Supporting information
Crystallographic Information File (CIF) https://doi.org/10.1107/S1600536806034751/ya2023sup1.cif | |
Structure factor file (CIF format) https://doi.org/10.1107/S1600536806034751/ya2023Isup2.hkl |
CCDC reference: 625054
Data collection: SMART (Bruker, 2000); cell refinement: SAINT (Bruker, 2000); data reduction: SAINT; program(s) used to solve structure: SHELXTL (Bruker, 2000); program(s) used to refine structure: SHELXTL; molecular graphics: SHELXTL; software used to prepare material for publication: SHELXTL.
C30H37N4Ni2O4+·ClO4−·0.5C2H3N | F(000) = 3144 |
Mr = 755.01 | Dx = 1.500 Mg m−3 |
Monoclinic, C2/c | Mo Kα radiation, λ = 0.71073 Å |
Hall symbol: -C 2yc | Cell parameters from 9027 reflections |
a = 31.353 (2) Å | θ = 2.4–26.3° |
b = 11.2316 (7) Å | µ = 1.26 mm−1 |
c = 21.2808 (14) Å | T = 298 K |
β = 116.875 (1)° | Block cut from needle, red |
V = 6684.6 (7) Å3 | 0.30 × 0.20 × 0.20 mm |
Z = 8 |
Bruker SMART APEX CCD area-detector diffractometer | 6572 independent reflections |
Radiation source: sealed tube | 5169 reflections with I > 2σ(I) |
Graphite monochromator | Rint = 0.048 |
φ and ω scans | θmax = 26.0°, θmin = 1.9° |
Absorption correction: multi-scan (SADABS; Bruker, 2000) | h = −38→38 |
Tmin = 0.703, Tmax = 0.786 | k = −13→13 |
28559 measured reflections | l = −24→26 |
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)] = 0.045 | Hydrogen site location: inferred from neighbouring sites |
wR(F2) = 0.101 | H-atom parameters constrained |
S = 1.06 | w = 1/[σ2(Fo2) + (0.05P)2 + 1.55P] where P = (Fo2 + 2Fc2)/3 |
6572 reflections | (Δ/σ)max < 0.001 |
425 parameters | Δρmax = 0.26 e Å−3 |
0 restraints | Δρmin = −0.40 e Å−3 |
Geometry. All e.s.d.'s (except the e.s.d. in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell e.s.d.'s are taken into account individually in the estimation of e.s.d.'s in distances, angles and torsion angles; correlations between e.s.d.'s in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell e.s.d.'s is used for estimating e.s.d.'s involving l.s. planes. |
Refinement. Refinement of F2 against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F2, conventional R-factors R are based on F, with F set to zero for negative F2. The threshold expression of F2 > σ(F2) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F2 are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. |
