Supporting information
Crystallographic Information File (CIF) https://doi.org/10.1107/S2053229620005008/qf3038sup1.cif | |
Structure factor file (CIF format) https://doi.org/10.1107/S2053229620005008/qf3038Isup2.hkl |
CCDC reference: 1995828
Data collection: CrysAlis PRO (Agilent, 2014); cell refinement: CrysAlis PRO (Agilent, 2014); data reduction: CrysAlis PRP (Agilent, 2014); program(s) used to solve structure: OLEX2 (Dolomanov et al., 2009); program(s) used to refine structure: SHELXL2018 (Sheldrick, 2015); molecular graphics: OLEX2 (Dolomanov et al., 2009); software used to prepare material for publication: publCIF (Westrip, 2010) and PLATON (Spek, 2020).
[Ni3(C18H13O8Si)2(C10H24N4)3]·4CH4O | F(000) = 1780 |
Mr = 1676.04 | Dx = 1.362 Mg m−3 |
Monoclinic, P21/c | Mo Kα radiation, λ = 0.71073 Å |
a = 13.5400 (7) Å | Cell parameters from 3580 reflections |
b = 14.0473 (6) Å | θ = 1.9–26.3° |
c = 22.0478 (12) Å | µ = 0.79 mm−1 |
β = 102.895 (5)° | T = 160 K |
V = 4087.7 (4) Å3 | Irregular, light violet |
Z = 2 | 0.25 × 0.10 × 0.03 mm |
Agilent Xcalibur Eos diffractometer | 5410 reflections with I > 2σ(I) |
Detector resolution: 8.0797 pixels mm-1 | Rint = 0.062 |
ω scans | θmax = 26.0°, θmin = 1.7° |
Absorption correction: multi-scan (CrysAlis PRO; Agilent, 2014) | h = −16→16 |
Tmin = 0.898, Tmax = 1.000 | k = −17→17 |
20822 measured reflections | l = −27→17 |
8041 independent reflections |
Refinement on F2 | 141 restraints |
Least-squares matrix: full | Hydrogen site location: mixed |
R[F2 > 2σ(F2)] = 0.068 | H-atom parameters constrained |
wR(F2) = 0.130 | w = 1/[σ2(Fo2) + (0.0379P)2 + 4.0667P] where P = (Fo2 + 2Fc2)/3 |
S = 1.05 | (Δ/σ)max < 0.001 |
8041 reflections | Δρmax = 0.64 e Å−3 |
519 parameters | Δρmin = −0.41 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. Crystallographic measurements were carried out with an Oxford-Diffraction Xcalibur E CCD diffractometer equipped with graphite-monochromated Mo-Ka radiation. The unit cell determination and data integration were carried out using the CrysAlis package of Oxford Diffraction. The structure was solved by direct methods using Olex2 and refined by full-matrix least-squares on F2. Atomic displacements for non-hydrogen atoms were refined using an anisotropic model. |
x | y | z | Uiso*/Ueq | Occ. (<1) | |
Ni1 | 0.500000 | 0.500000 | 0.500000 | 0.01529 (18) | |
Ni2 | −0.02509 (4) | 0.24865 (4) | 0.14648 (2) | 0.02124 (15) | |
Si1 | 0.45189 (9) | 0.02454 (7) | 0.36702 (5) | 0.0187 (3) | |
O1 | 0.5459 (2) | 0.35919 (18) | 0.48894 (13) | 0.0223 (7) | |
O2 | 0.7037 (2) | 0.3513 (2) | 0.54473 (14) | 0.0343 (8) | |
O3 | 0.8684 (2) | 0.19926 (18) | 0.56857 (12) | 0.0229 (7) | |
C31 | 0.1371 (3) | 0.2434 (3) | 0.26931 (19) | 0.0231 (10) | |
C2 | 0.5614 (4) | 0.5186 (3) | 0.6311 (2) | 0.0377 (13) | |
H2A | 0.527283 | 0.578512 | 0.634185 | 0.045* | |
H2B | 0.610634 | 0.508034 | 0.669774 | 0.045* | |
O4 | 0.8792 (2) | 0.2890 (2) | 0.48579 (13) | 0.0274 (7) | |
N2 | 0.6122 (3) | 0.5221 (2) | 0.57947 (15) | 0.0245 (9) | |
H2 | 0.656765 | 0.466421 | 0.583870 | 0.029* | |
N1 | 0.4131 (3) | 0.4540 (2) | 0.55990 (16) | 0.0280 (9) | |
H1 | 0.368437 | 0.506529 | 0.565598 | 0.034* | |
O5 | 0.0727 (2) | 0.19903 (19) | 0.22917 (13) | 0.0299 (8) | |
C16 | 0.6313 (3) | 0.3196 (3) | 0.50553 (18) | 0.0193 (9) | |
C7 | 0.1445 (9) | 0.2664 (8) | 0.0903 (8) | 0.027 (4) | 0.781 (3) |
H7A | 0.174283 | 0.258548 | 0.054451 | 0.032* | 0.781 (3) |
H7B | 0.197020 | 0.255712 | 0.127459 | 0.032* | 0.781 (3) |
O10X | 0.7373 (8) | 0.4040 (8) | 0.4033 (5) | 0.0358 (12)* | 0.48 (2) |
H10X | 0.771654 | 0.374972 | 0.432895 | 0.054* | 0.48 (2) |
O6 | 0.1691 (2) | 0.3255 (2) | 0.26436 (14) | 0.0379 (9) | |
N3 | 0.0532 (3) | 0.3723 (3) | 0.14296 (19) | 0.0255 (6) | 0.781 (3) |
H3 | 0.106903 | 0.373919 | 0.180989 | 0.031* | 0.781 (3) |
C30 | 0.1874 (3) | 0.1883 (3) | 0.32705 (19) | 0.0201 (10) | |
C5 | 0.3493 (4) | 0.3713 (3) | 0.5383 (2) | 0.0404 (13) | |
H5A | 0.311335 | 0.354649 | 0.569198 | 0.049* | |
H5B | 0.391985 | 0.317600 | 0.533610 | 0.049* | |
C12 | −0.2009 (5) | 0.2257 (5) | 0.1937 (3) | 0.0397 (18) | 0.781 (3) |
