Supporting information
Crystallographic Information File (CIF) https://doi.org/10.1107/S1600536802004658/ob6117sup1.cif | |
Structure factor file (CIF format) https://doi.org/10.1107/S1600536802004658/ob6117Isup2.hkl |
CCDC reference: 183767
Key indicators
- Single-crystal X-ray study
- T = 295 K
- Mean (C-C) = 0.015 Å
- R factor = 0.036
- wR factor = 0.079
- Data-to-parameter ratio = 9.6
checkCIF results
No syntax errors found ADDSYM reports no extra symmetry
Alert Level C:
STRVAL_01 From the CIF: _refine_ls_abs_structure_Flack 0.530 From the CIF: _refine_ls_abs_structure_Flack_su 0.030 Alert C Flack test results are ambiguous. General Notes
REFLT_03 From the CIF: _diffrn_reflns_theta_max 26.28 From the CIF: _reflns_number_total 2784 Count of symmetry unique reflns 2836 Completeness (_total/calc) 98.17% TEST3: Check Friedels for noncentro structure Estimate of Friedel pairs measured 0 Fraction of Friedel pairs measured 0.000 Are heavy atom types Z>Si present yes WARNING: Large fraction of Friedel related reflns may be needed to determine absolute structure
0 Alert Level A = Potentially serious problem
0 Alert Level B = Potential problem
1 Alert Level C = Please check
Data collection: CAD-4 EXPRESS (Enraf Nonius, 1994); cell refinement: CAD-4 EXPRESS; data reduction: XCAD4 (Harms & Wocadlo, 1995); program(s) used to solve structure: SHELXS97 (Sheldrick, 1997); program(s) used to refine structure: SHELXL97 (Sheldrick, 1997); molecular graphics: ORTEP-3 for Windows (Farrugia, 1997) and PLATON2000 (Spek, 2000); software used to prepare material for publication: WinGX (Farrugia, 1999).
[ZnNiBr2(C17H16N2O2)(C3H7NO)(CH4O)] | F(000) = 1336 |
Mr = 669.34 | Dx = 1.793 Mg m−3 |
Orthorhombic, P212121 | Mo Kα radiation, λ = 0.71073 Å |
Hall symbol: P 2ac 2ab | Cell parameters from 25 reflections |
a = 10.5304 (12) Å | θ = 10.2–18.2° |
b = 14.4184 (11) Å | µ = 4.98 mm−1 |
c = 16.3327 (13) Å | T = 295 K |
V = 2479.8 (4) Å3 | Prism, light blue |
Z = 4 | 0.25 × 0.20 × 0.15 mm |
Enraf Nonius CAD4 diffractometer | 1862 reflections with I > 2σ(I) |
Radiation source: fine-focus sealed tube | Rint = 0.064 |
Graphite monochromator | θmax = 26.3°, θmin = 2.4° |
ω/2θ scans | h = 0→13 |
Absorption correction: ψ scan (North et al., 1968) | k = 0→17 |
