Supporting information
Crystallographic Information File (CIF) https://doi.org/10.1107/S1600536806054080/ng2174sup1.cif | |
Structure factor file (CIF format) https://doi.org/10.1107/S1600536806054080/ng2174Isup2.hkl |
CCDC reference: 633971
Data collection: SMART (Bruker, 2002); cell refinement: SAINT-Plus (Bruker, 2003); data reduction: SAINT-Plus; program(s) used to solve structure: SHELXTL (Bruker, 2003); program(s) used to refine structure: SHELXTL; molecular graphics: SHELXTL; software used to prepare material for publication: SHELXTL.
[Ni2(C5H7O2)4(H2O)2]·0.5H2O | F(000) = 1192.0 |
Mr = 567.89 | Dx = 1.488 Mg m−3 |
Monoclinic, P21/c | Mo Kα radiation, λ = 0.71073 Å |
a = 14.6463 (6) Å | Cell parameters from 9703 reflections |
b = 17.1089 (7) Å | θ = 2.6–30.5° |
c = 10.1294 (4) Å | µ = 1.55 mm−1 |
β = 98.042 (1)° | T = 100 K |
V = 2513.28 (18) Å3 | Block, green |
Z = 4 | 0.50 × 0.42 × 0.33 mm |
Bruker SMART APEX CCD diffractometer | 6087 independent reflections |
Radiation source: fine-focus sealed tube | 5432 reflections with I > 2σ(I) |
Graphite monochromator | Rint = 0.016 |
ω scans | θmax = 28.3°, θmin = 1.8° |
Absorption correction: multi-scan (SADABS in SAINT-Plus; Bruker, 2003) | h = −19→18 |
Tmin = 0.510, Tmax = 0.600 | k = −22→22 |
12866 measured reflections | l = −13→10 |
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)] = 0.031 | Hydrogen site location: inferred from neighbouring sites |
wR(F2) = 0.087 | H atoms treated by a mixture of independent and constrained refinement |
S = 1.04 | w = 1/[σ2(Fo2) + (0.0465P)2 + 1.731P] where P = (Fo2 + 2Fc2)/3 |
6087 reflections | (Δ/σ)max = 0.001 |
324 parameters | Δρmax = 0.50 e Å−3 |
6 restraints | Δρmin = −0.71 e Å−3 |
Geometry. All e.s.d.'s (except the e.s.d. in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell e.s.d.'s are taken into account individually in the estimation of e.s.d.'s in distances, angles and torsion angles; correlations between e.s.d.'s in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell e.s.d.'s is used for estimating e.s.d.'s involving l.s. planes. |
Refinement. Refinement of F2 against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F2, conventional R-factors R are based on F, with F set to zero for negative F2. The threshold expression of F2 > σ(F2) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F2 are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. |
