Supporting information
Crystallographic Information File (CIF) https://doi.org/10.1107/S0108768112002728/ps5014sup1.cif | |
Structure factor file (CIF format) https://doi.org/10.1107/S0108768112002728/ps5014Isup2.hkl | |
Portable Document Format (PDF) file https://doi.org/10.1107/S0108768112002728/ps5014sup3.pdf |
CCDC reference: 879420
All H-atoms were placed in idealized locations and refined as riding with appropriate thermal displacement coefficients Uiso(H) = 1.2 or 1.5 times Ueq(bearing atom).
Data collection: APEX2 Ver. 2.1-4 (Bruker-AXS, 2007); cell refinement: SAINT Ver. 7.24A (Bruker-AXS, 2007); data reduction: SAINT Ver. 7.24A; program(s) used to solve structure: SHELXTL (Sheldrick, 2008); program(s) used to refine structure: SHELXTL; molecular graphics: SHELXTL; software used to prepare material for publication: SHELXTL.
| Figure 1. Molecular structure of (I). The thermal ellipsoids are shown at 50% probability level. |
C44H42Br5Fe3N6NiO4 | F(000) = 2644 |
Mr = 1344.65 | Dx = 1.895 Mg m−3 |
Monoclinic, Cc | Cu Kα radiation, λ = 1.54178 Å |
Hall symbol: C -2yc | Cell parameters from 999 reflections |
a = 15.2181 (3) Å | θ = 3.1–72.1° |
b = 22.0080 (3) Å | µ = 13.07 mm−1 |
c = 16.0005 (3) Å | T = 100 K |
β = 118.393 (2)° | Block, red |
V = 4714.25 (14) Å3 | 0.19 × 0.11 × 0.09 mm |
Z = 4 |
Bruker SMART APEX2 area detector diffractometer | 8033 independent reflections |
Radiation source: fine-focus sealed tube | 7903 reflections with I > 2σ(I) |
Graphite monochromator | Rint = 0.031 |
0.50° ω and 0.5 ° ϕ scans | θmax = 72.1°, θmin = 3.1° |
Absorption correction: analytical SADABS (Bruker-AXS, 2007) | h = −17→18 |
Tmin = 0.186, Tmax = 0.376 | k = −27→25 |
35920 measured reflections | l = −19→18 |
Refinement on F2 | Secondary atom site location: difference Fourier map |
Least-squares matrix: full | Hydrogen site location: inferred from neighbouring sites |
R[F2 > 2σ(F2)] = 0.032 | H-atom parameters constrained |
wR(F2) = 0.078 | w = 1/[σ2(Fo2) + (0.0581P)2] where P = (Fo2 + 2Fc2)/3 |
S = 1.05 | (Δ/σ)max = 0.001 |
8033 reflections | Δρmax = 0.70 e Å−3 |
599 parameters | Δρmin = −0.66 e Å−3 |
4 restraints | Absolute structure: Flack H D (1983), Acta Cryst. A39, 876-881 |
Primary atom site location: structure-invariant direct methods | Absolute structure parameter: −0.008 (4) |
C44H42Br5Fe3N6NiO4 | V = 4714.25 (14) Å3 |
Mr = 1344.65 | Z = 4 |
Monoclinic, Cc | Cu Kα radiation |
a = 15.2181 (3) Å | µ = 13.07 mm−1 |
b = 22.0080 (3) Å | T = 100 K |
c = 16.0005 (3) Å | 0.19 × 0.11 × 0.09 mm |
β = 118.393 (2)° |
Bruker SMART APEX2 area detector diffractometer | 8033 independent reflections |
Absorption correction: analytical SADABS (Bruker-AXS, 2007) | 7903 reflections with I > 2σ(I) |
Tmin = 0.186, Tmax = 0.376 | Rint = 0.031 |
35920 measured reflections |
R[F2 > 2σ(F2)] = 0.032 | H-atom parameters constrained |
wR(F2) = 0.078 | Δρmax = 0.70 e Å−3 |
S = 1.05 | Δρmin = −0.66 e Å−3 |
8033 reflections | Absolute structure: Flack H D (1983), Acta Cryst. A39, 876-881 |
599 parameters | Absolute structure parameter: −0.008 (4) |
4 restraints |
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) | |
Br1 | 0.29003 (5) | 0.62030 (3) | 0.66511 (4) | 0.02583 (15) | |
Ni1 | 0.20175 (8) | 0.62397 (5) | 0.49182 (7) | 0.01679 (19) | |
Fe1 | −0.07292 (7) | 0.58052 (5) | 0.59258 (7) | 0.0220 (2) | |
Fe2 | 0.58354 (7) | 0.67777 (5) | 0.59805 (8) | 0.0238 (2) | |
O1 | 0.0385 (4) | 0.3437 (2) | 0.4396 (5) | 0.0395 (13) | |
O2 | 0.1836 (4) | 0.3649 (2) | 0.4416 (5) | 0.0402 (14) | |
O3 | 0.2928 (4) | 0.9093 (2) | 0.4472 (4) | 0.0357 (12) | |
O4 | 0.1420 (4) | 0.8748 (2) | 0.4217 (5) | 0.0406 (15) | |
N1 | 0.2374 (4) | 0.5853 (2) | 0.3956 (4) | 0.0207 (11) | |
N2 | 0.1603 (4) | 0.4908 (2) | 0.4768 (4) | 0.0209 (11) | |
N3 | 0.1236 (4) | 0.5445 (2) | 0.4860 (4) | 0.0185 (10) | |
N4 | 0.0732 (4) | 0.6635 (2) | 0.3887 (4) | 0.0186 (10) | |
N5 | 0.2240 (4) | 0.7578 (2) | 0.4837 (4) | 0.0205 (11) | |
N6 | 0.2764 (4) | 0.7055 (2) | 0.4968 (4) | 0.0179 (10) | |
C1 | 0.2373 (5) | 0.6184 (3) | 0.3235 (5) | 0.0261 (15) | |
H1 | 0.2209 | 0.6603 | 0.3187 | 0.031* | |
C2 | 0.2597 (6) | 0.5933 (3) | 0.2586 (5) | 0.0303 (16) | |
H2 | 0.2603 | 0.6180 | 0.2102 | 0.036* | |
C3 | 0.2817 (6) | 0.5323 (3) | 0.2623 (6) | 0.0349 (17) | |
H3 | 0.2986 | 0.5145 | 0.2178 | 0.042* | |
C4 | 0.2784 (5) | 0.4988 (3) | 0.3316 (5) | 0.0273 (15) | |
H4 | 0.2910 | 0.4564 | 0.3348 | 0.033* | |
C5 | 0.2566 (4) | 0.5260 (3) | 0.3987 (4) | 0.0179 (13) | |
C6 | 0.2589 (5) | 0.4895 (3) | 0.4797 (5) | 0.0177 (12) | |
H6A | 0.2774 | 0.4470 | 0.4752 | 0.021* | |
H6B | 0.3102 | 0.5065 | 0.5409 | 0.021* | |
C7 | 0.0952 (5) | 0.4448 (3) | 0.4631 (5) | 0.0224 (14) | |
C8 | 0.1034 (5) | 0.3791 (3) | 0.4476 (5) | 0.0231 (14) | |
C9 | 0.1974 (7) | 0.3010 (3) | 0.4233 (6) | 0.043 (2) | |
H9A | 0.1501 | 0.2747 | 0.4328 | 0.051* | |
H9B | 0.2663 | 0.2876 | 0.4676 | 0.051* | |
C10 | 0.1785 (7) | 0.2960 (4) | 0.3214 (5) | 0.050 (2) | |
H10A | 0.1104 | 0.3097 | 0.2781 | 0.075* | |
H10B | 0.1865 | 0.2537 | 0.3073 | 0.075* | |
H10C | 0.2264 | 0.3216 | 0.3130 | 0.075* | |
C11 | 0.0135 (5) | 0.4709 (3) | 0.4681 (5) | 0.0202 (13) | |
H11 | −0.0444 | 0.4507 | 0.4621 | 0.024* | |
C12 | 0.0353 (5) | 0.5327 (3) | 0.4837 (5) | 0.0212 (13) | |
C13 | −0.0264 (5) | 0.5798 (3) | 0.4929 (5) | 0.0233 (13) | |
C14 | −0.1331 (5) | 0.5782 (4) | 0.4482 (5) | 0.0275 (15) | |
H14 | −0.1749 | 0.5473 | 0.4070 | 0.033* | |
C15 | −0.1652 (6) | 0.6317 (4) | 0.4767 (7) | 0.039 (2) | |
H15 | −0.2324 | 0.6429 | 0.4573 | 0.047* | |
C16 | −0.0794 (6) | 0.6652 (3) | 0.5390 (6) | 0.0344 (18) | |
H16 | −0.0797 | 0.7025 | 0.5686 | 0.041* | |
C17 | 0.0062 (6) | 0.6345 (3) | 0.5501 (6) | 0.0281 (15) | |
H17 | 0.0733 | 0.6473 | 0.5881 | 0.034* | |
C18 | 0.0213 (6) | 0.5606 (4) | 0.7314 (5) | 0.0311 (16) | |
H18 | 0.0876 | 0.5753 | 0.7679 | 0.037* | |
C19 | −0.0077 (6) | 0.5074 (3) | 0.6772 (5) | 0.0339 (16) | |
H19 | 0.0361 | 0.4797 | 0.6699 | 0.041* | |
C20 | −0.1128 (7) | 0.5014 (4) | 0.6349 (5) | 0.0377 (18) | |