x | y | z | Uiso*/Ueq | Occ. (<1) | |
C1 | −0.00045 (16) | 0.6164 (4) | −0.4381 (2) | 0.0857 (14) | |
H1A | 0.0280 | 0.5900 | −0.4402 | 0.129* | |
H1B | −0.0234 | 0.6427 | −0.4839 | 0.129* | |
H1C | −0.0137 | 0.5519 | −0.4230 | 0.129* | |
C2 | 0.01137 (14) | 0.7153 (3) | −0.38796 (18) | 0.0671 (11) | |
H2A | −0.0179 | 0.7451 | −0.3886 | 0.081* | |
H2B | 0.0253 | 0.7794 | −0.4031 | 0.081* | |
C3 | 0.04564 (12) | 0.6810 (4) | −0.31355 (18) | 0.0620 (10) | |
H3A | 0.0740 | 0.6460 | −0.3134 | 0.074* | |
H3B | 0.0308 | 0.6209 | −0.2972 | 0.074* | |
C4 | 0.06056 (13) | 0.7860 (3) | −0.26246 (18) | 0.0575 (9) | |
H4A | 0.0752 | 0.8457 | −0.2795 | 0.069* | |
H4B | 0.0319 | 0.8210 | −0.2637 | 0.069* | |
C5 | 0.09452 (11) | 0.7588 (3) | −0.18716 (16) | 0.0459 (7) | |
C6 | 0.13053 (11) | 0.8365 (3) | −0.14606 (17) | 0.0473 (7) | |
H6 | 0.1340 | 0.9066 | −0.1665 | 0.057* | |
C7 | 0.09132 (11) | 0.6530 (3) | −0.15529 (17) | 0.0462 (7) | |
H7 | 0.0686 | 0.5970 | −0.1824 | 0.055* | |
C8 | 0.16186 (11) | 0.8153 (3) | −0.07567 (17) | 0.0432 (7) | |
C9 | 0.12106 (9) | 0.6273 (2) | −0.08380 (15) | 0.0363 (6) | |
C10 | 0.15677 (10) | 0.7093 (2) | −0.04280 (16) | 0.0402 (6) | |
C11 | 0.19740 (11) | 0.9050 (2) | −0.03807 (18) | 0.0453 (7) | |
H11 | 0.1999 | 0.9690 | −0.0640 | 0.054* | |
C12 | 0.26128 (11) | 1.0008 (3) | 0.06166 (18) | 0.0504 (8) | |
H12A | 0.2477 | 1.0766 | 0.0401 | 0.060* | |
H12B | 0.2897 | 0.9863 | 0.0557 | 0.060* | |
C13 | 0.27354 (12) | 1.0025 (3) | 0.13820 (19) | 0.0524 (8) | |
H13A | 0.3043 | 1.0408 | 0.1650 | 0.063* | |
H13B | 0.2495 | 1.0464 | 0.1455 | 0.063* | |
C14 | 0.30428 (11) | 0.8396 (3) | 0.22282 (17) | 0.0441 (7) | |
H14 | 0.3256 | 0.8940 | 0.2543 | 0.053* | |
C15 | 0.30599 (10) | 0.7177 (3) | 0.24666 (16) | 0.0409 (7) | |
C16 | 0.34514 (11) | 0.6793 (3) | 0.30863 (16) | 0.0449 (7) | |
H16 | 0.3675 | 0.7358 | 0.3362 | 0.054* | |
C17 | 0.35233 (10) | 0.5625 (3) | 0.33098 (16) | 0.0445 (7) | |
C18 | 0.31843 (10) | 0.4810 (3) | 0.28694 (15) | 0.0437 (7) | |
H18 | 0.3230 | 0.4008 | 0.2990 | 0.052* | |
C19 | 0.27773 (9) | 0.5141 (2) | 0.22533 (15) | 0.0379 (6) | |
C20 | 0.27088 (9) | 0.6348 (2) | 0.20702 (14) | 0.0360 (6) | |