x | y | z | Uiso*/Ueq | ||
C11 | 0.55295 (13) | 0.48358 (12) | 0.35280 (18) | 0.0223 (4) | |
H11A | 0.5449 | 0.4521 | 0.4311 | 0.033* | |
H11B | 0.5534 | 0.5391 | 0.3764 | 0.033* | |
H11C | 0.6115 | 0.4699 | 0.3223 | 0.033* | |
C12 | 0.47512 (12) | 0.46781 (10) | 0.24352 (18) | 0.0167 (3) | |
C13 | 0.39935 (13) | 0.42577 (11) | 0.27441 (18) | 0.0196 (3) | |
H13 | 0.4014 | 0.4099 | 0.3646 | 0.024* | |
C14 | 0.32004 (12) | 0.40426 (10) | 0.18651 (18) | 0.0183 (3) | |
C15 | 0.24261 (13) | 0.36572 (12) | 0.24594 (19) | 0.0237 (4) | |
H15A | 0.2616 | 0.3131 | 0.2768 | 0.036* | |
H15B | 0.1880 | 0.3621 | 0.1782 | 0.036* | |
H15C | 0.2279 | 0.3968 | 0.3214 | 0.036* | |
C16 | 0.56726 (15) | 0.23548 (12) | −0.0258 (2) | 0.0287 (4) | |
H16A | 0.5469 | 0.2077 | 0.0495 | 0.043* | |
H16B | 0.6267 | 0.2608 | 0.0034 | 0.043* | |
H16C | 0.5740 | 0.1982 | −0.0973 | 0.043* | |
C17 | 0.49657 (12) | 0.29680 (10) | −0.07690 (19) | 0.0194 (3) | |
C18 | 0.44154 (13) | 0.28484 (11) | −0.19907 (19) | 0.0224 (4) | |
H18 | 0.4532 | 0.2394 | −0.2479 | 0.027* | |
C19 | 0.37041 (13) | 0.33425 (11) | −0.25588 (18) | 0.0198 (4) | |
C20 | 0.31892 (15) | 0.31323 (12) | −0.39129 (19) | 0.0282 (4) | |
H20A | 0.3360 | 0.3497 | −0.4583 | 0.042* | |
H20B | 0.2524 | 0.3165 | −0.3887 | 0.042* | |
H20C | 0.3351 | 0.2599 | −0.4146 | 0.042* | |
Ni1 | 0.410350 (15) | 0.449636 (13) | −0.04321 (2) | 0.01399 (7) | |
O6 | 0.48145 (8) | 0.49627 (7) | 0.12719 (12) | 0.0154 (2) | |
O7 | 0.30963 (8) | 0.41357 (7) | 0.06101 (12) | 0.0182 (3) | |
O8 | 0.49271 (9) | 0.35553 (7) | −0.00039 (13) | 0.0182 (3) | |
O9 | 0.34545 (9) | 0.39716 (8) | −0.20530 (12) | 0.0191 (3) | |
O10 | 0.34541 (9) | 0.55644 (8) | −0.08983 (13) | 0.0184 (3) | |
H10E | 0.3859 (15) | 0.5885 (13) | −0.067 (2) | 0.028* | |
H10D | 0.3009 (15) | 0.5679 (15) | −0.049 (2) | 0.028* | |
C1 | 0.18306 (18) | 0.68348 (15) | −0.3499 (2) | 0.0379 (5) | |
H1A | 0.2487 | 0.6754 | −0.3185 | 0.057* | |
H1B | 0.1723 | 0.7384 | −0.3745 | 0.057* | |
H1C | 0.1642 | 0.6503 | −0.4279 | 0.057* | |
C2 | 0.12759 (14) | 0.66233 (12) | −0.24058 (19) | 0.0257 (4) | |
C3 | 0.07519 (16) | 0.71996 (12) | −0.1882 (2) | 0.0309 (5) | |
H3 | 0.0784 | 0.7713 | −0.2229 | 0.037* | |
C4 | 0.01869 (14) | 0.70909 (12) | −0.0898 (2) | 0.0269 (4) | |
C5 | −0.04041 (18) | 0.77650 (14) | −0.0545 (3) | 0.0405 (6) | |
