Supporting information
Crystallographic Information File (CIF) https://doi.org/10.1107/S1600536807010653/bg2034sup1.cif | |
Structure factor file (CIF format) https://doi.org/10.1107/S1600536807010653/bg2034Isup2.hkl |
CCDC reference: 642906
Data collection: COLLECT (Nonius, 2000); cell refinement: SCALEPACK (Otwinowski & Minor, 1997); data reduction: SCALEPACK and DENZO (Otwinowski & Minor, 1997); program(s) used to solve structure: DIRDIFF99 (Beurskens et al., 1999); program(s) used to refine structure: SHELXL97 (Sheldrick, 1997); molecular graphics: X-SEED (Barbour, 2001); software used to prepare material for publication: WinGX (Farrugia, 1999).
[Ni(C13H12Br2N4)2](ClO4)2 | Z = 2 |
Mr = 1025.78 | F(000) = 1004 |
Triclinic, P1 | Dx = 2.037 Mg m−3 |
Hall symbol: -P 1 | Mo Kα radiation, λ = 0.71073 Å |
a = 9.1897 (3) Å | Cell parameters from 24601 reflections |
b = 12.9937 (3) Å | θ = 2.7–27.5° |
c = 15.0869 (5) Å | µ = 5.58 mm−1 |
α = 110.077 (2)° | T = 150 K |
β = 95.308 (2)° | Block, brown |
γ = 94.573 (2)° | 0.30 × 0.22 × 0.21 mm |
V = 1672.76 (9) Å3 |
Bruker–Nonius KappaCCD diffractometer | 7570 independent reflections |
Radiation source: fine-focus sealed tube | 4801 reflections with I > 2σ(I) |
Graphite monochromator | Rint = 0.156 |
φ and ω scans | θmax = 27.5°, θmin = 3.0° |
Absorption correction: multi-scan (SORTAV; Blessing, 1995) | h = −11→11 |
Tmin = 0.23, Tmax = 0.31 | k = −16→16 |
26603 measured reflections | l = −19→19 |
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)] = 0.064 | Hydrogen site location: inferred from neighbouring sites |
wR(F2) = 0.148 | H-atom parameters constrained |
S = 1.02 | w = 1/[σ2(Fo2) + (0.0417P)2 + 4.0795P] where P = (Fo2 + 2Fc2)/3 |
7570 reflections | (Δ/σ)max = 0.001 |
442 parameters | Δρmax = 1.35 e Å−3 |
0 restraints | Δρmin = −0.93 e Å−3 |
Experimental. m/z 579.00 (M+, 30%), calc. 579.85 (M+, 100%) for [NiL(CH3CN)]+(ClO4)-. IR (KBr disc): 1636.30(–C=N), 3405.67 (–NH2). |
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 | ||
C1 | 0.6524 (6) | 0.8316 (5) | 0.7649 (4) | 0.0201 (13) | |
C2 | 0.5748 (7) | 0.9242 (5) | 0.7542 (5) | 0.0225 (14) | |
C3 | 0.5682 (7) | 1.0204 (5) | 0.8302 (5) | 0.0281 (15) | |
H3 | 0.6191 | 1.0334 | 0.8915 | 0.034* | |
C4 | 0.4832 (8) | 1.0972 (5) | 0.8124 (5) | 0.0336 (17) | |