H20 | −0.1520 | 0.4690 | 0.5953 | 0.045* | |
C21 | −0.1484 (5) | 0.5529 (4) | 0.6630 (5) | 0.0311 (16) | |
H21 | −0.2165 | 0.5614 | 0.6445 | 0.037* | |
C22 | −0.0685 (7) | 0.5887 (4) | 0.7213 (6) | 0.0380 (18) | |
H22 | −0.0720 | 0.6258 | 0.7501 | 0.046* | |
C23 | 0.0101 (5) | 0.6323 (3) | 0.3113 (5) | 0.0238 (14) | |
H23 | 0.0239 | 0.5906 | 0.3071 | 0.029* | |
C24 | −0.0740 (5) | 0.6576 (3) | 0.2373 (5) | 0.0280 (15) | |
H24 | −0.1152 | 0.6346 | 0.1821 | 0.034* | |
C25 | −0.0966 (5) | 0.7178 (3) | 0.2460 (5) | 0.0267 (14) | |
H25 | −0.1553 | 0.7364 | 0.1979 | 0.032* | |
C26 | −0.0307 (5) | 0.7508 (3) | 0.3276 (5) | 0.0246 (14) | |
H26 | −0.0440 | 0.7921 | 0.3348 | 0.030* | |
C27 | 0.0531 (4) | 0.7224 (3) | 0.3965 (5) | 0.0194 (13) | |
C28 | 0.1286 (5) | 0.7547 (3) | 0.4849 (5) | 0.0223 (13) | |
H28A | 0.1048 | 0.7962 | 0.4872 | 0.027* | |
H28B | 0.1371 | 0.7324 | 0.5421 | 0.027* | |
C29 | 0.2752 (5) | 0.8057 (3) | 0.4748 (5) | 0.0206 (12) | |
C30 | 0.2389 (6) | 0.8699 (3) | 0.4486 (6) | 0.0281 (16) | |
C31 | 0.0928 (8) | 0.9307 (4) | 0.3692 (7) | 0.050 (2) | |
H31A | 0.0206 | 0.9235 | 0.3272 | 0.060* | |
H31B | 0.1232 | 0.9444 | 0.3299 | 0.060* | |
C32 | 0.1084 (10) | 0.9774 (4) | 0.4443 (7) | 0.070 (3) | |
H32A | 0.1017 | 0.9580 | 0.4961 | 0.106* | |
H32B | 0.0582 | 1.0096 | 0.4162 | 0.106* | |
H32C | 0.1753 | 0.9951 | 0.4693 | 0.106* | |
C33 | 0.3627 (5) | 0.7837 (3) | 0.4824 (5) | 0.0241 (13) | |
H33 | 0.4141 | 0.8064 | 0.4792 | 0.029* | |
C34 | 0.3610 (4) | 0.7204 (3) | 0.4961 (5) | 0.0204 (13) | |
C35 | 0.4356 (5) | 0.6761 (3) | 0.5031 (5) | 0.0243 (14) | |
C36 | 0.4924 (5) | 0.6820 (4) | 0.4538 (5) | 0.0306 (16) | |
H36 | 0.4885 | 0.7141 | 0.4124 | 0.037* | |
C37 | 0.5568 (6) | 0.6298 (3) | 0.4792 (6) | 0.0305 (16) | |
H37 | 0.6042 | 0.6215 | 0.4580 | 0.037* | |
C38 | 0.5377 (6) | 0.5926 (3) | 0.5413 (7) | 0.0380 (19) | |
H38 | 0.5695 | 0.5550 | 0.5676 | 0.046* | |
C39 | 0.4625 (6) | 0.6211 (3) | 0.5579 (6) | 0.0309 (16) | |
H39 | 0.4359 | 0.6066 | 0.5971 | 0.037* | |
C40 | 0.6302 (6) | 0.6998 (5) | 0.7369 (6) | 0.044 (2) | |
H40 | 0.5997 | 0.6875 | 0.7739 | 0.053* | |
C41 | 0.6084 (6) | 0.7525 (4) | 0.6815 (6) | 0.041 (2) | |
H41 | 0.5596 | 0.7820 | 0.6742 | 0.050* | |
C42 | 0.6707 (6) | 0.7548 (4) | 0.6383 (6) | 0.0374 (18) | |
H42 | 0.6713 | 0.7860 | 0.5976 | 0.045* | |
C43 | 0.7316 (6) | 0.7029 (4) | 0.6660 (6) | 0.0378 (18) | |
H43 | 0.7804 | 0.6930 | 0.6471 | 0.045* | |
C44 | 0.7076 (6) | 0.6672 (4) | 0.7275 (5) | 0.0386 (19) | |
H44 | 0.7369 | 0.6296 | 0.7564 | 0.046* | |
Br2 | 0.43364 (6) | 0.36557 (4) | 0.47749 (6) | 0.0455 (2) | |
Br3 | 0.49508 (8) | 0.47066 (4) | 0.68743 (8) | 0.0435 (3) | 0.852 (2) |
Br4 | 0.44443 (8) | 0.30422 (4) | 0.70425 (8) | 0.0384 (2) | 0.852 (2) |
Br5 | 0.68356 (7) | 0.35652 (4) | 0.69552 (7) | 0.0371 (2) | 0.852 (2) |
Br3A | 0.4315 (11) | 0.3893 (5) | 0.7007 (12) | 0.102 (4) | 0.148 (2) |
Br4A | 0.6172 (13) | 0.2750 (6) | 0.6963 (15) | 0.125 (6) | 0.148 (2) |
Br5A | 0.6694 (7) | 0.4413 (6) | 0.6917 (9) | 0.102 (4) | 0.148 (2) |
Fe3 | 0.51627 (9) | 0.37325 (6) | 0.64296 (8) | 0.0333 (3) |
U11 | U22 | U33 | U12 | U13 | U23 | |
Br1 | 0.0288 (4) | 0.0276 (3) | 0.0197 (3) | −0.0068 (3) | 0.0105 (3) | −0.0017 (3) |
Ni1 | 0.0160 (5) | 0.0167 (4) | 0.0183 (5) | −0.0022 (4) | 0.0087 (5) | −0.0014 (5) |
Fe1 | 0.0189 (5) | 0.0286 (5) | 0.0214 (6) | 0.0027 (4) | 0.0120 (5) | 0.0019 (4) |
Fe2 | 0.0190 (5) | 0.0317 (5) | 0.0237 (6) | 0.0048 (4) | 0.0125 (5) | 0.0013 (5) |
O1 | 0.037 (3) | 0.029 (3) | 0.060 (4) | −0.010 (2) | 0.029 (3) | −0.006 (2) |
O2 | 0.044 (3) | 0.021 (2) | 0.070 (4) | −0.006 (2) | 0.039 (3) | −0.008 (2) |
O3 | 0.035 (3) | 0.018 (2) | 0.053 (3) | −0.003 (2) | 0.020 (3) | 0.004 (2) |
O4 | 0.034 (3) | 0.026 (2) | 0.063 (4) | 0.012 (2) | 0.024 (3) | 0.024 (3) |
N1 | 0.019 (3) | 0.029 (3) | 0.021 (3) | −0.004 (2) | 0.015 (2) | −0.002 (2) |
N2 | 0.020 (3) | 0.024 (3) | 0.022 (3) | −0.002 (2) | 0.012 (2) | 0.001 (2) |
N3 | 0.024 (3) | 0.011 (2) | 0.025 (3) | −0.0046 (19) | 0.015 (2) | −0.002 (2) |
N4 | 0.020 (3) | 0.018 (2) | 0.019 (3) | −0.003 (2) | 0.011 (2) | −0.001 (2) |
N5 | 0.018 (3) | 0.021 (3) | 0.018 (3) | 0.001 (2) | 0.005 (2) | −0.001 (2) |
N6 | 0.018 (2) | 0.018 (2) | 0.018 (3) | −0.002 (2) | 0.009 (2) | −0.003 (2) |
C1 | 0.030 (4) | 0.020 (3) | 0.035 (4) | −0.004 (3) | 0.020 (3) | −0.005 (3) |
C2 | 0.046 (4) | 0.026 (3) | 0.026 (4) | −0.008 (3) | 0.024 (4) | −0.003 (3) |
C3 | 0.035 (4) | 0.033 (4) | 0.046 (5) | −0.008 (3) | 0.026 (4) | −0.007 (3) |
C4 | 0.032 (4) | 0.026 (3) | 0.032 (4) | −0.002 (3) | 0.022 (3) | −0.009 (3) |
C5 | 0.014 (3) | 0.018 (3) | 0.020 (3) | −0.002 (2) | 0.006 (2) | −0.001 (2) |
C6 | 0.017 (3) | 0.021 (3) | 0.020 (3) | −0.001 (2) | 0.012 (3) | −0.003 (2) |
C7 | 0.023 (3) | 0.028 (3) | 0.015 (3) | −0.004 (2) | 0.008 (3) | 0.002 (3) |
C8 | 0.025 (3) | 0.022 (3) | 0.025 (4) | −0.001 (3) | 0.014 (3) | −0.003 (2) |
C9 | 0.055 (5) | 0.016 (3) | 0.078 (6) | −0.002 (3) | 0.049 (5) | −0.005 (4) |
C10 | 0.057 (5) | 0.040 (5) | 0.060 (6) | −0.010 (4) | 0.034 (5) | −0.014 (4) |
C11 | 0.019 (3) | 0.027 (3) | 0.022 (3) | −0.005 (2) | 0.016 (3) | 0.000 (3) |
C12 | 0.020 (3) | 0.023 (3) | 0.018 (3) | −0.005 (2) | 0.007 (3) | 0.001 (3) |
C13 | 0.030 (3) | 0.033 (3) | 0.016 (3) | 0.000 (3) | 0.018 (3) | 0.004 (3) |
C14 | 0.011 (3) | 0.046 (4) | 0.022 (3) | 0.001 (3) | 0.005 (3) | 0.008 (3) |
C15 | 0.028 (4) | 0.058 (5) | 0.042 (5) | 0.026 (4) | 0.024 (4) | 0.023 (4) |
C16 | 0.046 (5) | 0.030 (4) | 0.033 (4) | 0.006 (3) | 0.023 (4) | −0.001 (3) |
C17 | 0.035 (4) | 0.028 (3) | 0.035 (4) | 0.000 (3) | 0.028 (3) | 0.004 (3) |
C18 | 0.025 (4) | 0.047 (4) | 0.020 (3) | 0.013 (3) | 0.010 (3) | 0.010 (3) |
C19 | 0.039 (4) | 0.038 (4) | 0.025 (4) | 0.014 (3) | 0.016 (3) | 0.015 (3) |
C20 | 0.045 (5) | 0.044 (4) | 0.027 (4) | −0.010 (4) | 0.019 (4) | 0.012 (3) |
C21 | 0.023 (4) | 0.050 (4) | 0.026 (4) | 0.005 (3) | 0.016 (3) | 0.009 (3) |
C22 | 0.044 (5) | 0.048 (4) | 0.027 (4) | 0.010 (4) | 0.021 (4) | −0.001 (3) |