H5A | −0.1057 | 0.7627 | −0.0769 | 0.061* | |
H5B | −0.0271 | 0.8230 | −0.1050 | 0.061* | |
H5C | −0.0267 | 0.7874 | 0.0412 | 0.061* | |
C6A | 0.04130 (17) | 0.4831 (2) | 0.3536 (2) | 0.0485 (8) | |
H6A | −0.0182 | 0.5084 | 0.3576 | 0.073* | |
H6B | 0.0819 | 0.4915 | 0.4378 | 0.073* | |
H6C | 0.0319 | 0.4269 | 0.3387 | 0.073* | |
C7 | 0.08459 (13) | 0.51728 (12) | 0.24156 (18) | 0.0222 (4) | |
C8 | 0.16802 (13) | 0.55714 (12) | 0.27275 (19) | 0.0242 (4) | |
H8 | 0.1897 | 0.5644 | 0.3648 | 0.029* | |
C9 | 0.22305 (12) | 0.58753 (10) | 0.18286 (19) | 0.0192 (4) | |
C10 | 0.31405 (13) | 0.62424 (12) | 0.2382 (2) | 0.0252 (4) | |
H10A | 0.3631 | 0.6020 | 0.1932 | 0.038* | |
H10B | 0.3273 | 0.6137 | 0.3341 | 0.038* | |
H10C | 0.3109 | 0.6808 | 0.2233 | 0.038* | |
Ni2 | 0.083411 (15) | 0.547886 (13) | −0.04688 (2) | 0.01583 (7) | |
O1 | 0.13137 (9) | 0.59080 (8) | −0.20634 (13) | 0.0221 (3) | |
O2 | 0.01126 (9) | 0.64619 (8) | −0.02487 (14) | 0.0232 (3) | |
O3 | 0.04295 (8) | 0.50577 (7) | 0.12348 (12) | 0.0173 (2) | |
O4 | 0.20334 (9) | 0.58637 (8) | 0.05629 (13) | 0.0198 (3) | |
O5 | 0.13496 (9) | 0.43697 (8) | −0.08245 (14) | 0.0207 (3) | |
H5D | 0.1868 (13) | 0.4263 (15) | −0.047 (2) | 0.031* | |
H5E | 0.0986 (16) | 0.4041 (13) | −0.059 (3) | 0.031* | |
O11 | 0.20986 (14) | 0.48668 (13) | −0.37718 (19) | 0.0503 (5) | |
H11D | 0.251 (2) | 0.4472 (17) | −0.334 (4) | 0.075* | |
H11E | 0.185 (2) | 0.5259 (18) | −0.323 (3) | 0.075* |
U11 | U22 | U33 | U12 | U13 | U23 | |
C11 | 0.0223 (9) | 0.0287 (10) | 0.0152 (8) | −0.0061 (7) | −0.0001 (7) | 0.0024 (7) |
C12 | 0.0161 (8) | 0.0163 (8) | 0.0177 (8) | 0.0014 (6) | 0.0026 (6) | 0.0009 (6) |
C13 | 0.0203 (9) | 0.0235 (9) | 0.0153 (8) | −0.0030 (7) | 0.0030 (7) | 0.0029 (7) |
C14 | 0.0167 (8) | 0.0166 (8) | 0.0219 (9) | 0.0007 (6) | 0.0041 (7) | 0.0016 (6) |
C15 | 0.0204 (9) | 0.0273 (10) | 0.0241 (9) | −0.0048 (7) | 0.0062 (7) | 0.0021 (8) |
C16 | 0.0279 (10) | 0.0214 (9) | 0.0364 (11) | 0.0064 (8) | 0.0032 (9) | 0.0025 (8) |
C17 | 0.0176 (8) | 0.0169 (8) | 0.0248 (9) | −0.0010 (6) | 0.0069 (7) | 0.0025 (7) |
C18 | 0.0263 (10) | 0.0182 (9) | 0.0233 (9) | −0.0023 (7) | 0.0062 (7) | −0.0036 (7) |
C19 | 0.0207 (9) | 0.0216 (9) | 0.0174 (8) | −0.0080 (7) | 0.0042 (7) | 0.0008 (7) |
C20 | 0.0343 (11) | 0.0289 (10) | 0.0205 (9) | −0.0102 (8) | 0.0011 (8) | −0.0013 (8) |