H4 | 0.4754 | 1.1641 | 0.8626 | 0.040* | |
C5 | 0.4112 (7) | 1.0774 (5) | 0.7239 (5) | 0.0319 (16) | |
H5 | 0.3526 | 1.1288 | 0.7108 | 0.038* | |
C6 | 0.4281 (7) | 0.9790 (5) | 0.6547 (5) | 0.0277 (15) | |
C7 | 0.7688 (6) | 0.7893 (5) | 0.7044 (4) | 0.0186 (13) | |
C8 | 0.8324 (7) | 0.8469 (5) | 0.6538 (5) | 0.0265 (14) | |
H8 | 0.7988 | 0.9139 | 0.6532 | 0.032* | |
C9 | 0.9469 (7) | 0.8050 (5) | 0.6038 (5) | 0.0305 (15) | |
H9 | 0.9964 | 0.8457 | 0.5715 | 0.037* | |
C10 | 0.9882 (7) | 0.7056 (6) | 0.6009 (5) | 0.0306 (16) | |
H10 | 1.0650 | 0.6752 | 0.5659 | 0.037* | |
C11 | 0.9145 (7) | 0.6501 (5) | 0.6508 (4) | 0.0260 (15) | |
C12 | 0.5068 (7) | 0.8104 (5) | 0.8843 (5) | 0.0277 (15) | |
H26A | 0.4288 | 0.8436 | 0.8573 | 0.033* | |
H26B | 0.5521 | 0.8650 | 0.9464 | 0.033* | |
C13 | 0.4410 (7) | 0.7049 (5) | 0.8971 (5) | 0.0265 (15) | |
H25A | 0.3839 | 0.7242 | 0.9519 | 0.032* | |
H25B | 0.3738 | 0.6591 | 0.8394 | 0.032* | |
C14 | 0.7363 (7) | 0.4128 (5) | 0.7723 (5) | 0.0228 (14) | |
C15 | 0.7982 (6) | 0.3134 (5) | 0.7799 (4) | 0.0226 (14) | |
C16 | 0.7890 (8) | 0.2825 (5) | 0.8573 (5) | 0.0333 (16) | |
H16 | 0.7348 | 0.3208 | 0.9066 | 0.040* | |
C17 | 0.8610 (7) | 0.1934 (5) | 0.8628 (5) | 0.0304 (16) | |
H17 | 0.8571 | 0.1701 | 0.9158 | 0.036* | |
C18 | 0.9378 (7) | 0.1405 (5) | 0.7891 (5) | 0.0298 (16) | |
H18 | 0.9890 | 0.0801 | 0.7900 | 0.036* | |
C19 | 0.9376 (7) | 0.1782 (5) | 0.7146 (5) | 0.0256 (14) | |
C20 | 0.6081 (7) | 0.4035 (5) | 0.7012 (4) | 0.0200 (13) | |
C21 | 0.5378 (7) | 0.3022 (5) | 0.6417 (5) | 0.0284 (15) | |
H21 | 0.5707 | 0.2364 | 0.6461 | 0.034* | |
C22 | 0.4198 (8) | 0.2961 (6) | 0.5757 (5) | 0.0394 (18) | |
H22 | 0.3717 | 0.2269 | 0.5335 | 0.047* | |
C23 | 0.3740 (8) | 0.3932 (6) | 0.5728 (5) | 0.0349 (17) | |
H23 | 0.2919 | 0.3927 | 0.5295 | 0.042* | |
C24 | 0.4509 (7) | 0.4922 (5) | 0.6350 (4) | 0.0250 (14) | |
C25 | 0.9272 (6) | 0.5349 (5) | 0.8917 (5) | 0.0247 (14) | |
H13A | 0.9949 | 0.4784 | 0.8696 | 0.030* | |
H13B | 0.8998 | 0.5352 | 0.9537 | 0.030* | |
C26 | 1.0008 (7) | 0.6485 (5) | 0.9015 (5) | 0.0260 (15) | |
H12A | 1.0803 | 0.6746 | 0.9558 | 0.031* | |
H12B | 1.0446 | 0.6443 | 0.8430 | 0.031* | |
N1 | 0.5086 (6) | 0.9035 (4) | 0.6666 (4) | 0.0247 (12) | |
N2 | 0.8093 (5) | 0.6899 (4) | 0.7044 (3) | 0.0212 (11) | |