Tmin = 0.315, Tmax = 0.474 | l = 0→20 |
2791 measured reflections | 3 standard reflections every 120 min |
2784 independent reflections | intensity decay: 2% |
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)] = 0.036 | H atoms treated by a mixture of independent and constrained refinement |
wR(F2) = 0.079 | w = 1/[σ2(Fo2) + (0.0354P)2] where P = (Fo2 + 2Fc2)/3 |
S = 1.02 | (Δ/σ)max < 0.001 |
2784 reflections | Δρmax = 0.50 e Å−3 |
291 parameters | Δρmin = −0.61 e Å−3 |
0 restraints | Absolute structure: (Flack, 1983) |
Primary atom site location: structure-invariant direct methods | Absolute structure parameter: 0.53 (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. Number of psi-scan sets used was 7 Theta correction was applied. Averaged transmission function was used. No Fourier smoothing was applied. 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 | 0.4943 (11) | 0.0265 (7) | 0.2899 (6) | 0.035 (3) | |
C2 | 0.5930 (11) | −0.0194 (9) | 0.3304 (6) | 0.042 (3) | |
H2 | 0.6609 | −0.0427 | 0.3003 | 0.050* | |
C3 | 0.5909 (12) | −0.0308 (8) | 0.4154 (6) | 0.047 (3) | |
H3 | 0.6549 | −0.0646 | 0.4408 | 0.056* | |
C4 | 0.4957 (11) | 0.0073 (11) | 0.4616 (6) | 0.054 (4) | |
H4 | 0.4967 | 0.0021 | 0.5184 | 0.065* | |
C5 | 0.3987 (12) | 0.0534 (9) | 0.4228 (6) | 0.049 (3) | |
H5 | 0.3334 | 0.0785 | 0.4541 | 0.059* | |
C6 | 0.3950 (9) | 0.0639 (7) | 0.3373 (5) | 0.029 (3) | |
C7 | 0.2870 (9) | 0.1150 (6) | 0.3048 (5) | 0.035 (2) | |
H7 | 0.2289 | 0.1361 | 0.3433 | 0.042* | |
C8 | 0.1477 (10) | 0.1880 (8) | 0.2147 (6) | 0.053 (3) | |
H81A | 0.1263 | 0.2227 | 0.2637 | 0.064* | |
H82B | 0.0785 | 0.1453 | 0.2039 | 0.064* | |
C9 | 0.1580 (11) | 0.2546 (8) | 0.1441 (7) | 0.067 (4) | |
H91A | 0.0894 | 0.2993 | 0.1481 | 0.080* | |
H92B | 0.2373 | 0.2884 | 0.1491 | 0.080* | |
C10 | 0.1531 (11) | 0.2105 (9) | 0.0615 (6) | 0.062 (4) | |
H10A | 0.0770 | 0.1728 | 0.0578 | 0.075* | |
H10B | 0.1471 | 0.2588 | 0.0203 | 0.075* | |
C11 | 0.2888 (10) | 0.1406 (7) | −0.0338 (6) | 0.041 (3) | |
H11 | 0.2359 | 0.1724 | −0.0697 | 0.049* | |
C12 | 0.3874 (10) | 0.0851 (7) | −0.0712 (5) | 0.034 (3) | |
C13 | 0.3840 (11) | 0.0768 (8) | −0.1567 (6) | 0.044 (3) | |
H13 | 0.3195 | 0.1070 | −0.1850 | 0.053* | |
C14 | 0.4688 (12) | 0.0275 (9) | −0.2000 (6) | 0.050 (3) | |