C21 | 0.24892 (10) | 0.4172 (2) | 0.17862 (15) | 0.0398 (6) | |
H21 | 0.2586 | 0.3393 | 0.1928 | 0.048* | |
C22 | 0.18825 (10) | 0.3313 (2) | 0.07386 (16) | 0.0421 (7) | |
H22A | 0.1921 | 0.2603 | 0.1018 | 0.051* | |
H22B | 0.2030 | 0.3169 | 0.0431 | 0.051* | |
C23 | 0.13583 (11) | 0.3575 (2) | 0.03021 (16) | 0.0445 (7) | |
H23A | 0.1221 | 0.3041 | −0.0099 | 0.053* | |
H23B | 0.1188 | 0.3472 | 0.0582 | 0.053* | |
C24 | 0.11625 (10) | 0.5093 (2) | −0.05737 (15) | 0.0405 (6) | |
H24 | 0.1002 | 0.4506 | −0.0905 | 0.049* | |
C25 | 0.39460 (11) | 0.5255 (3) | 0.39654 (18) | 0.0567 (8) | |
H25A | 0.4191 | 0.5863 | 0.4090 | 0.068* | |
H25B | 0.4074 | 0.4526 | 0.3872 | 0.068* | |
C26 | 0.38449 (12) | 0.5050 (3) | 0.45896 (18) | 0.0579 (9) | |
H26A | 0.3717 | 0.5778 | 0.4683 | 0.069* | |
H26B | 0.3601 | 0.4440 | 0.4466 | 0.069* | |
C27 | 0.42765 (14) | 0.4678 (4) | 0.5254 (2) | 0.0691 (10) | |
H27A | 0.4171 | 0.4434 | 0.5598 | 0.083* | |
H27B | 0.4420 | 0.3991 | 0.5149 | 0.083* | |
C28 | 0.46447 (16) | 0.5607 (4) | 0.5569 (2) | 0.0897 (14) | |
H28A | 0.4774 | 0.5804 | 0.5250 | 0.135* | |
H28B | 0.4896 | 0.5319 | 0.6004 | 0.135* | |
H28C | 0.4504 | 0.6304 | 0.5660 | 0.135* | |
C29 | 0.11556 (10) | 0.6390 (3) | 0.13521 (15) | 0.0409 (6) | |
C30 | 0.08026 (14) | 0.6736 (4) | 0.1610 (2) | 0.0680 (10) | |
H30A | 0.0969 | 0.6930 | 0.2102 | 0.102* | |
H30B | 0.0588 | 0.6085 | 0.1543 | 0.102* | |
H30C | 0.0624 | 0.7416 | 0.1352 | 0.102* | |
C31 | 0.5000 | 0.3090 (4) | 0.2500 | 0.0721 (16) | |
H31A | 0.4717 | 0.3375 | 0.2518 | 0.108* | 0.50 |
H31B | 0.5005 | 0.3375 | 0.2078 | 0.108* | 0.50 |
H31C | 0.5278 | 0.3375 | 0.2904 | 0.108* | 0.50 |
C32 | 0.5000 | 0.1829 (5) | 0.2500 | 0.0654 (14) | |
Cl1 | 0.34715 (3) | 0.29146 (8) | 0.13089 (5) | 0.0604 (2) | |
N1 | 0.22596 (8) | 0.90351 (19) | 0.02853 (14) | 0.0409 (6) | |
N2 | 0.27539 (9) | 0.8772 (2) | 0.16142 (14) | 0.0437 (6) | |
N3 | 0.13206 (8) | 0.4822 (2) | 0.00607 (12) | 0.0378 (5) | |
N4 | 0.21194 (8) | 0.43244 (19) | 0.12058 (13) | 0.0386 (5) | |
N5 | 0.5000 | 0.0838 (5) | 0.2500 | 0.0743 (13) | |
Ni1 | 0.171030 (13) | 0.58037 (3) | 0.090156 (19) | 0.03735 (11) | |
Ni2 | 0.229903 (13) | 0.78661 (3) | 0.09028 (2) | 0.03943 (11) | |
O1 | 0.18704 (7) | 0.68472 (16) | 0.02351 (10) | 0.0398 (4) | |
O2 | 0.23115 (7) | 0.67155 (17) | 0.15239 (10) | 0.0403 (4) | |