Ni1 | 0.01110 (12) | 0.01626 (12) | 0.01436 (11) | 0.00031 (7) | 0.00090 (8) | 0.00135 (8) |
O6 | 0.0134 (6) | 0.0187 (6) | 0.0145 (5) | 0.0003 (4) | 0.0028 (4) | 0.0021 (4) |
O7 | 0.0144 (6) | 0.0210 (6) | 0.0193 (6) | −0.0004 (5) | 0.0029 (5) | 0.0023 (5) |
O8 | 0.0157 (6) | 0.0180 (6) | 0.0204 (6) | 0.0010 (5) | 0.0005 (5) | 0.0012 (5) |
O9 | 0.0166 (6) | 0.0220 (6) | 0.0177 (6) | −0.0021 (5) | −0.0006 (5) | 0.0009 (5) |
O10 | 0.0135 (6) | 0.0200 (6) | 0.0217 (6) | 0.0010 (5) | 0.0023 (5) | 0.0008 (5) |
C1 | 0.0413 (13) | 0.0382 (13) | 0.0347 (12) | −0.0130 (10) | 0.0070 (10) | 0.0085 (10) |
C2 | 0.0233 (9) | 0.0300 (10) | 0.0217 (9) | −0.0097 (8) | −0.0042 (7) | 0.0031 (8) |
C3 | 0.0397 (12) | 0.0201 (10) | 0.0306 (11) | −0.0047 (8) | −0.0028 (9) | 0.0022 (8) |
C4 | 0.0250 (10) | 0.0218 (9) | 0.0305 (10) | 0.0009 (7) | −0.0082 (8) | −0.0054 (8) |
C5 | 0.0413 (13) | 0.0262 (11) | 0.0514 (15) | 0.0074 (10) | −0.0023 (11) | −0.0070 (10) |
C6A | 0.0248 (11) | 0.107 (2) | 0.0135 (9) | −0.0238 (13) | 0.0030 (8) | 0.0019 (12) |
C7 | 0.0149 (8) | 0.0346 (11) | 0.0170 (8) | 0.0012 (7) | 0.0020 (7) | −0.0041 (7) |
C8 | 0.0182 (9) | 0.0355 (11) | 0.0180 (8) | −0.0006 (7) | −0.0001 (7) | −0.0091 (7) |
C9 | 0.0144 (8) | 0.0171 (8) | 0.0252 (9) | 0.0019 (6) | −0.0004 (7) | −0.0048 (7) |
C10 | 0.0184 (9) | 0.0246 (10) | 0.0306 (10) | −0.0038 (7) | −0.0030 (8) | −0.0048 (8) |
Ni2 | 0.01107 (12) | 0.02000 (13) | 0.01611 (12) | 0.00043 (8) | 0.00084 (8) | 0.00029 (8) |
O1 | 0.0182 (6) | 0.0268 (7) | 0.0213 (6) | −0.0013 (5) | 0.0024 (5) | 0.0031 (5) |
O2 | 0.0185 (6) | 0.0229 (7) | 0.0272 (7) | 0.0029 (5) | −0.0001 (5) | −0.0022 (5) |
O3 | 0.0123 (6) | 0.0240 (6) | 0.0154 (5) | −0.0004 (5) | 0.0010 (4) | −0.0008 (5) |
O4 | 0.0140 (6) | 0.0233 (7) | 0.0212 (6) | −0.0017 (5) | −0.0001 (5) | 0.0004 (5) |
O5 | 0.0142 (6) | 0.0240 (7) | 0.0238 (7) | 0.0017 (5) | 0.0019 (5) | 0.0007 (5) |
O11 | 0.0447 (11) | 0.0678 (14) | 0.0368 (10) | 0.0120 (10) | −0.0003 (8) | −0.0017 (9) |
C11—C12 | 1.498 (2) | C1—H1A | 0.9800 |
C11—H11A | 0.9800 | C1—H1B | 0.9800 |
C11—H11B | 0.9800 | C1—H1C | 0.9800 |
C11—H11C | 0.9800 | C2—O1 | 1.271 (2) |
C12—O6 | 1.290 (2) | C2—C3 | 1.399 (3) |
C12—C13 | 1.394 (2) | C3—C4 | 1.394 (3) |
C13—C14 | 1.410 (3) | C3—H3 | 0.9500 |
C13—H13 | 0.9500 | C4—O2 | 1.274 (3) |
C14—O7 | 1.269 (2) | C4—C5 | 1.514 (3) |
C14—C15 | 1.508 (2) | C5—H5A | 0.9800 |
C15—H15A | 0.9800 | C5—H5B | 0.9800 |