H14 | 0.4635 | 0.0244 | −0.2567 | 0.060* | |
C15 | 0.5646 (12) | −0.0189 (9) | −0.1583 (6) | 0.049 (3) | |
H15 | 0.6233 | −0.0543 | −0.1872 | 0.059* | |
C16 | 0.5729 (11) | −0.0125 (9) | −0.0746 (6) | 0.047 (3) | |
H16 | 0.6382 | −0.0434 | −0.0477 | 0.056* | |
C17 | 0.4867 (9) | 0.0388 (7) | −0.0292 (5) | 0.032 (3) | |
C18 | 0.3100 (11) | −0.1069 (7) | 0.1134 (6) | 0.050 (3) | |
H18 | 0.3974 | −0.1052 | 0.1050 | 0.061* | |
C19 | 0.1194 (12) | −0.1993 (9) | 0.1223 (9) | 0.092 (4) | |
H19A | 0.0967 | −0.2636 | 0.1176 | 0.138* | |
H19B | 0.0737 | −0.1640 | 0.0821 | 0.138* | |
H19C | 0.0981 | −0.1773 | 0.1760 | 0.138* | |
C20 | 0.3247 (13) | −0.2731 (8) | 0.0917 (8) | 0.091 (5) | |
H20A | 0.2661 | −0.3241 | 0.0924 | 0.136* | |
H20B | 0.3888 | −0.2826 | 0.1326 | 0.136* | |
H20C | 0.3639 | −0.2692 | 0.0387 | 0.136* | |
C21 | 0.5242 (11) | 0.2619 (8) | 0.2089 (7) | 0.062 (3) | |
H21A | 0.5753 | 0.3147 | 0.1950 | 0.093* | |
H21B | 0.5738 | 0.2188 | 0.2402 | 0.093* | |
H21C | 0.4524 | 0.2817 | 0.2406 | 0.093* | |
Br1 | 0.70100 (14) | −0.14808 (8) | 0.12019 (9) | 0.0732 (4) | |
Br2 | 0.79403 (10) | 0.12241 (8) | 0.13298 (8) | 0.0611 (3) | |
N1 | 0.2615 (7) | 0.1347 (5) | 0.2307 (4) | 0.034 (2) | |
N2 | 0.2649 (7) | 0.1516 (6) | 0.0431 (5) | 0.038 (2) | |
N3 | 0.2578 (8) | −0.1885 (6) | 0.1085 (5) | 0.051 (2) | |
Ni | 0.36672 (10) | 0.09229 (7) | 0.13362 (7) | 0.0320 (3) | |
O1 | 0.4968 (6) | 0.0333 (4) | 0.2088 (3) | 0.0376 (18) | |
O2 | 0.4981 (6) | 0.0454 (5) | 0.0525 (3) | 0.0391 (18) | |
O3 | 0.2597 (5) | −0.0322 (4) | 0.1275 (5) | 0.0469 (17) | |
O4 | 0.4811 (6) | 0.2181 (5) | 0.1360 (5) | 0.0533 (18) | |
Zn | 0.63563 (9) | 0.00637 (7) | 0.12911 (7) | 0.0400 (3) | |
H4A | 0.5743 | 0.2167 | 0.1304 | 0.09 (4)* |
U11 | U22 | U33 | U12 | U13 | U23 | |
C1 | 0.047 (8) | 0.027 (6) | 0.032 (5) | −0.013 (5) | −0.007 (5) | 0.002 (5) |
C2 | 0.050 (8) | 0.049 (8) | 0.026 (5) | 0.006 (7) | 0.003 (5) | 0.008 (5) |
C3 | 0.052 (8) | 0.049 (8) | 0.041 (6) | −0.002 (7) | −0.008 (6) | 0.010 (6) |
C4 | 0.048 (8) | 0.079 (9) | 0.035 (6) | 0.009 (7) | −0.004 (6) | 0.005 (7) |
C5 | 0.051 (8) | 0.062 (9) | 0.034 (5) | 0.000 (7) | 0.012 (6) | −0.002 (6) |
C6 | 0.027 (6) | 0.031 (6) | 0.029 (5) | −0.006 (5) | 0.006 (4) | 0.002 (4) |