H12A | −0.249712 | 0.238567 | 0.155126 | 0.048* | 0.781 (3) |
H12B | −0.235158 | 0.231252 | 0.227702 | 0.048* | 0.781 (3) |
C23 | 0.5584 (3) | 0.1779 (3) | 0.44063 (17) | 0.0164 (9) | |
H23 | 0.494855 | 0.205301 | 0.437256 | 0.020* | |
O8 | 0.0036 (3) | 0.2773 (3) | 0.34502 (16) | 0.0547 (11) | |
C4 | 0.2763 (3) | 0.3906 (3) | 0.4768 (2) | 0.0391 (13) | |
H4A | 0.242931 | 0.450976 | 0.479881 | 0.047* | |
H4B | 0.224545 | 0.341594 | 0.470073 | 0.047* | |
C3 | 0.6773 (3) | 0.6059 (3) | 0.5797 (2) | 0.0353 (12) | |
H3A | 0.731066 | 0.604979 | 0.617034 | 0.042* | |
H3B | 0.637541 | 0.663123 | 0.580741 | 0.042* | |
C25 | 0.4601 (4) | 0.0213 (3) | 0.28406 (19) | 0.0361 (12) | |
H25A | 0.404628 | −0.015249 | 0.260554 | 0.054* | |
H25B | 0.522937 | −0.007625 | 0.280780 | 0.054* | |
H25C | 0.456913 | 0.084956 | 0.267961 | 0.054* | |
C28 | 0.2047 (3) | 0.1289 (3) | 0.43107 (19) | 0.0233 (10) | |
H28 | 0.180937 | 0.124394 | 0.467407 | 0.028* | |
C27 | 0.2943 (3) | 0.0831 (3) | 0.42732 (19) | 0.0253 (10) | |
H27 | 0.329588 | 0.048738 | 0.461375 | 0.030* | |
C17 | 0.6432 (3) | 0.2261 (3) | 0.47454 (18) | 0.0173 (9) | |
C33 | 0.2767 (3) | 0.1406 (3) | 0.32442 (18) | 0.0199 (9) | |
H33 | 0.300500 | 0.144355 | 0.288045 | 0.024* | |
C6 | 0.1043 (4) | 0.3649 (4) | 0.0911 (2) | 0.0291 (14) | 0.781 (3) |
H6A | 0.159366 | 0.410571 | 0.096377 | 0.035* | 0.781 (3) |
H6B | 0.056920 | 0.378511 | 0.052079 | 0.035* | 0.781 (3) |
N4 | 0.0623 (3) | 0.1956 (3) | 0.0874 (2) | 0.0255 (6) | 0.781 (3) |
H4 | 0.019763 | 0.199878 | 0.045252 | 0.031* | 0.781 (3) |
C29 | 0.1505 (3) | 0.1811 (3) | 0.38124 (19) | 0.0199 (9) | |
O7 | 0.0295 (3) | 0.2155 (3) | 0.43904 (15) | 0.0499 (10) | |
H7 | −0.023085 | 0.243948 | 0.439673 | 0.075* | |
C26 | 0.3318 (3) | 0.0875 (3) | 0.37398 (18) | 0.0186 (9) | |
N6 | −0.1174 (3) | 0.2954 (3) | 0.20186 (19) | 0.0255 (6) | 0.781 (3) |
H6 | −0.078942 | 0.289576 | 0.244970 | 0.031* | 0.781 (3) |
C32 | 0.0538 (3) | 0.2297 (3) | 0.3849 (2) | 0.0240 (10) | |
O9 | 0.3328 (7) | 0.3757 (7) | 0.2170 (6) | 0.0674 (17)* | 0.68 (4) |
H9 | 0.293274 | 0.367023 | 0.239736 | 0.101* | 0.68 (4) |
C19 | 0.8356 (3) | 0.2299 (3) | 0.51494 (19) | 0.0202 (9) | |
C24 | 0.4528 (3) | −0.0978 (3) | 0.3994 (2) | 0.0373 (12) | |
H24A | 0.398831 | −0.134264 | 0.374409 | 0.056* | |
H24B | 0.443588 | −0.094432 | 0.441319 | 0.056* | |
H24C | 0.516488 | −0.127749 | 0.399342 | 0.056* | |
C18 | 0.7381 (3) | 0.1856 (3) | 0.47911 (18) | 0.0181 (9) | |
C20 | 0.7464 (3) | 0.0995 (3) | 0.44918 (19) | 0.0241 (10) | |
H20 | 0.810144 | 0.073027 | 0.451680 | 0.029* | |
C22 | 0.5645 (3) | 0.0906 (3) | 0.41168 (18) | 0.0184 (9) | |
C11 | −0.1600 (6) | 0.1274 (5) | 0.1921 (3) | 0.0366 (19) | 0.781 (3) |
H11A | −0.113528 | 0.112984 | 0.231289 | 0.044* | 0.781 (3) |
H11B | −0.214852 | 0.081480 | 0.185587 | 0.044* | 0.781 (3) |
N5 | −0.1068 (3) | 0.1223 (3) | 0.1407 (2) | 0.0255 (6) | 0.781 (3) |
H5 | −0.158362 | 0.123963 | 0.101679 | 0.031* | 0.781 (3) |
C1 | 0.4855 (4) | 0.4385 (3) | 0.6197 (2) | 0.0374 (12) | |
H1A | 0.520227 | 0.378314 | 0.618742 | 0.045* | |
H1B | 0.449587 | 0.436097 | 0.653102 | 0.045* | |
C21 | 0.6620 (3) | 0.0527 (3) | 0.41600 (19) | 0.0252 (10) | |
H21 | 0.669602 | −0.004425 | 0.396246 | 0.030* | |
C14 | −0.0612 (7) | 0.4600 (4) | 0.1967 (4) | 0.043 (2) | 0.781 (3) |
H14A | −0.011748 | 0.443902 | 0.234370 | 0.051* | 0.781 (3) |
H14B | −0.084050 | 0.524325 | 0.201951 | 0.051* | 0.781 (3) |
C13 | −0.1487 (5) | 0.3959 (4) | 0.1925 (3) | 0.0352 (17) | 0.781 (3) |
H13A | −0.194052 | 0.403007 | 0.151986 | 0.042* | 0.781 (3) |
H13B | −0.185579 | 0.414038 | 0.223766 | 0.042* | 0.781 (3) |
C9 | 0.0076 (5) | 0.0287 (4) | 0.0886 (3) | 0.0377 (17) | 0.781 (3) |
H9A | −0.039755 | 0.042695 | 0.049630 | 0.045* | 0.781 (3) |
H9B | 0.031393 | −0.036033 | 0.085999 | 0.045* | 0.781 (3) |
C10 | −0.0483 (6) | 0.0339 (4) | 0.1407 (3) | 0.0317 (16) | 0.781 (3) |
H10A | −0.094128 | −0.019916 | 0.137349 | 0.038* | 0.781 (3) |
H10B | 0.000345 | 0.028587 | 0.180208 | 0.038* | 0.781 (3) |
C8 | 0.0974 (4) | 0.0958 (4) | 0.0954 (3) | 0.0321 (15) | 0.781 (3) |
H8A | 0.141564 | 0.087850 | 0.136290 | 0.039* | 0.781 (3) |