N3 | 0.6185 (5) | 0.7800 (4) | 0.8193 (4) | 0.0194 (11) | |
N4 | 0.5611 (5) | 0.6428 (4) | 0.9138 (4) | 0.0246 (12) | |
H4A | 0.5247 | 0.5716 | 0.9056 | 0.030* | |
H4B | 0.6087 | 0.6758 | 0.9748 | 0.030* | |
N5 | 0.8698 (6) | 0.2613 (4) | 0.7061 (4) | 0.0247 (12) | |
N6 | 0.5645 (5) | 0.5005 (4) | 0.7000 (3) | 0.0198 (11) | |
N7 | 0.7954 (5) | 0.5108 (4) | 0.8219 (4) | 0.0181 (11) | |
N8 | 0.8872 (5) | 0.7266 (4) | 0.9172 (4) | 0.0209 (11) | |
H5A | 0.9219 | 0.7908 | 0.9091 | 0.025* | |
H5B | 0.8613 | 0.7437 | 0.9776 | 0.025* | |
O1 | 0.0077 (5) | 0.0606 (4) | 0.1189 (4) | 0.0419 (13) | |
O2 | −0.1997 (6) | 0.0974 (4) | 0.1998 (4) | 0.0477 (14) | |
O3 | −0.2009 (5) | 0.1086 (4) | 0.0488 (4) | 0.0414 (13) | |
O4 | −0.2069 (6) | −0.0632 (4) | 0.0673 (4) | 0.0532 (15) | |
O5 | 0.2761 (6) | 0.4948 (4) | 0.9333 (4) | 0.0560 (16) | |
O6 | 0.2353 (7) | 0.3799 (6) | 0.7750 (4) | 0.077 (2) | |
O7 | 0.4538 (5) | 0.3833 (4) | 0.8690 (4) | 0.0433 (13) | |
O8 | 0.2333 (6) | 0.3053 (4) | 0.8945 (4) | 0.0506 (14) | |
Cl1 | −0.15091 (17) | 0.05028 (13) | 0.10838 (12) | 0.0271 (4) | |
Cl2 | 0.29863 (18) | 0.38968 (13) | 0.86626 (12) | 0.0287 (4) | |
Ni1 | 0.70626 (8) | 0.64307 (6) | 0.81450 (5) | 0.01821 (19) | |
Br1 | 0.32333 (9) | 0.94049 (7) | 0.52986 (6) | 0.0530 (3) | |
Br2 | 0.96357 (8) | 0.50814 (6) | 0.64089 (5) | 0.0389 (2) | |
Br3 | 1.04297 (9) | 0.10659 (6) | 0.61328 (5) | 0.0447 (2) | |
Br4 | 0.39281 (8) | 0.62512 (6) | 0.62567 (6) | 0.0419 (2) |
U11 | U22 | U33 | U12 | U13 | U23 | |
C1 | 0.016 (3) | 0.021 (3) | 0.027 (4) | 0.001 (2) | 0.006 (3) | 0.013 (3) |
C2 | 0.018 (3) | 0.022 (3) | 0.031 (4) | 0.001 (3) | 0.006 (3) | 0.013 (3) |
C3 | 0.035 (4) | 0.025 (4) | 0.023 (4) | 0.004 (3) | −0.002 (3) | 0.008 (3) |
C4 | 0.039 (4) | 0.020 (3) | 0.042 (4) | 0.008 (3) | 0.007 (3) | 0.010 (3) |
C5 | 0.026 (4) | 0.029 (4) | 0.048 (5) | 0.010 (3) | 0.005 (3) | 0.021 (3) |
C6 | 0.023 (4) | 0.035 (4) | 0.028 (4) | 0.005 (3) | −0.001 (3) | 0.017 (3) |
C7 | 0.016 (3) | 0.023 (3) | 0.017 (3) | 0.001 (2) | 0.004 (2) | 0.008 (3) |
C8 | 0.024 (4) | 0.026 (4) | 0.030 (4) | −0.001 (3) | 0.007 (3) | 0.010 (3) |
C9 | 0.027 (4) | 0.034 (4) | 0.029 (4) | −0.004 (3) | 0.002 (3) | 0.011 (3) |
C10 | 0.028 (4) | 0.041 (4) | 0.025 (4) | 0.010 (3) | 0.011 (3) | 0.011 (3) |