O3 | 0.12267 (8) | 0.70586 (18) | 0.09362 (12) | 0.0492 (5) | |
O4 | 0.13827 (7) | 0.54155 (18) | 0.15424 (11) | 0.0456 (5) | |
O5 | 0.36540 (11) | 0.1777 (3) | 0.15202 (15) | 0.0852 (9) | |
O6 | 0.35614 (9) | 0.3666 (2) | 0.18672 (14) | 0.0712 (7) | |
O7 | 0.29915 (9) | 0.2858 (2) | 0.08539 (14) | 0.0716 (8) | |
O8 | 0.36750 (10) | 0.3422 (2) | 0.09110 (14) | 0.0713 (7) |
U11 | U22 | U33 | U12 | U13 | U23 | |
C1 | 0.079 (3) | 0.082 (3) | 0.057 (2) | −0.019 (2) | −0.003 (2) | 0.005 (2) |
C2 | 0.066 (2) | 0.074 (3) | 0.0443 (19) | −0.0121 (18) | 0.0093 (17) | 0.0196 (17) |
C3 | 0.0508 (19) | 0.084 (3) | 0.050 (2) | −0.0038 (17) | 0.0213 (16) | 0.0219 (18) |
C4 | 0.058 (2) | 0.065 (2) | 0.056 (2) | 0.0162 (16) | 0.0312 (17) | 0.0227 (17) |
C5 | 0.0483 (16) | 0.0573 (18) | 0.0419 (17) | 0.0109 (14) | 0.0289 (14) | 0.0080 (14) |
C6 | 0.0564 (18) | 0.0408 (16) | 0.0557 (19) | 0.0064 (13) | 0.0352 (16) | 0.0126 (14) |
C7 | 0.0435 (16) | 0.0508 (18) | 0.0509 (18) | 0.0013 (13) | 0.0272 (14) | 0.0034 (14) |
C8 | 0.0515 (17) | 0.0365 (15) | 0.0537 (19) | 0.0011 (12) | 0.0344 (15) | 0.0047 (13) |
C9 | 0.0407 (14) | 0.0369 (14) | 0.0396 (15) | 0.0042 (11) | 0.0255 (12) | 0.0027 (12) |
C10 | 0.0481 (16) | 0.0363 (14) | 0.0462 (17) | 0.0023 (12) | 0.0302 (14) | 0.0030 (12) |
C11 | 0.0595 (18) | 0.0283 (14) | 0.065 (2) | 0.0061 (12) | 0.0435 (17) | 0.0086 (13) |
C12 | 0.0530 (18) | 0.0299 (14) | 0.076 (2) | −0.0101 (12) | 0.0356 (17) | −0.0043 (14) |
C13 | 0.0640 (19) | 0.0270 (14) | 0.074 (2) | −0.0099 (13) | 0.0382 (18) | −0.0092 (14) |
C14 | 0.0449 (16) | 0.0478 (17) | 0.0479 (18) | −0.0120 (13) | 0.0281 (14) | −0.0188 (14) |
C15 | 0.0482 (16) | 0.0409 (16) | 0.0425 (16) | −0.0091 (12) | 0.0282 (14) | −0.0140 (12) |
C16 | 0.0460 (16) | 0.0519 (18) | 0.0455 (17) | −0.0162 (13) | 0.0282 (14) | −0.0131 (14) |
C17 | 0.0394 (15) | 0.059 (2) | 0.0417 (16) | −0.0034 (13) | 0.0241 (13) | −0.0036 (13) |
C18 | 0.0502 (17) | 0.0477 (17) | 0.0397 (16) | 0.0050 (13) | 0.0259 (14) | −0.0003 (13) |
C19 | 0.0346 (13) | 0.0368 (14) | 0.0486 (16) | 0.0010 (11) | 0.0245 (13) | −0.0028 (12) |
C20 | 0.0364 (14) | 0.0404 (14) | 0.0356 (14) | −0.0010 (11) | 0.0199 (12) | −0.0033 (11) |
C21 | 0.0434 (15) | 0.0338 (14) | 0.0443 (16) | 0.0019 (11) | 0.0216 (13) | 0.0010 (12) |