C7 | 0.034 (5) | 0.041 (6) | 0.030 (5) | −0.003 (5) | 0.002 (4) | −0.003 (5) |
C8 | 0.042 (6) | 0.067 (8) | 0.050 (6) | 0.020 (6) | 0.007 (6) | −0.001 (6) |
C9 | 0.063 (7) | 0.063 (8) | 0.073 (9) | 0.026 (6) | 0.005 (7) | −0.001 (8) |
C10 | 0.055 (8) | 0.076 (9) | 0.056 (7) | 0.041 (7) | −0.014 (6) | 0.001 (7) |
C11 | 0.043 (6) | 0.043 (6) | 0.037 (6) | 0.002 (6) | −0.010 (5) | 0.010 (5) |
C12 | 0.041 (7) | 0.033 (6) | 0.027 (5) | −0.004 (6) | 0.001 (5) | 0.001 (5) |
C13 | 0.044 (6) | 0.052 (7) | 0.036 (5) | 0.002 (6) | −0.010 (5) | 0.005 (5) |
C14 | 0.057 (8) | 0.060 (8) | 0.033 (6) | −0.015 (7) | −0.003 (6) | −0.007 (6) |
C15 | 0.056 (8) | 0.048 (8) | 0.044 (6) | 0.002 (7) | 0.019 (6) | −0.015 (6) |
C16 | 0.043 (7) | 0.050 (8) | 0.047 (6) | −0.003 (7) | −0.003 (6) | −0.009 (6) |
C17 | 0.032 (6) | 0.043 (7) | 0.022 (5) | −0.009 (5) | 0.002 (4) | 0.003 (5) |
C18 | 0.066 (6) | 0.040 (6) | 0.045 (7) | −0.005 (6) | −0.015 (6) | 0.004 (6) |
C19 | 0.089 (9) | 0.074 (9) | 0.113 (11) | −0.032 (8) | 0.002 (12) | −0.004 (11) |
C20 | 0.098 (11) | 0.066 (9) | 0.109 (11) | 0.019 (8) | −0.031 (9) | −0.032 (8) |
C21 | 0.056 (7) | 0.063 (8) | 0.067 (8) | 0.000 (7) | 0.002 (7) | −0.012 (7) |
Br1 | 0.0979 (9) | 0.0551 (7) | 0.0665 (8) | 0.0341 (7) | 0.0222 (9) | 0.0112 (8) |
Br2 | 0.0465 (5) | 0.0717 (8) | 0.0650 (7) | −0.0042 (6) | 0.0009 (8) | 0.0060 (7) |
N1 | 0.032 (4) | 0.037 (5) | 0.034 (5) | 0.007 (4) | 0.004 (4) | 0.001 (4) |
N2 | 0.035 (5) | 0.042 (5) | 0.036 (5) | 0.008 (4) | −0.006 (4) | 0.002 (4) |
N3 | 0.070 (6) | 0.039 (5) | 0.044 (6) | −0.003 (5) | −0.007 (5) | 0.001 (5) |
Ni | 0.0330 (5) | 0.0333 (6) | 0.0298 (6) | 0.0056 (5) | 0.0002 (7) | 0.0015 (6) |
O1 | 0.040 (4) | 0.047 (4) | 0.026 (3) | 0.011 (3) | 0.001 (3) | 0.004 (3) |
O2 | 0.036 (4) | 0.054 (5) | 0.027 (3) | 0.008 (3) | −0.001 (3) | −0.002 (3) |
O3 | 0.049 (3) | 0.036 (4) | 0.056 (4) | −0.006 (3) | 0.000 (4) | 0.000 (5) |
O4 | 0.056 (4) | 0.052 (4) | 0.052 (4) | −0.007 (4) | −0.006 (5) | 0.003 (4) |
Zn | 0.0366 (5) | 0.0485 (7) | 0.0347 (6) | 0.0110 (5) | 0.0019 (7) | 0.0048 (7) |
Ni—Zn | 3.0917 (15) | C14—C15 | 1.388 (16) |
C1—O1 | 1.329 (10) | C14—H14 | 0.9300 |
C1—C2 | 1.397 (14) | C15—C16 | 1.373 (13) |
C1—C6 | 1.409 (13) | C15—H15 | 0.9300 |
C2—C3 | 1.398 (12) | C16—C17 | 1.385 (14) |