H8B | 0.135853 | 0.080462 | 0.064506 | 0.039* | 0.781 (3) |
C34 | 0.3987 (13) | 0.2921 (7) | 0.2204 (10) | 0.065 (3)* | 0.68 (4) |
H34A | 0.359812 | 0.238897 | 0.200761 | 0.097* | 0.68 (4) |
H34B | 0.427240 | 0.277048 | 0.263252 | 0.097* | 0.68 (4) |
H34C | 0.452256 | 0.305512 | 0.199579 | 0.097* | 0.68 (4) |
C35X | 0.7232 (12) | 0.3482 (13) | 0.3502 (5) | 0.051 (2)* | 0.48 (2) |
H35A | 0.677970 | 0.379938 | 0.316549 | 0.076* | 0.48 (2) |
H35B | 0.694675 | 0.288005 | 0.357888 | 0.076* | 0.48 (2) |
H35C | 0.787222 | 0.337907 | 0.339338 | 0.076* | 0.48 (2) |
N4X | 0.0201 (11) | 0.1303 (7) | 0.1066 (6) | 0.0255 (6) | 0.219 (3) |
H4X | −0.019083 | 0.128137 | 0.063519 | 0.031* | 0.219 (3) |
N3X | 0.0984 (8) | 0.3195 (9) | 0.1288 (7) | 0.0255 (6) | 0.219 (3) |
H3X | 0.149315 | 0.319445 | 0.168130 | 0.031* | 0.219 (3) |
N6X | −0.0630 (11) | 0.3656 (7) | 0.1946 (6) | 0.0255 (6) | 0.219 (3) |
H6X | −0.020204 | 0.361620 | 0.236711 | 0.031* | 0.219 (3) |
N5X | −0.1493 (9) | 0.1931 (12) | 0.1737 (7) | 0.0255 (6) | 0.219 (3) |
H5X | −0.203788 | 0.194857 | 0.136068 | 0.031* | 0.219 (3) |
C15X | 0.0851 (19) | 0.4200 (11) | 0.1095 (10) | 0.035 (6)* | 0.219 (3) |
H15A | 0.030887 | 0.423084 | 0.072469 | 0.042* | 0.219 (3) |
H15B | 0.146599 | 0.440705 | 0.097864 | 0.042* | 0.219 (3) |
C8X | 0.004 (2) | 0.0390 (15) | 0.1358 (14) | 0.046 (7)* | 0.219 (3) |
H8XA | 0.054247 | 0.031577 | 0.174365 | 0.056* | 0.219 (3) |
H8XB | 0.012144 | −0.012858 | 0.108325 | 0.056* | 0.219 (3) |
C14X | 0.062 (2) | 0.4892 (19) | 0.1551 (13) | 0.057 (8)* | 0.219 (3) |
H14C | 0.057803 | 0.553008 | 0.137897 | 0.068* | 0.219 (3) |
H14D | 0.115033 | 0.488245 | 0.192821 | 0.068* | 0.219 (3) |
C13X | −0.044 (3) | 0.4604 (14) | 0.1705 (15) | 0.039 (9)* | 0.219 (3) |
H13C | −0.056843 | 0.506664 | 0.200382 | 0.046* | 0.219 (3) |
H13D | −0.094894 | 0.470089 | 0.132627 | 0.046* | 0.219 (3) |
C9X | −0.1043 (19) | 0.0343 (18) | 0.1495 (12) | 0.039 (7)* | 0.219 (3) |
H9XA | −0.151109 | 0.043418 | 0.109622 | 0.047* | 0.219 (3) |
H9XB | −0.113088 | −0.031044 | 0.161511 | 0.047* | 0.219 (3) |
C12X | −0.1684 (13) | 0.3533 (18) | 0.2014 (13) | 0.036 (7)* | 0.219 (3) |
H12C | −0.181466 | 0.395671 | 0.233445 | 0.043* | 0.219 (3) |
H12D | −0.215185 | 0.369064 | 0.162573 | 0.043* | 0.219 (3) |
C11X | −0.183 (2) | 0.2582 (18) | 0.2176 (12) | 0.039 (8)* | 0.219 (3) |
H11C | −0.254210 | 0.247424 | 0.216380 | 0.047* | 0.219 (3) |
H11D | −0.144873 | 0.245821 | 0.259541 | 0.047* | 0.219 (3) |
C10X | −0.142 (3) | 0.0920 (13) | 0.1927 (17) | 0.046 (7)* | 0.219 (3) |
H10C | −0.097433 | 0.086340 | 0.233584 | 0.056* | 0.219 (3) |
H10D | −0.208581 | 0.069345 | 0.195522 | 0.056* | 0.219 (3) |
C7X | 0.1229 (14) | 0.162 (2) | 0.1048 (14) | 0.060 (8)* | 0.219 (3) |
H7XA | 0.165630 | 0.152089 | 0.145957 | 0.072* | 0.219 (3) |
H7XB | 0.147955 | 0.119703 | 0.076668 | 0.072* | 0.219 (3) |
C15 | −0.0057 (6) | 0.4615 (4) | 0.1426 (3) | 0.0365 (18) | 0.781 (3) |
H15C | −0.054644 | 0.467559 | 0.103307 | 0.044* | 0.781 (3) |
H15D | 0.039585 | 0.515858 | 0.147069 | 0.044* | 0.781 (3) |
C6X | 0.136 (4) | 0.253 (3) | 0.087 (3) | 0.036 (15)* | 0.219 (3) |
H6XA | 0.100185 | 0.263171 | 0.044684 | 0.043* | 0.219 (3) |
H6XB | 0.207842 | 0.264945 | 0.089899 | 0.043* | 0.219 (3) |
C34X | 0.423 (2) | 0.3000 (19) | 0.2420 (18) | 0.065 (3)* | 0.32 (4) |
H34D | 0.420272 | 0.237330 | 0.224267 | 0.097* | 0.32 (4) |
H34E | 0.413227 | 0.295689 | 0.283762 | 0.097* | 0.32 (4) |
H34F | 0.487360 | 0.328346 | 0.242411 | 0.097* | 0.32 (4) |
O9X | 0.3422 (17) | 0.3587 (19) | 0.2046 (11) | 0.0674 (17)* | 0.32 (4) |
H9X | 0.299893 | 0.366154 | 0.226772 | 0.101* | 0.32 (4) |
O10 | 0.7548 (8) | 0.4224 (7) | 0.4134 (4) | 0.0358 (12)* | 0.52 (2) |
H10 | 0.794450 | 0.390413 | 0.438930 | 0.054* | 0.52 (2) |
C35 | 0.7467 (11) | 0.3841 (13) | 0.3541 (5) | 0.051 (2)* | 0.52 (2) |
H35D | 0.738771 | 0.434726 | 0.324118 | 0.076* | 0.52 (2) |
H35E | 0.688918 | 0.342753 | 0.344327 | 0.076* | 0.52 (2) |
H35F | 0.806877 | 0.348627 | 0.353056 | 0.076* | 0.52 (2) |
U11 | U22 | U33 | U12 | U13 | U23 | |
Ni1 | 0.0109 (4) | 0.0181 (4) | 0.0156 (4) | 0.0010 (3) | 0.0003 (3) | −0.0051 (3) |