C23 | 0.020 (3) | 0.027 (3) | 0.024 (3) | −0.001 (2) | 0.010 (3) | −0.004 (3) |
C24 | 0.032 (4) | 0.028 (3) | 0.017 (3) | −0.004 (3) | 0.006 (3) | −0.005 (3) |
C25 | 0.019 (3) | 0.035 (4) | 0.021 (3) | 0.004 (3) | 0.005 (3) | 0.008 (3) |
C26 | 0.020 (3) | 0.022 (3) | 0.035 (4) | −0.005 (3) | 0.016 (3) | −0.006 (3) |
C27 | 0.017 (3) | 0.024 (3) | 0.023 (3) | −0.003 (2) | 0.014 (3) | −0.001 (2) |
C28 | 0.021 (3) | 0.014 (3) | 0.033 (4) | −0.001 (2) | 0.014 (3) | −0.008 (3) |
C29 | 0.017 (3) | 0.022 (3) | 0.019 (3) | −0.006 (2) | 0.005 (3) | −0.002 (3) |
C30 | 0.030 (4) | 0.030 (4) | 0.026 (4) | −0.001 (3) | 0.016 (3) | 0.000 (3) |
C31 | 0.048 (5) | 0.041 (4) | 0.066 (6) | 0.017 (4) | 0.031 (5) | 0.015 (4) |
C32 | 0.080 (8) | 0.059 (6) | 0.068 (7) | −0.008 (6) | 0.031 (6) | 0.015 (5) |
C33 | 0.025 (3) | 0.023 (3) | 0.026 (3) | −0.002 (3) | 0.013 (3) | 0.004 (3) |
C34 | 0.013 (3) | 0.024 (3) | 0.023 (3) | −0.001 (2) | 0.008 (2) | −0.004 (2) |
C35 | 0.013 (3) | 0.032 (3) | 0.027 (3) | −0.001 (2) | 0.009 (3) | −0.004 (3) |
C36 | 0.025 (4) | 0.040 (4) | 0.021 (4) | 0.002 (3) | 0.005 (3) | −0.004 (3) |
C37 | 0.031 (4) | 0.042 (4) | 0.025 (4) | −0.006 (3) | 0.019 (3) | −0.010 (3) |
C38 | 0.026 (4) | 0.027 (3) | 0.057 (6) | 0.004 (3) | 0.017 (4) | −0.011 (3) |
C39 | 0.024 (3) | 0.032 (3) | 0.048 (5) | 0.007 (3) | 0.026 (4) | 0.004 (3) |
C40 | 0.029 (4) | 0.071 (6) | 0.030 (4) | 0.007 (4) | 0.013 (3) | 0.000 (4) |
C41 | 0.029 (4) | 0.053 (5) | 0.032 (4) | 0.011 (3) | 0.007 (3) | −0.017 (4) |
C42 | 0.027 (4) | 0.035 (4) | 0.042 (4) | −0.006 (3) | 0.009 (3) | −0.008 (3) |
C43 | 0.017 (4) | 0.056 (5) | 0.030 (4) | −0.003 (3) | 0.003 (3) | −0.002 (4) |
C44 | 0.024 (4) | 0.063 (5) | 0.021 (4) | 0.015 (4) | 0.005 (3) | 0.007 (3) |
Br2 | 0.0361 (5) | 0.0623 (6) | 0.0334 (4) | 0.0137 (4) | 0.0126 (4) | −0.0062 (4) |
Br3 | 0.0405 (5) | 0.0342 (5) | 0.0392 (5) | 0.0055 (4) | 0.0054 (4) | −0.0105 (4) |
Br4 | 0.0439 (5) | 0.0414 (5) | 0.0418 (5) | −0.0085 (4) | 0.0300 (5) | −0.0053 (4) |
Br5 | 0.0197 (4) | 0.0515 (5) | 0.0361 (5) | 0.0053 (4) | 0.0099 (4) | 0.0034 (5) |
Br3A | 0.100 (8) | 0.130 (8) | 0.122 (10) | 0.023 (7) | 0.091 (9) | 0.026 (8) |
Br4A | 0.164 (15) | 0.101 (9) | 0.162 (14) | 0.003 (8) | 0.119 (13) | −0.032 (9) |
Br5A | 0.055 (5) | 0.147 (9) | 0.069 (7) | −0.013 (6) | 0.002 (5) | 0.042 (7) |
Fe3 | 0.0318 (7) | 0.0357 (5) | 0.0283 (6) | 0.0002 (5) | 0.0110 (5) | −0.0022 (5) |
Br1—Ni1 | 2.4407 (10) | C13—C17 | 1.450 (10) |
Ni1—N1 | 2.047 (5) | C14—C15 | 1.431 (11) |
Ni1—N4 | 2.058 (5) | C14—H14 | 0.9500 |
Ni1—N3 | 2.092 (5) | C15—C16 | 1.415 (13) |
Ni1—N6 | 2.105 (5) | C15—H15 | 0.9500 |
Fe1—C17 | 2.026 (7) | C16—C17 | 1.401 (10) |
Fe1—C13 | 2.030 (6) | C16—H16 | 0.9500 |
Fe1—C19 | 2.032 (7) | C17—H17 | 0.9500 |
Fe1—C16 | 2.033 (8) | C18—C19 | 1.398 (11) |
Fe1—C22 | 2.037 (8) | C18—C22 | 1.438 (11) |
Fe1—C18 | 2.038 (7) | C18—H18 | 0.9500 |
Fe1—C14 | 2.042 (7) | C19—C20 | 1.416 (12) |
Fe1—C21 | 2.047 (7) | C19—H19 | 0.9500 |
Fe1—C15 | 2.050 (8) | C20—C21 | 1.420 (12) |
Fe1—C20 | 2.062 (7) | C20—H20 | 0.9500 |
Fe2—C35 | 2.031 (7) | C21—C22 | 1.376 (12) |
Fe2—C41 | 2.038 (8) | C21—H21 | 0.9500 |
Fe2—C37 | 2.040 (7) | C22—H22 | 0.9500 |
Fe2—C40 | 2.042 (9) | C23—C24 | 1.381 (10) |
Fe2—C44 | 2.047 (7) | C23—H23 | 0.9500 |
Fe2—C36 | 2.053 (7) | C24—C25 | 1.394 (10) |
Fe2—C38 | 2.055 (8) | C24—H24 | 0.9500 |
Fe2—C43 | 2.057 (8) | C25—C26 | 1.411 (10) |
Fe2—C39 | 2.058 (7) | C25—H25 | 0.9500 |
Fe2—C42 | 2.058 (8) | C26—C27 | 1.376 (9) |
O1—C8 | 1.217 (9) | C26—H26 | 0.9500 |
O2—C8 | 1.307 (9) | C27—C28 | 1.510 (9) |
O2—C9 | 1.473 (8) | C28—H28A | 0.9900 |
O3—C30 | 1.201 (9) | C28—H28B | 0.9900 |
O4—C30 | 1.330 (9) | C29—C33 | 1.366 (10) |
O4—C31 | 1.475 (9) | C29—C30 | 1.503 (9) |
N1—C5 | 1.331 (8) | C31—C32 | 1.513 (4) |
N1—C1 | 1.363 (9) | C31—H31A | 0.9900 |
N2—N3 | 1.346 (7) | C31—H31B | 0.9900 |
N2—C7 | 1.360 (9) | C32—H32A | 0.9800 |
N2—C6 | 1.480 (8) | C32—H32B | 0.9800 |
N3—C12 | 1.351 (8) | C32—H32C | 0.9800 |
N4—C23 | 1.341 (9) | C33—C34 | 1.413 (9) |
N4—C27 | 1.353 (8) | C33—H33 | 0.9500 |
N5—C29 | 1.356 (8) | C34—C35 | 1.459 (9) |
N5—N6 | 1.358 (7) | C35—C36 | 1.427 (10) |
N5—C28 | 1.464 (8) | C35—C39 | 1.435 (10) |
N6—C34 | 1.335 (8) | C36—C37 | 1.438 (10) |
C1—C2 | 1.356 (10) | C36—H36 | 0.9500 |
C1—H1 | 0.9500 | C37—C38 | 1.420 (12) |
C2—C3 | 1.378 (10) | C37—H37 | 0.9500 |
C2—H2 | 0.9500 | C38—C39 | 1.436 (10) |
C3—C4 | 1.353 (11) | C38—H38 | 0.9500 |
C3—H3 | 0.9500 | C39—H39 | 0.9500 |
C4—C5 | 1.400 (9) | C40—C41 | 1.401 (13) |
C4—H4 | 0.9500 | C40—C44 | 1.445 (12) |
C5—C6 | 1.510 (9) | C40—H40 | 0.9500 |
C6—H6A | 0.9900 | C41—C42 | 1.416 (13) |
C6—H6B | 0.9900 | C41—H41 | 0.9500 |
C7—C11 | 1.405 (10) | C42—C43 | 1.402 (12) |
C7—C8 | 1.482 (9) | C42—H42 | 0.9500 |
C9—C10 | 1.519 (4) | C43—C44 | 1.436 (12) |
C9—H9A | 0.9900 | C43—H43 | 0.9500 |
C9—H9B | 0.9900 | C44—H44 | 0.9500 |
C10—H10A | 0.9800 | Br2—Fe3 | 2.3352 (13) |
C10—H10B | 0.9800 | Br3—Fe3 | 2.3290 (16) |
C10—H10C | 0.9800 | Br4—Fe3 | 2.3419 (16) |
C11—C12 | 1.395 (9) | Br5—Fe3 | 2.2995 (16) |
C11—H11 | 0.9500 | Br3A—Fe3 | 1.943 (10) |
C12—C13 | 1.451 (9) | Br4A—Fe3 | 2.553 (15) |
C13—C14 | 1.430 (9) | Br5A—Fe3 | 2.560 (11) |
N1—Ni1—N4 | 93.66 (19) | Fe1—C14—H14 | 126.4 |
N1—Ni1—N3 | 88.1 (2) | C16—C15—C14 | 108.2 (6) |
N4—Ni1—N3 | 90.8 (2) | C16—C15—Fe1 | 69.1 (5) |
N1—Ni1—N6 | 93.0 (2) | C14—C15—Fe1 | 69.2 (4) |
N4—Ni1—N6 | 87.7 (2) | C16—C15—H15 | 125.9 |
N3—Ni1—N6 | 178.2 (2) | C14—C15—H15 | 125.9 |
N1—Ni1—Br1 | 129.90 (17) | Fe1—C15—H15 | 127.3 |
N4—Ni1—Br1 | 136.43 (16) | C17—C16—C15 | 109.3 (6) |
N3—Ni1—Br1 | 90.97 (16) | C17—C16—Fe1 | 69.5 (4) |
N6—Ni1—Br1 | 89.41 (15) | C15—C16—Fe1 | 70.3 (4) |
C17—Fe1—C13 | 41.9 (3) | C17—C16—H16 | 125.4 |
C17—Fe1—C19 | 120.5 (3) | C15—C16—H16 | 125.4 |
C13—Fe1—C19 | 105.9 (3) | Fe1—C16—H16 | 126.3 |
C17—Fe1—C16 | 40.4 (3) | C16—C17—C13 | 107.6 (7) |
C13—Fe1—C16 | 68.9 (3) | C16—C17—Fe1 | 70.1 (4) |
C19—Fe1—C16 | 156.4 (3) | C13—C17—Fe1 | 69.2 (4) |
C17—Fe1—C22 | 123.3 (4) | C16—C17—H17 | 126.2 |