C22 | 0.0535 (17) | 0.0247 (13) | 0.0503 (17) | −0.0019 (11) | 0.0254 (14) | −0.0020 (12) |
C23 | 0.0548 (17) | 0.0280 (14) | 0.0471 (17) | −0.0132 (12) | 0.0198 (14) | −0.0015 (12) |
C24 | 0.0426 (15) | 0.0380 (15) | 0.0425 (16) | −0.0059 (12) | 0.0207 (13) | −0.0043 (12) |
C25 | 0.0450 (17) | 0.067 (2) | 0.0534 (19) | −0.0013 (15) | 0.0183 (15) | −0.0014 (17) |
C26 | 0.0524 (18) | 0.059 (2) | 0.059 (2) | 0.0062 (15) | 0.0223 (17) | 0.0124 (17) |
C27 | 0.078 (2) | 0.075 (2) | 0.054 (2) | 0.019 (2) | 0.0293 (19) | 0.0279 (19) |
C28 | 0.070 (3) | 0.098 (4) | 0.076 (3) | 0.009 (2) | 0.011 (2) | −0.012 (3) |
C29 | 0.0426 (15) | 0.0449 (17) | 0.0380 (15) | 0.0001 (12) | 0.0207 (12) | −0.0076 (13) |
C30 | 0.062 (2) | 0.082 (3) | 0.075 (3) | 0.0101 (19) | 0.045 (2) | −0.001 (2) |
C31 | 0.083 (4) | 0.050 (3) | 0.057 (3) | 0.000 | 0.009 (3) | 0.000 |
C32 | 0.071 (4) | 0.058 (3) | 0.062 (3) | 0.000 | 0.025 (3) | 0.000 |
Cl1 | 0.0657 (5) | 0.0561 (5) | 0.0660 (6) | 0.0003 (4) | 0.0357 (5) | −0.0041 (4) |
N1 | 0.0448 (13) | 0.0242 (11) | 0.0670 (17) | −0.0049 (9) | 0.0369 (13) | 0.0030 (11) |
N2 | 0.0509 (14) | 0.0298 (12) | 0.0590 (16) | −0.0099 (10) | 0.0325 (13) | −0.0084 (11) |
N3 | 0.0451 (13) | 0.0327 (12) | 0.0363 (13) | −0.0093 (10) | 0.0191 (11) | −0.0048 (9) |
N4 | 0.0413 (13) | 0.0280 (11) | 0.0495 (14) | −0.0075 (9) | 0.0231 (11) | −0.0034 (10) |
N5 | 0.051 (2) | 0.097 (4) | 0.065 (3) | 0.000 | 0.017 (2) | 0.000 |
Ni1 | 0.0431 (2) | 0.03001 (18) | 0.0405 (2) | −0.00374 (14) | 0.02019 (16) | −0.00054 (15) |
Ni2 | 0.0457 (2) | 0.02802 (19) | 0.0494 (2) | −0.00597 (14) | 0.02572 (18) | −0.00339 (15) |
O1 | 0.0495 (11) | 0.0312 (10) | 0.0402 (11) | −0.0069 (8) | 0.0216 (9) | −0.0011 (8) |
O2 | 0.0378 (10) | 0.0336 (10) | 0.0456 (11) | −0.0079 (8) | 0.0155 (9) | 0.0035 (8) |
O3 | 0.0564 (13) | 0.0415 (11) | 0.0536 (13) | 0.0072 (9) | 0.0284 (11) | 0.0056 (10) |
O4 | 0.0527 (12) | 0.0389 (11) | 0.0518 (12) | 0.0067 (9) | 0.0293 (10) | 0.0080 (9) |
O5 | 0.0801 (19) | 0.0733 (18) | 0.0654 (18) | −0.0146 (15) | 0.0004 (15) | 0.0067 (14) |
O6 | 0.0642 (15) | 0.0706 (17) | 0.0599 (15) | −0.0029 (13) | 0.0113 (12) | 0.0221 (13) |
O7 | 0.0516 (14) | 0.091 (2) | 0.0614 (16) | 0.0000 (13) | 0.0157 (12) | 0.0230 (14) |
