0.453 (3) |
C12' | 0.0616 (5) | 0.4477 (5) | 0.0080 (2) | 0.0687 (16) | 0.453 (3) |
H12D | 0.006092 | 0.423188 | −0.016282 | 0.103* | 0.453 (3) |
H12E | 0.117266 | 0.513325 | −0.003055 | 0.103* | 0.453 (3) |
H12F | 0.037522 | 0.455198 | 0.040781 | 0.103* | 0.453 (3) |
C13' | 0.1426 (4) | 0.3616 (5) | −0.03709 (15) | 0.0678 (16) | 0.453 (3) |
H13D | 0.095819 | 0.351707 | −0.064475 | 0.102* | 0.453 (3) |
H13E | 0.152718 | 0.303075 | −0.035197 | 0.102* | 0.453 (3) |
H13F | 0.207670 | 0.422946 | −0.043247 | 0.102* | 0.453 (3) |
U11 | U22 | U33 | U12 | U13 | U23 | |
Nb1 | 0.02093 (12) | 0.02093 (12) | 0.02681 (18) | 0.01047 (6) | 0.000 | 0.000 |
C1 | 0.0336 (8) | 0.0277 (8) | 0.0338 (8) | 0.0170 (7) | −0.0032 (6) | −0.0023 (6) |
N1 | 0.031 (3) | 0.0278 (9) | 0.0328 (19) | 0.0103 (10) | 0.0069 (16) | −0.0040 (11) |
C2 | 0.024 (3) | 0.0248 (8) | 0.0320 (12) | 0.0097 (9) | 0.0080 (16) | −0.0062 (8) |
C3 | 0.033 (2) | 0.0317 (11) | 0.0335 (13) | 0.0161 (15) | 0.0035 (14) | −0.0037 (9) |
C4 | 0.040 (3) | 0.0268 (10) | 0.0432 (13) | 0.0144 (15) | 0.006 (2) | 0.0009 (9) |
C5 | 0.034 (3) | 0.0284 (9) | 0.0517 (11) | 0.0089 (12) | −0.0019 (15) | −0.0111 (8) |
C6 | 0.0393 (12) | 0.0401 (9) | 0.0392 (11) | 0.0189 (8) | −0.0069 (8) | −0.0115 (8) |
C7 | 0.0362 (10) | 0.0320 (8) | 0.0338 (8) | 0.0175 (7) | 0.0024 (7) | −0.0049 (6) |
C8 | 0.0591 (17) | 0.0398 (10) | 0.0444 (12) | 0.0251 (11) | −0.0030 (11) | 0.0007 (8) |
C9 | 0.087 (3) | 0.066 (4) | 0.0761 (19) | 0.0375 (19) | 0.029 (2) | 0.029 (3) |
C10 | 0.105 (4) | 0.072 (3) | 0.080 (3) | 0.049 (3) | −0.031 (4) | 0.003 (2) |
C11 | 0.058 (3) | 0.045 (2) | 0.045 (2) | 0.028 (2) | −0.0046 (19) | −0.0044 (17) |
C12 | 0.063 (3) | 0.092 (4) | 0.062 (3) | 0.037 (3) | −0.022 (2) | −0.011 (3) |
C13 | 0.091 (4) | 0.082 (3) | 0.044 (2) | 0.041 (3) | −0.004 (2) | 0.014 (2) |
C1' | 0.0336 (8) | 0.0277 (8) | 0.0338 (8) | 0.0170 (7) | −0.0032 (6) | −0.0023 (6) |
N1' | 0.031 (3) | 0.0278 (9) | 0.0328 (19) | 0.0103 (10) | 0.0069 (16) | −0.0040 (11) |
C2' | 0.024 (3) | 0.0248 (8) | 0.0320 (12) | 0.0097 (9) | 0.0080 (16) | −0.0062 (8) |
C3' | 0.033 (2) | 0.0317 (11) | 0.0335 (13) | 0.0161 (15) | 0.0035 (14) | −0.0037 (9) |
C4' | 0.040 (3) | 0.0268 (10) | 0.0432 (13) | 0.0144 (15) | 0.006 (2) | 0.0009 (9) |
