Supporting information
Crystallographic Information File (CIF) https://doi.org/10.1107/S2052520617004334/eb5059sup1.cif | |
Structure factor file (CIF format) https://doi.org/10.1107/S2052520617004334/eb5059mn2293sup2.hkl | |
Structure factor file (CIF format) https://doi.org/10.1107/S2052520617004334/eb5059180csup3.hkl | |
Structure factor file (CIF format) https://doi.org/10.1107/S2052520617004334/eb5059298dsup4.hkl | |
Structure factor file (CIF format) https://doi.org/10.1107/S2052520617004334/eb5059280dsup5.hkl | |
Structure factor file (CIF format) https://doi.org/10.1107/S2052520617004334/eb5059260dsup6.hkl | |
Structure factor file (CIF format) https://doi.org/10.1107/S2052520617004334/eb5059240dsup7.hkl | |
Structure factor file (CIF format) https://doi.org/10.1107/S2052520617004334/eb5059220dsup8.hkl | |
Structure factor file (CIF format) https://doi.org/10.1107/S2052520617004334/eb5059200dsup9.hkl | |
Structure factor file (CIF format) https://doi.org/10.1107/S2052520617004334/eb5059160dsup10.hkl | |
Structure factor file (CIF format) https://doi.org/10.1107/S2052520617004334/eb5059140dsup11.hkl | |
Structure factor file (CIF format) https://doi.org/10.1107/S2052520617004334/eb5059120dsup12.hkl | |
Structure factor file (CIF format) https://doi.org/10.1107/S2052520617004334/eb5059100dsup13.hkl | |
Structure factor file (CIF format) https://doi.org/10.1107/S2052520617004334/eb5059150usup14.hkl | |
Structure factor file (CIF format) https://doi.org/10.1107/S2052520617004334/eb5059200usup15.hkl | |
Structure factor file (CIF format) https://doi.org/10.1107/S2052520617004334/eb5059250usup16.hkl | |
Structure factor file (CIF format) https://doi.org/10.1107/S2052520617004334/eb5059298usup17.hkl | |
Portable Document Format (PDF) file https://doi.org/10.1107/S2052520617004334/eb5059sup18.pdf |
Data collection: Apex 2 (Bruker, 2015) for mn2293; Apex 3 (Bruker, 2015) for 180c, 298d. Cell refinement: SAINT V8.37A (Bruker, 2015) for mn2293; SAINT (Bruker, 2015) for 180c, 298d. Data reduction: SAINT V8.37A (Bruker, 2015) for mn2293; SAINT (Bruker, 2015) for 180c, 298d. Program(s) used to solve structure: SHELXT (Sheldrick, 2015) for mn2293; SHELXS (Shedldrick, 2015) for 180c, 298d. For all compounds, program(s) used to refine structure: SHELXL2016/6 (Sheldrick, 2016); software used to prepare material for publication: SHELXL2016/6 (Sheldrick, 2016).
C14H12N2NiO10·2(C14H10N2NiO9)·C14H7N2NiO8·H3O·7(H2O) | Z = 2 |
Mr = 1779.92 | F(000) = 1824 |
Triclinic, P1 | Dx = 1.777 Mg m−3 |
a = 13.7266 (12) Å | Mo Kα radiation, λ = 0.71073 Å |
b = 16.9157 (15) Å | Cell parameters from 9917 reflections |
c = 16.9080 (14) Å | θ = 2.5–28.3° |
α = 69.7619 (11)° | µ = 1.24 mm−1 |
β = 69.3377 (11)° | T = 90 K |
γ = 69.3655 (11)° | Block, blue-green |
V = 3325.9 (5) Å3 | 0.41 × 0.25 × 0.17 mm |
Bruker Apex II diffractometer | 16469 independent reflections |
Radiation source: fine-focus sealed tube | 16170 reflections with I > 2σ(I) |
Detector resolution: 8.3 pixels mm-1 | Rint = 0.018 |
ω scans | θmax = 28.3°, θmin = 1.6° |
Absorption correction: multi-scan SADABS (Sheldrick, 2014) | h = −18→18 |
Tmin = 0.655, Tmax = 0.746 | k = −22→22 |
46008 measured reflections | l = −22→22 |
Refinement on F2 | 0 restraints |
Least-squares matrix: full | Hydrogen site location: mixed |
R[F2 > 2σ(F2)] = 0.020 | H atoms treated by a mixture of independent and constrained refinement |
wR(F2) = 0.055 | w = 1/[σ2(Fo2) + (0.0308P)2 + 0.791P] where P = (Fo2 + 2Fc2)/3 |
S = 1.03 | (Δ/σ)max = 0.002 |
16469 reflections | Δρmax = 0.50 e Å−3 |
1138 parameters | Δρmin = −0.59 e Å−3 |
Geometry. All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. |
Refinement. Refined as a 2-component twin. Hydrogen atoms not bonded to carbon were fully refined. |
x | y | z | Uiso*/Ueq | ||
Ni1 | 0.24678 (2) | 0.62448 (2) | 0.12902 (2) | 0.00918 (4) | |
O1 | 0.29354 (8) | 0.49888 (7) | 0.21576 (7) | 0.0124 (2) | |
O2 | 0.28983 (9) | 0.43838 (7) | 0.35757 (7) | 0.0142 (2) | |
O3 | 0.06519 (9) | 0.87063 (7) | 0.15950 (7) | 0.0186 (2) | |
O4 | 0.17118 (8) | 0.76087 (7) | 0.09594 (7) | 0.0132 (2) | |
O5 | 0.12593 (8) | 0.59332 (7) | 0.10481 (7) | 0.0127 (2) | |
O6 | 0.09988 (8) | 0.54432 (7) | 0.00856 (7) | 0.0138 (2) | |
O7 | 0.56025 (8) | 0.64301 (7) | −0.00611 (7) | 0.0147 (2) | |
O8 | 0.40549 (8) | 0.64381 (7) | 0.10108 (7) | 0.01242 (19) | |
N1 | 0.18288 (9) | 0.65059 (8) | 0.24453 (8) | 0.0097 (2) | |
N2 | 0.31990 (9) | 0.59977 (8) | 0.01385 (8) | 0.0097 (2) | |
C1 | 0.26525 (11) | 0.50131 (9) | 0.29390 (9) | 0.0110 (3) | |
C2 | 0.19698 (11) | 0.58628 (9) | 0.31601 (9) | 0.0105 (3) | |
C3 | 0.15309 (11) | 0.60120 (10) | 0.39871 (9) | 0.0137 (3) | |
H3 | 0.162028 | 0.555133 | 0.449441 | 0.016* | |
C4 | 0.09540 (12) | 0.68612 (11) | 0.40484 (10) | 0.0149 (3) | |
H4 | 0.065198 | 0.698597 | 0.460504 | 0.018* | |
C5 | 0.08173 (11) | 0.75267 (10) | 0.33013 (10) | 0.0131 (3) | |
H5 | 0.042378 | 0.810644 | 0.333798 | 0.016* | |
C6 | 0.12737 (11) | 0.73185 (9) | 0.24992 (9) | 0.0114 (3) | |
C7 | 0.11944 (11) | 0.79473 (9) | 0.16172 (10) | 0.0125 (3) | |
C8 | 0.15468 (11) | 0.57093 (9) | 0.03416 (9) | 0.0110 (3) | |
C9 | 0.26670 (11) | 0.57688 (9) | −0.02345 (9) | 0.0103 (2) | |
C10 | 0.31350 (11) | 0.56102 (10) | −0.10590 (9) | 0.0125 (3) | |
H10 | 0.275368 | 0.544710 | −0.132355 | 0.015* | |
C11 | 0.41804 (12) | 0.56972 (10) | −0.14869 (9) | 0.0131 (3) | |
H11 | 0.451859 | 0.559532 | −0.205190 | 0.016* | |
C12 | 0.47295 (11) | 0.59332 (9) | −0.10876 (9) | 0.0116 (3) | |
H12 | 0.544272 | 0.599215 | −0.136996 | 0.014* | |
C13 | 0.42023 (11) | 0.60788 (9) | −0.02665 (9) | 0.0103 (2) | |
C14 | 0.46563 (11) | 0.63352 (9) | 0.02710 (9) | 0.0109 (3) | |
Ni2 | 0.25329 (2) | 0.12175 (2) | 0.11808 (2) | 0.00967 (4) | |
O9 | 0.10055 (8) | 0.14844 (7) | 0.09529 (7) | 0.0135 (2) | |
O10 | −0.05740 (8) | 0.25189 (7) | 0.09740 (7) | 0.0161 (2) | |
O11 | 0.39904 (8) | 0.23826 (7) | 0.20297 (7) | 0.0142 (2) | |
O12 | 0.37077 (8) | 0.14356 (7) | 0.15385 (7) | 0.01317 (19) | |
O13 | 0.32874 (8) | 0.16257 (7) | −0.01668 (7) | 0.0136 (2) | |
O14 | 0.43321 (10) | 0.10624 (8) | −0.13125 (7) | 0.0208 (2) | |
O15 | 0.21858 (8) | −0.11661 (7) | 0.29451 (7) | 0.0148 (2) | |
H15 | 0.157 (2) | −0.099 (2) | 0.355 (2) | 0.067 (9)* | |
O16 | 0.21067 (8) | 0.02623 (7) | 0.24196 (7) | 0.0134 (2) | |
N3 | 0.17856 (10) | 0.23468 (8) | 0.14631 (8) | 0.0102 (2) | |
N4 | 0.31764 (9) | 0.00931 (8) | 0.08610 (8) | 0.0103 (2) | |
C15 | 0.03645 (11) | 0.22107 (9) | 0.10764 (9) | 0.0114 (3) | |
C16 | 0.07836 (11) | 0.27440 (9) | 0.13732 (9) | 0.0104 (3) | |
C17 | 0.02435 (11) | 0.35565 (9) | 0.15362 (9) | 0.0122 (3) | |
H17 | −0.047196 | 0.383352 | 0.148129 | 0.015* | |
C18 | 0.07831 (12) | 0.39569 (9) | 0.17840 (9) | 0.0125 (3) | |
H18 | 0.043361 | 0.451557 | 0.189867 | 0.015* | |
C19 | 0.18360 (12) | 0.35391 (9) | 0.18640 (9) | 0.0130 (3) | |
H19 | 0.221593 | 0.380934 | 0.202179 | 0.016* | |
C20 | 0.23069 (11) | 0.27167 (9) | 0.17053 (9) | 0.0106 (3) | |
C21 | 0.34265 (11) | 0.21374 (9) | 0.17667 (9) | 0.0112 (3) | |
C22 | 0.37979 (11) | 0.09982 (10) | −0.05469 (9) | 0.0135 (3) | |
C23 | 0.37138 (10) | 0.01018 (10) | 0.00321 (9) | 0.0115 (2) | |
C24 | 0.41561 (11) | −0.06645 (10) | −0.02480 (10) | 0.0138 (3) | |
H24 | 0.455010 | −0.065778 | −0.083758 | 0.017* | |
C25 | 0.40030 (12) | −0.14390 (10) | 0.03622 (10) | 0.0158 (3) | |
H25 | 0.428728 | −0.197056 | 0.018782 | 0.019* | |
C26 | 0.34346 (11) | −0.14421 (10) | 0.12291 (10) | 0.0140 (3) | |
H26 | 0.332848 | −0.196837 | 0.165194 | 0.017* | |
C27 | 0.30298 (11) | −0.06485 (9) | 0.14518 (9) | 0.0112 (3) | |
C28 | 0.23924 (11) | −0.04943 (10) | 0.23381 (9) | 0.0115 (3) | |
Ni3 | 0.75403 (2) | 0.35799 (2) | 0.37533 (2) | 0.00989 (4) | |
O17 | 0.69383 (8) | 0.30932 (7) | 0.50907 (7) | 0.0146 (2) | |
O18 | 0.60244 (9) | 0.35062 (8) | 0.63310 (7) | 0.0211 (2) | |
O19 | 0.76962 (9) | 0.60229 (7) | 0.20894 (7) | 0.0155 (2) | |
H19A | 0.824 (2) | 0.593 (2) | 0.151 (2) | 0.070 (9)* | |
O20 | 0.78817 (8) | 0.45783 (7) | 0.25591 (7) | 0.0138 (2) | |
O21 | 0.63035 (8) | 0.33731 (7) | 0.34342 (7) | 0.0139 (2) | |
O22 | 0.60517 (8) | 0.24845 (7) | 0.28405 (7) | 0.0142 (2) | |
