Bis[N-(2,6-dimethylphenyl)aminophenylglyoximato-κ2N,N′]nickel(II) dimethyl sulfoxide solvate
Supporting information
Crystallographic Information File (CIF) https://doi.org/10.1107/S1600536804020872/ob6405sup1.cif | |
Structure factor file (CIF format) https://doi.org/10.1107/S1600536804020872/ob6405Isup2.hkl |
CCDC reference: 251621
Key indicators
- Single-crystal X-ray study
- T = 293 K
- Mean (C-C) = 0.003 Å
- Disorder in solvent or counterion
- R factor = 0.037
- wR factor = 0.084
- Data-to-parameter ratio = 13.8
checkCIF/PLATON results
No syntax errors found
Alert level C PLAT063_ALERT_3_C Crystal Probably too Large for Beam Size ....... 0.70 mm PLAT243_ALERT_4_C High Solvent U(eq) as Compared to Neighbors for C17A PLAT244_ALERT_4_C Low Solvent U(eq) as Compared to Neighbors for S1 PLAT244_ALERT_4_C Low Solvent U(eq) as Compared to Neighbors for C17B PLAT301_ALERT_3_C Main Residue Disorder ......................... 22.00 Perc. PLAT302_ALERT_4_C Anion/Solvent Disorder ......................... 43.00 Perc.
0 ALERT level A = In general: serious problem 0 ALERT level B = Potentially serious problem 6 ALERT level C = Check and explain 0 ALERT level G = General alerts; check 0 ALERT type 1 CIF construction/syntax error, inconsistent or missing data 0 ALERT type 2 Indicator that the structure model may be wrong or deficient 2 ALERT type 3 Indicator that the structure quality may be low 4 ALERT type 4 Improvement, methodology, query or suggestion
Data collection: X-AREA (Stoe & Cie, 2002); cell refinement: X-AREA; data reduction: X-RED32 (Stoe & Cie, 2002); 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); software used to prepare material for publication: SHELXL97.
[Ni(C16H16N3O2)2]·C2H6OS | F(000) = 736 |
Mr = 701.47 | Dx = 1.369 Mg m−3 |
Monoclinic, P2/c | Mo Kα radiation, λ = 0.71073 Å |
Hall symbol: -P 2yc | Cell parameters from 9778 reflections |
a = 13.2381 (11) Å | θ = 2.5–27.6° |
b = 7.8171 (4) Å | µ = 0.68 mm−1 |
c = 16.5034 (14) Å | T = 293 K |
β = 94.654 (7)° | Plate, dark red |
V = 1702.2 (2) Å3 | 0.70 × 0.29 × 0.05 mm |
Z = 2 |
Stoe IPDS-2 diffractometer | 4027 independent reflections |
Radiation source: sealed X-ray tube, 12 x 0.4 mm long-fine focus | 2627 reflections with I > 2σ(I) |
Plane graphite monochromator | Rint = 0.069 |
Detector resolution: 6.67 pixels mm-1 | θmax = 27.8°, θmin = 2.5° |