C5' | 0.034 (3) | 0.0284 (9) | 0.0517 (11) | 0.0089 (12) | −0.0019 (15) | −0.0111 (8) |
C6' | 0.0393 (12) | 0.0401 (9) | 0.0392 (11) | 0.0189 (8) | −0.0069 (8) | −0.0115 (8) |
C7' | 0.0362 (10) | 0.0320 (8) | 0.0338 (8) | 0.0175 (7) | 0.0024 (7) | −0.0049 (6) |
C8' | 0.0591 (17) | 0.0398 (10) | 0.0444 (12) | 0.0251 (11) | −0.0030 (11) | 0.0007 (8) |
C9' | 0.087 (3) | 0.066 (4) | 0.0761 (19) | 0.0375 (19) | 0.029 (2) | 0.029 (3) |
C10' | 0.105 (4) | 0.072 (3) | 0.080 (3) | 0.049 (3) | −0.031 (4) | 0.003 (2) |
C11' | 0.044 (3) | 0.040 (2) | 0.038 (2) | 0.022 (3) | −0.004 (2) | 0.0000 (18) |
C12' | 0.086 (4) | 0.073 (4) | 0.066 (3) | 0.054 (3) | −0.022 (3) | −0.006 (3) |
C13' | 0.070 (3) | 0.090 (4) | 0.034 (2) | 0.033 (3) | −0.006 (2) | −0.012 (3) |
Nb1—C1i | 2.1542 (15) | C13—H13A | 0.9800 |
Nb1—C1ii | 2.1541 (15) | C13—H13B | 0.9800 |
Nb1—C1iii | 2.1541 (15) | C13—H13C | 0.9800 |
Nb1—C1' | 2.1542 (15) | C1'—N1' | 1.189 (2) |
Nb1—C1 | 2.1542 (15) | N1'—C2' | 1.391 (2) |
Nb1—C1iv | 2.1542 (15) | C2'—C3' | 1.401 (3) |
Nb1—C1v | 2.1542 (15) | C2'—C7' | 1.403 (3) |
C1—N1 | 1.187 (2) | C3'—C4' | 1.387 (3) |
N1—C2 | 1.389 (2) | C3'—C11' | 1.513 (3) |
C2—C3 | 1.401 (3) | C4'—C5' | 1.372 (3) |
C2—C7 | 1.404 (3) | C4'—H4B | 0.9500 |
C3—C4 | 1.387 (3) | C5'—C6' | 1.372 (3) |
C3—C11 | 1.518 (3) | C5'—H5B | 0.9500 |
C4—C5 | 1.371 (3) | C6'—C7' | 1.386 (3) |
C4—H4A | 0.9500 | C6'—H6B | 0.9500 |
C5—C6 | 1.372 (3) | C7'—C8' | 1.518 (3) |
C5—H5A | 0.9500 | C8'—C9' | 1.520 (4) |
C6—C7 | 1.387 (3) | C8'—C10' | 1.522 (4) |
C6—H6A | 0.9500 | C8'—H8B | 1.0000 |
C7—C8 | 1.518 (3) | C9'—H9D | 0.9853 |
C8—C9 | 1.519 (4) | C9'—H9E | 0.9855 |
C8—C10 | 1.523 (3) | C9'—H9F | 0.9868 |
C8—H8A | 1.0000 | C10'—H10D | 0.9874 |
C9—H9A | 0.9800 | C10'—H10E | 0.9889 |
C9—H9B | 0.9800 | C10'—H10F | 0.9831 |
C9—H9C | 0.9800 | C11'—C13' | 1.512 (4) |
C10—H10A | 0.9800 | C11'—C12' | 1.519 (3) |
C10—H10B | 0.9800 | C11'—H11B | 1.0000 |
C10—H10C | 0.9800 | C12'—H12D | 0.9800 |
C11—C13 | 1.517 (3) | C12'—H12E | 0.9800 |
C11—C12 | 1.523 (3) | C12'—H12F | 0.9800 |
C11—H11A | 1.0000 | C13'—H13D | 0.9800 |
C12—H12A | 0.9800 | C13'—H13E | 0.9800 |
C12—H12B | 0.9800 | C13'—H13F | 0.9800 |
C12—H12C | 0.9800 | ||
C1i—Nb1—C1ii | 95.46 (6) | H12A—C12—H12C | 109.5 |