C15—H15B | 0.9800 | C5—H5C | 0.9800 |
C15—H15C | 0.9800 | C6A—C7 | 1.494 (3) |
C16—C17 | 1.513 (3) | C6A—H6A | 0.9800 |
C16—H16A | 0.9800 | C6A—H6B | 0.9800 |
C16—H16B | 0.9800 | C6A—H6C | 0.9800 |
C16—H16C | 0.9800 | C7—O3 | 1.280 (2) |
C17—O8 | 1.275 (2) | C7—C8 | 1.397 (3) |
C17—C18 | 1.394 (3) | C8—C9 | 1.398 (3) |
C18—C19 | 1.401 (3) | C8—H8 | 0.9500 |
C18—H18 | 0.9500 | C9—O4 | 1.274 (2) |
C19—O9 | 1.268 (2) | C9—C10 | 1.509 (2) |
C19—C20 | 1.513 (3) | C10—H10A | 0.9800 |
C20—H20A | 0.9800 | C10—H10B | 0.9800 |
C20—H20B | 0.9800 | C10—H10C | 0.9800 |
C20—H20C | 0.9800 | Ni2—O1 | 1.9897 (13) |
Ni1—O9 | 1.9921 (13) | Ni2—O2 | 2.0151 (13) |
Ni1—O8 | 2.0221 (13) | Ni2—O4 | 2.0242 (13) |
Ni1—O7 | 2.0265 (12) | Ni2—O3 | 2.0333 (13) |
Ni1—O6 | 2.0487 (12) | Ni2—O5 | 2.0921 (14) |
Ni1—O10 | 2.0835 (13) | Ni2—O3ii | 2.1138 (12) |
Ni1—O6i | 2.1139 (12) | O3—Ni2ii | 2.1138 (12) |
O6—Ni1i | 2.1139 (12) | O5—H5D | 0.813 (17) |
O10—H10E | 0.816 (16) | O5—H5E | 0.831 (17) |
O10—H10D | 0.843 (16) | O11—H11D | 0.970 (18) |
C1—C2 | 1.506 (3) | O11—H11E | 0.972 (18) |
C12—C11—H11A | 109.5 | C2—C1—H1B | 109.5 |
C12—C11—H11B | 109.5 | H1A—C1—H1B | 109.5 |
H11A—C11—H11B | 109.5 | C2—C1—H1C | 109.5 |
C12—C11—H11C | 109.5 | H1A—C1—H1C | 109.5 |
H11A—C11—H11C | 109.5 | H1B—C1—H1C | 109.5 |
H11B—C11—H11C | 109.5 | O1—C2—C3 | 125.48 (19) |
O6—C12—C13 | 124.11 (16) | O1—C2—C1 | 115.1 (2) |
O6—C12—C11 | 117.54 (16) | C3—C2—C1 | 119.38 (19) |
C13—C12—C11 | 118.32 (16) | C4—C3—C2 | 126.10 (19) |
C12—C13—C14 | 127.17 (17) | C4—C3—H3 | 116.9 |
C12—C13—H13 | 116.4 | C2—C3—H3 | 116.9 |
C14—C13—H13 | 116.4 | O2—C4—C3 | 125.71 (19) |
O7—C14—C13 | 124.94 (16) | O2—C4—C5 | 115.4 (2) |
O7—C14—C15 | 117.59 (16) | C3—C4—C5 | 118.9 (2) |
C13—C14—C15 | 117.46 (16) | C4—C5—H5A | 109.5 |
C14—C15—H15A | 109.5 | C4—C5—H5B | 109.5 |
C14—C15—H15B | 109.5 | H5A—C5—H5B | 109.5 |
H15A—C15—H15B | 109.5 | C4—C5—H5C | 109.5 |
C14—C15—H15C | 109.5 | H5A—C5—H5C | 109.5 |
H15A—C15—H15C | 109.5 | H5B—C5—H5C | 109.5 |
H15B—C15—H15C | 109.5 | C7—C6A—H6A | 109.5 |
C17—C16—H16A | 109.5 | C7—C6A—H6B | 109.5 |
C17—C16—H16B | 109.5 | H6A—C6A—H6B | 109.5 |
H16A—C16—H16B | 109.5 | C7—C6A—H6C | 109.5 |
C17—C16—H16C | 109.5 | H6A—C6A—H6C | 109.5 |
H16A—C16—H16C | 109.5 | H6B—C6A—H6C | 109.5 |
H16B—C16—H16C | 109.5 | O3—C7—C8 | 125.04 (18) |
O8—C17—C18 | 125.86 (17) | O3—C7—C6A | 116.88 (17) |