φ scans | h = −17→17 |
Absorption correction: integration (X-RED32; Stoe & Cie, 2002) | k = −10→9 |
Tmin = 0.789, Tmax = 0.967 | l = −21→19 |
18574 measured reflections |
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)] = 0.037 | Hydrogen site location: mixed |
wR(F2) = 0.084 | H atoms treated by a mixture of independent and constrained refinement |
S = 0.91 | w = 1/[σ2(Fo2) + (0.0424P)2] where P = (Fo2 + 2Fc2)/3 |
4027 reflections | (Δ/σ)max < 0.001 |
291 parameters | Δρmax = 0.18 e Å−3 |
218 restraints | Δρmin = −0.40 e Å−3 |
Geometry. The r.m.s. deviations of the plane A (C1—C6), plane B'(C11A—C16A) and plane B''(C11B—C16B) are 0.010 0.014 and 0.011 Å, respectively. The dihedral angle between the least square planes of plane A—plane B' and plane A—plane B'' are 38.3 (6) ° and 38.3 (6) °. 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) | |
Ni1 | 0.0000 | 0.5000 | 0.0000 | 0.03790 (11) | |
O1 | −0.04525 (11) | 0.3119 (2) | 0.14245 (9) | 0.0501 (4) | |
H11 | −0.101 (2) | 0.371 (4) | 0.1212 (17) | 0.082 (9)* | |
O2 | 0.18652 (10) | 0.5250 (2) | −0.06883 (9) | 0.0526 (4) | |
N1 | 0.13373 (13) | 0.1741 (2) | 0.15883 (11) | 0.0445 (4) | |
H21 | 0.0907 (17) | 0.153 (3) | 0.1896 (14) | 0.051 (7)* | |
N2 | 0.02580 (11) | 0.3674 (2) | 0.09125 (10) | 0.0416 (4) | |
N3 | 0.13739 (12) | 0.4528 (2) | −0.01223 (10) | 0.0423 (4) | |
C1 | 0.21250 (14) | 0.0490 (3) | 0.16221 (12) | 0.0410 (5) | |
C2 | 0.22028 (17) | −0.0642 (3) | 0.09837 (13) | 0.0492 (5) | |
C3 | 0.2976 (2) | −0.1854 (3) | 0.10611 (17) | 0.0645 (7) | |
H3 | 0.3051 | −0.2627 | 0.0642 | 0.077* | |
C4 | 0.36294 (19) | −0.1917 (4) | 0.17491 (19) | 0.0726 (8) | |
H4 | 0.4153 | −0.2714 | 0.1786 | 0.087* | |
C5 | 0.35203 (17) | −0.0828 (4) | 0.23770 (17) | 0.0649 (7) | |
H5 | 0.3962 | −0.0908 | 0.2843 | 0.078* | |
C6 | 0.27654 (15) | 0.0397 (3) | 0.23359 (13) | 0.0494 (6) | |
C7 | 0.2620 (2) | 0.1535 (4) | 0.30390 (15) | 0.0730 (8) | |
H7A | 0.3133 | 0.1300 | 0.3469 | 0.088* | |
H7B | 0.1963 | 0.1332 | 0.3228 | 0.088* | |
H7C | 0.2668 | 0.2707 | 0.2873 | 0.088* | |
C8 | 0.1454 (2) | −0.0650 (4) | 0.02491 (15) | 0.0713 (7) | |
H8A | 0.0781 | −0.0512 | 0.0417 | 0.086* | |
H8B | 0.1498 | −0.1717 | −0.0034 | 0.086* | |
H8C | 0.1603 | 0.0274 | −0.0105 | 0.086* | |
C9 | 0.11353 (14) | 0.2918 (2) | 0.10093 (12) | 0.0387 (4) | |