O23 | 1.07128 (8) | 0.22781 (7) | 0.37710 (7) | 0.0147 (2) | |
O24 | 0.91384 (8) | 0.33175 (7) | 0.38746 (7) | 0.01260 (19) | |
N5 | 0.68758 (9) | 0.46617 (8) | 0.41561 (8) | 0.0119 (2) | |
N6 | 0.82746 (9) | 0.24807 (8) | 0.34004 (8) | 0.0100 (2) | |
C29 | 0.64462 (11) | 0.36635 (10) | 0.55327 (10) | 0.0140 (3) | |
C30 | 0.63951 (11) | 0.45993 (10) | 0.50049 (9) | 0.0121 (3) | |
C31 | 0.59124 (11) | 0.53454 (10) | 0.53213 (10) | 0.0157 (3) | |
H31 | 0.555781 | 0.530454 | 0.592310 | 0.019* | |
C32 | 0.59646 (12) | 0.61485 (11) | 0.47330 (11) | 0.0178 (3) | |
H32 | 0.564468 | 0.666583 | 0.493321 | 0.021* | |
C33 | 0.64838 (12) | 0.62033 (10) | 0.38477 (10) | 0.0157 (3) | |
H33 | 0.652713 | 0.675015 | 0.344057 | 0.019* | |
C34 | 0.69332 (11) | 0.54319 (10) | 0.35848 (9) | 0.0117 (3) | |
C35 | 0.75446 (11) | 0.53242 (10) | 0.26776 (10) | 0.0122 (3) | |
C36 | 0.65997 (11) | 0.27090 (9) | 0.31431 (9) | 0.0111 (3) | |
C37 | 0.77287 (11) | 0.21314 (9) | 0.31602 (9) | 0.0106 (3) | |
C38 | 0.81827 (12) | 0.13204 (10) | 0.29755 (9) | 0.0136 (3) | |
H38 | 0.778932 | 0.106974 | 0.280873 | 0.016* | |
C39 | 0.92377 (12) | 0.08822 (10) | 0.30420 (10) | 0.0138 (3) | |
H39 | 0.956969 | 0.032559 | 0.292000 | 0.017* | |
C40 | 0.98012 (11) | 0.12612 (9) | 0.32868 (9) | 0.0122 (3) | |
H40 | 1.051913 | 0.097328 | 0.333102 | 0.015* | |
C41 | 0.92815 (11) | 0.20720 (9) | 0.34639 (9) | 0.0104 (3) | |
C42 | 0.97505 (11) | 0.25954 (9) | 0.37279 (9) | 0.0111 (3) | |
Ni4 | 1.25272 (2) | 0.13793 (2) | 0.60421 (2) | 0.01043 (4) | |
O25 | 1.28403 (8) | 0.02147 (7) | 0.70974 (7) | 0.0139 (2) | |
O26 | 1.26696 (9) | −0.01781 (7) | 0.85421 (7) | 0.0174 (2) | |
H26A | 1.3133 (18) | −0.0767 (16) | 0.8458 (16) | 0.037 (6)* | |
O27 | 1.10148 (9) | 0.39723 (7) | 0.58434 (8) | 0.0198 (2) | |
O28 | 1.19134 (8) | 0.26965 (7) | 0.55008 (7) | 0.0142 (2) | |
O29 | 1.12944 (8) | 0.10217 (7) | 0.58858 (7) | 0.0138 (2) | |
O30 | 1.10129 (8) | 0.03963 (7) | 0.50430 (7) | 0.0141 (2) | |
O31 | 1.57283 (8) | 0.12944 (8) | 0.47660 (7) | 0.0164 (2) | |
H31A | 1.606 (2) | 0.143 (2) | 0.527 (2) | 0.070 (9)* | |
O32 | 1.41149 (8) | 0.15281 (7) | 0.57461 (7) | 0.0147 (2) | |
N7 | 1.18741 (10) | 0.18360 (8) | 0.70928 (8) | 0.0117 (2) | |
N8 | 1.32572 (9) | 0.09660 (8) | 0.49787 (8) | 0.0104 (2) | |
C43 | 1.25302 (11) | 0.03833 (10) | 0.78164 (10) | 0.0130 (3) | |
C44 | 1.19363 (11) | 0.13056 (10) | 0.78774 (10) | 0.0131 (3) | |
C45 | 1.14907 (12) | 0.16077 (10) | 0.86258 (10) | 0.0156 (3) | |
H45 | 1.154881 | 0.122658 | 0.918152 | 0.019* | |
C46 | 1.09540 (12) | 0.24905 (11) | 0.85350 (10) | 0.0170 (3) | |
H46 | 1.062553 | 0.271689 | 0.903662 | 0.020* | |
C47 | 1.08970 (11) | 0.30433 (10) | 0.77106 (10) | 0.0152 (3) | |
H47 | 1.053517 | 0.364636 | 0.764162 | 0.018* | |
C48 | 1.13858 (11) | 0.26858 (10) | 0.69915 (10) | 0.0125 (3) | |
C49 | 1.14269 (11) | 0.31791 (9) | 0.60439 (10) | 0.0132 (3) | |
C50 | 1.15749 (11) | 0.07093 (9) | 0.52331 (9) | 0.0113 (3) | |
C51 | 1.27044 (11) | 0.07139 (9) | 0.46459 (9) | 0.0107 (3) | |
C52 | 1.31630 (12) | 0.04892 (9) | 0.38525 (9) | 0.0127 (3) | |
H52 | 1.276076 | 0.032303 | 0.360932 | 0.015* | |
C53 | 1.42291 (12) | 0.05139 (10) | 0.34223 (10) | 0.0144 (3) | |
H53 | 1.456531 | 0.035649 | 0.288200 | 0.017* | |
C54 | 1.48032 (11) | 0.07697 (9) | 0.37851 (9) | 0.0124 (3) | |
H54 | 1.553181 | 0.078580 | 0.350190 | 0.015* | |
C55 | 1.42790 (11) | 0.09989 (9) | 0.45689 (9) | 0.0108 (3) | |
C56 | 1.47300 (11) | 0.13035 (9) | 0.50675 (9) | 0.0129 (3) | |
O1W | 1.15570 (9) | 0.32166 (8) | 0.39989 (7) | 0.0152 (2) | |
H1A | 1.115 (2) | 0.3733 (19) | 0.3887 (17) | 0.045 (7)* | |
H1B | 1.164 (2) | 0.293 (2) | 0.467 (2) | 0.068 (9)* | |
H1C | 1.117 (2) | 0.272 (2) | 0.395 (2) | 0.076 (10)* | |
O2W | 0.39736 (9) | 0.29718 (7) | 0.33030 (7) | 0.0141 (2) | |
H2A | 0.3820 (14) | 0.2799 (13) | 0.2956 (13) | 0.015 (4)* | |
H2B | 0.466 (2) | 0.2857 (19) | 0.3175 (19) | 0.057 (8)* | |
H2C | 0.350 (2) | 0.3660 (19) | 0.3413 (18) | 0.055 (8)* | |
O3W | 0.12798 (9) | 0.83936 (8) | −0.05238 (8) | 0.0193 (2) | |
H3A | 0.074 (2) | 0.8926 (17) | −0.0533 (16) | 0.042 (7)* | |
H3B | 0.1414 (17) | 0.8080 (15) | 0.0035 (15) | 0.030 (6)* | |
H3C | 0.099 (2) | 0.802 (2) | −0.0644 (19) | 0.065 (9)* | |
O4W | 1.64368 (9) | 0.15762 (8) | 0.57453 (8) | 0.0193 (2) | |
H4A | 1.6664 (16) | 0.2034 (14) | 0.5534 (13) | 0.017 (5)* | |
H4B | 1.602 (2) | 0.1615 (18) | 0.625 (2) | 0.051 (8)* | |
O5W | 0.64397 (9) | 0.68318 (8) | 0.07545 (7) | 0.0160 (2) | |
H5A | 0.6502 (19) | 0.7300 (17) | 0.0633 (16) | 0.035 (6)* | |
H5B | 0.613 (2) | 0.6642 (17) | 0.1335 (18) | 0.040 (7)* | |
H5C | 0.606 (2) | 0.661 (2) | 0.036 (2) | 0.081 (10)* | |
O6W | 1.38147 (9) | −0.16849 (8) | 0.83977 (8) | 0.0168 (2) | |
H6A | 1.443 (2) | −0.1814 (17) | 0.8323 (17) | 0.038 (7)* | |
H6B | 1.3679 (18) | −0.1971 (18) | 0.8134 (17) | 0.042 (7)* | |
O7W | 0.11206 (9) | −0.09167 (8) | 0.43920 (7) | 0.0156 (2) | |
H7A | 0.0435 (19) | −0.0760 (15) | 0.4491 (15) | 0.030 (6)* | |
H7B | 0.1287 (19) | −0.0526 (17) | 0.4504 (16) | 0.034 (6)* | |
O8W | 0.88656 (9) | 0.58139 (8) | 0.06530 (8) | 0.0164 (2) | |
H8A | 0.956 (2) | 0.5699 (16) | 0.0580 (16) | 0.033 (6)* | |
H8B | 0.8742 (17) | 0.5511 (15) | 0.0474 (15) | 0.023 (6)* | |
O9W | 0.52805 (9) | 0.60206 (8) | 0.22051 (8) | 0.0204 (2) | |
H9A | 0.4910 (19) | 0.6111 (17) | 0.2703 (18) | 0.046 (7)* | |
H9B | 0.4819 (18) | 0.6090 (16) | 0.1937 (16) | 0.035 (6)* | |
O10W | 1.01615 (9) | 0.46431 (8) | 0.34976 (8) | 0.0193 (2) | |
H10A | 0.9843 (19) | 0.5053 (18) | 0.3686 (17) | 0.042 (7)* | |
H10B | 0.970 (2) | 0.4394 (19) | 0.3590 (18) | 0.053 (8)* | |
O11W | 0.03939 (10) | 0.03378 (8) | 0.05294 (8) | 0.0244 (2) | |
H11A | 0.039 (3) | −0.017 (2) | 0.083 (2) | 0.075 (10)* | |
H11B | 0.0670 (19) | 0.0591 (17) | 0.0749 (17) | 0.044 (7)* | |
O12W | 1.50472 (12) | 0.20790 (10) | 0.71034 (9) | 0.0309 (3) | |
H12A | 1.477 (3) | 0.182 (2) | 0.766 (2) | 0.087 (11)* | |
H12B | 1.540 (3) | 0.251 (2) | 0.707 (2) | 0.103 (13)* |
U11 | U22 | U33 | U12 | U13 | U23 | |
Ni1 | 0.00980 (8) | 0.01074 (9) | 0.00775 (8) | −0.00310 (7) | −0.00144 (7) | −0.00368 (6) |
O1 | 0.0132 (5) | 0.0128 (5) | 0.0107 (5) | −0.0032 (4) | −0.0014 (4) | −0.0045 (4) |
O2 | 0.0181 (5) | 0.0112 (5) | 0.0128 (5) | −0.0033 (4) | −0.0054 (4) | −0.0018 (4) |
O3 | 0.0208 (5) | 0.0126 (5) | 0.0208 (6) | −0.0011 (4) | −0.0073 (4) | −0.0037 (4) |
O4 | 0.0154 (5) | 0.0137 (5) | 0.0108 (5) | −0.0039 (4) | −0.0043 (4) | −0.0023 (4) |
O5 | 0.0112 (5) | 0.0163 (5) | 0.0120 (5) | −0.0048 (4) | −0.0008 (4) | −0.0064 (4) |
O6 | 0.0138 (5) | 0.0165 (5) | 0.0146 (5) | −0.0062 (4) | −0.0043 (4) | −0.0050 (4) |
O7 | 0.0127 (5) | 0.0195 (5) | 0.0140 (5) | −0.0076 (4) | −0.0023 (4) | −0.0044 (4) |
O8 | 0.0127 (5) | 0.0154 (5) | 0.0116 (5) | −0.0050 (4) | −0.0029 (4) | −0.0052 (4) |
N1 | 0.0089 (5) | 0.0108 (6) | 0.0110 (6) | −0.0030 (4) | −0.0017 (4) | −0.0050 (4) |
N2 | 0.0109 (5) | 0.0103 (5) | 0.0082 (5) | −0.0033 (4) | −0.0020 (4) | −0.0026 (4) |
C1 | 0.0089 (6) | 0.0118 (6) | 0.0141 (6) | −0.0035 (5) | −0.0026 (5) | −0.0050 (5) |
C2 | 0.0103 (6) | 0.0129 (6) | 0.0100 (6) | −0.0043 (5) | −0.0025 (5) | −0.0037 (5) |
C3 | 0.0137 (6) | 0.0184 (7) | 0.0101 (6) | −0.0052 (5) | −0.0024 (5) | −0.0046 (5) |
C4 | 0.0139 (6) | 0.0211 (8) | 0.0123 (7) | −0.0052 (6) | −0.0010 (5) | −0.0091 (6) |
C5 | 0.0107 (6) | 0.0143 (7) | 0.0164 (7) | −0.0023 (5) | −0.0023 (5) | −0.0086 (5) |
C6 | 0.0106 (6) | 0.0129 (7) | 0.0127 (6) | −0.0048 (5) | −0.0037 (5) | −0.0033 (5) |
C7 | 0.0115 (6) | 0.0132 (7) | 0.0143 (6) | −0.0042 (5) | −0.0042 (5) | −0.0036 (5) |
C8 | 0.0111 (6) | 0.0102 (6) | 0.0115 (6) | −0.0031 (5) | −0.0032 (5) | −0.0020 (5) |
C9 | 0.0112 (6) | 0.0090 (6) | 0.0106 (6) | −0.0032 (5) | −0.0025 (5) | −0.0022 (5) |
C10 | 0.0149 (7) | 0.0140 (7) | 0.0105 (6) | −0.0050 (5) | −0.0039 (5) | −0.0037 (5) |
C11 | 0.0165 (7) | 0.0125 (7) | 0.0093 (6) | −0.0037 (5) | −0.0016 (5) | −0.0035 (5) |
C12 | 0.0117 (6) | 0.0107 (6) | 0.0096 (6) | −0.0030 (5) | −0.0008 (5) | −0.0013 (5) |
C13 | 0.0111 (6) | 0.0091 (6) | 0.0105 (6) | −0.0027 (5) | −0.0033 (5) | −0.0017 (5) |