C13—Fe1—C22 | 159.9 (3) | C13—C17—H17 | 126.2 |
C19—Fe1—C22 | 68.0 (3) | Fe1—C17—H17 | 126.0 |
C16—Fe1—C22 | 108.5 (3) | C19—C18—C22 | 106.8 (7) |
C17—Fe1—C18 | 105.6 (3) | C19—C18—Fe1 | 69.7 (4) |
C13—Fe1—C18 | 121.8 (3) | C22—C18—Fe1 | 69.3 (4) |
C19—Fe1—C18 | 40.2 (3) | C19—C18—H18 | 126.6 |
C16—Fe1—C18 | 121.6 (3) | C22—C18—H18 | 126.6 |
C22—Fe1—C18 | 41.3 (3) | Fe1—C18—H18 | 126.0 |
C17—Fe1—C14 | 69.7 (3) | C18—C19—C20 | 109.1 (7) |
C13—Fe1—C14 | 41.1 (3) | C18—C19—Fe1 | 70.1 (4) |
C19—Fe1—C14 | 123.2 (3) | C20—C19—Fe1 | 70.9 (4) |
C16—Fe1—C14 | 68.9 (3) | C18—C19—H19 | 125.5 |
C22—Fe1—C14 | 158.2 (3) | C20—C19—H19 | 125.5 |
C18—Fe1—C14 | 158.8 (3) | Fe1—C19—H19 | 125.1 |
C17—Fe1—C21 | 159.7 (3) | C19—C20—C21 | 106.8 (7) |
C13—Fe1—C21 | 158.0 (3) | C19—C20—Fe1 | 68.6 (4) |
C19—Fe1—C21 | 67.8 (3) | C21—C20—Fe1 | 69.2 (4) |
C16—Fe1—C21 | 125.2 (3) | C19—C20—H20 | 126.6 |
C22—Fe1—C21 | 39.4 (3) | C21—C20—H20 | 126.6 |
C18—Fe1—C21 | 68.0 (3) | Fe1—C20—H20 | 127.1 |
C14—Fe1—C21 | 123.3 (3) | C22—C21—C20 | 109.0 (7) |
C17—Fe1—C15 | 68.6 (3) | C22—C21—Fe1 | 69.9 (4) |
C13—Fe1—C15 | 68.8 (3) | C20—C21—Fe1 | 70.4 (4) |
C19—Fe1—C15 | 160.9 (4) | C22—C21—H21 | 125.5 |
C16—Fe1—C15 | 40.5 (4) | C20—C21—H21 | 125.5 |
C22—Fe1—C15 | 123.0 (3) | Fe1—C21—H21 | 125.8 |
C18—Fe1—C15 | 158.2 (3) | C21—C22—C18 | 108.5 (7) |
C14—Fe1—C15 | 41.0 (3) | C21—C22—Fe1 | 70.7 (4) |
C21—Fe1—C15 | 109.8 (3) | C18—C22—Fe1 | 69.4 (4) |
C17—Fe1—C20 | 157.0 (3) | C21—C22—H22 | 125.8 |
C13—Fe1—C20 | 121.2 (3) | C18—C22—H22 | 125.8 |
C19—Fe1—C20 | 40.5 (4) | Fe1—C22—H22 | 125.7 |
C16—Fe1—C20 | 161.7 (4) | N4—C23—C24 | 123.3 (6) |
C22—Fe1—C20 | 67.4 (3) | N4—C23—H23 | 118.3 |
C18—Fe1—C20 | 68.0 (3) | C24—C23—H23 | 118.3 |
C14—Fe1—C20 | 107.8 (3) | C23—C24—C25 | 118.1 (6) |
C21—Fe1—C20 | 40.4 (3) | C23—C24—H24 | 121.0 |
C15—Fe1—C20 | 125.4 (4) | C25—C24—H24 | 121.0 |
C35—Fe2—C41 | 107.4 (3) | C24—C25—C26 | 118.8 (6) |
C35—Fe2—C37 | 68.6 (3) | C24—C25—H25 | 120.6 |
C41—Fe2—C37 | 157.2 (3) | C26—C25—H25 | 120.6 |
C35—Fe2—C40 | 120.4 (3) | C27—C26—C25 | 119.2 (6) |
C41—Fe2—C40 | 40.2 (4) | C27—C26—H26 | 120.4 |
C37—Fe2—C40 | 161.5 (4) | C25—C26—H26 | 120.4 |
C35—Fe2—C44 | 156.3 (3) | N4—C27—C26 | 121.7 (6) |
C41—Fe2—C44 | 68.5 (3) | N4—C27—C28 | 115.6 (6) |
C37—Fe2—C44 | 124.3 (3) | C26—C27—C28 | 122.6 (6) |
C40—Fe2—C44 | 41.4 (3) | N5—C28—C27 | 109.1 (5) |
C35—Fe2—C36 | 40.9 (3) | N5—C28—H28A | 109.9 |
C41—Fe2—C36 | 121.0 (3) | C27—C28—H28A | 109.9 |
C37—Fe2—C36 | 41.1 (3) | N5—C28—H28B | 109.9 |
C40—Fe2—C36 | 155.7 (3) | C27—C28—H28B | 109.9 |
C44—Fe2—C36 | 161.4 (3) | H28A—C28—H28B | 108.3 |
C35—Fe2—C38 | 68.3 (3) | N5—C29—C33 | 107.5 (5) |
C41—Fe2—C38 | 160.8 (4) | N5—C29—C30 | 127.3 (6) |
C37—Fe2—C38 | 40.6 (3) | C33—C29—C30 | 124.8 (6) |
C40—Fe2—C38 | 124.5 (4) | O3—C30—O4 | 126.6 (7) |
C44—Fe2—C38 | 107.4 (3) | O3—C30—C29 | 121.4 (6) |
C36—Fe2—C38 | 68.8 (4) | O4—C30—C29 | 111.8 (6) |
C35—Fe2—C43 | 161.0 (3) | O4—C31—C32 | 105.6 (8) |
C41—Fe2—C43 | 67.8 (3) | O4—C31—H31A | 110.6 |
C37—Fe2—C43 | 108.3 (3) | C32—C31—H31A | 110.6 |
C40—Fe2—C43 | 68.6 (3) | O4—C31—H31B | 110.6 |
C44—Fe2—C43 | 40.9 (3) | C32—C31—H31B | 110.6 |
C36—Fe2—C43 | 124.5 (3) | H31A—C31—H31B | 108.7 |
C38—Fe2—C43 | 122.3 (3) | C29—C33—C34 | 105.9 (6) |
C35—Fe2—C39 | 41.1 (3) | C29—C33—H33 | 127.0 |
C41—Fe2—C39 | 123.6 (3) | C34—C33—H33 | 127.0 |
C37—Fe2—C39 | 69.1 (3) | N6—C34—C33 | 109.3 (5) |
C40—Fe2—C39 | 106.3 (4) | N6—C34—C35 | 123.7 (6) |
C44—Fe2—C39 | 120.4 (4) | C33—C34—C35 | 126.9 (6) |
C36—Fe2—C39 | 69.5 (3) | C36—C35—C39 | 110.0 (6) |
C38—Fe2—C39 | 40.9 (3) | C36—C35—C34 | 123.4 (6) |
C43—Fe2—C39 | 157.0 (3) | C39—C35—C34 | 126.6 (6) |
C35—Fe2—C42 | 124.7 (3) | C36—C35—Fe2 | 70.4 (4) |
C41—Fe2—C42 | 40.5 (4) | C39—C35—Fe2 | 70.4 (4) |
C37—Fe2—C42 | 122.1 (3) | C34—C35—Fe2 | 126.2 (5) |
C40—Fe2—C42 | 68.0 (4) | C35—C36—C37 | 106.3 (7) |
C44—Fe2—C42 | 68.2 (3) | C35—C36—Fe2 | 68.7 (4) |
C36—Fe2—C42 | 107.7 (3) | C37—C36—Fe2 | 68.9 (4) |
C38—Fe2—C42 | 157.3 (3) | C35—C36—H36 | 126.8 |
C43—Fe2—C42 | 39.8 (3) | C37—C36—H36 | 126.8 |
C39—Fe2—C42 | 160.9 (3) | Fe2—C36—H36 | 127.0 |
C8—O2—C9 | 118.0 (6) | C38—C37—C36 | 108.7 (6) |
C30—O4—C31 | 115.9 (6) | C38—C37—Fe2 | 70.3 (4) |
C5—N1—C1 | 117.9 (5) | C36—C37—Fe2 | 69.9 (4) |
C5—N1—Ni1 | 120.7 (4) | C38—C37—H37 | 125.6 |
C1—N1—Ni1 | 121.3 (4) | C36—C37—H37 | 125.6 |
N3—N2—C7 | 111.2 (5) | Fe2—C37—H37 | 125.7 |
N3—N2—C6 | 118.8 (5) | C37—C38—C39 | 108.8 (7) |
C7—N2—C6 | 130.0 (6) | C37—C38—Fe2 | 69.1 (4) |
N2—N3—C12 | 106.7 (5) | C39—C38—Fe2 | 69.7 (4) |
N2—N3—Ni1 | 118.8 (4) | C37—C38—H38 | 125.6 |
C12—N3—Ni1 | 134.3 (4) | C39—C38—H38 | 125.6 |
C23—N4—C27 | 118.9 (6) | Fe2—C38—H38 | 127.2 |
C23—N4—Ni1 | 120.9 (4) | C35—C39—C38 | 106.1 (7) |
C27—N4—Ni1 | 120.1 (4) | C35—C39—Fe2 | 68.5 (4) |
C29—N5—N6 | 110.5 (5) | C38—C39—Fe2 | 69.5 (4) |
C29—N5—C28 | 131.4 (5) | C35—C39—H39 | 127.0 |
N6—N5—C28 | 118.1 (5) | C38—C39—H39 | 127.0 |
C34—N6—N5 | 106.8 (5) | Fe2—C39—H39 | 126.7 |
C34—N6—Ni1 | 135.6 (4) | C41—C40—C44 | 107.8 (8) |
N5—N6—Ni1 | 116.8 (4) | C41—C40—Fe2 | 69.7 (5) |
C2—C1—N1 | 122.1 (6) | C44—C40—Fe2 | 69.5 (5) |
C2—C1—H1 | 119.0 | C41—C40—H40 | 126.1 |
N1—C1—H1 | 119.0 | C44—C40—H40 | 126.1 |
C1—C2—C3 | 120.5 (7) | Fe2—C40—H40 | 126.2 |
C1—C2—H2 | 119.7 | C40—C41—C42 | 108.9 (7) |
C3—C2—H2 | 119.7 | C40—C41—Fe2 | 70.1 (5) |
C4—C3—C2 | 117.6 (7) | C42—C41—Fe2 | 70.5 (4) |
C4—C3—H3 | 121.2 | C40—C41—H41 | 125.5 |
C2—C3—H3 | 121.2 | C42—C41—H41 | 125.5 |
C3—C4—C5 | 120.7 (6) | Fe2—C41—H41 | 125.4 |
C3—C4—H4 | 119.7 | C43—C42—C41 | 108.2 (8) |
C5—C4—H4 | 119.7 | C43—C42—Fe2 | 70.1 (4) |
N1—C5—C4 | 121.1 (6) | C41—C42—Fe2 | 69.0 (5) |
N1—C5—C6 | 118.0 (6) | C43—C42—H42 | 125.9 |
C4—C5—C6 | 120.8 (5) | C41—C42—H42 | 125.9 |
N2—C6—C5 | 110.7 (5) | Fe2—C42—H42 | 126.6 |
N2—C6—H6A | 109.5 | C42—C43—C44 | 108.5 (8) |
C5—C6—H6A | 109.5 | C42—C43—Fe2 | 70.1 (4) |
N2—C6—H6B | 109.5 | C44—C43—Fe2 | 69.1 (4) |
C5—C6—H6B | 109.5 | C42—C43—H43 | 125.8 |
H6A—C6—H6B | 108.1 | C44—C43—H43 | 125.8 |