C10 | 0.18384 (14) | 0.3541 (3) | 0.04260 (12) | 0.0401 (4) | |
C11A | 0.2951 (7) | 0.329 (3) | 0.0481 (11) | 0.0446 (19) | 0.46 (2) |
C12A | 0.3444 (8) | 0.282 (2) | −0.0188 (9) | 0.058 (2) | 0.46 (2) |
H12A | 0.3073 | 0.2605 | −0.0680 | 0.069* | 0.46 (2) |
C13A | 0.4480 (8) | 0.2659 (18) | −0.0131 (7) | 0.066 (2) | 0.46 (2) |
H13A | 0.4806 | 0.2291 | −0.0578 | 0.079* | 0.46 (2) |
C14A | 0.5034 (7) | 0.3039 (18) | 0.0581 (7) | 0.066 (2) | 0.46 (2) |
H14A | 0.5735 | 0.2925 | 0.0617 | 0.080* | 0.46 (2) |
C15A | 0.4563 (9) | 0.3585 (18) | 0.1236 (7) | 0.062 (2) | 0.46 (2) |
H15A | 0.4946 | 0.3891 | 0.1711 | 0.075* | 0.46 (2) |
C16A | 0.3511 (9) | 0.369 (3) | 0.1197 (9) | 0.054 (2) | 0.46 (2) |
H16A | 0.3187 | 0.4022 | 0.1651 | 0.065* | 0.46 (2) |
C11B | 0.2934 (6) | 0.313 (3) | 0.0439 (9) | 0.0448 (17) | 0.54 (2) |
C12B | 0.3322 (7) | 0.2439 (18) | −0.0239 (7) | 0.0555 (19) | 0.54 (2) |
H12B | 0.2897 | 0.2241 | −0.0706 | 0.067* | 0.54 (2) |
C13B | 0.4331 (7) | 0.2039 (16) | −0.0226 (5) | 0.0647 (19) | 0.54 (2) |
H13B | 0.4584 | 0.1547 | −0.0681 | 0.078* | 0.54 (2) |
C14B | 0.4966 (6) | 0.2358 (17) | 0.0450 (6) | 0.069 (2) | 0.54 (2) |
H14B | 0.5656 | 0.2131 | 0.0446 | 0.083* | 0.54 (2) |
C15B | 0.4593 (7) | 0.3006 (16) | 0.1131 (5) | 0.0627 (19) | 0.54 (2) |
H15B | 0.5024 | 0.3190 | 0.1597 | 0.075* | 0.54 (2) |
C16B | 0.3567 (8) | 0.339 (2) | 0.1132 (8) | 0.0532 (19) | 0.54 (2) |
H16B | 0.3311 | 0.3825 | 0.1599 | 0.064* | 0.54 (2) |
O3 | 0.0000 | 0.9612 (3) | 0.2500 | 0.0819 (8) | |
S1 | −0.00444 (9) | 0.78626 (17) | 0.21156 (8) | 0.0627 (3) | 0.50 |
C17A | 0.1012 (8) | 0.676 (2) | 0.2559 (10) | 0.113 (6) | 0.50 |
H17A | 0.1066 | 0.7007 | 0.3130 | 0.136* | 0.50 |
H17B | 0.1622 | 0.7106 | 0.2328 | 0.136* | 0.50 |
H17C | 0.0914 | 0.5550 | 0.2479 | 0.136* | 0.50 |
C17B | 0.0978 (6) | 0.6712 (14) | 0.2422 (9) | 0.067 (3) | 0.50 |
H17D | 0.1631 | 0.7219 | 0.2556 | 0.080* | 0.50 |
H17E | 0.0817 | 0.6768 | 0.1845 | 0.080* | 0.50 |
H17F | 0.0991 | 0.5538 | 0.2594 | 0.080* | 0.50 |
U11 | U22 | U33 | U12 | U13 | U23 | |
Ni1 | 0.03012 (16) | 0.04116 (19) | 0.04257 (19) | 0.00632 (17) | 0.00382 (12) | 0.00353 (18) |
O1 | 0.0377 (7) | 0.0642 (10) | 0.0496 (8) | 0.0104 (7) | 0.0114 (6) | 0.0138 (7) |
O2 | 0.0373 (7) | 0.0658 (10) | 0.0560 (8) | 0.0093 (7) | 0.0128 (6) | 0.0197 (8) |