C14 | 0.0116 (6) | 0.0099 (6) | 0.0109 (6) | −0.0031 (5) | −0.0038 (5) | −0.0013 (5) |
Ni2 | 0.01035 (8) | 0.00905 (9) | 0.01057 (10) | −0.00238 (7) | −0.00243 (7) | −0.00412 (7) |
O9 | 0.0130 (5) | 0.0133 (5) | 0.0171 (5) | −0.0030 (4) | −0.0053 (4) | −0.0065 (4) |
O10 | 0.0136 (5) | 0.0171 (5) | 0.0203 (5) | −0.0034 (4) | −0.0080 (4) | −0.0051 (4) |
O11 | 0.0130 (5) | 0.0172 (5) | 0.0160 (5) | −0.0050 (4) | −0.0051 (4) | −0.0061 (4) |
O12 | 0.0118 (4) | 0.0143 (5) | 0.0150 (5) | −0.0018 (4) | −0.0041 (4) | −0.0067 (4) |
O13 | 0.0162 (5) | 0.0125 (5) | 0.0123 (5) | −0.0058 (4) | −0.0027 (4) | −0.0025 (4) |
O14 | 0.0274 (6) | 0.0223 (6) | 0.0112 (5) | −0.0114 (5) | 0.0013 (4) | −0.0039 (4) |
O15 | 0.0172 (5) | 0.0140 (5) | 0.0121 (5) | −0.0066 (4) | −0.0010 (4) | −0.0024 (4) |
O16 | 0.0148 (5) | 0.0127 (5) | 0.0125 (5) | −0.0033 (4) | −0.0017 (4) | −0.0051 (4) |
N3 | 0.0112 (5) | 0.0100 (6) | 0.0094 (5) | −0.0034 (4) | −0.0026 (4) | −0.0022 (4) |
N4 | 0.0095 (5) | 0.0115 (6) | 0.0111 (5) | −0.0032 (4) | −0.0018 (4) | −0.0048 (4) |
C15 | 0.0147 (6) | 0.0124 (6) | 0.0080 (6) | −0.0060 (5) | −0.0025 (5) | −0.0016 (5) |
C16 | 0.0109 (6) | 0.0113 (6) | 0.0079 (6) | −0.0032 (5) | −0.0021 (5) | −0.0013 (5) |
C17 | 0.0128 (6) | 0.0131 (7) | 0.0099 (6) | −0.0036 (5) | −0.0026 (5) | −0.0021 (5) |
C18 | 0.0164 (7) | 0.0091 (6) | 0.0101 (6) | −0.0020 (5) | −0.0020 (5) | −0.0030 (5) |
C19 | 0.0176 (7) | 0.0131 (7) | 0.0107 (6) | −0.0065 (5) | −0.0043 (5) | −0.0028 (5) |
C20 | 0.0116 (6) | 0.0109 (6) | 0.0085 (6) | −0.0041 (5) | −0.0016 (5) | −0.0016 (5) |
C21 | 0.0113 (6) | 0.0122 (6) | 0.0087 (6) | −0.0042 (5) | −0.0011 (5) | −0.0013 (5) |
C22 | 0.0141 (6) | 0.0168 (7) | 0.0120 (6) | −0.0068 (5) | −0.0041 (5) | −0.0033 (5) |
C23 | 0.0098 (5) | 0.0162 (7) | 0.0104 (6) | −0.0049 (5) | −0.0017 (5) | −0.0051 (5) |
C24 | 0.0119 (6) | 0.0181 (7) | 0.0135 (6) | −0.0034 (5) | −0.0017 (5) | −0.0087 (6) |
C25 | 0.0144 (6) | 0.0148 (7) | 0.0209 (8) | −0.0018 (5) | −0.0036 (6) | −0.0108 (6) |
C26 | 0.0133 (6) | 0.0123 (7) | 0.0170 (7) | −0.0036 (5) | −0.0033 (5) | −0.0050 (5) |
C27 | 0.0086 (6) | 0.0142 (7) | 0.0121 (6) | −0.0036 (5) | −0.0025 (5) | −0.0045 (5) |
C28 | 0.0092 (6) | 0.0143 (7) | 0.0123 (6) | −0.0026 (5) | −0.0038 (5) | −0.0044 (5) |
Ni3 | 0.00954 (8) | 0.01104 (9) | 0.01006 (9) | −0.00251 (7) | −0.00174 (7) | −0.00488 (7) |
O17 | 0.0159 (5) | 0.0160 (5) | 0.0124 (5) | −0.0064 (4) | −0.0002 (4) | −0.0057 (4) |
O18 | 0.0250 (6) | 0.0264 (6) | 0.0125 (5) | −0.0116 (5) | 0.0015 (4) | −0.0074 (4) |
O19 | 0.0168 (5) | 0.0151 (5) | 0.0148 (5) | −0.0053 (4) | −0.0035 (4) | −0.0035 (4) |
O20 | 0.0147 (5) | 0.0144 (5) | 0.0126 (5) | −0.0034 (4) | −0.0025 (4) | −0.0051 (4) |
O21 | 0.0112 (4) | 0.0158 (5) | 0.0158 (5) | −0.0018 (4) | −0.0040 (4) | −0.0067 (4) |
O22 | 0.0120 (4) | 0.0175 (5) | 0.0165 (5) | −0.0050 (4) | −0.0050 (4) | −0.0060 (4) |
O23 | 0.0119 (5) | 0.0147 (5) | 0.0195 (5) | −0.0038 (4) | −0.0069 (4) | −0.0036 (4) |
O24 | 0.0121 (4) | 0.0148 (5) | 0.0133 (5) | −0.0038 (4) | −0.0036 (4) | −0.0059 (4) |
N5 | 0.0095 (5) | 0.0157 (6) | 0.0132 (6) | −0.0038 (4) | −0.0028 (4) | −0.0063 (5) |
N6 | 0.0110 (5) | 0.0101 (6) | 0.0079 (5) | −0.0034 (4) | −0.0011 (4) | −0.0017 (4) |
C29 | 0.0113 (6) | 0.0190 (7) | 0.0144 (7) | −0.0060 (5) | −0.0019 (5) | −0.0069 (5) |
C30 | 0.0090 (6) | 0.0173 (7) | 0.0131 (6) | −0.0036 (5) | −0.0026 (5) | −0.0075 (5) |
C31 | 0.0117 (6) | 0.0218 (8) | 0.0177 (7) | −0.0023 (6) | −0.0034 (5) | −0.0123 (6) |
C32 | 0.0152 (7) | 0.0188 (8) | 0.0231 (8) | −0.0006 (6) | −0.0053 (6) | −0.0136 (6) |
C33 | 0.0154 (6) | 0.0139 (7) | 0.0194 (7) | −0.0023 (5) | −0.0067 (6) | −0.0057 (5) |
C34 | 0.0093 (6) | 0.0144 (7) | 0.0137 (6) | −0.0029 (5) | −0.0039 (5) | −0.0058 (5) |
C35 | 0.0094 (6) | 0.0154 (7) | 0.0146 (7) | −0.0035 (5) | −0.0049 (5) | −0.0050 (5) |
C36 | 0.0110 (6) | 0.0136 (6) | 0.0089 (6) | −0.0049 (5) | −0.0020 (5) | −0.0021 (5) |
C37 | 0.0102 (6) | 0.0134 (6) | 0.0084 (6) | −0.0045 (5) | −0.0013 (5) | −0.0025 (5) |
C38 | 0.0159 (7) | 0.0126 (7) | 0.0140 (7) | −0.0051 (5) | −0.0041 (5) | −0.0041 (5) |
C39 | 0.0159 (7) | 0.0102 (7) | 0.0144 (7) | −0.0033 (5) | −0.0026 (5) | −0.0034 (5) |
C40 | 0.0106 (6) | 0.0119 (6) | 0.0116 (6) | −0.0024 (5) | −0.0016 (5) | −0.0018 (5) |
C41 | 0.0099 (6) | 0.0129 (6) | 0.0088 (6) | −0.0047 (5) | −0.0022 (5) | −0.0019 (5) |
C42 | 0.0127 (6) | 0.0134 (6) | 0.0075 (6) | −0.0056 (5) | −0.0019 (5) | −0.0015 (5) |
Ni4 | 0.00982 (8) | 0.01123 (9) | 0.01129 (8) | −0.00219 (7) | −0.00173 (7) | −0.00573 (6) |
O25 | 0.0140 (5) | 0.0132 (5) | 0.0141 (5) | −0.0017 (4) | −0.0025 (4) | −0.0063 (4) |
O26 | 0.0214 (5) | 0.0154 (5) | 0.0144 (5) | −0.0022 (4) | −0.0059 (4) | −0.0039 (4) |
O27 | 0.0217 (5) | 0.0132 (5) | 0.0242 (6) | −0.0002 (4) | −0.0072 (4) | −0.0078 (4) |
O28 | 0.0157 (5) | 0.0130 (5) | 0.0148 (5) | −0.0014 (4) | −0.0049 (4) | −0.0064 (4) |
O29 | 0.0110 (5) | 0.0168 (5) | 0.0158 (5) | −0.0040 (4) | −0.0011 (4) | −0.0086 (4) |
O30 | 0.0129 (5) | 0.0174 (5) | 0.0148 (5) | −0.0062 (4) | −0.0030 (4) | −0.0057 (4) |
O31 | 0.0128 (5) | 0.0218 (6) | 0.0156 (5) | −0.0082 (4) | −0.0037 (4) | −0.0022 (4) |
O32 | 0.0127 (5) | 0.0169 (5) | 0.0164 (5) | −0.0041 (4) | −0.0035 (4) | −0.0067 (4) |
N7 | 0.0094 (5) | 0.0145 (6) | 0.0134 (6) | −0.0039 (4) | −0.0027 (4) | −0.0057 (5) |
N8 | 0.0092 (5) | 0.0107 (6) | 0.0107 (5) | −0.0021 (4) | −0.0022 (4) | −0.0031 (4) |
C43 | 0.0100 (6) | 0.0151 (7) | 0.0155 (7) | −0.0047 (5) | −0.0025 (5) | −0.0050 (5) |
C44 | 0.0110 (6) | 0.0133 (7) | 0.0170 (7) | −0.0031 (5) | −0.0034 (5) | −0.0066 (5) |
C45 | 0.0159 (7) | 0.0188 (7) | 0.0140 (7) | −0.0057 (6) | −0.0022 (5) | −0.0071 (6) |
C46 | 0.0155 (6) | 0.0211 (8) | 0.0168 (7) | −0.0042 (6) | −0.0011 (6) | −0.0117 (6) |
C47 | 0.0125 (6) | 0.0174 (7) | 0.0196 (7) | −0.0044 (5) | −0.0026 (5) | −0.0108 (6) |
C48 | 0.0098 (6) | 0.0140 (7) | 0.0172 (7) | −0.0034 (5) | −0.0041 (5) | −0.0071 (5) |
C49 | 0.0113 (6) | 0.0130 (7) | 0.0180 (7) | −0.0026 (5) | −0.0055 (5) | −0.0059 (5) |
C50 | 0.0096 (6) | 0.0105 (6) | 0.0126 (6) | −0.0018 (5) | −0.0023 (5) | −0.0030 (5) |
C51 | 0.0107 (6) | 0.0097 (6) | 0.0111 (6) | −0.0023 (5) | −0.0023 (5) | −0.0030 (5) |
C52 | 0.0146 (6) | 0.0130 (7) | 0.0108 (6) | −0.0033 (5) | −0.0042 (5) | −0.0028 (5) |
C53 | 0.0168 (7) | 0.0144 (7) | 0.0094 (6) | −0.0025 (5) | −0.0015 (5) | −0.0035 (5) |
C54 | 0.0103 (6) | 0.0113 (6) | 0.0109 (6) | −0.0020 (5) | −0.0005 (5) | −0.0002 (5) |
C55 | 0.0101 (6) | 0.0093 (6) | 0.0118 (6) | −0.0027 (5) | −0.0030 (5) | −0.0008 (5) |
C56 | 0.0121 (6) | 0.0110 (6) | 0.0145 (7) | −0.0038 (5) | −0.0043 (5) | −0.0001 (5) |
O1W | 0.0151 (5) | 0.0160 (5) | 0.0171 (5) | −0.0050 (4) | −0.0062 (4) | −0.0042 (4) |
O2W | 0.0115 (5) | 0.0141 (5) | 0.0183 (5) | −0.0014 (4) | −0.0053 (4) | −0.0065 (4) |
O3W | 0.0225 (6) | 0.0212 (6) | 0.0180 (5) | −0.0101 (5) | −0.0100 (4) | −0.0002 (4) |
O4W | 0.0193 (5) | 0.0210 (6) | 0.0192 (6) | −0.0092 (5) | −0.0077 (5) | −0.0002 (5) |
O5W | 0.0187 (5) | 0.0161 (6) | 0.0153 (5) | −0.0080 (4) | −0.0063 (4) | −0.0008 (4) |
O6W | 0.0129 (5) | 0.0178 (6) | 0.0215 (6) | −0.0006 (4) | −0.0057 (4) | −0.0094 (4) |
O7W | 0.0122 (5) | 0.0206 (6) | 0.0144 (5) | −0.0060 (4) | 0.0001 (4) | −0.0068 (4) |
O8W | 0.0131 (5) | 0.0206 (6) | 0.0178 (5) | −0.0063 (4) | −0.0016 (4) | −0.0079 (4) |
O9W | 0.0181 (5) | 0.0318 (7) | 0.0149 (5) | −0.0085 (5) | −0.0015 (4) | −0.0111 (5) |
O10W | 0.0214 (6) | 0.0165 (6) | 0.0217 (6) | −0.0048 (5) | −0.0047 (4) | −0.0081 (4) |
O11W | 0.0339 (6) | 0.0161 (6) | 0.0292 (6) | −0.0081 (5) | −0.0182 (5) | −0.0010 (5) |
O12W | 0.0404 (8) | 0.0301 (7) | 0.0207 (6) | −0.0179 (6) | −0.0044 (6) | 0.0005 (5) |
Ni1—N2 | 1.9652 (12) | N5—C34 | 1.3359 (19) |
Ni1—N1 | 1.9732 (12) | N6—C37 | 1.3298 (18) |
Ni1—O5 | 2.1076 (11) | N6—C41 | 1.3340 (18) |
Ni1—O4 | 2.1312 (11) | C29—C30 | 1.515 (2) |
Ni1—O1 | 2.1504 (11) | C30—C31 | 1.3947 (19) |
Ni1—O8 | 2.1782 (10) | C31—C32 | 1.387 (2) |
O1—C1 | 1.2500 (17) | C31—H31 | 0.9500 |
O2—C1 | 1.2714 (18) | C32—C33 | 1.398 (2) |
O2—H2C | 1.27 (3) | C32—H32 | 0.9500 |
O3—C7 | 1.2316 (18) | C33—C34 | 1.386 (2) |
O4—C7 | 1.2908 (17) | C33—H33 | 0.9500 |