C11 | 0.035 (4) | 0.024 (3) | 0.020 (3) | 0.007 (3) | 0.004 (3) | 0.008 (3) |
C12 | 0.027 (4) | 0.033 (4) | 0.037 (4) | 0.021 (3) | 0.017 (3) | 0.023 (3) |
C13 | 0.017 (3) | 0.035 (4) | 0.036 (4) | 0.010 (3) | 0.008 (3) | 0.020 (3) |
C14 | 0.021 (3) | 0.024 (4) | 0.030 (4) | 0.007 (3) | 0.013 (3) | 0.015 (3) |
C15 | 0.018 (3) | 0.024 (3) | 0.028 (4) | 0.003 (3) | −0.001 (3) | 0.012 (3) |
C16 | 0.042 (4) | 0.028 (4) | 0.034 (4) | 0.007 (3) | 0.006 (3) | 0.015 (3) |
C17 | 0.038 (4) | 0.024 (4) | 0.030 (4) | −0.001 (3) | −0.001 (3) | 0.013 (3) |
C18 | 0.030 (4) | 0.019 (3) | 0.039 (4) | 0.002 (3) | −0.008 (3) | 0.011 (3) |
C19 | 0.025 (4) | 0.021 (3) | 0.025 (4) | 0.004 (3) | 0.000 (3) | 0.002 (3) |
C20 | 0.022 (3) | 0.019 (3) | 0.020 (3) | 0.005 (3) | 0.006 (3) | 0.008 (2) |
C21 | 0.038 (4) | 0.017 (3) | 0.025 (4) | 0.000 (3) | −0.003 (3) | 0.002 (3) |
C22 | 0.037 (4) | 0.032 (4) | 0.038 (5) | −0.004 (3) | −0.008 (3) | 0.003 (3) |
C23 | 0.035 (4) | 0.042 (4) | 0.026 (4) | 0.007 (3) | −0.007 (3) | 0.012 (3) |
C24 | 0.029 (4) | 0.027 (4) | 0.024 (4) | 0.005 (3) | 0.001 (3) | 0.016 (3) |
C25 | 0.018 (3) | 0.024 (3) | 0.029 (4) | 0.005 (3) | −0.007 (3) | 0.006 (3) |
C26 | 0.016 (3) | 0.026 (3) | 0.032 (4) | 0.005 (3) | −0.001 (3) | 0.005 (3) |
N1 | 0.024 (3) | 0.025 (3) | 0.027 (3) | 0.005 (2) | 0.005 (2) | 0.010 (2) |
N2 | 0.024 (3) | 0.022 (3) | 0.018 (3) | 0.009 (2) | 0.005 (2) | 0.005 (2) |
N3 | 0.017 (3) | 0.023 (3) | 0.022 (3) | 0.008 (2) | 0.006 (2) | 0.011 (2) |
N4 | 0.020 (3) | 0.023 (3) | 0.035 (3) | 0.004 (2) | 0.006 (2) | 0.014 (2) |
N5 | 0.029 (3) | 0.021 (3) | 0.022 (3) | 0.006 (2) | 0.000 (2) | 0.004 (2) |
N6 | 0.018 (3) | 0.016 (3) | 0.021 (3) | −0.003 (2) | −0.002 (2) | 0.003 (2) |
N7 | 0.013 (3) | 0.017 (3) | 0.027 (3) | 0.006 (2) | 0.002 (2) | 0.011 (2) |
N8 | 0.021 (3) | 0.016 (3) | 0.025 (3) | 0.001 (2) | 0.004 (2) | 0.007 (2) |
O1 | 0.026 (3) | 0.049 (3) | 0.058 (4) | −0.003 (2) | −0.002 (2) | 0.033 (3) |
O2 | 0.050 (3) | 0.057 (3) | 0.031 (3) | 0.000 (3) | 0.001 (3) | 0.012 (3) |
O3 | 0.035 (3) | 0.056 (3) | 0.047 (3) | 0.020 (2) | 0.008 (2) | 0.030 (3) |
O4 | 0.050 (3) | 0.029 (3) | 0.070 (4) | −0.005 (2) | 0.007 (3) | 0.007 (3) |
O5 | 0.040 (3) | 0.032 (3) | 0.090 (5) | 0.004 (2) | 0.020 (3) | 0.011 (3) |
O6 | 0.068 (4) | 0.125 (6) | 0.044 (4) | 0.004 (4) | −0.008 (3) | 0.041 (4) |