N1 | 0.0370 (9) | 0.0516 (11) | 0.0457 (10) | 0.0106 (8) | 0.0075 (8) | 0.0089 (8) |
N2 | 0.0313 (8) | 0.0482 (10) | 0.0461 (9) | 0.0070 (7) | 0.0080 (7) | 0.0051 (8) |
N3 | 0.0359 (8) | 0.0457 (10) | 0.0456 (9) | 0.0048 (7) | 0.0051 (7) | 0.0033 (7) |
C1 | 0.0336 (9) | 0.0422 (11) | 0.0475 (11) | 0.0045 (7) | 0.0040 (8) | 0.0064 (9) |
C2 | 0.0523 (12) | 0.0455 (11) | 0.0502 (13) | 0.0010 (10) | 0.0056 (10) | 0.0032 (10) |
C3 | 0.0686 (16) | 0.0508 (14) | 0.0773 (17) | 0.0098 (12) | 0.0257 (14) | −0.0059 (13) |
C4 | 0.0521 (14) | 0.0702 (18) | 0.098 (2) | 0.0246 (13) | 0.0178 (14) | 0.0191 (16) |
C5 | 0.0421 (12) | 0.0807 (17) | 0.0705 (16) | 0.0136 (12) | −0.0040 (11) | 0.0169 (15) |
C6 | 0.0386 (10) | 0.0610 (16) | 0.0481 (11) | 0.0071 (9) | 0.0007 (8) | 0.0074 (10) |
C7 | 0.0653 (16) | 0.101 (2) | 0.0510 (14) | 0.0068 (15) | −0.0091 (12) | −0.0070 (14) |
C8 | 0.088 (2) | 0.0661 (16) | 0.0583 (15) | −0.0072 (14) | −0.0033 (14) | −0.0113 (13) |
C9 | 0.0362 (9) | 0.0399 (11) | 0.0397 (10) | 0.0056 (8) | 0.0007 (8) | −0.0016 (9) |
C10 | 0.0340 (9) | 0.0423 (11) | 0.0442 (11) | 0.0062 (8) | 0.0031 (8) | 0.0013 (9) |
C11A | 0.035 (3) | 0.046 (4) | 0.054 (3) | 0.010 (3) | 0.008 (3) | 0.006 (3) |
C12A | 0.042 (3) | 0.068 (5) | 0.063 (3) | 0.011 (3) | 0.006 (3) | 0.001 (3) |
C13A | 0.043 (3) | 0.082 (5) | 0.074 (3) | 0.011 (4) | 0.022 (3) | 0.000 (4) |
C14A | 0.035 (2) | 0.083 (5) | 0.081 (4) | 0.010 (3) | 0.007 (3) | 0.009 (4) |
C15A | 0.040 (3) | 0.072 (5) | 0.073 (4) | 0.011 (4) | −0.006 (3) | 0.001 (3) |
C16A | 0.035 (3) | 0.061 (5) | 0.065 (3) | 0.005 (3) | −0.001 (3) | 0.006 (3) |
C11B | 0.034 (3) | 0.047 (4) | 0.054 (3) | 0.002 (2) | 0.002 (2) | 0.008 (3) |
C12B | 0.040 (3) | 0.067 (5) | 0.059 (3) | 0.007 (3) | 0.005 (2) | −0.005 (3) |
C13B | 0.046 (3) | 0.081 (5) | 0.067 (3) | 0.015 (3) | 0.007 (2) | −0.007 (3) |
C14B | 0.039 (3) | 0.093 (5) | 0.075 (3) | 0.019 (3) | 0.008 (2) | −0.003 (4) |
C15B | 0.037 (2) | 0.082 (5) | 0.067 (3) | 0.011 (3) | −0.007 (2) | 0.000 (3) |
C16B | 0.042 (3) | 0.064 (5) | 0.055 (3) | 0.008 (3) | 0.010 (2) | −0.002 (3) |
O3 | 0.0891 (19) | 0.0480 (16) | 0.115 (2) | 0.000 | 0.0477 (17) | 0.000 |
S1 | 0.0739 (8) | 0.0597 (7) | 0.0561 (6) | 0.0075 (6) | 0.0166 (6) | 0.0048 (6) |
C17A | 0.078 (8) | 0.094 (10) | 0.165 (14) | 0.021 (7) | −0.011 (7) | 0.038 (9) |