O5—C8 | 1.2654 (17) | C34—C35 | 1.5058 (19) |
O6—C8 | 1.2486 (17) | C36—C37 | 1.5173 (19) |
O7—C14 | 1.2641 (17) | C37—C38 | 1.387 (2) |
O7—H5C | 1.27 (3) | C38—C39 | 1.400 (2) |
O8—C14 | 1.2636 (17) | C38—H38 | 0.9500 |
N1—C6 | 1.3333 (18) | C39—C40 | 1.393 (2) |
N1—C2 | 1.3374 (18) | C39—H39 | 0.9500 |
N2—C9 | 1.3320 (18) | C40—C41 | 1.3870 (19) |
N2—C13 | 1.3368 (18) | C40—H40 | 0.9500 |
C1—C2 | 1.5029 (19) | C41—C42 | 1.5085 (19) |
C2—C3 | 1.3873 (19) | Ni4—N8 | 1.9572 (12) |
C3—C4 | 1.395 (2) | Ni4—N7 | 1.9732 (12) |
C3—H3 | 0.9500 | Ni4—O28 | 2.0789 (11) |
C4—C5 | 1.390 (2) | Ni4—O29 | 2.1087 (11) |
C4—H4 | 0.9500 | Ni4—O32 | 2.1433 (10) |
C5—C6 | 1.390 (2) | Ni4—O25 | 2.1822 (11) |
C5—H5 | 0.9500 | O25—C43 | 1.2367 (18) |
C6—C7 | 1.517 (2) | O26—C43 | 1.2944 (18) |
C8—C9 | 1.5190 (19) | O26—H26A | 1.00 (2) |
C9—C10 | 1.3905 (19) | O27—C49 | 1.2333 (18) |
C10—C11 | 1.395 (2) | O28—C49 | 1.2873 (17) |
C10—H10 | 0.9500 | O28—H1B | 1.47 (3) |
C11—C12 | 1.393 (2) | O29—C50 | 1.2671 (17) |
C11—H11 | 0.9500 | O30—C50 | 1.2486 (17) |
C12—C13 | 1.3833 (19) | O31—C56 | 1.2789 (17) |
C12—H12 | 0.9500 | O31—H31A | 1.20 (3) |
C13—C14 | 1.5050 (19) | O32—C56 | 1.2512 (18) |
Ni2—N3 | 1.9579 (12) | N7—C44 | 1.3322 (19) |
Ni2—N4 | 1.9698 (12) | N7—C48 | 1.3328 (19) |
Ni2—O12 | 2.0891 (10) | N8—C51 | 1.3302 (18) |
Ni2—O13 | 2.1193 (10) | N8—C55 | 1.3390 (18) |
Ni2—O9 | 2.1286 (10) | C43—C44 | 1.505 (2) |
Ni2—O16 | 2.1909 (11) | C44—C45 | 1.385 (2) |
O9—C15 | 1.2701 (17) | C45—C46 | 1.394 (2) |
O10—C15 | 1.2581 (18) | C45—H45 | 0.9500 |
O11—C21 | 1.2512 (17) | C46—C47 | 1.395 (2) |
O12—C21 | 1.2634 (17) | C46—H46 | 0.9500 |
O13—C22 | 1.2887 (18) | C47—C48 | 1.393 (2) |
O14—C22 | 1.2304 (18) | C47—H47 | 0.9500 |
O15—C28 | 1.2807 (18) | C48—C49 | 1.520 (2) |
O15—H15 | 1.13 (3) | C50—C51 | 1.5187 (19) |
O16—C28 | 1.2414 (18) | C51—C52 | 1.3887 (19) |
N3—C20 | 1.3308 (18) | C52—C53 | 1.394 (2) |
N3—C16 | 1.3386 (18) | C52—H52 | 0.9500 |
N4—C23 | 1.3313 (18) | C53—C54 | 1.396 (2) |
N4—C27 | 1.3346 (19) | C53—H53 | 0.9500 |
C15—C16 | 1.5099 (19) | C54—C55 | 1.3820 (19) |
C16—C17 | 1.3835 (19) | C54—H54 | 0.9500 |
C17—C18 | 1.397 (2) | C55—C56 | 1.501 (2) |
C17—H17 | 0.9500 | O1W—H1A | 0.85 (3) |
C18—C19 | 1.399 (2) | O1W—H1B | 1.10 (3) |
C18—H18 | 0.9500 | O1W—H1C | 1.18 (3) |
C19—C20 | 1.3883 (19) | O2W—H2A | 0.852 (19) |
C19—H19 | 0.9500 | O2W—H2B | 0.85 (3) |
C20—C21 | 1.5210 (19) | O2W—H2C | 1.16 (3) |
C22—C23 | 1.512 (2) | O3W—H3A | 0.94 (3) |
C23—C24 | 1.3928 (19) | O3W—H3B | 0.96 (2) |
C24—C25 | 1.390 (2) | O3W—H3C | 0.96 (3) |
C24—H24 | 0.9500 | O4W—H31A | 1.23 (3) |
C25—C26 | 1.396 (2) | O4W—H4A | 0.85 (2) |
C25—H25 | 0.9500 | O4W—H4B | 0.85 (3) |
C26—C27 | 1.3889 (19) | O5W—H5A | 0.77 (3) |
C26—H26 | 0.9500 | O5W—H5B | 0.91 (3) |
C27—C28 | 1.5044 (19) | O5W—H5C | 1.19 (3) |
Ni3—N6 | 1.9625 (12) | O6W—H6A | 0.76 (2) |
Ni3—N5 | 1.9728 (12) | O6W—H6B | 0.86 (2) |
Ni3—O17 | 2.0849 (11) | O7W—H15 | 1.37 (3) |
Ni3—O21 | 2.1193 (10) | O7W—H7A | 0.85 (2) |
Ni3—O24 | 2.1494 (10) | O7W—H7B | 0.87 (2) |
Ni3—O20 | 2.1632 (11) | O8W—H19A | 1.44 (3) |
O17—C29 | 1.2762 (18) | O8W—H8A | 0.88 (2) |
O18—C29 | 1.2396 (18) | O8W—H8B | 0.77 (2) |
O19—C35 | 1.2820 (18) | O9W—H9A | 0.85 (3) |
O19—H19A | 1.03 (3) | O9W—H9B | 0.86 (2) |
O20—C35 | 1.2427 (18) | O10W—H10A | 0.78 (3) |
O21—C36 | 1.2604 (17) | O10W—H10B | 0.82 (3) |
O22—C36 | 1.2567 (17) | O11W—H11A | 0.83 (4) |
O23—C42 | 1.2568 (18) | O11W—H11B | 0.89 (2) |
O23—H1C | 1.29 (3) | O12W—H12A | 0.90 (4) |
O24—C42 | 1.2644 (17) | O12W—H12B | 0.99 (4) |
N5—C30 | 1.3350 (18) | ||
N2—Ni1—N1 | 175.96 (5) | C29—O17—Ni3 | 115.70 (10) |
N2—Ni1—O5 | 78.59 (5) | C35—O19—H19A | 115.3 (18) |
N1—Ni1—O5 | 105.44 (4) | C35—O20—Ni3 | 112.78 (9) |
N2—Ni1—O4 | 102.50 (5) | C36—O21—Ni3 | 113.77 (9) |
N1—Ni1—O4 | 77.74 (5) | C42—O23—H1C | 119.6 (14) |
O5—Ni1—O4 | 92.16 (4) | C42—O24—Ni3 | 113.39 (9) |
N2—Ni1—O1 | 101.91 (5) | C30—N5—C34 | 121.61 (13) |
N1—Ni1—O1 | 77.80 (5) | C30—N5—Ni3 | 118.53 (10) |
O5—Ni1—O1 | 94.30 (4) | C34—N5—Ni3 | 119.84 (10) |
O4—Ni1—O1 | 155.54 (4) | C37—N6—C41 | 121.51 (12) |
N2—Ni1—O8 | 77.20 (4) | C37—N6—Ni3 | 118.95 (10) |
N1—Ni1—O8 | 98.77 (4) | C41—N6—Ni3 | 119.38 (10) |
O5—Ni1—O8 | 155.78 (4) | O18—C29—O17 | 125.43 (15) |
O4—Ni1—O8 | 93.56 (4) | O18—C29—C30 | 119.72 (13) |
O1—Ni1—O8 | 90.16 (4) | O17—C29—C30 | 114.85 (13) |
C1—O1—Ni1 | 112.98 (9) | N5—C30—C31 | 120.67 (14) |
C1—O2—H2C | 117.9 (13) | N5—C30—C29 | 112.56 (12) |
C7—O4—Ni1 | 114.92 (9) | C31—C30—C29 | 126.76 (13) |
C8—O5—Ni1 | 114.26 (9) | C32—C31—C30 | 118.15 (14) |
C14—O7—H5C | 120.7 (14) | C32—C31—H31 | 120.9 |
C14—O8—Ni1 | 113.14 (9) | C30—C31—H31 | 120.9 |
C6—N1—C2 | 121.25 (12) | C31—C32—C33 | 120.57 (14) |
C6—N1—Ni1 | 119.59 (10) | C31—C32—H32 | 119.7 |
C2—N1—Ni1 | 119.15 (10) | C33—C32—H32 | 119.7 |
C9—N2—C13 | 121.06 (12) | C34—C33—C32 | 117.68 (14) |
C9—N2—Ni1 | 118.72 (9) | C34—C33—H33 | 121.2 |
C13—N2—Ni1 | 120.21 (10) | C32—C33—H33 | 121.2 |
O1—C1—O2 | 126.12 (13) | N5—C34—C33 | 121.30 (13) |
O1—C1—C2 | 117.95 (13) | N5—C34—C35 | 111.33 (12) |
O2—C1—C2 | 115.92 (12) | C33—C34—C35 | 127.37 (14) |
N1—C2—C3 | 121.33 (13) | O20—C35—O19 | 125.29 (14) |
N1—C2—C1 | 111.91 (12) | O20—C35—C34 | 118.58 (13) |
C3—C2—C1 | 126.75 (13) | O19—C35—C34 | 116.11 (13) |
C2—C3—C4 | 117.74 (14) | O22—C36—O21 | 126.25 (13) |
C2—C3—H3 | 121.1 | O22—C36—C37 | 117.36 (12) |
C4—C3—H3 | 121.1 | O21—C36—C37 | 116.39 (12) |
C5—C4—C3 | 120.51 (13) | N6—C37—C38 | 121.09 (13) |
C5—C4—H4 | 119.7 | N6—C37—C36 | 112.09 (12) |
C3—C4—H4 | 119.7 | C38—C37—C36 | 126.80 (13) |
C6—C5—C4 | 118.01 (13) | C37—C38—C39 | 118.05 (13) |
C6—C5—H5 | 121.0 | C37—C38—H38 | 121.0 |
C4—C5—H5 | 121.0 | C39—C38—H38 | 121.0 |
N1—C6—C5 | 121.14 (13) | C40—C39—C38 | 120.10 (13) |
N1—C6—C7 | 113.06 (12) | C40—C39—H39 | 120.0 |
C5—C6—C7 | 125.78 (13) | C38—C39—H39 | 120.0 |
O3—C7—O4 | 126.89 (14) | C41—C40—C39 | 117.92 (13) |
O3—C7—C6 | 118.49 (13) | C41—C40—H40 | 121.0 |
O4—C7—C6 | 114.61 (12) | C39—C40—H40 | 121.0 |
O6—C8—O5 | 125.96 (13) | N6—C41—C40 | 121.32 (13) |
O6—C8—C9 | 118.01 (12) | N6—C41—C42 | 112.44 (12) |
O5—C8—C9 | 116.02 (12) | C40—C41—C42 | 126.23 (13) |
N2—C9—C10 | 121.11 (13) | O23—C42—O24 | 126.32 (13) |
N2—C9—C8 | 112.25 (12) | O23—C42—C41 | 117.04 (13) |
C10—C9—C8 | 126.65 (12) | O24—C42—C41 | 116.63 (12) |
C9—C10—C11 | 118.13 (13) | N8—Ni4—N7 | 175.93 (5) |
C9—C10—H10 | 120.9 | N8—Ni4—O28 | 100.13 (5) |
C11—C10—H10 | 120.9 | N7—Ni4—O28 | 78.71 (5) |
C12—C11—C10 | 120.17 (13) | N8—Ni4—O29 | 78.45 (5) |
C12—C11—H11 | 119.9 | N7—Ni4—O29 | 105.45 (5) |
C10—C11—H11 | 119.9 | O28—Ni4—O29 | 92.83 (4) |
C13—C12—C11 | 117.84 (13) | N8—Ni4—O32 | 78.11 (5) |
C13—C12—H12 | 121.1 | N7—Ni4—O32 | 98.01 (4) |
C11—C12—H12 | 121.1 | O28—Ni4—O32 | 92.59 (4) |
N2—C13—C12 | 121.70 (13) | O29—Ni4—O32 | 156.52 (4) |
N2—C13—C14 | 112.42 (12) | N8—Ni4—O25 | 104.23 (5) |
C12—C13—C14 | 125.88 (12) | N7—Ni4—O25 | 76.94 (5) |
O8—C14—O7 | 126.11 (13) | O28—Ni4—O25 | 155.63 (4) |
O8—C14—C13 | 116.97 (12) | O29—Ni4—O25 | 92.77 (4) |
O7—C14—C13 | 116.93 (12) | O32—Ni4—O25 | 91.65 (4) |
N3—Ni2—N4 | 174.99 (5) | C43—O25—Ni4 | 112.36 (9) |
N3—Ni2—O12 | 78.65 (5) | C43—O26—H26A | 112.8 (14) |
N4—Ni2—O12 | 106.32 (4) | C49—O28—Ni4 | 115.84 (10) |
N3—Ni2—O13 | 100.77 (5) | C49—O28—H1B | 121.2 (12) |
N4—Ni2—O13 | 78.72 (5) | Ni4—O28—H1B | 117.5 (12) |
O12—Ni2—O13 | 91.92 (4) | C50—O29—Ni4 | 114.20 (9) |
N3—Ni2—O9 | 78.08 (4) | C56—O31—H31A | 111.8 (14) |
N4—Ni2—O9 | 96.95 (4) | C56—O32—Ni4 | 112.73 (9) |
O12—Ni2—O9 | 156.72 (4) | C44—N7—C48 | 121.40 (13) |
O13—Ni2—O9 | 92.92 (4) | C44—N7—Ni4 | 120.41 (10) |
N3—Ni2—O16 | 103.97 (5) | C48—N7—Ni4 | 118.18 (10) |
N4—Ni2—O16 | 76.58 (5) | C51—N8—C55 | 121.30 (12) |
O12—Ni2—O16 | 93.39 (4) | C51—N8—Ni4 | 119.18 (9) |
O13—Ni2—O16 | 155.25 (4) | C55—N8—Ni4 | 119.35 (10) |
O9—Ni2—O16 | 91.68 (4) | O25—C43—O26 | 125.10 (14) |
C15—O9—Ni2 | 114.13 (9) | O25—C43—C44 | 119.01 (13) |
C21—O12—Ni2 | 114.83 (9) | O26—C43—C44 | 115.89 (13) |
C22—O13—Ni2 | 114.33 (9) | N7—C44—C45 | 121.74 (14) |
C28—O15—H15 | 112.4 (16) | N7—C44—C43 | 111.12 (13) |
C28—O16—Ni2 | 112.90 (9) | C45—C44—C43 | 127.14 (14) |