O7 | 0.026 (3) | 0.054 (3) | 0.051 (3) | 0.009 (2) | 0.013 (2) | 0.017 (3) |
O8 | 0.056 (4) | 0.041 (3) | 0.052 (4) | −0.016 (3) | 0.009 (3) | 0.017 (3) |
Cl1 | 0.0234 (8) | 0.0273 (9) | 0.0335 (9) | 0.0026 (6) | 0.0030 (7) | 0.0148 (7) |
Cl2 | 0.0257 (9) | 0.0299 (9) | 0.0312 (9) | −0.0006 (7) | 0.0021 (7) | 0.0129 (7) |
Ni1 | 0.0163 (4) | 0.0168 (4) | 0.0233 (4) | 0.0050 (3) | 0.0036 (3) | 0.0084 (3) |
Br1 | 0.0518 (5) | 0.0755 (6) | 0.0327 (5) | 0.0371 (5) | 0.0021 (4) | 0.0149 (4) |
Br2 | 0.0492 (5) | 0.0341 (4) | 0.0416 (5) | 0.0217 (3) | 0.0249 (4) | 0.0152 (3) |
Br3 | 0.0483 (5) | 0.0460 (5) | 0.0379 (5) | 0.0282 (4) | 0.0080 (4) | 0.0066 (3) |
Br4 | 0.0374 (4) | 0.0367 (4) | 0.0525 (5) | 0.0046 (3) | −0.0159 (4) | 0.0226 (4) |
C1—N3 | 1.270 (7) | C18—C19 | 1.371 (9) |
C1—C7 | 1.487 (8) | C18—H18 | 0.9500 |
C1—C2 | 1.494 (8) | C19—N5 | 1.327 (7) |
C2—N1 | 1.330 (8) | C19—Br3 | 1.893 (6) |
C2—C3 | 1.386 (9) | C20—N6 | 1.358 (7) |
C3—C4 | 1.395 (9) | C20—C21 | 1.379 (8) |
C3—H3 | 0.9500 | C21—C22 | 1.380 (9) |
C4—C5 | 1.364 (10) | C21—H21 | 0.9500 |
C4—H4 | 0.9500 | C22—C23 | 1.374 (9) |
C5—C6 | 1.376 (9) | C22—H22 | 0.9500 |
C5—H5 | 0.9500 | C23—C24 | 1.392 (9) |
C6—N1 | 1.325 (7) | C23—H23 | 0.9500 |
C6—Br1 | 1.914 (6) | C24—N6 | 1.336 (7) |
C7—N2 | 1.372 (7) | C24—Br4 | 1.894 (6) |
C7—C8 | 1.374 (8) | C25—N7 | 1.467 (7) |
C8—C9 | 1.389 (9) | C25—C26 | 1.527 (9) |
C8—H8 | 0.9500 | C25—H13A | 0.9900 |
C9—C10 | 1.363 (9) | C25—H13B | 0.9900 |
C9—H9 | 0.9500 | C26—N8 | 1.492 (7) |
C10—C11 | 1.391 (9) | C26—H12A | 0.9900 |
C10—H10 | 0.9500 | C26—H12B | 0.9900 |
C11—N2 | 1.339 (8) | N2—Ni1 | 2.218 (5) |
C11—Br2 | 1.893 (6) | N3—Ni1 | 1.993 (4) |
C12—N3 | 1.467 (7) | N4—Ni1 | 2.097 (5) |
C12—C13 | 1.535 (9) | N4—H4A | 0.9200 |
C12—H26A | 0.9900 | N4—H4B | 0.9200 |
C12—H26B | 0.9900 | N6—Ni1 | 2.261 (5) |
C13—N4 | 1.471 (7) | N7—Ni1 | 1.994 (4) |
C13—H25A | 0.9900 | N8—Ni1 | 2.103 (5) |
C13—H25B | 0.9900 | N8—H5A | 0.9200 |
C14—N7 | 1.279 (8) | N8—H5B | 0.9200 |
C14—C20 | 1.486 (9) | O1—Cl1 | 1.442 (5) |
C14—C15 | 1.486 (8) | O2—Cl1 | 1.434 (5) |
C15—N5 | 1.349 (8) | O3—Cl1 | 1.428 (5) |
C15—C16 | 1.367 (9) | O4—Cl1 | 1.419 (5) |
C16—C17 | 1.401 (9) | O5—Cl2 | 1.437 (5) |
C16—H16 | 0.9500 | O6—Cl2 | 1.404 (6) |
C17—C18 | 1.379 (9) | O7—Cl2 | 1.433 (5) |