C2—H2 | 0.9300 | C16—H16 | 0.9300 |
C3—C4 | 1.371 (15) | C17—O2 | 1.344 (10) |
C3—H3 | 0.9300 | C18—O3 | 1.223 (11) |
C4—C5 | 1.374 (15) | C18—N3 | 1.301 (12) |
C4—H4 | 0.9300 | C18—H18 | 0.9300 |
C5—C6 | 1.404 (12) | C19—N3 | 1.483 (14) |
C5—H5 | 0.9300 | C19—H19A | 0.9600 |
C6—C7 | 1.455 (13) | C19—H19B | 0.9600 |
C7—N1 | 1.271 (11) | C19—H19C | 0.9600 |
C7—H7 | 0.9300 | C20—N3 | 1.435 (14) |
C8—N1 | 1.447 (12) | C20—H20A | 0.9600 |
C8—C9 | 1.505 (15) | C20—H20B | 0.9600 |
C8—H81A | 0.9700 | C20—H20C | 0.9600 |
C8—H82B | 0.9700 | C21—H21A | 0.9600 |
C9—C10 | 1.493 (15) | C21—H21B | 0.9600 |
C9—H91A | 0.9700 | C21—H21C | 0.9600 |
C9—H92B | 0.9700 | Br1—Zn | 2.3356 (16) |
C10—N2 | 1.481 (12) | Br2—Zn | 2.3634 (15) |
C10—H10A | 0.9700 | N1—Ni | 2.028 (7) |
C10—H10B | 0.9700 | N2—Ni | 2.017 (8) |
C11—N2 | 1.290 (11) | Ni—O1 | 2.027 (6) |
C11—C12 | 1.447 (14) | Ni—O2 | 2.031 (6) |
C11—H11 | 0.9300 | Ni—O3 | 2.122 (6) |
C12—C13 | 1.402 (13) | Ni—O4 | 2.178 (6) |
C12—C17 | 1.417 (13) | O1—Zn | 1.996 (6) |
C13—C14 | 1.343 (15) | O2—Zn | 1.995 (6) |
C13—H13 | 0.9300 | O4—H4A | 0.985 |
O1—C1—C2 | 119.5 (10) | O3—C18—N3 | 128.7 (11) |
O1—C1—C6 | 122.3 (9) | O3—C18—H18 | 115.7 |
C2—C1—C6 | 118.3 (8) | N3—C18—H18 | 115.7 |
C3—C2—C1 | 120.9 (12) | N3—C19—H19A | 109.5 |
C3—C2—H2 | 119.6 | N3—C19—H19B | 109.5 |
C1—C2—H2 | 119.6 | H19A—C19—H19B | 109.5 |
C4—C3—C2 | 120.8 (13) | N3—C19—H19C | 109.5 |
C4—C3—H3 | 119.6 | H19A—C19—H19C | 109.5 |
C2—C3—H3 | 119.6 | H19B—C19—H19C | 109.5 |
C3—C4—C5 | 118.9 (10) | N3—C20—H20A | 109.5 |
C3—C4—H4 | 120.5 | N3—C20—H20B | 109.5 |
C5—C4—H4 | 120.5 | H20A—C20—H20B | 109.5 |
C4—C5—C6 | 122.1 (11) | N3—C20—H20C | 109.5 |
C4—C5—H5 | 118.9 | H20A—C20—H20C | 109.5 |
C6—C5—H5 | 118.9 | H20B—C20—H20C | 109.5 |
C5—C6—C1 | 119.0 (11) | O4—C21—H21A | 109.5 |
C5—C6—C7 | 116.1 (10) | O4—C21—H21B | 109.5 |
C1—C6—C7 | 125.0 (8) | H21A—C21—H21B | 109.5 |
N1—C7—C6 | 128.7 (9) | O4—C21—H21C | 109.5 |
N1—C7—H7 | 115.6 | H21A—C21—H21C | 109.5 |
C6—C7—H7 | 115.6 | H21B—C21—H21C | 109.5 |
N1—C8—C9 | 114.7 (9) | C7—N1—C8 | 117.7 (8) |
N1—C8—H81A | 108.6 | C7—N1—Ni | 124.1 (7) |
C9—C8—H81A | 108.6 | C8—N1—Ni | 118.1 (6) |
N1—C8—H82B | 108.6 | C11—N2—C10 | 115.0 (8) |
C9—C8—H82B | 108.6 | C11—N2—Ni | 123.9 (7) |
H81A—C8—H82B | 107.6 | C10—N2—Ni | 121.1 (6) |