O8 | 0.0787 (17) | 0.0722 (17) | 0.0636 (16) | 0.0137 (14) | 0.0326 (14) | 0.0259 (13) |
C1—C2 | 1.467 (6) | C22—N4 | 1.471 (3) |
C1—H1A | 0.9600 | C22—C23 | 1.507 (4) |
C1—H1B | 0.9600 | C22—H22A | 0.9700 |
C1—H1C | 0.9600 | C22—H22B | 0.9700 |
C2—C3 | 1.507 (4) | C23—N3 | 1.478 (3) |
C2—H2A | 0.9700 | C23—H23A | 0.9700 |
C2—H2B | 0.9700 | C23—H23B | 0.9700 |
C3—C4 | 1.527 (5) | C24—N3 | 1.247 (4) |
C3—H3A | 0.9700 | C24—H24 | 0.9300 |
C3—H3B | 0.9700 | C25—C26 | 1.516 (5) |
C4—C5 | 1.501 (4) | C25—H25A | 0.9700 |
C4—H4A | 0.9700 | C25—H25B | 0.9700 |
C4—H4B | 0.9700 | C26—C27 | 1.508 (5) |
C5—C6 | 1.381 (5) | C26—H26A | 0.9700 |
C5—C7 | 1.394 (4) | C26—H26B | 0.9700 |
C6—C8 | 1.391 (4) | C27—C28 | 1.474 (6) |
C6—H6 | 0.9300 | C27—H27A | 0.9700 |
C7—C9 | 1.409 (4) | C27—H27B | 0.9700 |
C7—H7 | 0.9300 | C28—H28A | 0.9600 |
C8—C10 | 1.426 (4) | C28—H28B | 0.9600 |
C8—C11 | 1.446 (4) | C28—H28C | 0.9600 |
C9—C10 | 1.407 (4) | C29—O3 | 1.255 (4) |
C9—C24 | 1.473 (4) | C29—O4 | 1.268 (3) |
C10—O1 | 1.326 (3) | C29—C30 | 1.493 (4) |
C11—N1 | 1.290 (4) | C29—Ni1 | 2.426 (3) |
C11—H11 | 0.9300 | C30—H30A | 0.9600 |
C12—N1 | 1.487 (3) | C30—H30B | 0.9600 |
C12—C13 | 1.495 (5) | C30—H30C | 0.9600 |
C12—H12A | 0.9700 | C31—C32 | 1.417 (7) |
C12—H12B | 0.9700 | C31—H31A | 0.9600 |
C13—N2 | 1.484 (4) | C31—H31B | 0.9600 |
C13—H13A | 0.9700 | C31—H31C | 0.9600 |
C13—H13B | 0.9700 | C32—N5 | 1.112 (7) |
C14—N2 | 1.279 (4) | Cl1—O7 | 1.374 (3) |
C14—C15 | 1.453 (4) | Cl1—O6 | 1.379 (3) |
C14—H14 | 0.9300 | Cl1—O5 | 1.389 (3) |
C15—C20 | 1.396 (4) | Cl1—O8 | 1.392 (3) |
C15—C16 | 1.403 (4) | Ni1—Ni2 | 2.9612 (5) |
C16—C17 | 1.379 (4) | Ni1—O1 | 2.0692 (19) |
C16—H16 | 0.9300 | Ni1—O2 | 2.0245 (18) |
C17—C18 | 1.395 (4) | Ni1—O3 | 2.096 (2) |
C17—C25 | 1.485 (4) | Ni1—O4 | 2.091 (2) |
C18—C19 | 1.405 (4) | Ni1—N3 | 1.983 (2) |
C18—H18 | 0.9300 | Ni1—N4 | 2.018 (2) |
C19—C20 | 1.400 (4) | Ni2—O1 | 1.8461 (19) |
C19—C21 | 1.476 (4) | Ni2—O2 | 1.8364 (19) |
C20—O2 | 1.328 (3) | Ni2—N1 | 1.822 (2) |
C21—N4 | 1.267 (4) | Ni2—N2 | 1.846 (2) |
C21—H21 | 0.9300 | ||
C2—C1—H1A | 109.5 | C27—C26—C25 | 114.1 (3) |
C2—C1—H1B | 109.5 | C27—C26—H26A | 108.7 |
H1A—C1—H1B | 109.5 | C25—C26—H26A | 108.7 |
C2—C1—H1C | 109.5 | C27—C26—H26B | 108.7 |
H1A—C1—H1C | 109.5 | C25—C26—H26B | 108.7 |
H1B—C1—H1C | 109.5 | H26A—C26—H26B | 107.6 |