N2—C7—C11 | 106.5 (6) | Fe2—C43—H43 | 126.6 |
N2—C7—C8 | 129.7 (6) | C43—C44—C40 | 106.6 (7) |
C11—C7—C8 | 123.8 (6) | C43—C44—Fe2 | 69.9 (4) |
O1—C8—O2 | 125.4 (6) | C40—C44—Fe2 | 69.1 (5) |
O1—C8—C7 | 120.9 (6) | C43—C44—H44 | 126.7 |
O2—C8—C7 | 113.7 (6) | C40—C44—H44 | 126.7 |
O2—C9—C10 | 108.0 (6) | Fe2—C44—H44 | 125.8 |
O2—C9—H9A | 110.1 | Br3A—Fe3—Br5 | 136.5 (5) |
C10—C9—H9A | 110.1 | Br3A—Fe3—Br3 | 57.9 (4) |
O2—C9—H9B | 110.1 | Br5—Fe3—Br3 | 109.01 (6) |
C10—C9—H9B | 110.1 | Br3A—Fe3—Br2 | 115.5 (5) |
H9A—C9—H9B | 108.4 | Br5—Fe3—Br2 | 107.98 (6) |
C12—C11—C7 | 105.5 (6) | Br3—Fe3—Br2 | 109.57 (6) |
C12—C11—H11 | 127.2 | Br3A—Fe3—Br4 | 51.0 (3) |
C7—C11—H11 | 127.2 | Br5—Fe3—Br4 | 113.52 (7) |
N3—C12—C11 | 109.9 (6) | Br3—Fe3—Br4 | 108.00 (7) |
N3—C12—C13 | 122.9 (6) | Br2—Fe3—Br4 | 108.71 (6) |
C11—C12—C13 | 127.1 (6) | Br3A—Fe3—Br4A | 115.1 (5) |
C14—C13—C17 | 107.6 (6) | Br5—Fe3—Br4A | 49.9 (3) |
C14—C13—C12 | 124.5 (7) | Br3—Fe3—Br4A | 145.7 (4) |
C17—C13—C12 | 127.8 (6) | Br2—Fe3—Br4A | 103.4 (4) |
C14—C13—Fe1 | 69.9 (4) | Br4—Fe3—Br4A | 68.7 (3) |
C17—C13—Fe1 | 68.9 (4) | Br3A—Fe3—Br5A | 117.6 (6) |
C12—C13—Fe1 | 124.7 (5) | Br5—Fe3—Br5A | 45.0 (3) |
C13—C14—C15 | 107.4 (7) | Br3—Fe3—Br5A | 66.9 (3) |
C13—C14—Fe1 | 69.0 (4) | Br2—Fe3—Br5A | 108.0 (3) |
C15—C14—Fe1 | 69.8 (5) | Br4—Fe3—Br5A | 142.2 (3) |
C13—C14—H14 | 126.3 | Br4A—Fe3—Br5A | 94.5 (4) |
C15—C14—H14 | 126.3 | ||
N4—Ni1—N1—C5 | −127.2 (5) | Fe1—C18—C22—C21 | 60.2 (6) |
N3—Ni1—N1—C5 | −36.5 (5) | C19—C18—C22—Fe1 | −59.9 (5) |
N6—Ni1—N1—C5 | 144.9 (5) | C17—Fe1—C22—C21 | 165.6 (4) |
Br1—Ni1—N1—C5 | 53.2 (5) | C13—Fe1—C22—C21 | −157.4 (8) |
N4—Ni1—N1—C1 | 49.3 (6) | C19—Fe1—C22—C21 | −81.4 (5) |
N3—Ni1—N1—C1 | 140.0 (5) | C16—Fe1—C22—C21 | 123.4 (5) |
N6—Ni1—N1—C1 | −38.6 (5) | C18—Fe1—C22—C21 | −119.3 (7) |
Br1—Ni1—N1—C1 | −130.3 (5) | C14—Fe1—C22—C21 | 44.2 (11) |
C7—N2—N3—C12 | 3.5 (8) | C15—Fe1—C22—C21 | 81.0 (6) |
C6—N2—N3—C12 | −178.3 (6) | C20—Fe1—C22—C21 | −37.5 (5) |
C7—N2—N3—Ni1 | −172.9 (4) | C17—Fe1—C22—C18 | −75.1 (6) |
C6—N2—N3—Ni1 | 5.3 (8) | C13—Fe1—C22—C18 | −38.1 (11) |
N1—Ni1—N3—N2 | 36.3 (5) | C19—Fe1—C22—C18 | 37.9 (5) |
N4—Ni1—N3—N2 | 130.0 (5) | C16—Fe1—C22—C18 | −117.2 (5) |
Br1—Ni1—N3—N2 | −93.5 (5) | C14—Fe1—C22—C18 | 163.5 (8) |
N1—Ni1—N3—C12 | −138.8 (7) | C21—Fe1—C22—C18 | 119.3 (7) |
N4—Ni1—N3—C12 | −45.1 (7) | C15—Fe1—C22—C18 | −159.6 (5) |
Br1—Ni1—N3—C12 | 91.3 (7) | C20—Fe1—C22—C18 | 81.8 (5) |
N1—Ni1—N4—C23 | 44.4 (5) | C27—N4—C23—C24 | 1.5 (10) |
N3—Ni1—N4—C23 | −43.8 (5) | Ni1—N4—C23—C24 | −176.0 (5) |
N6—Ni1—N4—C23 | 137.2 (5) | N4—C23—C24—C25 | −3.2 (11) |
Br1—Ni1—N4—C23 | −136.1 (4) | C23—C24—C25—C26 | 2.7 (11) |
N1—Ni1—N4—C27 | −133.1 (5) | C24—C25—C26—C27 | −0.8 (10) |
N3—Ni1—N4—C27 | 138.7 (5) | C23—N4—C27—C26 | 0.6 (9) |
N6—Ni1—N4—C27 | −40.2 (5) | Ni1—N4—C27—C26 | 178.1 (5) |
Br1—Ni1—N4—C27 | 46.5 (6) | C23—N4—C27—C28 | −179.0 (6) |
C29—N5—N6—C34 | 0.0 (7) | Ni1—N4—C27—C28 | −1.5 (7) |
C28—N5—N6—C34 | −177.9 (6) | C25—C26—C27—N4 | −0.9 (10) |
C29—N5—N6—Ni1 | −171.1 (4) | C25—C26—C27—C28 | 178.7 (6) |
C28—N5—N6—Ni1 | 11.0 (7) | C29—N5—C28—C27 | 112.3 (7) |
N1—Ni1—N6—C34 | −38.9 (7) | N6—N5—C28—C27 | −70.4 (7) |
N4—Ni1—N6—C34 | −132.4 (7) | N4—C27—C28—N5 | 64.4 (7) |
Br1—Ni1—N6—C34 | 91.0 (7) | C26—C27—C28—N5 | −115.2 (6) |
N1—Ni1—N6—N5 | 128.9 (4) | N6—N5—C29—C33 | −0.1 (8) |
N4—Ni1—N6—N5 | 35.3 (5) | C28—N5—C29—C33 | 177.4 (7) |
Br1—Ni1—N6—N5 | −101.2 (4) | N6—N5—C29—C30 | 172.4 (6) |
C5—N1—C1—C2 | −2.7 (10) | C28—N5—C29—C30 | −10.1 (12) |
Ni1—N1—C1—C2 | −179.3 (6) | C31—O4—C30—O3 | 11.9 (12) |
N1—C1—C2—C3 | 1.4 (11) | C31—O4—C30—C29 | −163.2 (7) |
C1—C2—C3—C4 | 1.0 (11) | N5—C29—C30—O3 | 176.4 (7) |
C2—C3—C4—C5 | −2.1 (11) | C33—C29—C30—O3 | −12.3 (12) |
C1—N1—C5—C4 | 1.6 (9) | N5—C29—C30—O4 | −8.2 (10) |
Ni1—N1—C5—C4 | 178.2 (5) | C33—C29—C30—O4 | 163.1 (7) |
C1—N1—C5—C6 | 178.7 (6) | C30—O4—C31—C32 | −86.7 (9) |
Ni1—N1—C5—C6 | −4.6 (7) | N5—C29—C33—C34 | 0.1 (8) |
C3—C4—C5—N1 | 0.8 (10) | C30—C29—C33—C34 | −172.6 (6) |
C3—C4—C5—C6 | −176.3 (7) | N5—N6—C34—C33 | 0.1 (8) |
N3—N2—C6—C5 | −62.0 (8) | Ni1—N6—C34—C33 | 168.7 (5) |
C7—N2—C6—C5 | 115.9 (7) | N5—N6—C34—C35 | −176.7 (6) |
N1—C5—C6—N2 | 62.2 (7) | Ni1—N6—C34—C35 | −8.0 (11) |
C4—C5—C6—N2 | −120.7 (6) | C29—C33—C34—N6 | −0.1 (8) |
N3—N2—C7—C11 | −2.6 (8) | C29—C33—C34—C35 | 176.5 (6) |
C6—N2—C7—C11 | 179.4 (6) | N6—C34—C35—C36 | 144.1 (7) |
N3—N2—C7—C8 | 178.5 (6) | C33—C34—C35—C36 | −32.0 (11) |
C6—N2—C7—C8 | 0.5 (12) | N6—C34—C35—C39 | −35.3 (11) |
C9—O2—C8—O1 | 0.2 (12) | C33—C34—C35—C39 | 148.5 (8) |
C9—O2—C8—C7 | −178.2 (6) | N6—C34—C35—Fe2 | −126.8 (6) |
N2—C7—C8—O1 | 177.5 (7) | C33—C34—C35—Fe2 | 57.0 (10) |
C11—C7—C8—O1 | −1.2 (11) | C41—Fe2—C35—C36 | 117.6 (5) |
N2—C7—C8—O2 | −3.9 (11) | C37—Fe2—C35—C36 | −38.5 (4) |
C11—C7—C8—O2 | 177.4 (7) | C40—Fe2—C35—C36 | 159.5 (5) |
C8—O2—C9—C10 | 106.9 (8) | C44—Fe2—C35—C36 | −166.3 (8) |
N2—C7—C11—C12 | 0.8 (8) | C38—Fe2—C35—C36 | −82.3 (5) |
C8—C7—C11—C12 | 179.7 (6) | C43—Fe2—C35—C36 | 45.6 (11) |
N2—N3—C12—C11 | −2.9 (8) | C39—Fe2—C35—C36 | −120.8 (6) |
Ni1—N3—C12—C11 | 172.6 (5) | C42—Fe2—C35—C36 | 76.5 (5) |
N2—N3—C12—C13 | 179.2 (6) | C41—Fe2—C35—C39 | −121.5 (5) |
Ni1—N3—C12—C13 | −5.3 (11) | C37—Fe2—C35—C39 | 82.3 (4) |
C7—C11—C12—N3 | 1.3 (8) | C40—Fe2—C35—C39 | −79.7 (5) |
C7—C11—C12—C13 | 179.1 (6) | C44—Fe2—C35—C39 | −45.5 (9) |
N3—C12—C13—C14 | 148.3 (7) | C36—Fe2—C35—C39 | 120.8 (6) |
C11—C12—C13—C14 | −29.3 (11) | C38—Fe2—C35—C39 | 38.5 (5) |
N3—C12—C13—C17 | −34.5 (10) | C43—Fe2—C35—C39 | 166.4 (9) |
C11—C12—C13—C17 | 148.0 (7) | C42—Fe2—C35—C39 | −162.7 (5) |
N3—C12—C13—Fe1 | −123.5 (7) | C41—Fe2—C35—C34 | 0.0 (7) |
C11—C12—C13—Fe1 | 59.0 (9) | C37—Fe2—C35—C34 | −156.1 (7) |
C17—Fe1—C13—C14 | −119.1 (6) | C40—Fe2—C35—C34 | 41.9 (8) |
C19—Fe1—C13—C14 | 122.6 (5) | C44—Fe2—C35—C34 | 76.1 (10) |
C16—Fe1—C13—C14 | −81.6 (5) | C36—Fe2—C35—C34 | −117.6 (8) |
C22—Fe1—C13—C14 | −168.0 (9) | C38—Fe2—C35—C34 | 160.1 (7) |