C10—C9—C8 | 114.8 (10) | C18—N3—C20 | 125.0 (10) |
C10—C9—H91A | 108.6 | C18—N3—C19 | 120.1 (11) |
C8—C9—H91A | 108.6 | C20—N3—C19 | 115.0 (11) |
C10—C9—H92B | 108.6 | N2—Ni—O1 | 169.0 (3) |
C8—C9—H92B | 108.6 | N2—Ni—N1 | 98.9 (3) |
H91A—C9—H92B | 107.6 | O1—Ni—N1 | 91.2 (3) |
N2—C10—C9 | 113.6 (9) | N2—Ni—O2 | 91.4 (3) |
N2—C10—H10A | 108.8 | O1—Ni—O2 | 78.2 (2) |
C9—C10—H10A | 108.8 | N1—Ni—O2 | 169.1 (3) |
N2—C10—H10B | 108.8 | N2—Ni—O3 | 92.4 (3) |
C9—C10—H10B | 108.8 | O1—Ni—O3 | 91.9 (3) |
H10A—C10—H10B | 107.7 | N1—Ni—O3 | 90.1 (3) |
N2—C11—C12 | 128.3 (9) | O2—Ni—O3 | 92.9 (3) |
N2—C11—H11 | 115.8 | N2—Ni—O4 | 87.4 (3) |
C12—C11—H11 | 115.8 | O1—Ni—O4 | 88.0 (3) |
C13—C12—C17 | 117.4 (11) | N1—Ni—O4 | 92.1 (3) |
C13—C12—C11 | 116.7 (10) | O2—Ni—O4 | 85.0 (3) |
C17—C12—C11 | 125.8 (8) | O3—Ni—O4 | 177.8 (3) |
C14—C13—C12 | 123.5 (11) | C1—O1—Zn | 130.6 (6) |
C14—C13—H13 | 118.3 | C1—O1—Ni | 128.5 (6) |
C12—C13—H13 | 118.3 | Zn—O1—Ni | 100.5 (3) |
C13—C14—C15 | 118.7 (9) | C17—O2—Zn | 131.9 (6) |
C13—C14—H14 | 120.6 | C17—O2—Ni | 127.7 (6) |
C15—C14—H14 | 120.6 | Zn—O2—Ni | 100.3 (2) |
C16—C15—C14 | 120.1 (12) | C18—O3—Ni | 121.6 (7) |
C16—C15—H15 | 119.9 | C21—O4—Ni | 124.1 (6) |
C14—C15—H15 | 119.9 | Ni—O4—H4A | 122.1 |
C15—C16—C17 | 121.8 (13) | O2—Zn—O1 | 79.8 (2) |
C15—C16—H16 | 119.1 | O2—Zn—Br1 | 116.4 (2) |
C17—C16—H16 | 119.1 | O1—Zn—Br1 | 116.26 (19) |
O2—C17—C16 | 120.7 (10) | O2—Zn—Br2 | 109.2 (2) |
O2—C17—C12 | 120.8 (9) | O1—Zn—Br2 | 111.20 (19) |
C16—C17—C12 | 118.4 (9) | Br1—Zn—Br2 | 117.95 (6) |
O1—C1—C2—C3 | −177.7 (12) | C7—N1—Ni—O3 | 87.8 (8) |
C6—C1—C2—C3 | 2.2 (18) | C8—N1—Ni—O3 | −90.0 (7) |
C1—C2—C3—C4 | −4 (2) | C7—N1—Ni—O4 | −92.1 (8) |
C2—C3—C4—C5 | 3 (2) | C8—N1—Ni—O4 | 90.1 (7) |
C3—C4—C5—C6 | −1 (2) | C2—C1—O1—Zn | −11.5 (14) |
C4—C5—C6—C1 | 0 (2) | C6—C1—O1—Zn | 168.6 (7) |
C4—C5—C6—C7 | −179.5 (10) | C2—C1—O1—Ni | 178.3 (7) |
O1—C1—C6—C5 | 179.7 (10) | C6—C1—O1—Ni | −1.6 (14) |
C2—C1—C6—C5 | −0.2 (16) | N2—Ni—O1—C1 | 160.6 (15) |
O1—C1—C6—C7 | −1.3 (16) | N1—Ni—O1—C1 | 3.6 (8) |
C2—C1—C6—C7 | 178.8 (10) | O2—Ni—O1—C1 | −179.1 (8) |
C5—C6—C7—N1 | 179.5 (11) | O3—Ni—O1—C1 | −86.5 (8) |
C1—C6—C7—N1 | 0.4 (17) | O4—Ni—O1—C1 | 95.6 (8) |
N1—C8—C9—C10 | 75.3 (13) | N2—Ni—O1—Zn | −11.8 (18) |