C1—C2—C3 | 113.3 (3) | C28—C27—C26 | 114.7 (3) |
C1—C2—H2A | 108.9 | C28—C27—H27A | 108.6 |
C3—C2—H2A | 108.9 | C26—C27—H27A | 108.6 |
C1—C2—H2B | 108.9 | C28—C27—H27B | 108.6 |
C3—C2—H2B | 108.9 | C26—C27—H27B | 108.6 |
H2A—C2—H2B | 107.7 | H27A—C27—H27B | 107.6 |
C2—C3—C4 | 113.2 (3) | C27—C28—H28A | 109.5 |
C2—C3—H3A | 108.9 | C27—C28—H28B | 109.5 |
C4—C3—H3A | 108.9 | H28A—C28—H28B | 109.5 |
C2—C3—H3B | 108.9 | C27—C28—H28C | 109.5 |
C4—C3—H3B | 108.9 | H28A—C28—H28C | 109.5 |
H3A—C3—H3B | 107.8 | H28B—C28—H28C | 109.5 |
C5—C4—C3 | 116.4 (3) | O3—C29—O4 | 119.2 (3) |
C5—C4—H4A | 108.2 | O3—C29—C30 | 120.1 (3) |
C3—C4—H4A | 108.2 | O4—C29—C30 | 120.7 (3) |
C5—C4—H4B | 108.2 | O3—C29—Ni1 | 59.74 (15) |
C3—C4—H4B | 108.2 | O4—C29—Ni1 | 59.50 (15) |
H4A—C4—H4B | 107.3 | C30—C29—Ni1 | 178.3 (2) |
C6—C5—C7 | 116.6 (3) | C29—C30—H30A | 109.5 |
C6—C5—C4 | 122.0 (3) | C29—C30—H30B | 109.5 |
C7—C5—C4 | 121.4 (3) | H30A—C30—H30B | 109.5 |
C5—C6—C8 | 123.5 (3) | C29—C30—H30C | 109.5 |
C5—C6—H6 | 118.3 | H30A—C30—H30C | 109.5 |
C8—C6—H6 | 118.3 | H30B—C30—H30C | 109.5 |
C5—C7—C9 | 122.8 (3) | C32—C31—H31A | 109.5 |
C5—C7—H7 | 118.6 | C32—C31—H31B | 109.5 |
C9—C7—H7 | 118.6 | H31A—C31—H31B | 109.5 |
C6—C8—C10 | 119.3 (3) | C32—C31—H31C | 109.5 |
C6—C8—C11 | 118.0 (3) | H31A—C31—H31C | 109.5 |
C10—C8—C11 | 122.6 (3) | H31B—C31—H31C | 109.5 |
C10—C9—C7 | 119.2 (3) | N5—C32—C31 | 180.000 (2) |
C10—C9—C24 | 122.8 (3) | O7—Cl1—O6 | 111.57 (18) |
C7—C9—C24 | 117.7 (3) | O7—Cl1—O5 | 110.18 (17) |
O1—C10—C9 | 120.6 (2) | O6—Cl1—O5 | 112.98 (17) |
O1—C10—C8 | 120.7 (3) | O7—Cl1—O8 | 104.33 (17) |
C9—C10—C8 | 118.5 (3) | O6—Cl1—O8 | 107.57 (18) |
N1—C11—C8 | 125.3 (3) | O5—Cl1—O8 | 109.80 (19) |
N1—C11—H11 | 117.4 | C11—N1—C12 | 120.6 (2) |
C8—C11—H11 | 117.4 | C11—N1—Ni2 | 126.10 (19) |
N1—C12—C13 | 107.2 (2) | C12—N1—Ni2 | 113.2 (2) |
N1—C12—H12A | 110.3 | C14—N2—C13 | 123.8 (3) |
C13—C12—H12A | 110.3 | C14—N2—Ni2 | 125.7 (2) |
N1—C12—H12B | 110.3 | C13—N2—Ni2 | 110.5 (2) |
C13—C12—H12B | 110.3 | C24—N3—C23 | 122.5 (2) |
H12A—C12—H12B | 108.5 | C24—N3—Ni1 | 128.5 (2) |
N2—C13—C12 | 107.6 (2) | C23—N3—Ni1 | 107.05 (17) |
N2—C13—H13A | 110.2 | C21—N4—C22 | 121.0 (2) |
C12—C13—H13A | 110.2 | C21—N4—Ni1 | 126.38 (19) |
N2—C13—H13B | 110.2 | C22—N4—Ni1 | 111.42 (17) |