Ni2 | 0.0139 (3) | 0.0239 (3) | 0.0236 (3) | 0.0023 (3) | −0.0008 (2) | 0.0066 (2) |
Si1 | 0.0174 (6) | 0.0192 (6) | 0.0165 (6) | 0.0000 (5) | −0.0024 (5) | −0.0034 (5) |
O1 | 0.0123 (14) | 0.0202 (14) | 0.0316 (17) | 0.0048 (13) | −0.0012 (13) | −0.0091 (13) |
O2 | 0.0201 (17) | 0.0324 (17) | 0.043 (2) | 0.0071 (15) | −0.0089 (15) | −0.0219 (15) |
O3 | 0.0206 (16) | 0.0264 (15) | 0.0186 (16) | −0.0065 (14) | −0.0027 (13) | −0.0037 (13) |
C31 | 0.020 (2) | 0.024 (2) | 0.023 (2) | 0.005 (2) | −0.0006 (19) | 0.0066 (19) |
C2 | 0.033 (3) | 0.054 (3) | 0.022 (3) | 0.014 (3) | −0.002 (2) | −0.010 (2) |
O4 | 0.0184 (16) | 0.0333 (17) | 0.0291 (18) | 0.0000 (14) | 0.0026 (14) | 0.0016 (14) |
N2 | 0.0192 (19) | 0.0255 (19) | 0.025 (2) | 0.0058 (17) | −0.0034 (16) | −0.0097 (16) |
N1 | 0.023 (2) | 0.031 (2) | 0.031 (2) | 0.0024 (18) | 0.0099 (18) | 0.0001 (17) |
O5 | 0.0236 (17) | 0.0259 (16) | 0.0308 (18) | −0.0038 (14) | −0.0136 (15) | 0.0085 (14) |
C16 | 0.016 (2) | 0.021 (2) | 0.020 (2) | 0.0002 (19) | 0.0025 (19) | −0.0035 (18) |
C7 | 0.022 (5) | 0.038 (6) | 0.022 (5) | −0.004 (4) | 0.008 (3) | 0.003 (3) |
O6 | 0.045 (2) | 0.0265 (17) | 0.0320 (19) | −0.0087 (16) | −0.0140 (16) | 0.0089 (14) |
N3 | 0.0211 (13) | 0.0298 (13) | 0.0212 (12) | 0.0014 (11) | −0.0047 (10) | 0.0019 (10) |
C30 | 0.021 (2) | 0.0124 (19) | 0.023 (2) | −0.0031 (19) | −0.0036 (19) | −0.0010 (17) |
C5 | 0.029 (3) | 0.038 (3) | 0.057 (4) | −0.006 (2) | 0.014 (3) | 0.002 (3) |
C12 | 0.031 (4) | 0.055 (5) | 0.033 (4) | 0.006 (4) | 0.008 (3) | −0.003 (4) |
C23 | 0.012 (2) | 0.018 (2) | 0.018 (2) | 0.0049 (18) | 0.0027 (17) | −0.0007 (16) |
O8 | 0.044 (2) | 0.077 (3) | 0.046 (2) | 0.038 (2) | 0.0169 (19) | 0.026 (2) |
C4 | 0.019 (3) | 0.031 (3) | 0.064 (4) | −0.011 (2) | 0.003 (3) | −0.008 (2) |
C3 | 0.023 (3) | 0.031 (3) | 0.045 (3) | 0.002 (2) | −0.008 (2) | −0.018 (2) |
C25 | 0.032 (3) | 0.049 (3) | 0.025 (3) | 0.009 (2) | 0.000 (2) | −0.009 (2) |
C28 | 0.022 (2) | 0.031 (2) | 0.017 (2) | −0.002 (2) | 0.0033 (19) | 0.0016 (19) |
C27 | 0.022 (2) | 0.030 (2) | 0.021 (2) | 0.000 (2) | −0.002 (2) | 0.0021 (19) |
C17 | 0.016 (2) | 0.015 (2) | 0.020 (2) | 0.0013 (18) | 0.0029 (18) | −0.0010 (16) |
C33 | 0.019 (2) | 0.024 (2) | 0.014 (2) | −0.005 (2) | −0.0006 (18) | 0.0003 (18) |
C6 | 0.025 (3) | 0.025 (3) | 0.035 (4) | −0.004 (3) | 0.004 (3) | 0.012 (3) |
N4 | 0.0211 (13) | 0.0298 (13) | 0.0212 (12) | 0.0014 (11) | −0.0047 (10) | 0.0019 (10) |
C29 | 0.015 (2) | 0.021 (2) | 0.021 (2) | −0.0027 (19) | −0.0024 (18) | −0.0035 (17) |
O7 | 0.033 (2) | 0.081 (3) | 0.039 (2) | 0.030 (2) | 0.0160 (18) | 0.0093 (19) |
C26 | 0.015 (2) | 0.017 (2) | 0.020 (2) | −0.0014 (18) | −0.0047 (18) | −0.0013 (17) |
N6 | 0.0211 (13) | 0.0298 (13) | 0.0212 (12) | 0.0014 (11) | −0.0047 (10) | 0.0019 (10) |
C32 | 0.022 (2) | 0.026 (2) | 0.022 (2) | −0.001 (2) | 0.001 (2) | −0.0058 (19) |
C19 | 0.015 (2) | 0.020 (2) | 0.024 (2) | 0.0072 (19) | 0.0020 (19) | −0.0036 (18) |
C24 | 0.030 (3) | 0.029 (2) | 0.049 (3) | −0.003 (2) | 0.001 (3) | 0.001 (2) |
C18 | 0.017 (2) | 0.020 (2) | 0.016 (2) | 0.0023 (19) | 0.0005 (18) | −0.0021 (17) |
C20 | 0.015 (2) | 0.023 (2) | 0.032 (3) | 0.007 (2) | −0.001 (2) | −0.0060 (19) |
C22 | 0.016 (2) | 0.021 (2) | 0.015 (2) | 0.0035 (19) | −0.0025 (18) | −0.0007 (17) |
C11 | 0.030 (4) | 0.043 (5) | 0.033 (4) | −0.016 (4) | −0.002 (3) | 0.008 (4) |
N5 | 0.0211 (13) | 0.0298 (13) | 0.0212 (12) | 0.0014 (11) | −0.0047 (10) | 0.0019 (10) |
C1 | 0.041 (3) | 0.054 (3) | 0.021 (3) | 0.002 (3) | 0.015 (2) | 0.008 (2) |
C21 | 0.023 (2) | 0.020 (2) | 0.030 (3) | 0.003 (2) | −0.001 (2) | −0.0134 (19) |
C14 | 0.064 (6) | 0.032 (4) | 0.029 (4) | 0.026 (4) | 0.005 (4) | −0.010 (3) |
C13 | 0.041 (4) | 0.033 (4) | 0.033 (4) | 0.019 (4) | 0.011 (3) | 0.000 (3) |
C9 | 0.036 (4) | 0.020 (3) | 0.053 (5) | 0.002 (3) | 0.001 (3) | −0.005 (3) |
C10 | 0.033 (4) | 0.025 (3) | 0.036 (4) | 0.002 (3) | 0.004 (3) | 0.007 (3) |
C8 | 0.024 (3) | 0.032 (3) | 0.040 (4) | 0.014 (3) | 0.007 (3) | 0.006 (3) |
N4X | 0.0211 (13) | 0.0298 (13) | 0.0212 (12) | 0.0014 (11) | −0.0047 (10) | 0.0019 (10) |