O8—C17—C16 | 115.15 (17) | C8—C7—C6A | 118.05 (17) |
C18—C17—C16 | 118.99 (17) | C7—C8—C9 | 126.89 (18) |
C17—C18—C19 | 125.47 (17) | C7—C8—H8 | 116.6 |
C17—C18—H18 | 117.3 | C9—C8—H8 | 116.6 |
C19—C18—H18 | 117.3 | O4—C9—C8 | 125.41 (17) |
O9—C19—C18 | 125.88 (17) | O4—C9—C10 | 116.38 (17) |
O9—C19—C20 | 115.65 (17) | C8—C9—C10 | 118.21 (17) |
C18—C19—C20 | 118.46 (17) | C9—C10—H10A | 109.5 |
C19—C20—H20A | 109.5 | C9—C10—H10B | 109.5 |
C19—C20—H20B | 109.5 | H10A—C10—H10B | 109.5 |
H20A—C20—H20B | 109.5 | C9—C10—H10C | 109.5 |
C19—C20—H20C | 109.5 | H10A—C10—H10C | 109.5 |
H20A—C20—H20C | 109.5 | H10B—C10—H10C | 109.5 |
H20B—C20—H20C | 109.5 | O1—Ni2—O2 | 91.83 (6) |
O9—Ni1—O8 | 91.12 (5) | O1—Ni2—O4 | 85.39 (5) |
O9—Ni1—O7 | 89.65 (5) | O2—Ni2—O4 | 95.85 (5) |
O8—Ni1—O7 | 95.84 (5) | O1—Ni2—O3 | 176.06 (5) |
O9—Ni1—O6 | 175.99 (5) | O2—Ni2—O3 | 88.99 (5) |
O8—Ni1—O6 | 84.94 (5) | O4—Ni2—O3 | 90.69 (5) |
O7—Ni1—O6 | 90.05 (5) | O1—Ni2—O5 | 91.03 (6) |
O9—Ni1—O10 | 93.35 (5) | O2—Ni2—O5 | 169.58 (6) |
O8—Ni1—O10 | 170.62 (5) | O4—Ni2—O5 | 94.36 (5) |
O7—Ni1—O10 | 92.44 (5) | O3—Ni2—O5 | 88.84 (5) |
O6—Ni1—O10 | 90.66 (5) | O1—Ni2—O3ii | 104.64 (5) |
O9—Ni1—O6i | 99.43 (5) | O2—Ni2—O3ii | 87.55 (5) |
O8—Ni1—O6i | 88.66 (5) | O4—Ni2—O3ii | 169.34 (5) |
O7—Ni1—O6i | 169.80 (5) | O3—Ni2—O3ii | 79.25 (5) |
O6—Ni1—O6i | 81.21 (5) | O5—Ni2—O3ii | 82.03 (5) |
O10—Ni1—O6i | 82.47 (5) | C2—O1—Ni2 | 124.74 (13) |
C12—O6—Ni1 | 121.97 (11) | C4—O2—Ni2 | 124.35 (13) |
C12—O6—Ni1i | 133.34 (11) | C7—O3—Ni2 | 125.55 (12) |
Ni1—O6—Ni1i | 98.79 (5) | C7—O3—Ni2ii | 133.49 (12) |
C14—O7—Ni1 | 124.46 (12) | Ni2—O3—Ni2ii | 100.75 (5) |
C17—O8—Ni1 | 124.96 (12) | C9—O4—Ni2 | 125.63 (12) |
C19—O9—Ni1 | 125.76 (12) | Ni2—O5—H5D | 117.7 (19) |
Ni1—O10—H10E | 103.6 (18) | Ni2—O5—H5E | 107.7 (18) |
Ni1—O10—H10D | 116.9 (17) | H5D—O5—H5E | 109 (3) |
H10E—O10—H10D | 107 (2) | H11D—O11—H11E | 119 (3) |
C2—C1—H1A | 109.5 | ||
O6—C12—C13—C14 | 2.9 (3) | C1—C2—C3—C4 | 178.2 (2) |
C11—C12—C13—C14 | −179.35 (18) | C2—C3—C4—O2 | 5.6 (3) |
C12—C13—C14—O7 | 7.4 (3) | C2—C3—C4—C5 | −174.1 (2) |
C12—C13—C14—C15 | −173.97 (18) | O3—C7—C8—C9 | −3.7 (3) |
O8—C17—C18—C19 | −2.4 (3) | C6A—C7—C8—C9 | 174.3 (2) |
C16—C17—C18—C19 | 176.68 (18) | C7—C8—C9—O4 | 3.2 (3) |
C17—C18—C19—O9 | 0.2 (3) | C7—C8—C9—C10 | −176.18 (19) |
C17—C18—C19—C20 | 178.60 (18) | C3—C2—O1—Ni2 | −12.4 (3) |