C1i—Nb1—C1iii | 84.54 (6) | H12B—C12—H12C | 109.5 |
C1ii—Nb1—C1iii | 180.00 (15) | C11—C13—H13A | 109.5 |
C1i—Nb1—C1 | 180.0 | C11—C13—H13B | 109.5 |
C1ii—Nb1—C1 | 84.54 (6) | H13A—C13—H13B | 109.5 |
C1iii—Nb1—C1 | 95.46 (6) | C11—C13—H13C | 109.5 |
C1i—Nb1—C1iv | 95.46 (6) | H13A—C13—H13C | 109.5 |
C1ii—Nb1—C1iv | 95.46 (6) | H13B—C13—H13C | 109.5 |
C1iii—Nb1—C1iv | 84.54 (6) | N1'—C1'—Nb1 | 173.2 (4) |
C1'—Nb1—C1iv | 84.54 (6) | C1'—N1'—C2' | 157.7 (6) |
C1—Nb1—C1iv | 84.54 (6) | N1'—C2'—C3' | 118.7 (4) |
C1i—Nb1—C1v | 84.54 (6) | N1'—C2'—C7' | 118.4 (4) |
C1ii—Nb1—C1v | 84.54 (6) | C3'—C2'—C7' | 122.8 (3) |
C1iii—Nb1—C1v | 95.46 (6) | C4'—C3'—C2' | 116.8 (3) |
C1'—Nb1—C1v | 95.46 (6) | C4'—C3'—C11' | 122.5 (4) |
C1—Nb1—C1v | 95.46 (6) | C2'—C3'—C11' | 120.7 (3) |
C1iv—Nb1—C1v | 180.00 (10) | C5'—C4'—C3' | 121.5 (4) |
N1—C1—Nb1 | 168.3 (3) | C5'—C4'—H4B | 119.3 |
C1—N1—C2 | 177.6 (6) | C3'—C4'—H4B | 119.3 |
N1—C2—C3 | 118.0 (3) | C6'—C5'—C4' | 120.5 (4) |
N1—C2—C7 | 119.0 (3) | C6'—C5'—H5B | 119.7 |
C3—C2—C7 | 123.0 (3) | C4'—C5'—H5B | 119.7 |
C4—C3—C2 | 116.8 (3) | C5'—C6'—C7' | 121.2 (4) |
C4—C3—C11 | 122.1 (3) | C5'—C6'—H6B | 119.4 |
C2—C3—C11 | 121.1 (3) | C7'—C6'—H6B | 119.4 |
C5—C4—C3 | 121.5 (3) | C6'—C7'—C2' | 117.1 (3) |
C5—C4—H4A | 119.2 | C6'—C7'—C8' | 122.7 (4) |
C3—C4—H4A | 119.2 | C2'—C7'—C8' | 120.2 (4) |
C6—C5—C4 | 120.5 (3) | C7'—C8'—C9' | 110.7 (4) |
C6—C5—H5A | 119.8 | C7'—C8'—C10' | 112.7 (5) |
C4—C5—H5A | 119.8 | C9'—C8'—C10' | 110.6 (5) |
C5—C6—C7 | 121.4 (3) | C7'—C8'—H8B | 107.5 |
C5—C6—H6A | 119.3 | C9'—C8'—H8B | 107.5 |
C7—C6—H6A | 119.3 | C10'—C8'—H8B | 107.5 |
C6—C7—C2 | 116.8 (3) | C8'—C9'—H9D | 111.2 |
C6—C7—C8 | 122.3 (3) | C8'—C9'—H9E | 106.0 |
C2—C7—C8 | 120.9 (3) | H9D—C9'—H9E | 109.0 |
C7—C8—C9 | 111.1 (4) | C8'—C9'—H9F | 111.2 |
C7—C8—C10 | 112.7 (4) | H9D—C9'—H9F | 109.0 |
C9—C8—C10 | 110.6 (4) | H9E—C9'—H9F | 110.4 |
C7—C8—H8A | 107.4 | C8'—C10'—H10D | 111.1 |
C9—C8—H8A | 107.4 | C8'—C10'—H10E | 108.8 |
C10—C8—H8A | 107.4 | H10D—C10'—H10E | 109.2 |
C8—C9—H9A | 109.5 | C8'—C10'—H10F | 108.4 |
C8—C9—H9B | 109.5 | H10D—C10'—H10F | 109.0 |
H9A—C9—H9B | 109.5 | H10E—C10'—H10F | 110.3 |
C8—C9—H9C | 109.5 | C13'—C11'—C3' | 112.7 (3) |
H9A—C9—H9C | 109.5 | C13'—C11'—C12' | 112.2 (4) |