C17B | 0.069 (6) | 0.046 (5) | 0.089 (5) | −0.004 (4) | 0.030 (4) | 0.003 (4) |
Ni1—N2i | 1.8370 (16) | C11A—C16A | 1.379 (6) |
Ni1—N2 | 1.8370 (16) | C12A—C13A | 1.373 (6) |
Ni1—N3i | 1.8827 (15) | C12A—H12A | 0.9300 |
Ni1—N3 | 1.8827 (15) | C13A—C14A | 1.366 (7) |
O1—N2 | 1.384 (2) | C13A—H13A | 0.9300 |
O1—H11 | 0.92 (3) | C14A—C15A | 1.360 (7) |
O2—N3 | 1.309 (2) | C14A—H14A | 0.9300 |
N1—C9 | 1.338 (3) | C15A—C16A | 1.392 (6) |
N1—C1 | 1.427 (2) | C15A—H15A | 0.9300 |
N1—H21 | 0.81 (2) | C16A—H16A | 0.9300 |
N2—C9 | 1.302 (2) | C11B—C16B | 1.377 (5) |
N3—C10 | 1.305 (2) | C11B—C12B | 1.380 (5) |
C1—C2 | 1.386 (3) | C12B—C13B | 1.371 (5) |
C1—C6 | 1.396 (3) | C12B—H12B | 0.9300 |
C2—C3 | 1.393 (3) | C13B—C14B | 1.365 (6) |
C2—C8 | 1.503 (3) | C13B—H13B | 0.9300 |
C3—C4 | 1.371 (4) | C14B—C15B | 1.362 (6) |
C3—H3 | 0.9300 | C14B—H14B | 0.9300 |
C4—C5 | 1.358 (4) | C15B—C16B | 1.391 (5) |
C4—H4 | 0.9300 | C15B—H15B | 0.9300 |
C5—C6 | 1.382 (3) | C16B—H16B | 0.9300 |
C5—H5 | 0.9300 | O3—S1ii | 1.507 (2) |
C6—C7 | 1.487 (3) | O3—S1 | 1.507 (2) |
C7—H7A | 0.9600 | S1—C17B | 1.670 (7) |
C7—H7B | 0.9600 | S1—C17Aii | 1.670 (7) |
C7—H7C | 0.9600 | S1—C17A | 1.753 (7) |
C8—H8A | 0.9600 | S1—C17Bii | 1.753 (6) |
C8—H8B | 0.9600 | C17A—H17A | 0.9600 |
C8—H8C | 0.9600 | C17A—H17B | 0.9600 |
C9—C10 | 1.475 (3) | C17A—H17C | 0.9600 |
C10—C11A | 1.481 (9) | C17B—H17D | 0.9600 |
C10—C11B | 1.483 (8) | C17B—H17E | 0.9600 |
C11A—C12A | 1.377 (6) | C17B—H17F | 0.9600 |
N2i—Ni1—N2 | 180.00 (10) | C12A—C11A—C10 | 121.4 (9) |
N2i—Ni1—N3i | 81.97 (7) | C16A—C11A—C10 | 119.0 (9) |
N2—Ni1—N3i | 98.03 (7) | C13A—C12A—C11A | 120.4 (4) |
N2i—Ni1—N3 | 98.03 (7) | C13A—C12A—H12A | 119.8 |
N2—Ni1—N3 | 81.97 (7) | C11A—C12A—H12A | 119.8 |
N3i—Ni1—N3 | 180.00 (10) | C14A—C13A—C12A | 120.2 (4) |
N2—O1—H11 | 100.0 (17) | C14A—C13A—H13A | 119.9 |
C9—N1—C1 | 127.03 (17) | C12A—C13A—H13A | 119.9 |
C9—N1—H21 | 118.4 (16) | C15A—C14A—C13A | 120.2 (4) |
C1—N1—H21 | 112.8 (16) | C15A—C14A—H14A | 119.9 |
C9—N2—O1 | 115.22 (16) | C13A—C14A—H14A | 119.9 |
C9—N2—Ni1 | 117.49 (13) | C14A—C15A—C16A | 120.2 (4) |
O1—N2—Ni1 | 125.95 (12) | C14A—C15A—H15A | 119.9 |
C10—N3—O2 | 121.11 (16) | C16A—C15A—H15A | 119.9 |
C10—N3—Ni1 | 116.54 (13) | C11A—C16A—C15A | 119.5 (4) |
O2—N3—Ni1 | 122.15 (12) | C11A—C16A—H16A | 120.2 |