C20—N3—C16 | 121.65 (12) | C44—C45—C46 | 117.66 (14) |
C20—N3—Ni2 | 118.88 (10) | C44—C45—H45 | 121.2 |
C16—N3—Ni2 | 119.41 (10) | C46—C45—H45 | 121.2 |
C23—N4—C27 | 121.23 (12) | C45—C46—C47 | 120.29 (14) |
C23—N4—Ni2 | 118.06 (10) | C45—C46—H46 | 119.9 |
C27—N4—Ni2 | 120.63 (10) | C47—C46—H46 | 119.9 |
O10—C15—O9 | 126.10 (13) | C48—C47—C46 | 118.12 (14) |
O10—C15—C16 | 117.88 (13) | C48—C47—H47 | 120.9 |
O9—C15—C16 | 116.03 (12) | C46—C47—H47 | 120.9 |
N3—C16—C17 | 121.14 (13) | N7—C48—C47 | 120.76 (14) |
N3—C16—C15 | 112.32 (12) | N7—C48—C49 | 113.16 (12) |
C17—C16—C15 | 126.54 (13) | C47—C48—C49 | 126.08 (13) |
C16—C17—C18 | 117.92 (13) | O27—C49—O28 | 124.99 (14) |
C16—C17—H17 | 121.0 | O27—C49—C48 | 120.90 (13) |
C18—C17—H17 | 121.0 | O28—C49—C48 | 114.11 (12) |
C17—C18—C19 | 120.34 (13) | O30—C50—O29 | 125.87 (13) |
C17—C18—H18 | 119.8 | O30—C50—C51 | 118.23 (12) |
C19—C18—H18 | 119.8 | O29—C50—C51 | 115.90 (12) |
C20—C19—C18 | 117.79 (13) | N8—C51—C52 | 121.03 (13) |
C20—C19—H19 | 121.1 | N8—C51—C50 | 111.90 (12) |
C18—C19—H19 | 121.1 | C52—C51—C50 | 127.08 (13) |
N3—C20—C19 | 121.15 (13) | C51—C52—C53 | 118.25 (13) |
N3—C20—C21 | 111.84 (12) | C51—C52—H52 | 120.9 |
C19—C20—C21 | 127.01 (13) | C53—C52—H52 | 120.9 |
O11—C21—O12 | 125.39 (13) | C52—C53—C54 | 120.03 (13) |
O11—C21—C20 | 118.92 (12) | C52—C53—H53 | 120.0 |
O12—C21—C20 | 115.69 (12) | C54—C53—H53 | 120.0 |
O14—C22—O13 | 126.70 (14) | C55—C54—C53 | 117.97 (13) |
O14—C22—C23 | 118.61 (13) | C55—C54—H54 | 121.0 |
O13—C22—C23 | 114.69 (12) | C53—C54—H54 | 121.0 |
N4—C23—C24 | 121.22 (14) | N8—C55—C54 | 121.39 (13) |
N4—C23—C22 | 114.10 (12) | N8—C55—C56 | 111.55 (12) |
C24—C23—C22 | 124.67 (13) | C54—C55—C56 | 127.06 (13) |
C25—C24—C23 | 117.91 (13) | O32—C56—O31 | 125.36 (14) |
C25—C24—H24 | 121.0 | O32—C56—C55 | 118.11 (12) |
C23—C24—H24 | 121.0 | O31—C56—C55 | 116.51 (13) |
C24—C25—C26 | 120.51 (13) | H1A—O1W—H1B | 117 (2) |
C24—C25—H25 | 119.7 | H1A—O1W—H1C | 110 (2) |
C26—C25—H25 | 119.7 | H1B—O1W—H1C | 100 (2) |
C27—C26—C25 | 117.65 (14) | H2A—O2W—H2B | 107 (2) |
C27—C26—H26 | 121.2 | H2A—O2W—H2C | 118.3 (18) |
C25—C26—H26 | 121.2 | H2B—O2W—H2C | 116 (2) |
N4—C27—C26 | 121.47 (13) | H3A—O3W—H3B | 115.1 (19) |
N4—C27—C28 | 111.60 (12) | H3A—O3W—H3C | 106 (2) |
C26—C27—C28 | 126.93 (13) | H3B—O3W—H3C | 103 (2) |
O16—C28—O15 | 125.72 (13) | H31A—O4W—H4A | 115 (2) |
O16—C28—C27 | 118.07 (13) | H31A—O4W—H4B | 116 (2) |
O15—C28—C27 | 116.20 (13) | H4A—O4W—H4B | 105 (2) |
N6—Ni3—N5 | 175.97 (5) | H5A—O5W—H5B | 112 (2) |
N6—Ni3—O17 | 99.97 (5) | H5A—O5W—H5C | 123 (2) |
N5—Ni3—O17 | 78.36 (5) | H5B—O5W—H5C | 107 (2) |
N6—Ni3—O21 | 78.43 (4) | H6A—O6W—H6B | 107 (2) |
N5—Ni3—O21 | 105.25 (4) | H15—O7W—H7A | 109.3 (19) |
O17—Ni3—O21 | 93.27 (4) | H15—O7W—H7B | 114 (2) |
N6—Ni3—O24 | 77.82 (4) | H7A—O7W—H7B | 106 (2) |
N5—Ni3—O24 | 98.54 (4) | H19A—O8W—H8A | 113.0 (19) |
O17—Ni3—O24 | 92.63 (4) | H19A—O8W—H8B | 118 (2) |
O21—Ni3—O24 | 156.18 (4) | H8A—O8W—H8B | 111 (2) |
N6—Ni3—O20 | 104.14 (4) | H9A—O9W—H9B | 105 (2) |
N5—Ni3—O20 | 77.42 (5) | H10A—O10W—H10B | 104 (2) |
O17—Ni3—O20 | 155.76 (4) | H11A—O11W—H11B | 111 (3) |
O21—Ni3—O20 | 93.95 (4) | H12A—O12W—H12B | 111 (3) |
O24—Ni3—O20 | 90.03 (4) | ||
Ni1—O1—C1—O2 | −173.90 (11) | Ni3—O17—C29—O18 | 179.31 (12) |
Ni1—O1—C1—C2 | 5.19 (15) | Ni3—O17—C29—C30 | −0.54 (15) |
C6—N1—C2—C3 | 1.0 (2) | C34—N5—C30—C31 | 1.4 (2) |
Ni1—N1—C2—C3 | −179.58 (10) | Ni3—N5—C30—C31 | −179.90 (10) |
C6—N1—C2—C1 | −177.94 (12) | C34—N5—C30—C29 | −178.78 (12) |
Ni1—N1—C2—C1 | 1.50 (15) | Ni3—N5—C30—C29 | −0.12 (15) |
O1—C1—C2—N1 | −4.64 (18) | O18—C29—C30—N5 | −179.42 (13) |
O2—C1—C2—N1 | 174.55 (12) | O17—C29—C30—N5 | 0.45 (18) |
O1—C1—C2—C3 | 176.52 (13) | O18—C29—C30—C31 | 0.4 (2) |
O2—C1—C2—C3 | −4.3 (2) | O17—C29—C30—C31 | −179.79 (13) |
N1—C2—C3—C4 | −1.3 (2) | N5—C30—C31—C32 | −1.2 (2) |
C1—C2—C3—C4 | 177.47 (13) | C29—C30—C31—C32 | 179.06 (13) |
C2—C3—C4—C5 | 0.9 (2) | C30—C31—C32—C33 | 0.3 (2) |
C3—C4—C5—C6 | −0.2 (2) | C31—C32—C33—C34 | 0.4 (2) |
C2—N1—C6—C5 | −0.2 (2) | C30—N5—C34—C33 | −0.7 (2) |
Ni1—N1—C6—C5 | −179.67 (10) | Ni3—N5—C34—C33 | −179.39 (10) |
C2—N1—C6—C7 | −179.25 (12) | C30—N5—C34—C35 | 178.13 (12) |
Ni1—N1—C6—C7 | 1.31 (16) | Ni3—N5—C34—C35 | −0.51 (16) |
C4—C5—C6—N1 | −0.2 (2) | C32—C33—C34—N5 | −0.2 (2) |
C4—C5—C6—C7 | 178.72 (13) | C32—C33—C34—C35 | −178.84 (13) |
Ni1—O4—C7—O3 | −176.11 (12) | Ni3—O20—C35—O19 | 175.72 (11) |
Ni1—O4—C7—C6 | 3.11 (15) | Ni3—O20—C35—C34 | −2.42 (15) |
N1—C6—C7—O3 | 176.34 (12) | N5—C34—C35—O20 | 2.05 (18) |
C5—C6—C7—O3 | −2.6 (2) | C33—C34—C35—O20 | −179.16 (14) |
N1—C6—C7—O4 | −2.96 (17) | N5—C34—C35—O19 | −176.26 (12) |
C5—C6—C7—O4 | 178.08 (13) | C33—C34—C35—O19 | 2.5 (2) |
Ni1—O5—C8—O6 | 175.14 (12) | Ni3—O21—C36—O22 | −173.69 (11) |
Ni1—O5—C8—C9 | −4.40 (16) | Ni3—O21—C36—C37 | 6.12 (15) |
C13—N2—C9—C10 | −0.3 (2) | C41—N6—C37—C38 | 0.8 (2) |
Ni1—N2—C9—C10 | 178.21 (11) | Ni3—N6—C37—C38 | −174.57 (11) |
C13—N2—C9—C8 | 179.57 (12) | C41—N6—C37—C36 | 179.43 (12) |
Ni1—N2—C9—C8 | −1.93 (16) | Ni3—N6—C37—C36 | 4.09 (15) |
O6—C8—C9—N2 | −175.31 (13) | O22—C36—C37—N6 | 172.99 (12) |
O5—C8—C9—N2 | 4.27 (18) | O21—C36—C37—N6 | −6.84 (18) |
O6—C8—C9—C10 | 4.5 (2) | O22—C36—C37—C38 | −8.4 (2) |
O5—C8—C9—C10 | −175.88 (14) | O21—C36—C37—C38 | 171.73 (14) |
N2—C9—C10—C11 | 0.0 (2) | N6—C37—C38—C39 | −0.5 (2) |
C8—C9—C10—C11 | −179.82 (13) | C36—C37—C38—C39 | −178.99 (13) |
C9—C10—C11—C12 | 0.3 (2) | C37—C38—C39—C40 | −0.1 (2) |
C10—C11—C12—C13 | −0.3 (2) | C38—C39—C40—C41 | 0.4 (2) |
C9—N2—C13—C12 | 0.3 (2) | C37—N6—C41—C40 | −0.4 (2) |
Ni1—N2—C13—C12 | −178.21 (10) | Ni3—N6—C41—C40 | 174.93 (10) |
C9—N2—C13—C14 | −179.56 (12) | C37—N6—C41—C42 | 178.81 (12) |
Ni1—N2—C13—C14 | 1.96 (16) | Ni3—N6—C41—C42 | −5.86 (15) |
C11—C12—C13—N2 | 0.0 (2) | C39—C40—C41—N6 | −0.2 (2) |
C11—C12—C13—C14 | 179.83 (13) | C39—C40—C41—C42 | −179.29 (13) |
Ni1—O8—C14—O7 | 178.10 (12) | Ni3—O24—C42—O23 | −178.53 (12) |
Ni1—O8—C14—C13 | −1.68 (15) | Ni3—O24—C42—C41 | 2.35 (15) |
N2—C13—C14—O8 | 0.01 (18) | N6—C41—C42—O23 | −177.26 (12) |
C12—C13—C14—O8 | −179.81 (13) | C40—C41—C42—O23 | 1.9 (2) |
N2—C13—C14—O7 | −179.79 (12) | N6—C41—C42—O24 | 1.94 (18) |
C12—C13—C14—O7 | 0.4 (2) | C40—C41—C42—O24 | −178.90 (13) |
Ni2—O9—C15—O10 | 179.01 (12) | Ni4—O25—C43—O26 | −176.02 (11) |
Ni2—O9—C15—C16 | −0.96 (15) | Ni4—O25—C43—C44 | 4.34 (15) |
C20—N3—C16—C17 | −0.5 (2) | C48—N7—C44—C45 | 0.5 (2) |
Ni2—N3—C16—C17 | −177.67 (10) | Ni4—N7—C44—C45 | 179.68 (11) |
C20—N3—C16—C15 | 178.85 (12) | C48—N7—C44—C43 | −179.64 (12) |
Ni2—N3—C16—C15 | 1.70 (15) | Ni4—N7—C44—C43 | −0.51 (16) |
O10—C15—C16—N3 | 179.65 (12) | O25—C43—C44—N7 | −2.83 (19) |
O9—C15—C16—N3 | −0.38 (18) | O26—C43—C44—N7 | 177.50 (12) |
O10—C15—C16—C17 | −1.0 (2) | O25—C43—C44—C45 | 176.97 (14) |
O9—C15—C16—C17 | 178.96 (13) | O26—C43—C44—C45 | −2.7 (2) |
N3—C16—C17—C18 | 1.0 (2) | N7—C44—C45—C46 | 1.0 (2) |
C15—C16—C17—C18 | −178.25 (13) | C43—C44—C45—C46 | −178.77 (13) |
C16—C17—C18—C19 | −0.2 (2) | C44—C45—C46—C47 | −1.3 (2) |
C17—C18—C19—C20 | −1.1 (2) | C45—C46—C47—C48 | 0.2 (2) |
C16—N3—C20—C19 | −0.9 (2) | C44—N7—C48—C47 | −1.8 (2) |
Ni2—N3—C20—C19 | 176.28 (10) | Ni4—N7—C48—C47 | 179.10 (10) |
C16—N3—C20—C21 | 179.64 (12) | C44—N7—C48—C49 | 178.58 (12) |
Ni2—N3—C20—C21 | −3.19 (15) | Ni4—N7—C48—C49 | −0.57 (15) |
C18—C19—C20—N3 | 1.7 (2) | C46—C47—C48—N7 | 1.4 (2) |
C18—C19—C20—C21 | −178.92 (13) | C46—C47—C48—C49 | −179.03 (13) |
Ni2—O12—C21—O11 | 177.73 (11) | Ni4—O28—C49—O27 | 179.86 (11) |
Ni2—O12—C21—C20 | −2.48 (15) | Ni4—O28—C49—C48 | −0.46 (15) |
N3—C20—C21—O11 | −176.50 (12) | N7—C48—C49—O27 | −179.64 (13) |
C19—C20—C21—O11 | 4.1 (2) | C47—C48—C49—O27 | 0.7 (2) |
N3—C20—C21—O12 | 3.70 (18) | N7—C48—C49—O28 | 0.67 (18) |
C19—C20—C21—O12 | −175.74 (14) | C47—C48—C49—O28 | −178.98 (13) |
Ni2—O13—C22—O14 | −177.02 (12) | Ni4—O29—C50—O30 | 174.62 (12) |
Ni2—O13—C22—C23 | 2.74 (15) | Ni4—O29—C50—C51 | −4.61 (16) |
C27—N4—C23—C24 | −0.9 (2) | C55—N8—C51—C52 | −1.1 (2) |
Ni2—N4—C23—C24 | −177.63 (10) | Ni4—N8—C51—C52 | 174.30 (11) |
C27—N4—C23—C22 | 179.73 (12) | C55—N8—C51—C50 | 178.74 (12) |