N3X | 0.0211 (13) | 0.0298 (13) | 0.0212 (12) | 0.0014 (11) | −0.0047 (10) | 0.0019 (10) |
N6X | 0.0211 (13) | 0.0298 (13) | 0.0212 (12) | 0.0014 (11) | −0.0047 (10) | 0.0019 (10) |
N5X | 0.0211 (13) | 0.0298 (13) | 0.0212 (12) | 0.0014 (11) | −0.0047 (10) | 0.0019 (10) |
C15 | 0.050 (5) | 0.014 (3) | 0.037 (4) | 0.003 (3) | −0.006 (4) | 0.016 (3) |
Ni1—N1i | 2.059 (4) | C19—C18 | 1.513 (5) |
Ni1—N1 | 2.059 (4) | C24—H24A | 0.9600 |
Ni1—N2i | 2.070 (3) | C24—H24B | 0.9600 |
Ni1—N2 | 2.070 (3) | C24—H24C | 0.9600 |
Ni1—O1i | 2.104 (2) | C18—C20 | 1.395 (5) |
Ni1—O1 | 2.104 (2) | C20—C21 | 1.378 (5) |
Ni2—N4X | 2.037 (7) | C20—H20 | 0.9300 |
Ni2—N6 | 2.041 (4) | C22—C21 | 1.407 (5) |
Ni2—N3 | 2.045 (4) | C11—N5 | 1.474 (6) |
Ni2—N3X | 2.057 (7) | C11—H11A | 0.9700 |
Ni2—N5X | 2.060 (8) | C11—H11B | 0.9700 |
Ni2—N5 | 2.080 (4) | N5—C10 | 1.472 (5) |
Ni2—N6X | 2.081 (7) | N5—H5 | 0.9800 |
Ni2—N4 | 2.083 (4) | C1—H1A | 0.9700 |
Ni2—O3ii | 2.112 (3) | C1—H1B | 0.9700 |
Ni2—O5 | 2.118 (3) | C21—H21 | 0.9300 |
Si1—C25 | 1.858 (4) | C14—C13 | 1.475 (10) |
Si1—C24 | 1.860 (4) | C14—C15 | 1.545 (10) |
Si1—C22 | 1.867 (4) | C14—H14A | 0.9700 |
Si1—C26 | 1.887 (4) | C14—H14B | 0.9700 |
O1—C16 | 1.262 (4) | C13—H13A | 0.9700 |
O2—C16 | 1.236 (4) | C13—H13B | 0.9700 |
O3—C19 | 1.243 (4) | C9—C10 | 1.514 (9) |
C31—O6 | 1.246 (5) | C9—C8 | 1.519 (8) |
C31—O5 | 1.260 (5) | C9—H9A | 0.9700 |
C31—C30 | 1.515 (5) | C9—H9B | 0.9700 |
C2—N2 | 1.455 (5) | C10—H10A | 0.9700 |
C2—C1 | 1.507 (6) | C10—H10B | 0.9700 |
C2—H2A | 0.9700 | C8—H8A | 0.9700 |
C2—H2B | 0.9700 | C8—H8B | 0.9700 |
O4—C19 | 1.273 (5) | C34—H34A | 0.9600 |
N2—C3 | 1.470 (5) | C34—H34B | 0.9600 |
N2—H2 | 0.9800 | C34—H34C | 0.9600 |
N1—C5 | 1.462 (5) | C35X—H35A | 0.9600 |
N1—C1 | 1.472 (5) | C35X—H35B | 0.9600 |
N1—H1 | 0.9800 | C35X—H35C | 0.9600 |
C16—C17 | 1.506 (5) | N4X—C7X | 1.469 (8) |
C7—N4 | 1.483 (8) | N4X—C8X | 1.473 (8) |
C7—C6 | 1.489 (14) | N4X—H4X | 0.9800 |
C7—H7A | 0.9700 | N3X—C15X | 1.473 (8) |
C7—H7B | 0.9700 | N3X—C6X | 1.476 (8) |
O10X—C35X | 1.387 (8) | N3X—H3X | 0.9800 |
O10X—H10X | 0.8199 | N6X—C13X | 1.478 (8) |
N3—C6 | 1.467 (5) | N6X—C12X | 1.479 (8) |
N3—C15 | 1.485 (5) | N6X—H6X | 0.9800 |
N3—H3 | 0.9800 | N5X—C11X | 1.48 (3) |
C30—C33 | 1.395 (5) | N5X—C10X | 1.477 (8) |
C30—C29 | 1.398 (6) | N5X—H5X | 0.9800 |
C5—C4 | 1.513 (6) | C15X—C14X | 1.48 (3) |
C5—H5A | 0.9700 | C15X—H15A | 0.9700 |
C5—H5B | 0.9700 | C15X—H15B | 0.9700 |
C12—N6 | 1.476 (6) | C8X—C9X | 1.56 (3) |
C12—C11 | 1.490 (9) | C8X—H8XA | 0.9700 |
C12—H12A | 0.9700 | C8X—H8XB | 0.9700 |
C12—H12B | 0.9700 | C14X—C13X | 1.59 (4) |
C23—C22 | 1.393 (5) | C14X—H14C | 0.9700 |
C23—C17 | 1.398 (5) | C14X—H14D | 0.9700 |
C23—H23 | 0.9300 | C13X—H13C | 0.9700 |
O8—C32 | 1.190 (5) | C13X—H13D | 0.9700 |
C4—C3i | 1.516 (7) | C9X—C10X | 1.43 (4) |
C4—H4A | 0.9700 | C9X—H9XA | 0.9700 |
C4—H4B | 0.9700 | C9X—H9XB | 0.9700 |
C3—H3A | 0.9700 | C12X—C11X | 1.41 (3) |
C3—H3B | 0.9700 | C12X—H12C | 0.9700 |
C25—H25A | 0.9600 | C12X—H12D | 0.9700 |
C25—H25B | 0.9600 | C11X—H11C | 0.9700 |
C25—H25C | 0.9600 | C11X—H11D | 0.9700 |
C28—C29 | 1.388 (5) | C10X—H10C | 0.9700 |
C28—C27 | 1.391 (6) | C10X—H10D | 0.9700 |
C28—H28 | 0.9300 | C7X—C6X | 1.37 (6) |
C27—C26 | 1.383 (6) | C7X—H7XA | 0.9700 |
C27—H27 | 0.9300 | C7X—H7XB | 0.9700 |
C17—C18 | 1.388 (5) | C15—H15C | 0.9700 |
C33—C26 | 1.394 (5) | C15—H15D | 0.9700 |
C33—H33 | 0.9300 | C6X—H6XA | 0.9700 |
C6—H6A | 0.9700 | C6X—H6XB | 0.9700 |
C6—H6B | 0.9700 | C34X—O9X | 1.466 (10) |
N4—C8 | 1.479 (5) | C34X—H34D | 0.9600 |
N4—H4 | 0.9800 | C34X—H34E | 0.9600 |
C29—C32 | 1.494 (6) | C34X—H34F | 0.9600 |
O7—C32 | 1.321 (5) | O9X—H9X | 0.8394 |
O7—H7 | 0.8200 | O10—C35 | 1.396 (8) |
N6—C13 | 1.475 (5) | O10—H10 | 0.8200 |
N6—H6 | 0.9800 | C35—H35D | 0.9600 |
O9—C34 | 1.467 (8) | C35—H35E | 0.9600 |
O9—H9 | 0.8199 | C35—H35F | 0.9600 |
N1i—Ni1—N1 | 180.0 | C20—C18—C19 | 116.8 (3) |
N1i—Ni1—N2i | 85.45 (14) | C21—C20—C18 | 121.3 (4) |
N1—Ni1—N2i | 94.56 (14) | C21—C20—H20 | 119.3 |
N1i—Ni1—N2 | 94.56 (14) | C18—C20—H20 | 119.3 |
N1—Ni1—N2 | 85.44 (14) | C23—C22—C21 | 116.9 (4) |
N2i—Ni1—N2 | 180.0 (2) | C23—C22—Si1 | 123.7 (3) |