C2—C1—C6 | 122.03 (19) | C15A—C16A—H16A | 120.2 |
C2—C1—N1 | 120.46 (19) | C16B—C11B—C12B | 119.3 (3) |
C6—C1—N1 | 117.41 (18) | C16B—C11B—C10 | 120.6 (8) |
C1—C2—C3 | 117.6 (2) | C12B—C11B—C10 | 120.0 (8) |
C1—C2—C8 | 122.1 (2) | C13B—C12B—C11B | 120.3 (4) |
C3—C2—C8 | 120.2 (2) | C13B—C12B—H12B | 119.9 |
C4—C3—C2 | 120.7 (2) | C11B—C12B—H12B | 119.9 |
C4—C3—H3 | 119.7 | C14B—C13B—C12B | 120.4 (4) |
C2—C3—H3 | 119.7 | C14B—C13B—H13B | 119.8 |
C5—C4—C3 | 120.7 (2) | C12B—C13B—H13B | 119.8 |
C5—C4—H4 | 119.7 | C15B—C14B—C13B | 120.1 (4) |
C3—C4—H4 | 119.7 | C15B—C14B—H14B | 119.9 |
C4—C5—C6 | 121.2 (2) | C13B—C14B—H14B | 119.9 |
C4—C5—H5 | 119.4 | C14B—C15B—C16B | 120.1 (4) |
C6—C5—H5 | 119.4 | C14B—C15B—H15B | 120.0 |
C5—C6—C1 | 117.7 (2) | C16B—C15B—H15B | 120.0 |
C5—C6—C7 | 121.0 (2) | C11B—C16B—C15B | 119.8 (4) |
C1—C6—C7 | 121.24 (19) | C11B—C16B—H16B | 120.1 |
C6—C7—H7A | 109.5 | C15B—C16B—H16B | 120.1 |
C6—C7—H7B | 109.5 | O3—S1—C17B | 111.0 (5) |
H7A—C7—H7B | 109.5 | O3—S1—C17Aii | 109.8 (6) |
C6—C7—H7C | 109.5 | C17B—S1—C17Aii | 104.4 (5) |
H7A—C7—H7C | 109.5 | O3—S1—C17A | 105.6 (6) |
H7B—C7—H7C | 109.5 | C17Aii—S1—C17A | 102.5 (11) |
C2—C8—H8A | 109.5 | O3—S1—C17Bii | 106.7 (4) |
C2—C8—H8B | 109.5 | C17A—S1—C17Bii | 97.6 (6) |
H8A—C8—H8B | 109.5 | S1—C17A—H17A | 107.7 |
C2—C8—H8C | 109.5 | S1—C17A—H17B | 111.3 |
H8A—C8—H8C | 109.5 | H17A—C17A—H17B | 109.5 |
H8B—C8—H8C | 109.5 | S1—C17A—H17C | 109.5 |
N2—C9—N1 | 121.66 (17) | H17A—C17A—H17C | 109.5 |
N2—C9—C10 | 111.96 (17) | H17B—C17A—H17C | 109.5 |
N1—C9—C10 | 126.37 (17) | S1ii—C17B—H17D | 110.0 |
N3—C10—C9 | 111.16 (16) | S1ii—C17B—H17E | 107.4 |
N3—C10—C11A | 122.1 (10) | H17D—C17B—H17E | 109.5 |
C9—C10—C11A | 126.4 (9) | S1ii—C17B—H17F | 111.0 |
N3—C10—C11B | 122.8 (8) | H17D—C17B—H17F | 109.5 |
C9—C10—C11B | 126.0 (8) | H17E—C17B—H17F | 109.5 |
C12A—C11A—C16A | 119.4 (4) | ||
N3i—Ni1—N2—C9 | 172.90 (15) | N1—C9—C10—C11B | −8.0 (9) |
N3—Ni1—N2—C9 | −7.10 (15) | N3—C10—C11A—C12A | −51.8 (18) |
N3i—Ni1—N2—O1 | 6.77 (17) | C9—C10—C11A—C12A | 135.6 (11) |
N3—Ni1—N2—O1 | −173.23 (17) | C11B—C10—C11A—C12A | 47 (16) |
N2i—Ni1—N3—C10 | −178.51 (15) | N3—C10—C11A—C16A | 122.1 (13) |
N2—Ni1—N3—C10 | 1.49 (15) | C9—C10—C11A—C16A | −50 (2) |
N2i—Ni1—N3—O2 | 6.65 (17) | C11B—C10—C11A—C16A | −139 (19) |