Ni2—N4—C23—C22 | 2.95 (15) | Ni4—N8—C51—C50 | −5.88 (16) |
O14—C22—C23—N4 | 176.02 (13) | O30—C50—C51—N8 | −172.44 (13) |
O13—C22—C23—N4 | −3.76 (17) | O29—C50—C51—N8 | 6.85 (18) |
O14—C22—C23—C24 | −3.4 (2) | O30—C50—C51—C52 | 7.4 (2) |
O13—C22—C23—C24 | 176.85 (13) | O29—C50—C51—C52 | −173.35 (14) |
N4—C23—C24—C25 | 1.1 (2) | N8—C51—C52—C53 | 1.5 (2) |
C22—C23—C24—C25 | −179.53 (13) | C50—C51—C52—C53 | −178.24 (13) |
C23—C24—C25—C26 | −0.8 (2) | C51—C52—C53—C54 | −0.8 (2) |
C24—C25—C26—C27 | 0.3 (2) | C52—C53—C54—C55 | −0.5 (2) |
C23—N4—C27—C26 | 0.3 (2) | C51—N8—C55—C54 | −0.2 (2) |
Ni2—N4—C27—C26 | 176.98 (10) | Ni4—N8—C55—C54 | −175.59 (11) |
C23—N4—C27—C28 | −179.45 (12) | C51—N8—C55—C56 | 179.85 (13) |
Ni2—N4—C27—C28 | −2.76 (16) | Ni4—N8—C55—C56 | 4.48 (16) |
C25—C26—C27—N4 | 0.0 (2) | C53—C54—C55—N8 | 1.0 (2) |
C25—C26—C27—C28 | 179.68 (13) | C53—C54—C55—C56 | −179.11 (14) |
Ni2—O16—C28—O15 | −175.40 (11) | Ni4—O32—C56—O31 | −177.03 (12) |
Ni2—O16—C28—C27 | 4.02 (15) | Ni4—O32—C56—C55 | 1.53 (16) |
N4—C27—C28—O16 | −1.23 (18) | N8—C55—C56—O32 | −3.86 (19) |
C26—C27—C28—O16 | 179.06 (14) | C54—C55—C56—O32 | 176.22 (14) |
N4—C27—C28—O15 | 178.24 (12) | N8—C55—C56—O31 | 174.83 (13) |
C26—C27—C28—O15 | −1.5 (2) | C54—C55—C56—O31 | −5.1 (2) |
D—H···A | D—H | H···A | D···A | D—H···A |
O15—H15···O7W | 1.13 (3) | 1.37 (3) | 2.4609 (15) | 161 (3) |
O19—H19A···O8W | 1.03 (3) | 1.44 (3) | 2.4581 (16) | 171 (3) |
O26—H26A···O6W | 1.00 (2) | 1.52 (2) | 2.5224 (16) | 176 (2) |
O31—H31A···O4W | 1.20 (3) | 1.23 (3) | 2.4339 (16) | 177 (3) |
O1W—H1A···O10W | 0.85 (3) | 1.76 (3) | 2.5852 (17) | 162 (2) |
O1W—H1B···O28 | 1.10 (3) | 1.47 (3) | 2.5475 (15) | 167 (3) |
O1W—H1C···O23 | 1.18 (3) | 1.29 (3) | 2.4590 (15) | 170 (3) |
O2W—H2A···O11 | 0.852 (19) | 1.84 (2) | 2.6575 (15) | 160.1 (17) |
O2W—H2B···O22 | 0.85 (3) | 1.74 (3) | 2.5772 (15) | 170 (3) |
O2W—H2C···O2 | 1.16 (3) | 1.27 (3) | 2.4275 (15) | 174 (2) |
O3W—H3A···O11Wi | 0.94 (3) | 1.62 (3) | 2.5317 (18) | 163 (2) |
O3W—H3B···O4 | 0.96 (2) | 1.61 (2) | 2.5679 (16) | 175 (2) |
O3W—H3C···O10i | 0.96 (3) | 1.55 (3) | 2.5076 (16) | 172 (3) |
O4W—H4A···O17ii | 0.85 (2) | 1.81 (2) | 2.6507 (16) | 171.4 (19) |
O4W—H4B···O12W | 0.85 (3) | 1.78 (3) | 2.5983 (19) | 160 (3) |
O5W—H5A···O13iii | 0.77 (3) | 1.80 (3) | 2.5628 (16) | 170 (3) |
O5W—H5B···O9W | 0.91 (3) | 1.79 (3) | 2.6242 (17) | 151 (2) |
O5W—H5C···O7 | 1.19 (3) | 1.27 (3) | 2.4499 (15) | 176 (3) |
O6W—H6A···O11iv | 0.76 (2) | 2.00 (2) | 2.7459 (15) | 164 (2) |
O6W—H6B···O22iv | 0.86 (2) | 1.99 (2) | 2.7856 (15) | 154 (2) |
O7W—H7A···O30v | 0.85 (2) | 1.82 (2) | 2.6560 (15) | 166 (2) |
O7W—H7B···O30vi | 0.87 (2) | 1.93 (2) | 2.7408 (16) | 155 (2) |
O8W—H8A···O6ii | 0.88 (2) | 1.81 (2) | 2.6509 (15) | 161 (2) |
O8W—H8B···O6iii | 0.77 (2) | 2.01 (2) | 2.7405 (16) | 159 (2) |
O9W—H9A···O18vii | 0.85 (3) | 1.84 (3) | 2.6846 (16) | 170 (3) |
O9W—H9B···O8 | 0.86 (2) | 2.00 (2) | 2.8250 (16) | 162 (2) |
O10W—H10A···O27viii | 0.78 (3) | 1.90 (3) | 2.6842 (16) | 176 (2) |
O10W—H10B···O24 | 0.82 (3) | 2.07 (3) | 2.8293 (16) | 155 (3) |
O11W—H11A···O3ix | 0.83 (4) | 1.89 (4) | 2.7037 (17) | 166 (3) |
O11W—H11B···O9 | 0.89 (2) | 1.89 (3) | 2.7406 (16) | 159 (2) |
O12W—H12A···O14x | 0.90 (4) | 1.81 (4) | 2.6912 (17) | 166 (3) |
O12W—H12B···O18ii | 0.99 (4) | 1.98 (4) | 2.8633 (18) | 148 (3) |
Symmetry codes: (i) −x, −y+1, −z; (ii) x+1, y, z; (iii) −x+1, −y+1, −z; (iv) −x+2, −y, −z+1; (v) −x+1, −y, −z+1; (vi) x−1, y, z; (vii) −x+1, −y+1, −z+1; (viii) −x+2, −y+1, −z+1; (ix) x, y−1, z; (x) x+1, y, z+1. |
3(C14H6N2NiO8)·C14H8N2NiO8·3(H3O)·4(H2O)·HO·4(O) | F(000) = 3600 |
Mr = 1767.75 | Dx = 1.745 Mg m−3 |
Monoclinic, Cc | Mo Kα radiation, λ = 0.71073 Å |
a = 27.5303 (18) Å | Cell parameters from 9820 reflections |
b = 19.6477 (13) Å | θ = 2.7–27.5° |
c = 13.7534 (9) Å | µ = 1.22 mm−1 |
β = 115.261 (2)° | T = 180 K |
V = 6727.9 (8) Å3 | Block, blue-green |
Z = 4 | 0.47 × 0.40 × 0.34 mm |
Bruker Kappa DUO with Photon 100 detector diffractometer | 14609 independent reflections |
Radiation source: microsource | 13325 reflections with I > 2σ(I) |
Detector resolution: 10.42 pixels mm-1 | Rint = 0.022 |
ω and φ scans | θmax = 27.6°, θmin = 2.4° |
Absorption correction: multi-scan SADABS (Sheldrick, 2015) | h = −35→35 |
Tmin = 0.667, Tmax = 0.746 | k = −25→23 |
30960 measured reflections | l = −17→15 |
Refinement on F2 | Secondary atom site location: difference Fourier map |
Least-squares matrix: full | Hydrogen site location: mixed |
R[F2 > 2σ(F2)] = 0.041 | H atoms treated by a mixture of independent and constrained refinement |
wR(F2) = 0.113 | w = 1/[σ2(Fo2) + (0.0385P)2 + 29.8338P] where P = (Fo2 + 2Fc2)/3 |
S = 1.03 | (Δ/σ)max < 0.001 |
14609 reflections | Δρmax = 0.89 e Å−3 |
1069 parameters | Δρmin = −0.72 e Å−3 |
33 restraints | Absolute structure: Refined as an inversion twin. |
Primary atom site location: structure-invariant direct methods | Absolute structure parameter: 0.50 (2) |
Geometry. All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. |
Refinement. Seven solvate waters experience disorder and hydrogen atoms could not be reliably added. Refined as a 2-component inversion twin. |
x | y | z | Uiso*/Ueq | Occ. (<1) | |
Ni1 | 0.38091 (3) | 0.87394 (4) | 0.75039 (7) | 0.01359 (18) | |
O1 | 0.3526 (2) | 0.8674 (2) | 0.8677 (5) | 0.0185 (11) | |
O2 | 0.2807 (2) | 0.8891 (3) | 0.8993 (5) | 0.0213 (11) | |
O3 | 0.37738 (18) | 0.8992 (3) | 0.5944 (4) | 0.0200 (10) | |
O4 | 0.32294 (19) | 0.9516 (3) | 0.4388 (4) | 0.0202 (10) | |
O5 | 0.42857 (17) | 0.9584 (2) | 0.8239 (4) | 0.0158 (9) | |
O6 | 0.5150 (2) | 0.9870 (3) | 0.9272 (5) | 0.0358 (12) | |
O7 | 0.3643 (2) | 0.7676 (3) | 0.7063 (5) | 0.0230 (11) | |
O8 | 0.4077 (2) | 0.6685 (2) | 0.7153 (5) | 0.0295 (12) | |
N1 | 0.3101 (2) | 0.9185 (3) | 0.6775 (5) | 0.0155 (12) | |
N2 | 0.4530 (2) | 0.8333 (3) | 0.8163 (4) | 0.0155 (11) | |
C1 | 0.3065 (3) | 0.8919 (4) | 0.8426 (6) | 0.0165 (13) | |
C2 | 0.2803 (2) | 0.9226 (3) | 0.7323 (6) | 0.0150 (13) | |
C3 | 0.2317 (2) | 0.9575 (3) | 0.6862 (6) | 0.0124 (12) | |
H3 | 0.211068 | 0.964624 | 0.725859 | 0.015* | |
C4 | 0.2135 (3) | 0.9819 (4) | 0.5810 (6) | 0.0186 (14) | |
H4 | 0.179228 | 1.002989 | 0.547146 | 0.022* | |
C5 | 0.2456 (2) | 0.9751 (3) | 0.5253 (6) | 0.0143 (12) | |
H5 | 0.234396 | 0.991933 | 0.454228 | 0.017* | |
C6 | 0.2950 (2) | 0.9425 (3) | 0.5798 (6) | 0.0129 (12) | |
C7 | 0.3343 (2) | 0.9304 (3) | 0.5324 (6) | 0.0146 (12) | |
C8 | 0.4800 (2) | 0.9459 (3) | 0.8755 (5) | 0.0191 (13) | |
C9 | 0.4954 (3) | 0.8711 (3) | 0.8701 (6) | 0.0194 (14) | |
C10 | 0.5461 (3) | 0.8475 (4) | 0.9164 (6) | 0.0249 (14) | |
H10 | 0.575748 | 0.876599 | 0.954826 | 0.030* | |
C11 | 0.5530 (3) | 0.7766 (4) | 0.9048 (7) | 0.0306 (17) | |
H11 | 0.587716 | 0.756657 | 0.937446 | 0.037* | |
C12 | 0.5087 (3) | 0.7372 (4) | 0.8455 (6) | 0.0266 (15) | |
H12 | 0.512940 | 0.690243 | 0.834586 | 0.032* | |
C13 | 0.4587 (3) | 0.7657 (3) | 0.8026 (6) | 0.0190 (13) | |
C14 | 0.4060 (3) | 0.7324 (3) | 0.7354 (6) | 0.0225 (14) | |
Ni2 | 0.37233 (3) | 0.38450 (5) | 0.74654 (6) | 0.0178 (2) | |
O9 | 0.3642 (2) | 0.2766 (3) | 0.7109 (5) | 0.0240 (11) | |
O10 | 0.4157 (2) | 0.1837 (3) | 0.7289 (5) | 0.0315 (12) | |
H10A | 0.384 (2) | 0.161 (3) | 0.688 (4) | 0.002 (12)* | |
O11 | 0.41370 (19) | 0.4734 (3) | 0.8103 (4) | 0.0275 (12) | |
O12 | 0.4961 (2) | 0.5161 (3) | 0.9043 (5) | 0.0414 (13) | |
O13 | 0.3458 (2) | 0.3767 (3) | 0.8665 (5) | 0.0213 (11) | |
O14 | 0.2726 (2) | 0.3897 (3) | 0.8986 (5) | 0.0222 (11) | |
O15 | 0.36589 (19) | 0.4067 (3) | 0.5890 (4) | 0.0219 (10) | |
O16 | 0.3085 (2) | 0.4518 (3) | 0.4315 (4) | 0.0246 (11) | |
H16 | 0.338 (3) | 0.442 (4) | 0.418 (6) | 0.04 (2)* | |
N3 | 0.4469 (2) | 0.3523 (3) | 0.8141 (5) | 0.0202 (12) | |
N4 | 0.2982 (2) | 0.4223 (3) | 0.6724 (5) | 0.0150 (11) | |
C15 | 0.4088 (3) | 0.2477 (4) | 0.7442 (6) | 0.0274 (16) | |
C16 | 0.4587 (3) | 0.2862 (4) | 0.8073 (6) | 0.0256 (15) | |
C17 | 0.5107 (3) | 0.2628 (4) | 0.8516 (6) | 0.0258 (15) | |
H17 | 0.518301 | 0.216208 | 0.845382 | 0.031* | |
C18 | 0.5523 (3) | 0.3089 (5) | 0.9062 (7) | 0.039 (2) | |
H18 | 0.588706 | 0.294413 | 0.937862 | 0.047* | |