N1i—Ni1—O1i | 90.28 (13) | C21—C22—Si1 | 119.4 (3) |
N1—Ni1—O1i | 89.72 (13) | N5—C11—C12 | 108.1 (5) |
N2i—Ni1—O1i | 93.42 (11) | N5—C11—H11A | 110.1 |
N2—Ni1—O1i | 86.58 (11) | C12—C11—H11A | 110.1 |
N1i—Ni1—O1 | 89.72 (13) | N5—C11—H11B | 110.1 |
N1—Ni1—O1 | 90.28 (13) | C12—C11—H11B | 110.1 |
N2i—Ni1—O1 | 86.58 (11) | H11A—C11—H11B | 108.4 |
N2—Ni1—O1 | 93.42 (11) | C10—N5—C11 | 113.3 (5) |
O1i—Ni1—O1 | 180.0 | C10—N5—Ni2 | 116.2 (4) |
N6—Ni2—N3 | 98.11 (17) | C11—N5—Ni2 | 104.8 (3) |
N4X—Ni2—N3X | 88.7 (6) | C10—N5—H5 | 107.4 |
N4X—Ni2—N5X | 99.2 (6) | C11—N5—H5 | 107.4 |
N3X—Ni2—N5X | 171.6 (7) | Ni2—N5—H5 | 107.4 |
N6—Ni2—N5 | 85.61 (17) | N1—C1—C2 | 109.4 (4) |
N3—Ni2—N5 | 174.42 (17) | N1—C1—H1A | 109.8 |
N4X—Ni2—N6X | 174.9 (6) | C2—C1—H1A | 109.8 |
N3X—Ni2—N6X | 91.0 (6) | N1—C1—H1B | 109.8 |
N5X—Ni2—N6X | 80.8 (6) | C2—C1—H1B | 109.8 |
N6—Ni2—N4 | 176.65 (17) | H1A—C1—H1B | 108.2 |
N3—Ni2—N4 | 84.73 (17) | C20—C21—C22 | 120.7 (4) |
N5—Ni2—N4 | 91.43 (17) | C20—C21—H21 | 119.7 |
N6—Ni2—O3ii | 88.66 (14) | C22—C21—H21 | 119.7 |
N3—Ni2—O3ii | 86.59 (14) | C13—C14—C15 | 118.9 (6) |
N5—Ni2—O3ii | 89.34 (14) | C13—C14—H14A | 107.6 |
N4—Ni2—O3ii | 89.74 (14) | C15—C14—H14A | 107.6 |
N4X—Ni2—O5 | 85.0 (4) | C13—C14—H14B | 107.6 |
N6—Ni2—O5 | 86.54 (15) | C15—C14—H14B | 107.6 |
N3—Ni2—O5 | 94.73 (14) | H14A—C14—H14B | 107.0 |
N3X—Ni2—O5 | 86.8 (4) | C14—C13—N6 | 111.9 (5) |
N5X—Ni2—O5 | 91.1 (4) | C14—C13—H13A | 109.2 |
N5—Ni2—O5 | 89.64 (14) | N6—C13—H13A | 109.2 |
N6X—Ni2—O5 | 89.9 (4) | C14—C13—H13B | 109.2 |
N4—Ni2—O5 | 95.01 (15) | N6—C13—H13B | 109.2 |
O3ii—Ni2—O5 | 175.16 (12) | H13A—C13—H13B | 107.9 |
C25—Si1—C24 | 111.0 (2) | C10—C9—C8 | 114.8 (6) |
C25—Si1—C22 | 108.1 (2) | C10—C9—H9A | 108.6 |
C24—Si1—C22 | 108.79 (19) | C8—C9—H9A | 108.6 |
C25—Si1—C26 | 109.48 (19) | C10—C9—H9B | 108.6 |
C24—Si1—C26 | 109.5 (2) | C8—C9—H9B | 108.6 |
C22—Si1—C26 | 109.92 (17) | H9A—C9—H9B | 107.6 |
C16—O1—Ni1 | 131.0 (2) | N5—C10—C9 | 113.6 (5) |
C19—O3—Ni2iii | 133.4 (3) | N5—C10—H10A | 108.8 |
O6—C31—O5 | 126.6 (4) | C9—C10—H10A | 108.8 |
O6—C31—C30 | 116.5 (4) | N5—C10—H10B | 108.8 |
O5—C31—C30 | 116.7 (4) | C9—C10—H10B | 108.8 |
N2—C2—C1 | 108.6 (4) | H10A—C10—H10B | 107.7 |
N2—C2—H2A | 110.0 | N4—C8—C9 | 110.4 (4) |
C1—C2—H2A | 110.0 | N4—C8—H8A | 109.6 |
N2—C2—H2B | 110.0 | C9—C8—H8A | 109.6 |
C1—C2—H2B | 110.0 | N4—C8—H8B | 109.6 |
H2A—C2—H2B | 108.4 | C9—C8—H8B | 109.6 |
C2—N2—C3 | 114.3 (4) | H8A—C8—H8B | 108.1 |
C2—N2—Ni1 | 105.7 (3) | O9—C34—H34A | 109.5 |
C3—N2—Ni1 | 116.7 (3) | O9—C34—H34B | 109.5 |
C2—N2—H2 | 106.5 | H34A—C34—H34B | 109.5 |
C3—N2—H2 | 106.5 | O9—C34—H34C | 109.5 |
Ni1—N2—H2 | 106.5 | H34A—C34—H34C | 109.5 |
C5—N1—C1 | 113.7 (3) | H34B—C34—H34C | 109.5 |
C5—N1—Ni1 | 114.9 (3) | O10X—C35X—H35A | 109.5 |
C1—N1—Ni1 | 105.0 (3) | O10X—C35X—H35B | 109.5 |
C5—N1—H1 | 107.6 | H35A—C35X—H35B | 109.5 |
C1—N1—H1 | 107.6 | O10X—C35X—H35C | 109.5 |
Ni1—N1—H1 | 107.6 | H35A—C35X—H35C | 109.5 |
C31—O5—Ni2 | 130.1 (3) | H35B—C35X—H35C | 109.5 |
O2—C16—O1 | 125.2 (4) | C7X—N4X—C8X | 120.5 (19) |
O2—C16—C17 | 118.9 (3) | C7X—N4X—Ni2 | 98.4 (13) |
O1—C16—C17 | 115.9 (3) | C8X—N4X—Ni2 | 115.7 (15) |
N4—C7—C6 | 110.6 (8) | C7X—N4X—H4X | 107.1 |
N4—C7—H7A | 109.5 | C8X—N4X—H4X | 107.1 |
C6—C7—H7A | 109.5 | Ni2—N4X—H4X | 107.1 |
N4—C7—H7B | 109.5 | C15X—N3X—C6X | 118 (3) |
C6—C7—H7B | 109.5 | C15X—N3X—Ni2 | 117.8 (12) |
H7A—C7—H7B | 108.1 | C6X—N3X—Ni2 | 102.9 (18) |
C35X—O10X—H10X | 109.7 | C15X—N3X—H3X | 105.8 |
C6—N3—C15 | 113.7 (5) | C6X—N3X—H3X | 105.8 |
C6—N3—Ni2 | 108.0 (3) | Ni2—N3X—H3X | 105.8 |
C15—N3—Ni2 | 115.8 (4) | C13X—N6X—C12X | 113.3 (19) |
C6—N3—H3 | 106.2 | C13X—N6X—Ni2 | 116.4 (15) |
C15—N3—H3 | 106.2 | C12X—N6X—Ni2 | 108.2 (12) |
Ni2—N3—H3 | 106.2 | C13X—N6X—H6X | 106.1 |
C33—C30—C29 | 118.6 (4) | C12X—N6X—H6X | 106.1 |
C33—C30—C31 | 116.2 (4) | Ni2—N6X—H6X | 106.1 |
C29—C30—C31 | 125.1 (4) | C11X—N5X—C10X | 114.8 (19) |
N1—C5—C4 | 111.7 (4) | C11X—N5X—Ni2 | 110.4 (13) |
N1—C5—H5A | 109.3 | C10X—N5X—Ni2 | 116.1 (19) |
C4—C5—H5A | 109.3 | C11X—N5X—H5X | 104.7 |
N1—C5—H5B | 109.3 | C10X—N5X—H5X | 104.7 |
C4—C5—H5B | 109.3 | Ni2—N5X—H5X | 104.7 |