N2—Ni1—N3—O2 | −173.35 (17) | C16A—C11A—C12A—C13A | 3.4 (15) |
C9—N1—C1—C2 | −55.9 (3) | C10—C11A—C12A—C13A | 177.3 (18) |
C9—N1—C1—C6 | 127.8 (2) | C11A—C12A—C13A—C14A | −2.8 (11) |
C6—C1—C2—C3 | −2.6 (3) | C12A—C13A—C14A—C15A | −0.3 (13) |
N1—C1—C2—C3 | −178.8 (2) | C13A—C14A—C15A—C16A | 2.9 (14) |
C6—C1—C2—C8 | 174.1 (2) | C12A—C11A—C16A—C15A | −0.9 (19) |
N1—C1—C2—C8 | −2.1 (3) | C10—C11A—C16A—C15A | −174.9 (18) |
C1—C2—C3—C4 | 0.4 (3) | C14A—C15A—C16A—C11A | −2.2 (18) |
C8—C2—C3—C4 | −176.4 (2) | N3—C10—C11B—C16B | 126.9 (12) |
C2—C3—C4—C5 | 1.6 (4) | C9—C10—C11B—C16B | −53.0 (17) |
C3—C4—C5—C6 | −1.4 (4) | C11A—C10—C11B—C16B | 43 (17) |
C4—C5—C6—C1 | −0.7 (4) | N3—C10—C11B—C12B | −55.2 (15) |
C4—C5—C6—C7 | 177.2 (2) | C9—C10—C11B—C12B | 124.9 (9) |
C2—C1—C6—C5 | 2.8 (3) | C11A—C10—C11B—C12B | −140 (19) |
N1—C1—C6—C5 | 179.1 (2) | C16B—C11B—C12B—C13B | −1.2 (13) |
C2—C1—C6—C7 | −175.2 (2) | C10—C11B—C12B—C13B | −179.1 (15) |
N1—C1—C6—C7 | 1.1 (3) | C11B—C12B—C13B—C14B | −1.4 (10) |
O1—N2—C9—N1 | −2.7 (3) | C12B—C13B—C14B—C15B | 3.0 (11) |
Ni1—N2—C9—N1 | −170.31 (15) | C13B—C14B—C15B—C16B | −1.9 (12) |
O1—N2—C9—C10 | 178.21 (16) | C12B—C11B—C16B—C15B | 2.2 (17) |
Ni1—N2—C9—C10 | 10.6 (2) | C10—C11B—C16B—C15B | −179.9 (15) |
C1—N1—C9—N2 | 160.8 (2) | C14B—C15B—C16B—C11B | −0.7 (15) |
C1—N1—C9—C10 | −20.2 (3) | S1ii—O3—S1—C17B | −57.0 (5) |
O2—N3—C10—C9 | 178.40 (17) | S1ii—O3—S1—C17Aii | 57.9 (6) |
Ni1—N3—C10—C9 | 3.5 (2) | S1ii—O3—S1—C17A | −52.0 (5) |
O2—N3—C10—C11A | 4.9 (9) | S1ii—O3—S1—C17Bii | 51.1 (5) |
Ni1—N3—C10—C11A | −170.0 (9) | O3—S1—C17A—S1ii | 52.2 (4) |
O2—N3—C10—C11B | −1.5 (8) | C17B—S1—C17A—S1ii | −168 (8) |
Ni1—N3—C10—C11B | −176.4 (8) | C17Aii—S1—C17A—S1ii | −62.8 (8) |
N2—C9—C10—N3 | −8.9 (2) | C17Bii—S1—C17A—S1ii | −57.6 (5) |
N1—C9—C10—N3 | 172.11 (19) | O3—S1—C17B—S1ii | 53.2 (3) |
N2—C9—C10—C11A | 164.3 (10) | C17Aii—S1—C17B—S1ii | −65.0 (6) |
N1—C9—C10—C11A | −14.7 (10) | C17A—S1—C17B—S1ii | 11 (8) |
N2—C9—C10—C11B | 171.0 (8) | C17Bii—S1—C17B—S1ii | −59.2 (5) |
Symmetry codes: (i) −x, −y+1, −z; (ii) −x, y, −z+1/2. |
D—H···A | D—H | H···A | D···A | D—H···A |
O1—H11···O2i | 0.92 (3) | 1.59 (3) | 2.496 (2) | 169 (3) |
N1—H21···O3iii | 0.81 (2) | 2.21 (2) | 2.933 (2) | 149 (2) |
Symmetry codes: (i) −x, −y+1, −z; (iii) x, y−1, z. |
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