C18—Fe1—C13—C14 | 163.4 (5) | C43—Fe2—C35—C34 | −72.0 (12) |
C21—Fe1—C13—C14 | 52.5 (9) | C39—Fe2—C35—C34 | 121.6 (8) |
C15—Fe1—C13—C14 | −38.0 (5) | C42—Fe2—C35—C34 | −41.1 (7) |
C20—Fe1—C13—C14 | 81.4 (5) | C39—C35—C36—C37 | −0.5 (8) |
C19—Fe1—C13—C17 | −118.2 (5) | C34—C35—C36—C37 | 180.0 (6) |
C16—Fe1—C13—C17 | 37.5 (4) | Fe2—C35—C36—C37 | 58.9 (5) |
C22—Fe1—C13—C17 | −48.9 (11) | C39—C35—C36—Fe2 | −59.5 (5) |
C18—Fe1—C13—C17 | −77.5 (5) | C34—C35—C36—Fe2 | 121.0 (6) |
C14—Fe1—C13—C17 | 119.1 (6) | C41—Fe2—C36—C35 | −80.7 (5) |
C21—Fe1—C13—C17 | 171.6 (7) | C37—Fe2—C36—C35 | 118.2 (6) |
C15—Fe1—C13—C17 | 81.1 (5) | C40—Fe2—C36—C35 | −47.3 (10) |
C20—Fe1—C13—C17 | −159.5 (5) | C44—Fe2—C36—C35 | 162.7 (10) |
C17—Fe1—C13—C12 | 122.1 (8) | C38—Fe2—C36—C35 | 80.9 (5) |
C19—Fe1—C13—C12 | 3.9 (7) | C43—Fe2—C36—C35 | −163.6 (4) |
C16—Fe1—C13—C12 | 159.6 (7) | C39—Fe2—C36—C35 | 37.0 (4) |
C22—Fe1—C13—C12 | 73.3 (11) | C42—Fe2—C36—C35 | −122.9 (4) |
C18—Fe1—C13—C12 | 44.6 (7) | C35—Fe2—C36—C37 | −118.2 (6) |
C14—Fe1—C13—C12 | −118.7 (8) | C41—Fe2—C36—C37 | 161.1 (4) |
C21—Fe1—C13—C12 | −66.2 (10) | C40—Fe2—C36—C37 | −165.5 (8) |
C15—Fe1—C13—C12 | −156.8 (7) | C44—Fe2—C36—C37 | 44.4 (13) |
C20—Fe1—C13—C12 | −37.3 (7) | C38—Fe2—C36—C37 | −37.3 (4) |
C17—C13—C14—C15 | 0.8 (8) | C43—Fe2—C36—C37 | 78.1 (5) |
C12—C13—C14—C15 | 178.5 (6) | C39—Fe2—C36—C37 | −81.2 (4) |
Fe1—C13—C14—C15 | 59.5 (5) | C42—Fe2—C36—C37 | 118.8 (5) |
C17—C13—C14—Fe1 | −58.8 (5) | C35—C36—C37—C38 | 1.0 (8) |
C12—C13—C14—Fe1 | 119.0 (6) | Fe2—C36—C37—C38 | 59.8 (6) |
C17—Fe1—C14—C13 | 38.5 (4) | C35—C36—C37—Fe2 | −58.8 (5) |
C19—Fe1—C14—C13 | −75.4 (5) | C35—Fe2—C37—C38 | −81.3 (5) |
C16—Fe1—C14—C13 | 81.7 (5) | C41—Fe2—C37—C38 | −165.2 (7) |
C22—Fe1—C14—C13 | 168.9 (8) | C40—Fe2—C37—C38 | 41.5 (12) |
C18—Fe1—C14—C13 | −42.4 (11) | C44—Fe2—C37—C38 | 76.1 (5) |
C21—Fe1—C14—C13 | −159.2 (4) | C36—Fe2—C37—C38 | −119.6 (6) |
C15—Fe1—C14—C13 | 118.8 (6) | C43—Fe2—C37—C38 | 118.6 (5) |
C20—Fe1—C14—C13 | −117.3 (5) | C39—Fe2—C37—C38 | −37.1 (4) |
C17—Fe1—C14—C15 | −80.3 (5) | C42—Fe2—C37—C38 | 160.3 (4) |
C13—Fe1—C14—C15 | −118.8 (6) | C35—Fe2—C37—C36 | 38.3 (4) |
C19—Fe1—C14—C15 | 165.8 (5) | C41—Fe2—C37—C36 | −45.7 (10) |
C16—Fe1—C14—C15 | −37.0 (5) | C40—Fe2—C37—C36 | 161.0 (10) |
C22—Fe1—C14—C15 | 50.1 (11) | C44—Fe2—C37—C36 | −164.3 (5) |
C18—Fe1—C14—C15 | −161.1 (8) | C38—Fe2—C37—C36 | 119.6 (6) |
C21—Fe1—C14—C15 | 82.0 (5) | C43—Fe2—C37—C36 | −121.8 (5) |
C20—Fe1—C14—C15 | 123.9 (5) | C39—Fe2—C37—C36 | 82.5 (5) |
C13—C14—C15—C16 | −0.7 (9) | C42—Fe2—C37—C36 | −80.1 (5) |
Fe1—C14—C15—C16 | 58.3 (6) | C36—C37—C38—C39 | −1.1 (9) |
C13—C14—C15—Fe1 | −59.0 (5) | Fe2—C37—C38—C39 | 58.5 (6) |
C17—Fe1—C15—C16 | −36.8 (4) | C36—C37—C38—Fe2 | −59.6 (5) |
C13—Fe1—C15—C16 | −82.0 (5) | C35—Fe2—C38—C37 | 81.9 (5) |
C19—Fe1—C15—C16 | −159.2 (9) | C41—Fe2—C38—C37 | 162.5 (9) |
C22—Fe1—C15—C16 | 79.7 (6) | C40—Fe2—C38—C37 | −165.2 (5) |
C18—Fe1—C15—C16 | 41.5 (10) | C44—Fe2—C38—C37 | −122.8 (5) |
C14—Fe1—C15—C16 | −120.2 (6) | C36—Fe2—C38—C37 | 37.8 (4) |
C21—Fe1—C15—C16 | 121.5 (5) | C43—Fe2—C38—C37 | −80.4 (5) |
C20—Fe1—C15—C16 | 164.0 (5) | C39—Fe2—C38—C37 | 120.7 (7) |
C17—Fe1—C15—C14 | 83.3 (5) | C42—Fe2—C38—C37 | −47.6 (11) |
C13—Fe1—C15—C14 | 38.2 (4) | C35—Fe2—C38—C39 | −38.7 (5) |
C19—Fe1—C15—C14 | −39.1 (12) | C41—Fe2—C38—C39 | 41.9 (12) |
C16—Fe1—C15—C14 | 120.2 (6) | C37—Fe2—C38—C39 | −120.7 (7) |
C22—Fe1—C15—C14 | −160.1 (5) | C40—Fe2—C38—C39 | 74.1 (6) |
C18—Fe1—C15—C14 | 161.7 (8) | C44—Fe2—C38—C39 | 116.5 (5) |
C21—Fe1—C15—C14 | −118.4 (5) | C36—Fe2—C38—C39 | −82.8 (5) |
C20—Fe1—C15—C14 | −75.8 (5) | C43—Fe2—C38—C39 | 158.9 (5) |
C14—C15—C16—C17 | 0.5 (9) | C42—Fe2—C38—C39 | −168.3 (8) |
Fe1—C15—C16—C17 | 58.8 (5) | C36—C35—C39—C38 | −0.1 (9) |
C14—C15—C16—Fe1 | −58.3 (5) | C34—C35—C39—C38 | 179.3 (7) |
C13—Fe1—C16—C17 | −38.9 (5) | Fe2—C35—C39—C38 | −59.6 (5) |
C19—Fe1—C16—C17 | 42.7 (10) | C36—C35—C39—Fe2 | 59.4 (5) |
C22—Fe1—C16—C17 | 120.0 (5) | C34—C35—C39—Fe2 | −121.1 (7) |
C18—Fe1—C16—C17 | 76.4 (5) | C37—C38—C39—C35 | 0.8 (9) |
C14—Fe1—C16—C17 | −83.1 (5) | Fe2—C38—C39—C35 | 58.9 (5) |
C21—Fe1—C16—C17 | 160.4 (5) | C37—C38—C39—Fe2 | −58.1 (6) |
C15—Fe1—C16—C17 | −120.5 (7) | C41—Fe2—C39—C35 | 77.5 (5) |
C20—Fe1—C16—C17 | −166.1 (9) | C37—Fe2—C39—C35 | −81.0 (5) |
C17—Fe1—C16—C15 | 120.5 (7) | C40—Fe2—C39—C35 | 117.9 (5) |
C13—Fe1—C16—C15 | 81.6 (5) | C44—Fe2—C39—C35 | 160.6 (4) |
C19—Fe1—C16—C15 | 163.2 (7) | C36—Fe2—C39—C35 | −36.9 (4) |
C22—Fe1—C16—C15 | −119.6 (5) | C38—Fe2—C39—C35 | −117.8 (7) |
C18—Fe1—C16—C15 | −163.2 (4) | C43—Fe2—C39—C35 | −168.7 (8) |
C14—Fe1—C16—C15 | 37.4 (4) | C42—Fe2—C39—C35 | 48.4 (12) |
C21—Fe1—C16—C15 | −79.2 (5) | C35—Fe2—C39—C38 | 117.8 (7) |
C20—Fe1—C16—C15 | −45.7 (12) | C41—Fe2—C39—C38 | −164.7 (5) |
C15—C16—C17—C13 | 0.0 (8) | C37—Fe2—C39—C38 | 36.8 (5) |
Fe1—C16—C17—C13 | 59.3 (5) | C40—Fe2—C39—C38 | −124.3 (5) |
C15—C16—C17—Fe1 | −59.3 (6) | C44—Fe2—C39—C38 | −81.6 (6) |
C14—C13—C17—C16 | −0.5 (8) | C36—Fe2—C39—C38 | 80.9 (6) |
C12—C13—C17—C16 | −178.1 (6) | C43—Fe2—C39—C38 | −51.0 (11) |
Fe1—C13—C17—C16 | −59.9 (5) | C42—Fe2—C39—C38 | 166.1 (10) |
C14—C13—C17—Fe1 | 59.4 (5) | C35—Fe2—C40—C41 | −80.9 (6) |
C12—C13—C17—Fe1 | −118.3 (7) | C37—Fe2—C40—C41 | 164.3 (9) |
C13—Fe1—C17—C16 | 118.7 (7) | C44—Fe2—C40—C41 | 119.1 (7) |
C19—Fe1—C17—C16 | −161.7 (5) | C36—Fe2—C40—C41 | −47.0 (11) |
C22—Fe1—C17—C16 | −79.3 (6) | C38—Fe2—C40—C41 | −164.2 (5) |
C18—Fe1—C17—C16 | −120.8 (5) | C43—Fe2—C40—C41 | 80.5 (5) |
C14—Fe1—C17—C16 | 81.0 (5) | C39—Fe2—C40—C41 | −123.2 (5) |
C21—Fe1—C17—C16 | −52.3 (11) | C42—Fe2—C40—C41 | 37.5 (5) |
C15—Fe1—C17—C16 | 37.0 (5) | C35—Fe2—C40—C44 | 160.0 (5) |
C20—Fe1—C17—C16 | 168.9 (8) | C41—Fe2—C40—C44 | −119.1 (7) |
C19—Fe1—C17—C13 | 79.6 (5) | C37—Fe2—C40—C44 | 45.2 (13) |
C16—Fe1—C17—C13 | −118.7 (7) | C36—Fe2—C40—C44 | −166.1 (8) |
C22—Fe1—C17—C13 | 162.0 (4) | C38—Fe2—C40—C44 | 76.7 (6) |
C18—Fe1—C17—C13 | 120.5 (4) | C43—Fe2—C40—C44 | −38.6 (5) |