C19 | 0.5389 (3) | 0.3769 (4) | 0.9128 (6) | 0.0300 (16) | |
H19 | 0.566375 | 0.408705 | 0.951179 | 0.036* | |
C20 | 0.4854 (3) | 0.3985 (4) | 0.8635 (6) | 0.0274 (16) | |
C21 | 0.4654 (3) | 0.4692 (4) | 0.8603 (6) | 0.0271 (15) | |
C22 | 0.3213 (3) | 0.4334 (3) | 0.5272 (6) | 0.0179 (13) | |
C23 | 0.2822 (3) | 0.4442 (3) | 0.5752 (6) | 0.0162 (13) | |
C24 | 0.2316 (3) | 0.4732 (3) | 0.5213 (6) | 0.0198 (14) | |
H24 | 0.218943 | 0.488614 | 0.449161 | 0.024* | |
C25 | 0.2002 (3) | 0.4785 (4) | 0.5781 (6) | 0.0228 (15) | |
H25 | 0.165296 | 0.497887 | 0.544773 | 0.027* | |
C26 | 0.2200 (3) | 0.4555 (3) | 0.6835 (6) | 0.0223 (15) | |
H26 | 0.199354 | 0.461343 | 0.723339 | 0.027* | |
C27 | 0.2698 (3) | 0.4240 (3) | 0.7307 (6) | 0.0188 (14) | |
C28 | 0.2978 (3) | 0.3955 (4) | 0.8420 (6) | 0.0199 (14) | |
Ni3 | 0.63070 (4) | 0.62559 (5) | 0.75260 (7) | 0.0185 (2) | |
O17 | 0.6581 (2) | 0.6201 (3) | 0.6292 (5) | 0.0222 (12) | |
O18 | 0.7319 (2) | 0.6420 (3) | 0.6057 (5) | 0.0230 (11) | |
O19 | 0.6359 (2) | 0.6483 (3) | 0.9118 (4) | 0.0217 (10) | |
O20 | 0.6910 (3) | 0.6999 (3) | 1.0636 (5) | 0.0328 (13) | |
O21 | 0.64563 (19) | 0.5184 (2) | 0.7952 (4) | 0.0190 (10) | |
O22 | 0.6004 (2) | 0.4226 (3) | 0.7801 (5) | 0.0249 (11) | |
O23 | 0.5813 (3) | 0.7121 (3) | 0.6816 (5) | 0.0395 (15) | |
O24 | 0.4956 (3) | 0.7396 (4) | 0.5817 (6) | 0.069 (2) | |
N5 | 0.7014 (2) | 0.6659 (3) | 0.8237 (5) | 0.0148 (11) | |
N6 | 0.5575 (2) | 0.5846 (3) | 0.6895 (5) | 0.0219 (13) | |
C29 | 0.7056 (3) | 0.6420 (3) | 0.6606 (6) | 0.0166 (13) | |
C30 | 0.7322 (3) | 0.6743 (3) | 0.7724 (6) | 0.0166 (13) | |
C31 | 0.7821 (3) | 0.7050 (4) | 0.8155 (7) | 0.0267 (16) | |
H31 | 0.804120 | 0.706909 | 0.778001 | 0.032* | |
C32 | 0.7979 (3) | 0.7329 (4) | 0.9175 (7) | 0.0263 (17) | |
H32 | 0.831053 | 0.756675 | 0.950031 | 0.032* | |
C33 | 0.7664 (3) | 0.7264 (3) | 0.9718 (6) | 0.0246 (15) | |
H33 | 0.777499 | 0.745714 | 1.041359 | 0.030* | |
C34 | 0.7191 (3) | 0.6923 (4) | 0.9254 (6) | 0.0192 (14) | |
C35 | 0.6776 (3) | 0.6786 (4) | 0.9684 (6) | 0.0226 (14) | |
C36 | 0.5318 (4) | 0.6985 (5) | 0.6320 (7) | 0.038 (2) | |
C37 | 0.5162 (3) | 0.6274 (4) | 0.6350 (6) | 0.0258 (17) | |
C38 | 0.4634 (3) | 0.5979 (7) | 0.5886 (6) | 0.047 (3) | |
H38 | 0.433005 | 0.625720 | 0.549564 | 0.056* | |
C39 | 0.4569 (3) | 0.5328 (6) | 0.5998 (7) | 0.051 (3) | |
H39 | 0.421583 | 0.514535 | 0.570359 | 0.061* | |
C40 | 0.5012 (3) | 0.4886 (5) | 0.6548 (7) | 0.040 (2) | |
H40 | 0.496996 | 0.441003 | 0.660897 | 0.047* | |
C41 | 0.5514 (2) | 0.5206 (4) | 0.6991 (6) | 0.0216 (14) | |
C42 | 0.6032 (2) | 0.4848 (3) | 0.7615 (5) | 0.0152 (12) | |
Ni4 | 0.62611 (4) | 0.86765 (5) | 0.25176 (7) | 0.0205 (2) | |
O25 | 0.63616 (19) | 0.9776 (3) | 0.2900 (5) | 0.0218 (11) | |
O26 | 0.5890 (2) | 1.0725 (3) | 0.2741 (5) | 0.0302 (12) | |
O27 | 0.5823 (2) | 0.7780 (3) | 0.1813 (5) | 0.0340 (13) | |
O28 | 0.4979 (3) | 0.7446 (4) | 0.0831 (6) | 0.066 (2) | |
O29 | 0.6543 (2) | 0.8772 (3) | 0.1309 (5) | 0.0250 (12) | |
O30 | 0.7273 (2) | 0.8577 (3) | 0.1056 (5) | 0.0257 (12) | |
O31 | 0.6298 (2) | 0.8428 (3) | 0.4075 (4) | 0.0262 (11) | |
O32 | 0.6865 (3) | 0.7959 (3) | 0.5630 (5) | 0.0413 (16) | |
N7 | 0.5522 (2) | 0.9052 (4) | 0.1859 (5) | 0.0244 (13) | |
N8 | 0.6981 (2) | 0.8314 (3) | 0.3246 (5) | 0.0169 (12) | |
C43 | 0.5941 (2) | 1.0088 (4) | 0.2569 (6) | 0.0203 (14) | |
C44 | 0.5429 (3) | 0.9696 (4) | 0.1951 (6) | 0.0223 (15) | |
C45 | 0.4901 (3) | 0.9982 (5) | 0.1482 (7) | 0.039 (2) | |
H45 | 0.483382 | 1.045048 | 0.154066 | 0.047* | |
C46 | 0.4492 (3) | 0.9518 (5) | 0.0931 (7) | 0.038 (2) | |
H46 | 0.413167 | 0.967459 | 0.060971 | 0.045* | |
C47 | 0.4591 (3) | 0.8849 (6) | 0.0836 (6) | 0.046 (3) | |
H47 | 0.430427 | 0.854613 | 0.044887 | 0.055* | |
C48 | 0.5127 (3) | 0.8609 (4) | 0.1323 (6) | 0.0232 (15) | |
C49 | 0.5314 (3) | 0.7887 (4) | 0.1317 (7) | 0.037 (2) | |
C50 | 0.6727 (3) | 0.8160 (4) | 0.4661 (6) | 0.0247 (15) | |
C51 | 0.7161 (3) | 0.8054 (4) | 0.4264 (6) | 0.0225 (15) | |
C52 | 0.7651 (3) | 0.7741 (4) | 0.4750 (7) | 0.0292 (18) | |
H52 | 0.777081 | 0.756561 | 0.545806 | 0.035* | |
C53 | 0.7968 (3) | 0.7681 (4) | 0.4209 (7) | 0.0294 (18) | |
H53 | 0.830235 | 0.745153 | 0.453871 | 0.035* | |
C54 | 0.7803 (3) | 0.7955 (4) | 0.3176 (7) | 0.0290 (17) | |
H54 | 0.802439 | 0.794426 | 0.280246 | 0.035* | |
C55 | 0.7293 (3) | 0.8245 (3) | 0.2735 (6) | 0.0170 (13) | |
C56 | 0.7020 (3) | 0.8565 (3) | 0.1610 (6) | 0.0174 (13) | |
O1W | 0.3860 (2) | 1.0707 (3) | 0.8587 (5) | 0.0334 (12) | |
H1A | 0.403 (2) | 1.035 (2) | 0.838 (5) | 0.040* | |
H1B | 0.3599 (19) | 1.053 (3) | 0.879 (5) | 0.040* | |
H1C | 0.4119 (17) | 1.094 (3) | 0.918 (3) | 0.040* | |
O2W | 0.6725 (2) | 1.1360 (3) | 0.3886 (5) | 0.0302 (13) | |
H2A | 0.7040 (16) | 1.137 (4) | 0.376 (5) | 0.036* | |
H2B | 0.686 (2) | 1.143 (4) | 0.4647 (16) | 0.036* | |
O3W | 0.6833 (2) | 0.3622 (3) | 0.8930 (5) | 0.0234 (11) | |
H3A | 0.7120 (17) | 0.362 (3) | 0.872 (4) | 0.028* | |
H3B | 0.697 (2) | 0.355 (3) | 0.9682 (16) | 0.028* | |
O4W | 0.3677 (2) | 0.5796 (3) | −0.1507 (5) | 0.0316 (12) | |
H4A | 0.4040 (12) | 0.592 (4) | −0.104 (5) | 0.038* | |
O5W | 0.3335 (2) | 0.8788 (3) | 1.1137 (5) | 0.0274 (13) | |
H5A | 0.319 (2) | 0.875 (3) | 1.0375 (14) | 0.033* | |
H5B | 0.3060 (19) | 0.865 (3) | 1.134 (5) | 0.033* | |
O6W | 0.3238 (3) | 0.6107 (3) | 0.6076 (5) | 0.0321 (13) | |
H6A | 0.2953 (16) | 0.630 (3) | 0.620 (5) | 0.039* | |
H6B | 0.316 (2) | 0.623 (3) | 0.5345 (18) | 0.039* | |
H6C | 0.3551 (15) | 0.638 (3) | 0.648 (4) | 0.039* | |
O7W | 0.6311 (3) | 0.6769 (3) | 1.1516 (5) | 0.0363 (14) | |
H7A | 0.651 (2) | 0.683 (3) | 1.110 (5) | 0.044* | |
H7B | 0.609 (2) | 0.6374 (19) | 1.126 (5) | 0.044* | |
H7C | 0.607 (2) | 0.715 (2) | 1.136 (5) | 0.044* | |
O8W | 0.6206 (3) | 0.8186 (3) | 0.6397 (6) | 0.0447 (16) | |
H8A | 0.622 (3) | 0.776 (2) | 0.675 (6) | 0.054* | |
H8B | 0.6566 (12) | 0.828 (4) | 0.651 (7) | 0.054* | |
O9W | 0.5921 (2) | 0.5689 (3) | 1.0253 (5) | 0.0429 (13) | |
O10W | 0.5579 (5) | 0.8895 (6) | 0.4803 (9) | 0.059 (3)* | 0.6 |
O11W | 0.4232 (4) | 0.8299 (5) | 0.4777 (8) | 0.050 (2)* | 0.6 |
O12W | 0.4150 (4) | 0.6721 (5) | −0.0202 (8) | 0.048 (2)* | 0.6 |
O13W | 0.5350 (6) | 0.8825 (8) | 0.5059 (13) | 0.055 (4)* | 0.4 |
O14W | 0.4577 (7) | 0.8597 (8) | 0.5232 (14) | 0.060 (4)* | 0.4 |
O15W | 0.4593 (7) | 0.6283 (8) | −0.0091 (13) | 0.059 (4)* | 0.4 |
U11 | U22 | U33 | U12 | U13 | U23 | |
Ni1 | 0.0087 (4) | 0.0159 (3) | 0.0158 (4) | 0.0071 (2) | 0.0049 (3) | 0.0019 (3) |
O1 | 0.014 (2) | 0.025 (2) | 0.017 (3) | 0.0061 (16) | 0.007 (2) | 0.0023 (18) |
O2 | 0.017 (2) | 0.027 (2) | 0.022 (3) | −0.0004 (18) | 0.010 (2) | 0.003 (2) |
O3 | 0.0132 (19) | 0.026 (2) | 0.023 (2) | 0.0076 (17) | 0.0103 (18) | 0.0051 (18) |
O4 | 0.020 (2) | 0.026 (2) | 0.017 (2) | 0.0049 (17) | 0.0105 (18) | 0.0055 (18) |
O5 | 0.0119 (18) | 0.0165 (19) | 0.020 (2) | 0.0056 (14) | 0.0079 (16) | 0.0003 (16) |
O6 | 0.027 (2) | 0.031 (2) | 0.046 (3) | −0.007 (2) | 0.012 (2) | −0.008 (2) |
O7 | 0.015 (2) | 0.026 (2) | 0.021 (3) | −0.0006 (18) | 0.0018 (18) | −0.0054 (19) |
O8 | 0.042 (3) | 0.015 (2) | 0.034 (3) | 0.0076 (19) | 0.018 (2) | −0.0070 (19) |
N1 | 0.012 (2) | 0.019 (3) | 0.020 (3) | −0.0022 (19) | 0.011 (2) | −0.001 (2) |
N2 | 0.017 (2) | 0.021 (3) | 0.007 (2) | 0.0070 (19) | 0.0026 (18) | 0.0004 (19) |
C1 | 0.015 (3) | 0.020 (3) | 0.014 (3) | 0.004 (2) | 0.006 (2) | −0.001 (3) |
C2 | 0.007 (2) | 0.020 (3) | 0.018 (3) | 0.002 (2) | 0.006 (2) | 0.000 (2) |
C3 | 0.007 (2) | 0.015 (2) | 0.020 (3) | 0.0017 (19) | 0.011 (2) | 0.000 (2) |
C4 | 0.010 (2) | 0.025 (3) | 0.023 (4) | 0.007 (2) | 0.009 (2) | 0.004 (3) |
C5 | 0.012 (2) | 0.018 (3) | 0.016 (3) | 0.006 (2) | 0.009 (2) | 0.002 (2) |
C6 | 0.007 (2) | 0.009 (2) | 0.018 (3) | 0.0019 (19) | 0.000 (2) | −0.004 (2) |
C7 | 0.013 (2) | 0.011 (2) | 0.023 (3) | 0.002 (2) | 0.011 (2) | 0.001 (2) |
C8 | 0.015 (3) | 0.027 (3) | 0.016 (3) | 0.001 (2) | 0.008 (2) | 0.003 (2) |
C9 | 0.022 (3) | 0.022 (3) | 0.018 (3) | 0.006 (2) | 0.012 (3) | 0.000 (2) |
C10 | 0.020 (3) | 0.035 (4) | 0.019 (3) | 0.006 (3) | 0.008 (3) | 0.001 (3) |
C11 | 0.021 (3) | 0.039 (4) | 0.031 (4) | 0.023 (3) | 0.010 (3) | 0.002 (3) |