C12—C13—H13B | 110.2 | N3—Ni1—N4 | 82.82 (9) |
H13A—C13—H13B | 108.5 | N3—Ni1—O2 | 152.02 (9) |
N2—C14—C15 | 124.4 (3) | N4—Ni1—O2 | 86.43 (8) |
N2—C14—H14 | 117.8 | N3—Ni1—O1 | 86.43 (9) |
C15—C14—H14 | 117.8 | N4—Ni1—O1 | 111.73 (9) |
C20—C15—C16 | 118.6 (3) | O2—Ni1—O1 | 73.70 (8) |
C20—C15—C14 | 121.5 (3) | N3—Ni1—O4 | 100.88 (9) |
C16—C15—C14 | 119.8 (3) | N4—Ni1—O4 | 92.72 (9) |
C17—C16—C15 | 123.6 (3) | O2—Ni1—O4 | 105.39 (8) |
C17—C16—H16 | 118.2 | O1—Ni1—O4 | 155.26 (8) |
C15—C16—H16 | 118.2 | N3—Ni1—O3 | 104.18 (9) |
C16—C17—C18 | 115.9 (3) | N4—Ni1—O3 | 155.13 (9) |
C16—C17—C25 | 121.9 (3) | O2—Ni1—O3 | 96.38 (8) |
C18—C17—C25 | 122.2 (3) | O1—Ni1—O3 | 92.68 (8) |
C17—C18—C19 | 123.3 (3) | O4—Ni1—O3 | 62.66 (8) |
C17—C18—H18 | 118.4 | N3—Ni1—C29 | 104.37 (10) |
C19—C18—H18 | 118.4 | N4—Ni1—C29 | 124.19 (10) |
C20—C19—C18 | 118.5 (3) | O2—Ni1—C29 | 103.05 (9) |
C20—C19—C21 | 123.8 (3) | O1—Ni1—C29 | 123.82 (9) |
C18—C19—C21 | 117.0 (3) | O4—Ni1—C29 | 31.52 (9) |
O2—C20—C15 | 119.5 (3) | O3—Ni1—C29 | 31.15 (9) |
O2—C20—C19 | 120.6 (2) | N3—Ni1—Ni2 | 124.41 (7) |
C15—C20—C19 | 119.8 (3) | N4—Ni1—Ni2 | 109.76 (6) |
N4—C21—C19 | 124.6 (3) | O2—Ni1—Ni2 | 37.64 (5) |
N4—C21—H21 | 117.7 | O1—Ni1—Ni2 | 38.11 (5) |
C19—C21—H21 | 117.7 | O4—Ni1—Ni2 | 130.72 (6) |
N4—C22—C23 | 110.0 (2) | O3—Ni1—Ni2 | 86.24 (6) |
N4—C22—H22A | 109.7 | C29—Ni1—Ni2 | 110.19 (7) |
C23—C22—H22A | 109.7 | N1—Ni2—O2 | 177.19 (9) |
N4—C22—H22B | 109.7 | N1—Ni2—O1 | 95.92 (10) |
C23—C22—H22B | 109.7 | O2—Ni2—O1 | 83.63 (8) |
H22A—C22—H22B | 108.2 | N1—Ni2—N2 | 88.27 (11) |
N3—C23—C22 | 107.0 (2) | O2—Ni2—N2 | 92.31 (10) |
N3—C23—H23A | 110.3 | O1—Ni2—N2 | 175.13 (10) |
C22—C23—H23A | 110.3 | N1—Ni2—Ni1 | 136.39 (8) |
N3—C23—H23B | 110.3 | O2—Ni2—Ni1 | 42.31 (6) |
C22—C23—H23B | 110.3 | O1—Ni2—Ni1 | 43.77 (6) |
H23A—C23—H23B | 108.6 | N2—Ni2—Ni1 | 132.99 (8) |
N3—C24—C9 | 125.0 (3) | C10—O1—Ni2 | 127.73 (17) |
N3—C24—H24 | 117.5 | C10—O1—Ni1 | 124.67 (17) |
C9—C24—H24 | 117.5 | Ni2—O1—Ni1 | 98.12 (9) |
C17—C25—C26 | 114.5 (3) | C20—O2—Ni2 | 123.69 (17) |
C17—C25—H25A | 108.6 | C20—O2—Ni1 | 130.03 (17) |
C26—C25—H25A | 108.6 | Ni2—O2—Ni1 | 100.05 (9) |
C17—C25—H25B | 108.6 | C29—O3—Ni1 | 89.12 (17) |
C26—C25—H25B | 108.6 | C29—O4—Ni1 | 88.98 (17) |
H25A—C25—H25B | 107.6 |