C14—Fe1—C17—C13 | −37.8 (4) | C39—Fe2—C40—C44 | 117.7 (5) |
C21—Fe1—C17—C13 | −171.0 (8) | C42—Fe2—C40—C44 | −81.6 (6) |
C15—Fe1—C17—C13 | −81.7 (5) | C44—C40—C41—C42 | −0.8 (9) |
C20—Fe1—C17—C13 | 50.2 (10) | Fe2—C40—C41—C42 | −60.0 (5) |
C17—Fe1—C18—C19 | −119.1 (5) | C44—C40—C41—Fe2 | 59.3 (6) |
C13—Fe1—C18—C19 | −76.5 (6) | C35—Fe2—C41—C40 | 116.9 (5) |
C16—Fe1—C18—C19 | −159.9 (5) | C37—Fe2—C41—C40 | −167.2 (7) |
C22—Fe1—C18—C19 | 117.9 (7) | C44—Fe2—C41—C40 | −38.4 (5) |
C14—Fe1—C18—C19 | −45.1 (11) | C36—Fe2—C41—C40 | 159.5 (5) |
C21—Fe1—C18—C19 | 81.3 (5) | C38—Fe2—C41—C40 | 43.0 (12) |
C15—Fe1—C18—C19 | 169.7 (8) | C43—Fe2—C41—C40 | −82.7 (5) |
C20—Fe1—C18—C19 | 37.5 (5) | C39—Fe2—C41—C40 | 74.6 (6) |
C17—Fe1—C18—C22 | 123.0 (5) | C42—Fe2—C41—C40 | −119.6 (7) |
C13—Fe1—C18—C22 | 165.6 (5) | C35—Fe2—C41—C42 | −123.5 (5) |
C19—Fe1—C18—C22 | −117.9 (7) | C37—Fe2—C41—C42 | −47.6 (10) |
C16—Fe1—C18—C22 | 82.1 (6) | C40—Fe2—C41—C42 | 119.6 (7) |
C14—Fe1—C18—C22 | −163.0 (8) | C44—Fe2—C41—C42 | 81.2 (5) |
C21—Fe1—C18—C22 | −36.6 (5) | C36—Fe2—C41—C42 | −80.9 (5) |
C15—Fe1—C18—C22 | 51.7 (11) | C38—Fe2—C41—C42 | 162.6 (9) |
C20—Fe1—C18—C22 | −80.4 (5) | C43—Fe2—C41—C42 | 37.0 (5) |
C22—C18—C19—C20 | −0.8 (8) | C39—Fe2—C41—C42 | −165.8 (5) |
Fe1—C18—C19—C20 | −60.5 (5) | C40—C41—C42—C43 | 0.5 (9) |
C22—C18—C19—Fe1 | 59.7 (5) | Fe2—C41—C42—C43 | −59.3 (5) |
C17—Fe1—C19—C18 | 77.7 (5) | C40—C41—C42—Fe2 | 59.8 (6) |
C13—Fe1—C19—C18 | 120.8 (5) | C35—Fe2—C42—C43 | −164.9 (5) |
C16—Fe1—C19—C18 | 47.0 (10) | C41—Fe2—C42—C43 | 119.7 (7) |
C22—Fe1—C19—C18 | −39.0 (5) | C37—Fe2—C42—C43 | −80.1 (6) |
C14—Fe1—C19—C18 | 162.2 (4) | C40—Fe2—C42—C43 | 82.5 (6) |
C21—Fe1—C19—C18 | −81.6 (5) | C44—Fe2—C42—C43 | 37.7 (5) |
C15—Fe1—C19—C18 | −168.2 (9) | C36—Fe2—C42—C43 | −123.0 (5) |
C20—Fe1—C19—C18 | −119.5 (7) | C38—Fe2—C42—C43 | −45.5 (12) |
C17—Fe1—C19—C20 | −162.8 (5) | C39—Fe2—C42—C43 | 158.4 (10) |
C13—Fe1—C19—C20 | −119.7 (5) | C35—Fe2—C42—C41 | 75.4 (5) |
C16—Fe1—C19—C20 | 166.5 (7) | C37—Fe2—C42—C41 | 160.2 (5) |
C22—Fe1—C19—C20 | 80.5 (5) | C40—Fe2—C42—C41 | −37.2 (5) |
C18—Fe1—C19—C20 | 119.5 (7) | C44—Fe2—C42—C41 | −82.0 (5) |
C14—Fe1—C19—C20 | −78.3 (5) | C36—Fe2—C42—C41 | 117.3 (5) |
C21—Fe1—C19—C20 | 37.9 (5) | C38—Fe2—C42—C41 | −165.2 (9) |
C15—Fe1—C19—C20 | −48.7 (12) | C43—Fe2—C42—C41 | −119.7 (7) |
C18—C19—C20—C21 | 1.1 (8) | C39—Fe2—C42—C41 | 38.7 (12) |
Fe1—C19—C20—C21 | −58.9 (5) | C41—C42—C43—C44 | 0.0 (9) |
C18—C19—C20—Fe1 | 60.0 (5) | Fe2—C42—C43—C44 | −58.6 (6) |
C17—Fe1—C20—C19 | 40.7 (10) | C41—C42—C43—Fe2 | 58.7 (5) |
C13—Fe1—C20—C19 | 77.5 (5) | C35—Fe2—C43—C42 | 41.2 (12) |
C16—Fe1—C20—C19 | −162.7 (9) | C41—Fe2—C43—C42 | −37.5 (5) |
C22—Fe1—C20—C19 | −82.1 (5) | C37—Fe2—C43—C42 | 118.5 (5) |
C18—Fe1—C20—C19 | −37.3 (4) | C40—Fe2—C43—C42 | −80.9 (6) |
C14—Fe1—C20—C19 | 120.6 (5) | C44—Fe2—C43—C42 | −119.9 (8) |
C21—Fe1—C20—C19 | −118.7 (6) | C36—Fe2—C43—C42 | 75.8 (6) |
C15—Fe1—C20—C19 | 162.5 (5) | C38—Fe2—C43—C42 | 161.0 (5) |
C17—Fe1—C20—C21 | 159.4 (8) | C39—Fe2—C43—C42 | −162.0 (8) |
C13—Fe1—C20—C21 | −163.8 (4) | C35—Fe2—C43—C44 | 161.1 (8) |
C19—Fe1—C20—C21 | 118.7 (6) | C41—Fe2—C43—C44 | 82.4 (6) |
C16—Fe1—C20—C21 | −44.1 (12) | C37—Fe2—C43—C44 | −121.6 (5) |
C22—Fe1—C20—C21 | 36.6 (5) | C40—Fe2—C43—C44 | 39.0 (5) |
C18—Fe1—C20—C21 | 81.4 (5) | C36—Fe2—C43—C44 | −164.3 (5) |
C14—Fe1—C20—C21 | −120.7 (5) | C38—Fe2—C43—C44 | −79.1 (6) |
C15—Fe1—C20—C21 | −78.8 (5) | C39—Fe2—C43—C44 | −42.1 (11) |
C19—C20—C21—C22 | −0.9 (8) | C42—Fe2—C43—C44 | 119.9 (8) |
Fe1—C20—C21—C22 | −59.5 (5) | C42—C43—C44—C40 | −0.5 (9) |
C19—C20—C21—Fe1 | 58.6 (5) | Fe2—C43—C44—C40 | −59.7 (6) |
C17—Fe1—C21—C22 | −36.8 (11) | C42—C43—C44—Fe2 | 59.2 (5) |
C13—Fe1—C21—C22 | 159.4 (7) | C41—C40—C44—C43 | 0.8 (9) |
C19—Fe1—C21—C22 | 81.9 (5) | Fe2—C40—C44—C43 | 60.2 (6) |
C16—Fe1—C21—C22 | −75.6 (6) | C41—C40—C44—Fe2 | −59.4 (6) |
C18—Fe1—C21—C22 | 38.4 (5) | C35—Fe2—C44—C43 | −164.8 (7) |
C14—Fe1—C21—C22 | −162.0 (5) | C41—Fe2—C44—C43 | −80.4 (6) |
C15—Fe1—C21—C22 | −118.3 (5) | C37—Fe2—C44—C43 | 78.1 (6) |
C20—Fe1—C21—C22 | 119.8 (7) | C40—Fe2—C44—C43 | −117.7 (7) |
C17—Fe1—C21—C20 | −156.6 (9) | C36—Fe2—C44—C43 | 44.3 (13) |
C13—Fe1—C21—C20 | 39.6 (10) | C38—Fe2—C44—C43 | 119.6 (5) |
C19—Fe1—C21—C20 | −37.9 (5) | C39—Fe2—C44—C43 | 162.3 (5) |
C16—Fe1—C21—C20 | 164.5 (5) | C42—Fe2—C44—C43 | −36.7 (5) |
C22—Fe1—C21—C20 | −119.8 (7) | C35—Fe2—C44—C40 | −47.1 (10) |
C18—Fe1—C21—C20 | −81.5 (5) | C41—Fe2—C44—C40 | 37.3 (6) |
C14—Fe1—C21—C20 | 78.2 (5) | C37—Fe2—C44—C40 | −164.2 (5) |
C15—Fe1—C21—C20 | 121.8 (5) | C36—Fe2—C44—C40 | 161.9 (10) |
C20—C21—C22—C18 | 0.4 (9) | C38—Fe2—C44—C40 | −122.7 (6) |
Fe1—C21—C22—C18 | −59.3 (5) | C43—Fe2—C44—C40 | 117.7 (7) |
C20—C21—C22—Fe1 | 59.7 (5) | C39—Fe2—C44—C40 | −80.0 (6) |
C19—C18—C22—C21 | 0.2 (9) | C42—Fe2—C44—C40 | 81.0 (6) |
Experimental details
Crystal data | |
Chemical formula | C44H42Br5Fe3N6NiO4 |
Mr | 1344.65 |
Crystal system, space group | Monoclinic, Cc |
Temperature (K) | 100 |
a, b, c (Å) | 15.2181 (3), 22.0080 (3), 16.0005 (3) |
β (°) | 118.393 (2) |
V (Å3) | 4714.25 (14) |
Z | 4 |
Radiation type | Cu Kα |
µ (mm−1) | 13.07 |
Crystal size (mm) | 0.19 × 0.11 × 0.09 |
Data collection | |
Diffractometer | Bruker SMART APEX2 area detector diffractometer |
Absorption correction | Analytical SADABS (Bruker-AXS, 2007) |
Tmin, Tmax | 0.186, 0.376 |
No. of measured, independent and observed [I > 2σ(I)] reflections | 35920, 8033, 7903 |
Rint | 0.031 |
(sin θ/λ)max (Å−1) | 0.617 |
Refinement | |
R[F2 > 2σ(F2)], wR(F2), S | 0.032, 0.078, 1.05 |
No. of reflections | 8033 |
No. of parameters | 599 |
No. of restraints | 4 |
H-atom treatment | H-atom parameters constrained |
Δρmax, Δρmin (e Å−3) | 0.70, −0.66 |
Absolute structure | Flack H D (1983), Acta Cryst. A39, 876-881 |
Absolute structure parameter | −0.008 (4) |
Computer programs: APEX2 Ver. 2.1-4 (Bruker-AXS, 2007), SAINT Ver. 7.24A (Bruker-AXS, 2007), SAINT Ver. 7.24A, SHELXTL (Sheldrick, 2008), SHELXTL.