C13—C12—O6—Ni1 | −25.2 (2) | C1—C2—O1—Ni2 | 169.49 (14) |
C11—C12—O6—Ni1 | 156.99 (13) | O2—Ni2—O1—C2 | 14.50 (15) |
C13—C12—O6—Ni1i | −172.02 (13) | O4—Ni2—O1—C2 | −81.22 (15) |
C11—C12—O6—Ni1i | 10.2 (2) | O5—Ni2—O1—C2 | −175.51 (15) |
O8—Ni1—O6—C12 | −66.81 (13) | O3ii—Ni2—O1—C2 | 102.45 (15) |
O7—Ni1—O6—C12 | 29.04 (13) | C3—C4—O2—Ni2 | 1.8 (3) |
O10—Ni1—O6—C12 | 121.48 (13) | C5—C4—O2—Ni2 | −178.43 (14) |
O6i—Ni1—O6—C12 | −156.24 (15) | O1—Ni2—O2—C4 | −9.40 (15) |
O8—Ni1—O6—Ni1i | 89.42 (5) | O4—Ni2—O2—C4 | 76.16 (15) |
O7—Ni1—O6—Ni1i | −174.72 (5) | O3—Ni2—O2—C4 | 166.74 (15) |
O10—Ni1—O6—Ni1i | −82.28 (5) | O5—Ni2—O2—C4 | −115.3 (3) |
O6i—Ni1—O6—Ni1i | 0.0 | O3ii—Ni2—O2—C4 | −113.98 (15) |
C13—C14—O7—Ni1 | 7.6 (3) | C8—C7—O3—Ni2 | −3.9 (3) |
C15—C14—O7—Ni1 | −171.04 (12) | C6A—C7—O3—Ni2 | 178.03 (17) |
O9—Ni1—O7—C14 | 155.30 (14) | C8—C7—O3—Ni2ii | −177.62 (14) |
O8—Ni1—O7—C14 | 64.21 (14) | C6A—C7—O3—Ni2ii | 4.3 (3) |
O6—Ni1—O7—C14 | −20.70 (14) | O2—Ni2—O3—C7 | −87.69 (15) |
O10—Ni1—O7—C14 | −111.37 (14) | O4—Ni2—O3—C7 | 8.16 (15) |
O6i—Ni1—O7—C14 | −51.6 (3) | O5—Ni2—O3—C7 | 102.50 (15) |
C18—C17—O8—Ni1 | −3.9 (3) | O3ii—Ni2—O3—C7 | −175.39 (17) |
C16—C17—O8—Ni1 | 176.92 (12) | O2—Ni2—O3—Ni2ii | 87.70 (6) |
O9—Ni1—O8—C17 | 8.40 (14) | O4—Ni2—O3—Ni2ii | −176.46 (6) |
O7—Ni1—O8—C17 | 98.16 (14) | O5—Ni2—O3—Ni2ii | −82.11 (6) |
O6—Ni1—O8—C17 | −172.30 (14) | O3ii—Ni2—O3—Ni2ii | 0.0 |
O6i—Ni1—O8—C17 | −91.01 (14) | C8—C9—O4—Ni2 | 5.0 (3) |
C18—C19—O9—Ni1 | 8.2 (3) | C10—C9—O4—Ni2 | −175.70 (12) |
C20—C19—O9—Ni1 | −170.28 (12) | O1—Ni2—O4—C9 | 171.75 (15) |
O8—Ni1—O9—C19 | −10.46 (14) | O2—Ni2—O4—C9 | 80.38 (15) |
O7—Ni1—O9—C19 | −106.30 (14) | O3—Ni2—O4—C9 | −8.67 (15) |
O10—Ni1—O9—C19 | 161.28 (14) | O5—Ni2—O4—C9 | −97.56 (15) |
O6i—Ni1—O9—C19 | 78.37 (14) | O3ii—Ni2—O4—C9 | −27.8 (4) |
O1—C2—C3—C4 | 0.2 (3) |
Symmetry codes: (i) −x+1, −y+1, −z; (ii) −x, −y+1, −z. |
D—H···A | D—H | H···A | D···A | D—H···A |
O5—H5D···O7 | 0.81 (2) | 1.98 (2) | 2.7887 (18) | 170 (3) |
O5—H5E···O2ii | 0.83 (2) | 2.11 (2) | 2.906 (2) | 161 (2) |
O10—H10E···O8i | 0.82 (2) | 2.05 (2) | 2.8494 (18) | 166 (2) |
O10—H10D···O4 | 0.84 (2) | 1.92 (2) | 2.7649 (19) | 175 (3) |
O11—H11D···O9 | 0.97 (2) | 1.96 (2) | 2.890 (2) | 160 (3) |
O11—H11E···O1 | 0.97 (2) | 1.87 (2) | 2.836 (2) | 173 (3) |
Symmetry codes: (i) −x+1, −y+1, −z; (ii) −x, −y+1, −z. |