H5A—C5—H5B | 107.9 | N3X—C15X—C14X | 118 (2) |
N6—C12—C11 | 109.8 (5) | N3X—C15X—H15A | 107.9 |
N6—C12—H12A | 109.7 | C14X—C15X—H15A | 107.9 |
C11—C12—H12A | 109.7 | N3X—C15X—H15B | 107.9 |
N6—C12—H12B | 109.7 | C14X—C15X—H15B | 107.9 |
C11—C12—H12B | 109.7 | H15A—C15X—H15B | 107.2 |
H12A—C12—H12B | 108.2 | N4X—C8X—C9X | 111 (2) |
C22—C23—C17 | 123.1 (4) | N4X—C8X—H8XA | 109.4 |
C22—C23—H23 | 118.5 | C9X—C8X—H8XA | 109.4 |
C17—C23—H23 | 118.5 | N4X—C8X—H8XB | 109.4 |
C5—C4—C3i | 115.7 (4) | C9X—C8X—H8XB | 109.4 |
C5—C4—H4A | 108.4 | H8XA—C8X—H8XB | 108.0 |
C3i—C4—H4A | 108.4 | C15X—C14X—C13X | 108 (2) |
C5—C4—H4B | 108.4 | C15X—C14X—H14C | 110.0 |
C3i—C4—H4B | 108.4 | C13X—C14X—H14C | 110.0 |
H4A—C4—H4B | 107.4 | C15X—C14X—H14D | 110.0 |
N2—C3—C4i | 112.4 (4) | C13X—C14X—H14D | 110.0 |
N2—C3—H3A | 109.1 | H14C—C14X—H14D | 108.4 |
C4i—C3—H3A | 109.1 | N6X—C13X—C14X | 123 (2) |
N2—C3—H3B | 109.1 | N6X—C13X—H13C | 106.6 |
C4i—C3—H3B | 109.1 | C14X—C13X—H13C | 106.6 |
H3A—C3—H3B | 107.9 | N6X—C13X—H13D | 106.6 |
Si1—C25—H25A | 109.5 | C14X—C13X—H13D | 106.6 |
Si1—C25—H25B | 109.5 | H13C—C13X—H13D | 106.5 |
H25A—C25—H25B | 109.5 | C10X—C9X—C8X | 126 (3) |
Si1—C25—H25C | 109.5 | C10X—C9X—H9XA | 105.7 |
H25A—C25—H25C | 109.5 | C8X—C9X—H9XA | 105.7 |
H25B—C25—H25C | 109.5 | C10X—C9X—H9XB | 105.7 |
C29—C28—C27 | 120.8 (4) | C8X—C9X—H9XB | 105.7 |
C29—C28—H28 | 119.6 | H9XA—C9X—H9XB | 106.1 |
C27—C28—H28 | 119.6 | C11X—C12X—N6X | 109 (2) |
C26—C27—C28 | 121.3 (4) | C11X—C12X—H12C | 109.8 |
C26—C27—H27 | 119.3 | N6X—C12X—H12C | 109.8 |
C28—C27—H27 | 119.3 | C11X—C12X—H12D | 109.8 |
C18—C17—C23 | 118.5 (3) | N6X—C12X—H12D | 109.8 |
C18—C17—C16 | 121.0 (3) | H12C—C12X—H12D | 108.3 |
C23—C17—C16 | 120.5 (3) | C12X—C11X—N5X | 110 (2) |
C26—C33—C30 | 122.8 (4) | C12X—C11X—H11C | 109.7 |
C26—C33—H33 | 118.6 | N5X—C11X—H11C | 109.7 |
C30—C33—H33 | 118.6 | C12X—C11X—H11D | 109.7 |
N3—C6—C7 | 108.1 (6) | N5X—C11X—H11D | 109.7 |
N3—C6—H6A | 110.1 | H11C—C11X—H11D | 108.2 |
C7—C6—H6A | 110.1 | C9X—C10X—N5X | 111 (3) |
N3—C6—H6B | 110.1 | C9X—C10X—H10C | 109.3 |
C7—C6—H6B | 110.1 | N5X—C10X—H10C | 109.3 |
H6A—C6—H6B | 108.4 | C9X—C10X—H10D | 109.3 |
C8—N4—C7 | 114.3 (7) | N5X—C10X—H10D | 109.3 |
C8—N4—Ni2 | 118.5 (3) | H10C—C10X—H10D | 108.0 |
C7—N4—Ni2 | 105.1 (3) | C6X—C7X—N4X | 118 (3) |
C8—N4—H4 | 106.0 | C6X—C7X—H7XA | 107.7 |
C7—N4—H4 | 106.0 | N4X—C7X—H7XA | 107.7 |
Ni2—N4—H4 | 106.0 | C6X—C7X—H7XB | 107.7 |
C28—C29—C30 | 119.2 (4) | N4X—C7X—H7XB | 107.7 |
C28—C29—C32 | 120.9 (4) | H7XA—C7X—H7XB | 107.1 |
C30—C29—C32 | 119.9 (4) | N3—C15—C14 | 109.7 (5) |
C32—O7—H7 | 109.5 | N3—C15—H15C | 109.7 |
C27—C26—C33 | 117.2 (4) | C14—C15—H15C | 109.7 |
C27—C26—Si1 | 122.3 (3) | N3—C15—H15D | 109.7 |
C33—C26—Si1 | 120.5 (3) | C14—C15—H15D | 109.7 |
C13—N6—C12 | 115.4 (5) | H15C—C15—H15D | 108.2 |
C13—N6—Ni2 | 114.9 (4) | C7X—C6X—N3X | 109 (4) |
C12—N6—Ni2 | 105.5 (4) | C7X—C6X—H6XA | 109.8 |
C13—N6—H6 | 106.8 | N3X—C6X—H6XA | 109.8 |
C12—N6—H6 | 106.8 | C7X—C6X—H6XB | 109.8 |
Ni2—N6—H6 | 106.8 | N3X—C6X—H6XB | 109.8 |
O8—C32—O7 | 122.5 (4) | H6XA—C6X—H6XB | 108.2 |
O8—C32—C29 | 125.4 (4) | O9X—C34X—H34D | 109.5 |
O7—C32—C29 | 112.2 (4) | O9X—C34X—H34E | 109.5 |
C34—O9—H9 | 108.8 | H34D—C34X—H34E | 109.5 |
O3—C19—O4 | 126.8 (4) | O9X—C34X—H34F | 109.5 |
O3—C19—C18 | 116.0 (4) | H34D—C34X—H34F | 109.5 |
O4—C19—C18 | 117.0 (4) | H34E—C34X—H34F | 109.5 |
Si1—C24—H24A | 109.5 | C34X—O9X—H9X | 105.1 |
Si1—C24—H24B | 109.5 | C35—O10—H10 | 109.5 |
H24A—C24—H24B | 109.5 | O10—C35—H35D | 109.5 |
Si1—C24—H24C | 109.5 | O10—C35—H35E | 109.5 |
H24A—C24—H24C | 109.5 | H35D—C35—H35E | 109.5 |
H24B—C24—H24C | 109.5 | O10—C35—H35F | 109.5 |
C17—C18—C20 | 119.5 (4) | H35D—C35—H35F | 109.5 |
C17—C18—C19 | 123.7 (3) | H35E—C35—H35F | 109.5 |
C1—C2—N2—C3 | 171.2 (4) | O3—C19—C18—C17 | 97.3 (5) |
C1—C2—N2—Ni1 | 41.4 (4) | O4—C19—C18—C17 | −87.7 (5) |
O6—C31—O5—Ni2 | −11.9 (7) | O3—C19—C18—C20 | −83.0 (5) |
C30—C31—O5—Ni2 | 173.8 (3) | O4—C19—C18—C20 | 91.9 (4) |
Ni1—O1—C16—O2 | 17.1 (7) | C17—C18—C20—C21 | −1.2 (6) |
Ni1—O1—C16—C17 | −163.4 (3) | C19—C18—C20—C21 | 179.2 (4) |