Br1—Ni1 | 2.4407 (10) | Fe2—C41 | 2.038 (8) |
Ni1—N1 | 2.047 (5) | Fe2—C37 | 2.040 (7) |
Ni1—N4 | 2.058 (5) | Fe2—C40 | 2.042 (9) |
Ni1—N3 | 2.092 (5) | Fe2—C44 | 2.047 (7) |
Ni1—N6 | 2.105 (5) | Fe2—C36 | 2.053 (7) |
Fe1—C17 | 2.026 (7) | Fe2—C38 | 2.055 (8) |
Fe1—C13 | 2.030 (6) | Fe2—C43 | 2.057 (8) |
Fe1—C19 | 2.032 (7) | Fe2—C39 | 2.058 (7) |
Fe1—C16 | 2.033 (8) | Fe2—C42 | 2.058 (8) |
Fe1—C22 | 2.037 (8) | Br2—Fe3 | 2.3352 (13) |
Fe1—C18 | 2.038 (7) | Br3—Fe3 | 2.3290 (16) |
Fe1—C14 | 2.042 (7) | Br4—Fe3 | 2.3419 (16) |
Fe1—C21 | 2.047 (7) | Br5—Fe3 | 2.2995 (16) |
Fe1—C15 | 2.050 (8) | Br3A—Fe3 | 1.943 (10) |
Fe1—C20 | 2.062 (7) | Br4A—Fe3 | 2.553 (15) |
Fe2—C35 | 2.031 (7) | Br5A—Fe3 | 2.560 (11) |
N1—Ni1—N4 | 93.66 (19) | C35—Fe2—C44 | 156.3 (3) |
N1—Ni1—N3 | 88.1 (2) | C41—Fe2—C44 | 68.5 (3) |
N4—Ni1—N3 | 90.8 (2) | C37—Fe2—C44 | 124.3 (3) |
N1—Ni1—N6 | 93.0 (2) | C40—Fe2—C44 | 41.4 (3) |
N4—Ni1—N6 | 87.7 (2) | C35—Fe2—C36 | 40.9 (3) |
N3—Ni1—N6 | 178.2 (2) | C41—Fe2—C36 | 121.0 (3) |
N1—Ni1—Br1 | 129.90 (17) | C37—Fe2—C36 | 41.1 (3) |
N4—Ni1—Br1 | 136.43 (16) | C40—Fe2—C36 | 155.7 (3) |
N3—Ni1—Br1 | 90.97 (16) | C44—Fe2—C36 | 161.4 (3) |
N6—Ni1—Br1 | 89.41 (15) | C35—Fe2—C38 | 68.3 (3) |
C17—Fe1—C13 | 41.9 (3) | C41—Fe2—C38 | 160.8 (4) |
C17—Fe1—C19 | 120.5 (3) | C37—Fe2—C38 | 40.6 (3) |
C13—Fe1—C19 | 105.9 (3) | C40—Fe2—C38 | 124.5 (4) |
C17—Fe1—C16 | 40.4 (3) | C44—Fe2—C38 | 107.4 (3) |
C13—Fe1—C16 | 68.9 (3) | C36—Fe2—C38 | 68.8 (4) |
C19—Fe1—C16 | 156.4 (3) | C35—Fe2—C43 | 161.0 (3) |
C17—Fe1—C22 | 123.3 (4) | C41—Fe2—C43 | 67.8 (3) |
C13—Fe1—C22 | 159.9 (3) | C37—Fe2—C43 | 108.3 (3) |
C19—Fe1—C22 | 68.0 (3) | C40—Fe2—C43 | 68.6 (3) |
C16—Fe1—C22 | 108.5 (3) | C44—Fe2—C43 | 40.9 (3) |
C17—Fe1—C18 | 105.6 (3) | C36—Fe2—C43 | 124.5 (3) |
C13—Fe1—C18 | 121.8 (3) | C38—Fe2—C43 | 122.3 (3) |
C19—Fe1—C18 | 40.2 (3) | C35—Fe2—C39 | 41.1 (3) |
C16—Fe1—C18 | 121.6 (3) | C41—Fe2—C39 | 123.6 (3) |
C22—Fe1—C18 | 41.3 (3) | C37—Fe2—C39 | 69.1 (3) |
C17—Fe1—C14 | 69.7 (3) | C40—Fe2—C39 | 106.3 (4) |
C13—Fe1—C14 | 41.1 (3) | C44—Fe2—C39 | 120.4 (4) |
C19—Fe1—C14 | 123.2 (3) | C36—Fe2—C39 | 69.5 (3) |
C16—Fe1—C14 | 68.9 (3) | C38—Fe2—C39 | 40.9 (3) |
C22—Fe1—C14 | 158.2 (3) | C43—Fe2—C39 | 157.0 (3) |
C18—Fe1—C14 | 158.8 (3) | C35—Fe2—C42 | 124.7 (3) |
C17—Fe1—C21 | 159.7 (3) | C41—Fe2—C42 | 40.5 (4) |
C13—Fe1—C21 | 158.0 (3) | C37—Fe2—C42 | 122.1 (3) |
C19—Fe1—C21 | 67.8 (3) | C40—Fe2—C42 | 68.0 (4) |
C16—Fe1—C21 | 125.2 (3) | C44—Fe2—C42 | 68.2 (3) |
C22—Fe1—C21 | 39.4 (3) | C36—Fe2—C42 | 107.7 (3) |
C18—Fe1—C21 | 68.0 (3) | C38—Fe2—C42 | 157.3 (3) |
C14—Fe1—C21 | 123.3 (3) | C43—Fe2—C42 | 39.8 (3) |
C17—Fe1—C15 | 68.6 (3) | C39—Fe2—C42 | 160.9 (3) |
C13—Fe1—C15 | 68.8 (3) | Br3A—Fe3—Br5 | 136.5 (5) |
C19—Fe1—C15 | 160.9 (4) | Br3A—Fe3—Br3 | 57.9 (4) |
C16—Fe1—C15 | 40.5 (4) | Br5—Fe3—Br3 | 109.01 (6) |
C22—Fe1—C15 | 123.0 (3) | Br3A—Fe3—Br2 | 115.5 (5) |
C18—Fe1—C15 | 158.2 (3) | Br5—Fe3—Br2 | 107.98 (6) |
C14—Fe1—C15 | 41.0 (3) | Br3—Fe3—Br2 | 109.57 (6) |
C21—Fe1—C15 | 109.8 (3) | Br3A—Fe3—Br4 | 51.0 (3) |
C17—Fe1—C20 | 157.0 (3) | Br5—Fe3—Br4 | 113.52 (7) |
C13—Fe1—C20 | 121.2 (3) | Br3—Fe3—Br4 | 108.00 (7) |
C19—Fe1—C20 | 40.5 (4) | Br2—Fe3—Br4 | 108.71 (6) |
C16—Fe1—C20 | 161.7 (4) | Br3A—Fe3—Br4A | 115.1 (5) |
C22—Fe1—C20 | 67.4 (3) | Br5—Fe3—Br4A | 49.9 (3) |
C18—Fe1—C20 | 68.0 (3) | Br3—Fe3—Br4A | 145.7 (4) |
C14—Fe1—C20 | 107.8 (3) | Br2—Fe3—Br4A | 103.4 (4) |
C21—Fe1—C20 | 40.4 (3) | Br4—Fe3—Br4A | 68.7 (3) |
C15—Fe1—C20 | 125.4 (4) | Br3A—Fe3—Br5A | 117.6 (6) |
C35—Fe2—C41 | 107.4 (3) | Br5—Fe3—Br5A | 45.0 (3) |
C35—Fe2—C37 | 68.6 (3) | Br3—Fe3—Br5A | 66.9 (3) |
C41—Fe2—C37 | 157.2 (3) | Br2—Fe3—Br5A | 108.0 (3) |
C35—Fe2—C40 | 120.4 (3) | Br4—Fe3—Br5A | 142.2 (3) |
C41—Fe2—C40 | 40.2 (4) | Br4A—Fe3—Br5A | 94.5 (4) |
C37—Fe2—C40 | 161.5 (4) |