C17—H17 | 0.9500 | O8—Cl2 | 1.416 (5) |
N3—C1—C7 | 116.2 (5) | C22—C23—C24 | 118.4 (6) |
N3—C1—C2 | 123.7 (5) | C22—C23—H23 | 120.8 |
C7—C1—C2 | 119.9 (5) | C24—C23—H23 | 120.8 |
N1—C2—C3 | 123.8 (5) | N6—C24—C23 | 124.8 (5) |
N1—C2—C1 | 113.8 (5) | N6—C24—Br4 | 117.3 (5) |
C3—C2—C1 | 122.4 (6) | C23—C24—Br4 | 117.9 (5) |
C2—C3—C4 | 116.8 (6) | N7—C25—C26 | 106.7 (5) |
C2—C3—H3 | 121.6 | N7—C25—H13A | 110.4 |
C4—C3—H3 | 121.6 | C26—C25—H13A | 110.4 |
C5—C4—C3 | 120.9 (6) | N7—C25—H13B | 110.4 |
C5—C4—H4 | 119.6 | C26—C25—H13B | 110.4 |
C3—C4—H4 | 119.6 | H13A—C25—H13B | 108.6 |
C4—C5—C6 | 116.3 (6) | N8—C26—C25 | 108.5 (5) |
C4—C5—H5 | 121.8 | N8—C26—H12A | 110.0 |
C6—C5—H5 | 121.8 | C25—C26—H12A | 110.0 |
N1—C6—C5 | 125.8 (6) | N8—C26—H12B | 110.0 |
N1—C6—Br1 | 114.8 (5) | C25—C26—H12B | 110.0 |
C5—C6—Br1 | 119.4 (5) | H12A—C26—H12B | 108.4 |
N2—C7—C8 | 122.9 (5) | C6—N1—C2 | 116.4 (5) |
N2—C7—C1 | 115.0 (5) | C11—N2—C7 | 116.2 (5) |
C8—C7—C1 | 122.1 (5) | C11—N2—Ni1 | 133.1 (4) |
C7—C8—C9 | 118.6 (6) | C7—N2—Ni1 | 109.9 (4) |
C7—C8—H8 | 120.7 | C1—N3—C12 | 123.7 (5) |
C9—C8—H8 | 120.7 | C1—N3—Ni1 | 120.9 (4) |
C10—C9—C8 | 120.0 (6) | C12—N3—Ni1 | 115.2 (4) |
C10—C9—H9 | 120.0 | C13—N4—Ni1 | 106.7 (4) |
C8—C9—H9 | 120.0 | C13—N4—H4A | 110.4 |
C9—C10—C11 | 117.9 (6) | Ni1—N4—H4A | 110.4 |
C9—C10—H10 | 121.0 | C13—N4—H4B | 110.4 |
C11—C10—H10 | 121.0 | Ni1—N4—H4B | 110.4 |
N2—C11—C10 | 124.2 (6) | H4A—N4—H4B | 108.6 |
N2—C11—Br2 | 117.7 (5) | C19—N5—C15 | 115.2 (5) |
C10—C11—Br2 | 118.0 (5) | C24—N6—C20 | 115.7 (5) |
N3—C12—C13 | 107.6 (5) | C24—N6—Ni1 | 134.5 (4) |
N3—C12—H26A | 110.2 | C20—N6—Ni1 | 109.8 (4) |
C13—C12—H26A | 110.2 | C14—N7—C25 | 123.3 (5) |
N3—C12—H26B | 110.2 | C14—N7—Ni1 | 121.7 (4) |
C13—C12—H26B | 110.2 | C25—N7—Ni1 | 115.0 (4) |
H26A—C12—H26B | 108.5 | C26—N8—Ni1 | 105.3 (4) |
N4—C13—C12 | 109.1 (5) | C26—N8—H5A | 110.7 |
N4—C13—H25A | 109.9 | Ni1—N8—H5A | 110.7 |
C12—C13—H25A | 109.9 | C26—N8—H5B | 110.7 |
N4—C13—H25B | 109.9 | Ni1—N8—H5B | 110.7 |
C12—C13—H25B | 109.9 | H5A—N8—H5B | 108.8 |
H25A—C13—H25B | 108.3 | O4—Cl1—O3 | 110.5 (3) |
N7—C14—C20 | 116.1 (5) | O4—Cl1—O2 | 109.7 (3) |
N7—C14—C15 | 122.3 (6) | O3—Cl1—O2 | 109.1 (3) |
C20—C14—C15 | 121.5 (5) | O4—Cl1—O1 | 109.1 (3) |
N5—C15—C16 | 123.9 (5) | O3—Cl1—O1 | 108.9 (3) |