O6—C31—C30—C33 | −84.5 (5) | C17—C23—C22—C21 | −2.1 (6) |
O5—C31—C30—C33 | 90.4 (5) | C17—C23—C22—Si1 | 179.2 (3) |
O6—C31—C30—C29 | 96.5 (5) | C25—Si1—C22—C23 | 114.2 (4) |
O5—C31—C30—C29 | −88.6 (5) | C24—Si1—C22—C23 | −125.2 (4) |
C1—N1—C5—C4 | 180.0 (4) | C26—Si1—C22—C23 | −5.3 (4) |
Ni1—N1—C5—C4 | −59.0 (4) | C25—Si1—C22—C21 | −64.5 (4) |
N1—C5—C4—C3i | 73.3 (5) | C24—Si1—C22—C21 | 56.2 (4) |
C2—N2—C3—C4i | −176.7 (4) | C26—Si1—C22—C21 | 176.1 (3) |
Ni1—N2—C3—C4i | −52.6 (4) | N6—C12—C11—N5 | −58.2 (7) |
C29—C28—C27—C26 | −0.4 (6) | C12—C11—N5—C10 | 170.3 (5) |
C22—C23—C17—C18 | 0.6 (6) | C12—C11—N5—Ni2 | 42.6 (6) |
C22—C23—C17—C16 | −179.1 (4) | C5—N1—C1—C2 | 168.1 (4) |
O2—C16—C17—C18 | −13.7 (6) | Ni1—N1—C1—C2 | 41.8 (4) |
O1—C16—C17—C18 | 166.8 (4) | N2—C2—C1—N1 | −58.0 (5) |
O2—C16—C17—C23 | 166.0 (4) | C18—C20—C21—C22 | −0.4 (7) |
O1—C16—C17—C23 | −13.5 (6) | C23—C22—C21—C20 | 1.9 (6) |
C29—C30—C33—C26 | −1.3 (6) | Si1—C22—C21—C20 | −179.3 (3) |
C31—C30—C33—C26 | 179.6 (4) | C15—C14—C13—N6 | 73.3 (7) |
C15—N3—C6—C7 | −170.0 (7) | C12—N6—C13—C14 | −175.5 (6) |
Ni2—N3—C6—C7 | −40.1 (7) | Ni2—N6—C13—C14 | −52.4 (6) |
N4—C7—C6—N3 | 55.0 (12) | C11—N5—C10—C9 | −179.3 (6) |
C6—C7—N4—C8 | −171.7 (8) | Ni2—N5—C10—C9 | −57.8 (6) |
C6—C7—N4—Ni2 | −40.2 (12) | C8—C9—C10—N5 | 70.8 (7) |
C27—C28—C29—C30 | −0.7 (6) | C7—N4—C8—C9 | −177.1 (8) |
C27—C28—C29—C32 | 179.5 (4) | Ni2—N4—C8—C9 | 58.1 (6) |
C33—C30—C29—C28 | 1.5 (6) | C10—C9—C8—N4 | −69.2 (7) |
C31—C30—C29—C28 | −179.5 (4) | C6X—N3X—C15X—C14X | −171 (3) |
C33—C30—C29—C32 | −178.7 (3) | Ni2—N3X—C15X—C14X | 65 (2) |
C31—C30—C29—C32 | 0.3 (6) | C7X—N4X—C8X—C9X | 164 (2) |
C28—C27—C26—C33 | 0.6 (6) | Ni2—N4X—C8X—C9X | 46 (3) |
C28—C27—C26—Si1 | −179.0 (3) | N3X—C15X—C14X—C13X | −62 (3) |
C30—C33—C26—C27 | 0.2 (6) | C12X—N6X—C13X—C14X | −176 (3) |
C30—C33—C26—Si1 | 179.8 (3) | Ni2—N6X—C13X—C14X | −50 (3) |
C25—Si1—C26—C27 | 165.7 (3) | C15X—C14X—C13X—N6X | 57 (3) |
C24—Si1—C26—C27 | 43.8 (4) | N4X—C8X—C9X—C10X | −66 (4) |
C22—Si1—C26—C27 | −75.7 (4) | C13X—N6X—C12X—C11X | 173 (2) |
C25—Si1—C26—C33 | −13.9 (4) | Ni2—N6X—C12X—C11X | 43 (2) |
C24—Si1—C26—C33 | −135.8 (3) | N6X—C12X—C11X—N5X | −51 (3) |
C22—Si1—C26—C33 | 104.7 (3) | C10X—N5X—C11X—C12X | 169 (2) |
C11—C12—N6—C13 | 169.1 (5) | Ni2—N5X—C11X—C12X | 35 (2) |
C11—C12—N6—Ni2 | 41.1 (6) | C8X—C9X—C10X—N5X | 66 (4) |
C28—C29—C32—O8 | 178.5 (4) | C11X—N5X—C10X—C9X | −177 (2) |
C30—C29—C32—O8 | −1.3 (6) | Ni2—N5X—C10X—C9X | −46 (3) |
C28—C29—C32—O7 | −0.4 (5) | C8X—N4X—C7X—C6X | −169 (3) |
C30—C29—C32—O7 | 179.7 (4) | Ni2—N4X—C7X—C6X | −42 (3) |
Ni2iii—O3—C19—O4 | 22.7 (6) | C6—N3—C15—C14 | 176.9 (5) |
Ni2iii—O3—C19—C18 | −162.8 (2) | Ni2—N3—C15—C14 | 51.0 (6) |
C23—C17—C18—C20 | 1.1 (6) | C13—C14—C15—N3 | −72.0 (7) |
C16—C17—C18—C20 | −179.2 (4) | N4X—C7X—C6X—N3X | 57 (6) |
C23—C17—C18—C19 | −179.3 (4) | C15X—N3X—C6X—C7X | −167 (3) |
C16—C17—C18—C19 | 0.4 (6) | Ni2—N3X—C6X—C7X | −35 (5) |
Symmetry codes: (i) −x+1, −y+1, −z+1; (ii) x−1, −y+1/2, z−1/2; (iii) x+1, −y+1/2, z+1/2. |
D—H···A | D—H | H···A | D···A | D—H···A |
N2—H2···O2 | 0.98 | 2.00 | 2.882 (4) | 148 |
N3—H3···O6 | 0.98 | 1.96 | 2.861 (5) | 151 |
N4—H4···O4ii | 0.98 | 2.06 | 2.955 (5) | 151 |
N5—H5···O2ii | 0.98 | 2.03 | 2.962 (5) | 157 |
N6—H6···O8 | 0.98 | 2.25 | 3.225 (5) | 178 |
O7—H7···O4iv | 0.82 | 1.95 | 2.684 (5) | 150 |
N4—H4···O7v | 0.98 | 2.66 | 3.437 (6) | 137 |
N1—H1···O10i | 0.98 | 2.08 | 3.021 (9) | 160 |
O9—H9···O6 | 0.82 | 1.97 | 2.745 (11) | 158 |
O10—H10···O4 | 0.82 | 1.97 | 2.775 (9) | 166 |
Symmetry codes: (i) −x+1, −y+1, −z+1; (ii) x−1, −y+1/2, z−1/2; (iv) x−1, y, z; (v) x, −y+1/2, z−1/2. |
Distances | Bite angles | |||
Ni1—N1 | 2.059 (4) | N1—Ni1—N2 | 85.44 (14) | |
Ni1—N2 | 2.070 (3) | N1—Ni1—N2i | 94.55 (14) | |
Ni1—O1 | 2.104 (2) | |||
Ni2—N3 | 2.045 (4) | N3—Ni2—N4 | 84.73 (17) | |
Ni2—N4 | 2.083 (4) | N5—Ni2—N6 | 85.61 (17) | |
Ni2—N5 | 2.041 (4) | N4—Ni2—N5 | 91.43 (17) | |
Ni2—N6 | 2.080 (4) | N3—Ni2—N6 | 98.11 (17) | |
Ni2—O3ii | 2.112 (3) | |||
Ni2—O5 | 2.118 (3) |
Symmetry codes: (i) -x+1, -y+1, -z+1; (ii) x-1, -y+1/2, z-1/2. |
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