H9B—C9—H9C | 109.5 | C3'—C11'—C12' | 113.0 (3) |
C8—C10—H10A | 109.5 | C13'—C11'—H11B | 106.1 |
C8—C10—H10B | 109.5 | C3'—C11'—H11B | 106.1 |
H10A—C10—H10B | 109.5 | C12'—C11'—H11B | 106.1 |
C8—C10—H10C | 109.5 | C11'—C12'—H12D | 109.5 |
H10A—C10—H10C | 109.5 | C11'—C12'—H12E | 109.5 |
H10B—C10—H10C | 109.5 | H12D—C12'—H12E | 109.5 |
C13—C11—C3 | 113.5 (3) | C11'—C12'—H12F | 109.5 |
C13—C11—C12 | 110.0 (3) | H12D—C12'—H12F | 109.5 |
C3—C11—C12 | 109.5 (3) | H12E—C12'—H12F | 109.5 |
C13—C11—H11A | 107.9 | C11'—C13'—H13D | 109.5 |
C3—C11—H11A | 107.9 | C11'—C13'—H13E | 109.5 |
C12—C11—H11A | 107.9 | H13D—C13'—H13E | 109.5 |
C11—C12—H12A | 109.5 | C11'—C13'—H13F | 109.5 |
C11—C12—H12B | 109.5 | H13D—C13'—H13F | 109.5 |
H12A—C12—H12B | 109.5 | H13E—C13'—H13F | 109.5 |
C11—C12—H12C | 109.5 | ||
N1—C2—C3—C4 | −176.8 (4) | C1'—N1'—C2'—C7' | −98 (2) |
C7—C2—C3—C4 | 1.6 (7) | N1'—C2'—C3'—C4' | −176.2 (6) |
N1—C2—C3—C11 | 1.8 (7) | C7'—C2'—C3'—C4' | 1.0 (10) |
C7—C2—C3—C11 | −179.8 (5) | N1'—C2'—C3'—C11' | 2.6 (9) |
C2—C3—C4—C5 | 0.0 (8) | C7'—C2'—C3'—C11' | 179.7 (6) |
C11—C3—C4—C5 | −178.5 (6) | C2'—C3'—C4'—C5' | −1.1 (10) |
C3—C4—C5—C6 | −2.0 (11) | C11'—C3'—C4'—C5' | −179.8 (8) |
C4—C5—C6—C7 | 2.3 (13) | C3'—C4'—C5'—C6' | 0.5 (14) |
C5—C6—C7—C2 | −0.6 (11) | C4'—C5'—C6'—C7' | 0.3 (16) |
C5—C6—C7—C8 | 179.8 (8) | C5'—C6'—C7'—C2' | −0.4 (13) |
N1—C2—C7—C6 | 177.0 (6) | C5'—C6'—C7'—C8' | −178.6 (9) |
C3—C2—C7—C6 | −1.4 (8) | N1'—C2'—C7'—C6' | 176.9 (7) |
N1—C2—C7—C8 | −3.4 (8) | C3'—C2'—C7'—C6' | −0.2 (10) |
C3—C2—C7—C8 | 178.2 (6) | N1'—C2'—C7'—C8' | −4.9 (10) |
C6—C7—C8—C9 | 101.3 (17) | C3'—C2'—C7'—C8' | 178.0 (7) |
C2—C7—C8—C9 | −78.3 (17) | C6'—C7'—C8'—C9' | 109 (2) |
C6—C7—C8—C10 | −23.5 (18) | C2'—C7'—C8'—C9' | −69 (2) |
C2—C7—C8—C10 | 156.9 (18) | C6'—C7'—C8'—C10' | −15 (2) |
C4—C3—C11—C13 | 22.5 (5) | C2'—C7'—C8'—C10' | 167 (2) |
C2—C3—C11—C13 | −156.0 (5) | C4'—C3'—C11'—C13' | 90.8 (5) |
C4—C3—C11—C12 | −100.8 (4) | C2'—C3'—C11'—C13' | −87.8 (6) |
C2—C3—C11—C12 | 80.7 (5) | C4'—C3'—C11'—C12' | −37.7 (6) |
C1'—N1'—C2'—C3' | 79 (2) | C2'—C3'—C11'—C12' | 143.7 (6) |
Symmetry codes: (i) −x, −y, −z; (ii) y, −x+y, −z; (iii) −y, x−y, z; (iv) x−y, x, −z; (v) −x+y, −x, z. |
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