C8—C9—C10—N2 | −67.3 (13) | N1—Ni—O1—Zn | −168.9 (3) |
N2—C11—C12—C13 | 173.0 (11) | O2—Ni—O1—Zn | 8.5 (2) |
N2—C11—C12—C17 | −7.0 (17) | O3—Ni—O1—Zn | 101.0 (3) |
C17—C12—C13—C14 | 0.2 (19) | O4—Ni—O1—Zn | −76.8 (3) |
C11—C12—C13—C14 | −179.8 (10) | C16—C17—O2—Zn | 9.0 (14) |
C12—C13—C14—C15 | 0.7 (19) | C12—C17—O2—Zn | −170.0 (6) |
C13—C14—C15—C16 | −1 (2) | C16—C17—O2—Ni | −166.1 (8) |
C14—C15—C16—C17 | 1 (2) | C12—C17—O2—Ni | 14.9 (13) |
C15—C16—C17—O2 | −178.8 (13) | N2—Ni—O2—C17 | −16.0 (8) |
C15—C16—C17—C12 | 0.3 (18) | O1—Ni—O2—C17 | 167.8 (9) |
C13—C12—C17—O2 | 178.3 (10) | N1—Ni—O2—C17 | −178.1 (14) |
C11—C12—C17—O2 | −1.6 (15) | O3—Ni—O2—C17 | 76.5 (8) |
C13—C12—C17—C16 | −0.7 (15) | O4—Ni—O2—C17 | −103.2 (8) |
C11—C12—C17—C16 | 179.3 (11) | N2—Ni—O2—Zn | 167.7 (3) |
C6—C7—N1—C8 | −179.1 (9) | O1—Ni—O2—Zn | −8.5 (2) |
C6—C7—N1—Ni | 3.1 (14) | N1—Ni—O2—Zn | 5.7 (17) |
C9—C8—N1—C7 | 145.4 (10) | O3—Ni—O2—Zn | −99.8 (3) |
C9—C8—N1—Ni | −36.6 (12) | O4—Ni—O2—Zn | 80.5 (3) |
C12—C11—N2—C10 | −177.6 (10) | N3—C18—O3—Ni | 179.3 (8) |
C12—C11—N2—Ni | 1.0 (16) | N2—Ni—O3—C18 | 121.5 (9) |
C9—C10—N2—C11 | −155.6 (10) | O1—Ni—O3—C18 | −48.4 (9) |
C9—C10—N2—Ni | 25.7 (13) | N1—Ni—O3—C18 | −139.6 (9) |
O3—C18—N3—C20 | −179.9 (11) | O2—Ni—O3—C18 | 29.9 (9) |
O3—C18—N3—C19 | −1.0 (18) | N2—Ni—O4—C21 | 138.7 (8) |
C11—N2—Ni—O1 | 28 (2) | O1—Ni—O4—C21 | −51.3 (8) |
C10—N2—Ni—O1 | −153.9 (15) | N1—Ni—O4—C21 | 39.8 (8) |
C11—N2—Ni—N1 | −175.7 (9) | O2—Ni—O4—C21 | −129.6 (8) |
C10—N2—Ni—N1 | 2.9 (8) | C17—O2—Zn—O1 | −167.5 (9) |
C11—N2—Ni—O2 | 7.7 (9) | Ni—O2—Zn—O1 | 8.6 (2) |
C10—N2—Ni—O2 | −173.7 (8) | C17—O2—Zn—Br1 | −53.1 (9) |
C11—N2—Ni—O3 | −85.2 (9) | Ni—O2—Zn—Br1 | 122.9 (2) |
C10—N2—Ni—O3 | 93.4 (8) | C17—O2—Zn—Br2 | 83.5 (8) |
C11—N2—Ni—O4 | 92.6 (9) | Ni—O2—Zn—Br2 | −100.5 (2) |
C10—N2—Ni—O4 | −88.8 (8) | C1—O1—Zn—O2 | 179.2 (9) |
C7—N1—Ni—N2 | −179.8 (8) | Ni—O1—Zn—O2 | −8.6 (2) |
C8—N1—Ni—N2 | 2.4 (7) | C1—O1—Zn—Br1 | 64.7 (8) |
C7—N1—Ni—O1 | −4.1 (8) | Ni—O1—Zn—Br1 | −123.1 (2) |
C8—N1—Ni—O1 | 178.1 (7) | C1—O1—Zn—Br2 | −74.0 (8) |
C7—N1—Ni—O2 | −18 (2) | Ni—O1—Zn—Br2 | 98.2 (2) |
C8—N1—Ni—O2 | 164.3 (14) |
D—H···A | D—H | H···A | D···A | D—H···A |
O4—H4A···Br2 | 0.99 | 2.68 | 3.572 (6) | 150 |
C18—H18···O2 | 0.93 | 2.56 | 3.120 (13) | 119 |