N5—C15—C14 | 113.7 (5) | O2—Cl1—O1 | 109.6 (3) |
C16—C15—C14 | 122.3 (6) | O6—Cl2—O8 | 110.9 (4) |
C15—C16—C17 | 118.8 (6) | O6—Cl2—O7 | 110.9 (4) |
C15—C16—H16 | 120.6 | O8—Cl2—O7 | 108.8 (3) |
C17—C16—H16 | 120.6 | O6—Cl2—O5 | 109.3 (4) |
C18—C17—C16 | 118.2 (6) | O8—Cl2—O5 | 108.6 (3) |
C18—C17—H17 | 120.9 | O7—Cl2—O5 | 108.3 (3) |
C16—C17—H17 | 120.9 | N3—Ni1—N7 | 175.0 (2) |
C19—C18—C17 | 117.7 (6) | N3—Ni1—N4 | 82.12 (19) |
C19—C18—H18 | 121.2 | N7—Ni1—N4 | 94.34 (19) |
C17—C18—H18 | 121.2 | N3—Ni1—N8 | 94.53 (19) |
N5—C19—C18 | 126.1 (6) | N7—Ni1—N8 | 82.28 (19) |
N5—C19—Br3 | 115.8 (5) | N4—Ni1—N8 | 95.0 (2) |
C18—C19—Br3 | 118.1 (5) | N3—Ni1—N2 | 77.32 (18) |
N6—C20—C21 | 122.8 (6) | N7—Ni1—N2 | 106.45 (18) |
N6—C20—C14 | 115.7 (5) | N4—Ni1—N2 | 158.97 (18) |
C21—C20—C14 | 121.5 (5) | N8—Ni1—N2 | 91.03 (19) |
C20—C21—C22 | 120.2 (6) | N3—Ni1—N6 | 107.07 (19) |
C20—C21—H21 | 119.9 | N7—Ni1—N6 | 76.38 (19) |
C22—C21—H21 | 119.9 | N4—Ni1—N6 | 91.5 (2) |
C23—C22—C21 | 118.1 (6) | N8—Ni1—N6 | 158.12 (17) |
C23—C22—H22 | 120.9 | N2—Ni1—N6 | 90.38 (18) |
C21—C22—H22 | 120.9 | ||
N3—C1—C2—N1 | −117.6 (7) | C16—C15—N5—C19 | −2.4 (9) |
C7—C1—C2—N1 | 57.5 (8) | C14—C15—N5—C19 | 174.2 (6) |
N3—C1—C2—C3 | 59.8 (9) | C23—C24—N6—C20 | 2.3 (9) |
C7—C1—C2—C3 | −125.1 (7) | Br4—C24—N6—C20 | −176.6 (4) |
N1—C2—C3—C4 | 1.8 (10) | C23—C24—N6—Ni1 | −176.8 (5) |
C1—C2—C3—C4 | −175.3 (6) | Br4—C24—N6—Ni1 | 4.2 (8) |
C2—C3—C4—C5 | −0.2 (10) | C21—C20—N6—C24 | −2.0 (9) |
C3—C4—C5—C6 | −0.3 (10) | C14—C20—N6—C24 | 178.9 (5) |
C4—C5—C6—N1 | −0.6 (11) | C21—C20—N6—Ni1 | 177.3 (5) |
C4—C5—C6—Br1 | 176.8 (5) | C14—C20—N6—Ni1 | −1.7 (6) |
N3—C1—C7—N2 | 9.4 (8) | C20—C14—N7—C25 | −176.7 (5) |
C2—C1—C7—N2 | −166.1 (5) | C15—C14—N7—C25 | −1.1 (9) |
N3—C1—C7—C8 | −169.4 (6) | C20—C14—N7—Ni1 | 6.8 (7) |
C2—C1—C7—C8 | 15.1 (9) | C15—C14—N7—Ni1 | −177.5 (4) |
N2—C7—C8—C9 | −2.8 (10) | C26—C25—N7—C14 | 155.1 (5) |
C1—C7—C8—C9 | 176.0 (6) | C26—C25—N7—Ni1 | −28.3 (6) |
C7—C8—C9—C10 | 3.8 (10) | C25—C26—N8—Ni1 | −46.8 (5) |
C8—C9—C10—C11 | −1.3 (10) | C1—N3—Ni1—N4 | −175.6 (5) |
C9—C10—C11—N2 | −2.7 (10) | C12—N3—Ni1—N4 | 0.3 (4) |
C9—C10—C11—Br2 | 176.4 (5) | C1—N3—Ni1—N8 | 90.0 (5) |
N3—C12—C13—N4 | 45.7 (7) | C12—N3—Ni1—N8 | −94.1 (4) |
N7—C14—C15—N5 | −104.5 (7) | C1—N3—Ni1—N2 | 0.0 (5) |
C20—C14—C15—N5 | 70.9 (7) | C12—N3—Ni1—N2 | 175.9 (5) |
N7—C14—C15—C16 | 72.2 (8) | C1—N3—Ni1—N6 | −86.4 (5) |
C20—C14—C15—C16 | −112.4 (7) | C12—N3—Ni1—N6 | 89.4 (5) |
N5—C15—C16—C17 | 1.8 (10) | C14—N7—Ni1—N4 | 84.6 (5) |
C14—C15—C16—C17 | −174.6 (6) | C25—N7—Ni1—N4 | −92.2 (4) |
C15—C16—C17—C18 | −0.2 (10) | C14—N7—Ni1—N8 | 179.0 (5) |
C16—C17—C18—C19 | −0.6 (10) | C25—N7—Ni1—N8 | 2.3 (4) |
C17—C18—C19—N5 | −0.2 (10) | C14—N7—Ni1—N2 | −92.2 (5) |
C17—C18—C19—Br3 | 179.8 (5) | C25—N7—Ni1—N2 | 91.1 (4) |
N7—C14—C20—N6 | −2.8 (8) | C14—N7—Ni1—N6 | −5.9 (5) |
C15—C14—C20—N6 | −178.4 (5) | C25—N7—Ni1—N6 | 177.4 (4) |
N7—C14—C20—C21 | 178.1 (6) | C13—N4—Ni1—N3 | 24.9 (4) |
C15—C14—C20—C21 | 2.4 (9) | C13—N4—Ni1—N7 | −158.6 (4) |
N6—C20—C21—C22 | 1.6 (10) | C13—N4—Ni1—N8 | 118.8 (4) |
C14—C20—C21—C22 | −179.4 (6) | C13—N4—Ni1—N2 | 12.8 (8) |
C20—C21—C22—C23 | −1.2 (11) | C13—N4—Ni1—N6 | −82.1 (4) |
C21—C22—C23—C24 | 1.4 (11) | C26—N8—Ni1—N3 | −159.1 (4) |
C22—C23—C24—N6 | −2.1 (11) | C26—N8—Ni1—N7 | 24.7 (4) |
C22—C23—C24—Br4 | 176.8 (5) | C26—N8—Ni1—N4 | 118.4 (4) |
N7—C25—C26—N8 | 49.6 (6) | C26—N8—Ni1—N2 | −81.8 (4) |
C5—C6—N1—C2 | 2.0 (10) | C26—N8—Ni1—N6 | 11.8 (7) |
Br1—C6—N1—C2 | −175.5 (4) | C11—N2—Ni1—N3 | 173.9 (6) |
C3—C2—N1—C6 | −2.6 (9) | C7—N2—Ni1—N3 | 5.0 (4) |
C1—C2—N1—C6 | 174.7 (5) | C11—N2—Ni1—N7 | −2.7 (6) |
C10—C11—N2—C7 | 3.7 (9) | C7—N2—Ni1—N7 | −171.7 (4) |
Br2—C11—N2—C7 | −175.3 (4) | C11—N2—Ni1—N4 | −173.8 (6) |
C10—C11—N2—Ni1 | −164.7 (5) | C7—N2—Ni1—N4 | 17.3 (8) |
Br2—C11—N2—Ni1 | 16.3 (8) | C11—N2—Ni1—N8 | 79.5 (6) |
C8—C7—N2—C11 | −0.9 (9) | C7—N2—Ni1—N8 | −89.4 (4) |
C1—C7—N2—C11 | −179.7 (5) | C11—N2—Ni1—N6 | −78.6 (6) |
C8—C7—N2—Ni1 | 170.1 (5) | C7—N2—Ni1—N6 | 112.4 (4) |
C1—C7—N2—Ni1 | −8.7 (6) | C24—N6—Ni1—N3 | 6.6 (6) |
C7—C1—N3—C12 | 179.6 (6) | C20—N6—Ni1—N3 | −172.6 (4) |
C2—C1—N3—C12 | −5.1 (10) | C24—N6—Ni1—N7 | −177.0 (6) |
C7—C1—N3—Ni1 | −4.9 (8) | C20—N6—Ni1—N7 | 3.8 (4) |
C2—C1—N3—Ni1 | 170.4 (5) | C24—N6—Ni1—N4 | 88.9 (6) |
C13—C12—N3—C1 | 151.3 (6) | C20—N6—Ni1—N4 | −90.4 (4) |
C13—C12—N3—Ni1 | −24.4 (6) | C24—N6—Ni1—N8 | −163.9 (6) |
C12—C13—N4—Ni1 | −44.7 (6) | C20—N6—Ni1—N8 | 16.9 (7) |
C18—C19—N5—C15 | 1.6 (9) | C24—N6—Ni1—N2 | −70.2 (6) |
Br3—C19—N5—C15 | −178.4 (4) | C20—N6—Ni1—N2 | 110.6 (4) |