C12 | 0.023 (3) | 0.033 (3) | 0.019 (3) | 0.017 (3) | 0.005 (2) | −0.002 (3) |
C13 | 0.028 (3) | 0.015 (3) | 0.016 (3) | 0.014 (2) | 0.012 (2) | 0.004 (2) |
C14 | 0.041 (4) | 0.014 (3) | 0.014 (3) | 0.007 (2) | 0.013 (3) | 0.000 (2) |
Ni2 | 0.0117 (4) | 0.0255 (4) | 0.0149 (4) | 0.0002 (3) | 0.0046 (3) | −0.0005 (4) |
O9 | 0.016 (2) | 0.026 (2) | 0.025 (3) | 0.0019 (17) | 0.0042 (19) | −0.0064 (19) |
O10 | 0.033 (3) | 0.025 (2) | 0.039 (3) | 0.006 (2) | 0.017 (2) | −0.006 (2) |
O11 | 0.0126 (19) | 0.046 (3) | 0.022 (2) | −0.0129 (19) | 0.0059 (17) | −0.009 (2) |
O12 | 0.023 (2) | 0.054 (3) | 0.043 (3) | −0.018 (2) | 0.010 (2) | −0.014 (3) |
O13 | 0.014 (2) | 0.032 (3) | 0.015 (3) | 0.0021 (18) | 0.002 (2) | 0.0032 (19) |
O14 | 0.021 (2) | 0.029 (2) | 0.020 (3) | −0.0049 (19) | 0.012 (2) | 0.004 (2) |
O15 | 0.015 (2) | 0.032 (2) | 0.020 (2) | 0.0032 (18) | 0.0080 (18) | 0.0025 (19) |
O16 | 0.036 (3) | 0.025 (2) | 0.014 (2) | 0.007 (2) | 0.011 (2) | 0.0061 (19) |
N3 | 0.021 (2) | 0.028 (3) | 0.014 (3) | 0.001 (2) | 0.010 (2) | −0.002 (2) |
N4 | 0.010 (2) | 0.016 (2) | 0.016 (3) | 0.0050 (17) | 0.0030 (19) | −0.001 (2) |
C15 | 0.039 (4) | 0.022 (3) | 0.022 (3) | 0.006 (3) | 0.014 (3) | 0.007 (3) |
C16 | 0.032 (3) | 0.030 (4) | 0.015 (3) | 0.008 (3) | 0.010 (3) | 0.000 (3) |
C17 | 0.016 (3) | 0.042 (4) | 0.023 (3) | 0.011 (3) | 0.010 (2) | 0.008 (3) |
C18 | 0.024 (3) | 0.063 (6) | 0.029 (4) | 0.012 (3) | 0.009 (3) | 0.004 (4) |
C19 | 0.020 (3) | 0.053 (4) | 0.018 (3) | −0.002 (3) | 0.010 (2) | 0.002 (3) |
C20 | 0.020 (3) | 0.047 (4) | 0.014 (3) | 0.000 (3) | 0.006 (2) | 0.001 (3) |
C21 | 0.015 (3) | 0.049 (4) | 0.021 (3) | −0.012 (3) | 0.011 (2) | −0.011 (3) |
C22 | 0.021 (3) | 0.008 (2) | 0.019 (3) | −0.004 (2) | 0.003 (2) | −0.002 (2) |
C23 | 0.022 (3) | 0.011 (2) | 0.015 (3) | −0.004 (2) | 0.007 (2) | −0.007 (2) |
C24 | 0.023 (3) | 0.017 (3) | 0.012 (3) | −0.002 (2) | 0.000 (2) | −0.002 (2) |
C25 | 0.017 (3) | 0.025 (3) | 0.024 (4) | 0.001 (2) | 0.006 (3) | 0.002 (3) |
C26 | 0.025 (3) | 0.020 (3) | 0.021 (4) | 0.008 (3) | 0.010 (3) | 0.000 (3) |
C27 | 0.015 (3) | 0.022 (3) | 0.022 (3) | −0.004 (2) | 0.011 (2) | −0.003 (3) |
C28 | 0.023 (3) | 0.020 (3) | 0.014 (3) | 0.002 (2) | 0.006 (3) | −0.002 (3) |
Ni3 | 0.0203 (4) | 0.0218 (4) | 0.0148 (4) | 0.0061 (3) | 0.0087 (3) | 0.0009 (3) |
O17 | 0.023 (3) | 0.030 (3) | 0.017 (3) | 0.0018 (18) | 0.012 (2) | −0.0041 (18) |
O18 | 0.030 (2) | 0.030 (2) | 0.016 (3) | −0.007 (2) | 0.017 (2) | −0.004 (2) |
O19 | 0.030 (2) | 0.023 (2) | 0.017 (2) | 0.0024 (18) | 0.0136 (19) | 0.0009 (18) |
O20 | 0.055 (3) | 0.032 (3) | 0.021 (3) | −0.010 (2) | 0.025 (2) | −0.008 (2) |
O21 | 0.015 (2) | 0.018 (2) | 0.022 (2) | −0.0010 (16) | 0.0066 (18) | −0.0059 (18) |
O22 | 0.021 (2) | 0.028 (2) | 0.029 (3) | −0.0034 (18) | 0.0134 (19) | −0.0077 (19) |
O23 | 0.062 (4) | 0.030 (3) | 0.040 (3) | 0.023 (3) | 0.035 (3) | 0.015 (2) |
O24 | 0.084 (5) | 0.078 (5) | 0.062 (4) | 0.067 (4) | 0.047 (4) | 0.050 (4) |
N5 | 0.022 (2) | 0.012 (2) | 0.010 (2) | 0.0010 (19) | 0.006 (2) | −0.0033 (19) |
N6 | 0.011 (2) | 0.043 (3) | 0.013 (3) | 0.013 (2) | 0.0066 (19) | 0.002 (2) |
C29 | 0.020 (3) | 0.014 (3) | 0.020 (3) | 0.005 (2) | 0.012 (3) | 0.000 (3) |
C30 | 0.029 (3) | 0.011 (3) | 0.011 (3) | 0.000 (2) | 0.010 (2) | −0.001 (2) |
C31 | 0.027 (3) | 0.031 (4) | 0.027 (4) | 0.001 (3) | 0.016 (3) | 0.000 (3) |
C32 | 0.031 (4) | 0.016 (3) | 0.025 (4) | −0.008 (3) | 0.006 (3) | 0.002 (3) |
C33 | 0.037 (4) | 0.016 (3) | 0.017 (3) | 0.001 (3) | 0.008 (3) | −0.001 (2) |
C34 | 0.027 (3) | 0.020 (3) | 0.013 (3) | 0.003 (2) | 0.010 (3) | −0.003 (2) |
C35 | 0.038 (4) | 0.023 (3) | 0.014 (3) | 0.004 (3) | 0.018 (3) | 0.001 (3) |
C36 | 0.046 (4) | 0.050 (5) | 0.032 (4) | 0.036 (4) | 0.028 (4) | 0.021 (3) |
C37 | 0.014 (3) | 0.056 (5) | 0.011 (3) | 0.018 (3) | 0.008 (2) | 0.006 (3) |
C38 | 0.014 (3) | 0.111 (8) | 0.016 (3) | 0.024 (4) | 0.008 (3) | 0.013 (5) |
C39 | 0.010 (3) | 0.122 (10) | 0.019 (4) | 0.001 (4) | 0.004 (3) | 0.000 (4) |
C40 | 0.028 (4) | 0.069 (6) | 0.026 (4) | −0.004 (4) | 0.016 (3) | −0.008 (4) |
C41 | 0.007 (2) | 0.046 (4) | 0.013 (3) | 0.002 (2) | 0.006 (2) | −0.002 (3) |
C42 | 0.008 (2) | 0.031 (3) | 0.010 (3) | 0.002 (2) | 0.007 (2) | −0.004 (2) |
Ni4 | 0.0194 (4) | 0.0276 (5) | 0.0148 (4) | −0.0058 (4) | 0.0077 (3) | 0.0002 (4) |
O25 | 0.012 (2) | 0.030 (2) | 0.023 (3) | 0.0019 (17) | 0.0069 (18) | 0.0097 (19) |
O26 | 0.027 (2) | 0.033 (3) | 0.029 (3) | 0.004 (2) | 0.010 (2) | 0.005 (2) |
O27 | 0.053 (3) | 0.021 (2) | 0.037 (3) | −0.017 (2) | 0.029 (3) | −0.011 (2) |
O28 | 0.071 (4) | 0.082 (5) | 0.063 (4) | −0.062 (4) | 0.044 (4) | −0.049 (4) |
O29 | 0.020 (2) | 0.038 (3) | 0.015 (3) | −0.003 (2) | 0.006 (2) | 0.006 (2) |
O30 | 0.031 (3) | 0.035 (3) | 0.017 (3) | 0.004 (2) | 0.016 (2) | 0.005 (2) |
O31 | 0.036 (3) | 0.029 (2) | 0.020 (2) | −0.006 (2) | 0.018 (2) | −0.001 (2) |
O32 | 0.074 (4) | 0.035 (3) | 0.024 (3) | 0.007 (3) | 0.029 (3) | 0.006 (2) |
N7 | 0.009 (2) | 0.048 (3) | 0.019 (3) | −0.005 (2) | 0.009 (2) | 0.002 (2) |
N8 | 0.023 (3) | 0.013 (2) | 0.011 (3) | −0.002 (2) | 0.003 (2) | 0.0013 (19) |
C43 | 0.010 (2) | 0.039 (4) | 0.012 (3) | −0.002 (2) | 0.006 (2) | 0.002 (3) |
C44 | 0.014 (3) | 0.042 (4) | 0.010 (3) | −0.004 (2) | 0.005 (2) | 0.001 (3) |
C45 | 0.018 (3) | 0.075 (6) | 0.025 (4) | 0.006 (3) | 0.010 (3) | 0.007 (4) |
C46 | 0.009 (3) | 0.077 (6) | 0.022 (4) | 0.001 (3) | 0.003 (2) | 0.011 (4) |
C47 | 0.013 (3) | 0.107 (8) | 0.016 (3) | −0.022 (4) | 0.004 (3) | −0.004 (4) |
C48 | 0.014 (3) | 0.049 (4) | 0.009 (3) | −0.013 (3) | 0.007 (2) | −0.008 (2) |
C49 | 0.041 (4) | 0.051 (5) | 0.029 (4) | −0.025 (3) | 0.025 (3) | −0.016 (3) |
C50 | 0.042 (4) | 0.023 (3) | 0.015 (3) | −0.008 (3) | 0.018 (3) | −0.005 (3) |
C51 | 0.037 (4) | 0.019 (3) | 0.012 (3) | 0.000 (3) | 0.010 (3) | 0.003 (2) |
C52 | 0.045 (4) | 0.015 (3) | 0.019 (4) | 0.001 (3) | 0.006 (3) | 0.004 (3) |
C53 | 0.035 (4) | 0.018 (3) | 0.023 (4) | 0.008 (3) | 0.002 (3) | 0.002 (3) |
C54 | 0.030 (4) | 0.025 (3) | 0.030 (4) | −0.002 (3) | 0.010 (3) | −0.001 (3) |
C55 | 0.027 (3) | 0.010 (3) | 0.013 (3) | −0.001 (2) | 0.008 (2) | 0.002 (2) |
C56 | 0.021 (3) | 0.017 (3) | 0.016 (3) | −0.006 (2) | 0.009 (3) | 0.000 (3) |
O1W | 0.046 (3) | 0.028 (3) | 0.040 (3) | 0.001 (2) | 0.032 (3) | −0.001 (2) |
O2W | 0.030 (3) | 0.034 (3) | 0.025 (3) | 0.003 (2) | 0.010 (2) | −0.004 (2) |
O3W | 0.023 (2) | 0.029 (2) | 0.022 (3) | 0.0031 (19) | 0.012 (2) | 0.003 (2) |
O4W | 0.045 (3) | 0.026 (2) | 0.031 (3) | 0.002 (2) | 0.023 (2) | −0.003 (2) |
O5W | 0.029 (3) | 0.038 (3) | 0.018 (3) | 0.0070 (19) | 0.013 (2) | 0.0034 (19) |
O6W | 0.040 (3) | 0.039 (3) | 0.018 (3) | −0.003 (2) | 0.013 (2) | −0.007 (2) |
O7W | 0.054 (3) | 0.035 (3) | 0.025 (3) | −0.023 (2) | 0.021 (2) | −0.003 (2) |
O8W | 0.075 (4) | 0.030 (3) | 0.043 (4) | 0.002 (3) | 0.037 (3) | −0.007 (2) |
O9W | 0.033 (2) | 0.043 (3) | 0.048 (3) | −0.017 (2) | 0.013 (2) | −0.009 (2) |
Ni1—N2 | 1.965 (5) | O19—C35 | 1.232 (9) |
Ni1—N1 | 1.976 (6) | O20—C35 | 1.270 (10) |
Ni1—O1 | 2.075 (6) | O21—C42 | 1.248 (8) |
Ni1—O5 | 2.089 (5) | O22—C42 | 1.258 (9) |
Ni1—O3 | 2.163 (6) | O23—C36 | 1.265 (11) |
Ni1—O7 | 2.169 (5) | O24—C36 | 1.239 (9) |
O1—C1 | 1.259 (8) | N5—C30 | 1.325 (9) |
O2—C1 | 1.261 (9) | N5—C34 | 1.371 (9) |
O3—C7 | 1.284 (8) | N6—C41 | 1.284 (10) |
O4—C7 | 1.259 (9) | N6—C37 | 1.355 (8) |
O5—C8 | 1.308 (7) | C29—C30 | 1.530 (10) |
O6—C8 | 1.225 (8) | C30—C31 | 1.380 (10) |
O7—C14 | 1.253 (9) | C31—C32 | 1.392 (12) |
O8—C14 | 1.290 (8) | C31—H31 | 0.9500 |
O8—H6C | 1.471 (18) | C32—C33 | 1.372 (11) |
N1—C6 | 1.313 (9) | C32—H32 | 0.9500 |
N1—C2 | 1.332 (9) | C33—C34 | 1.358 (10) |
N2—C9 | 1.314 (9) | C33—H33 | 0.9500 |
N2—C13 | 1.361 (8) | C34—C35 | 1.517 (10) |
C1—C2 | 1.500 (10) | C36—C37 | 1.467 (12) |
C2—C3 | 1.393 (8) | C37—C38 | 1.438 (12) |
C3—C4 | 1.399 (10) | C38—C39 | 1.309 (15) |
C3—H3 | 0.9500 | C38—H38 | 0.9500 |
C4—C5 | 1.402 (9) | C39—C40 | 1.424 (13) |
C4—H4 | 0.9500 | C39—H39 | 0.9500 |
C5—C6 | 1.398 (8) | C40—C41 | 1.399 (10) |
C5—H5 | 0.9500 | C40—H40 | 0.9500 |
C6—C7 | 1.500 (9) | C41—C42 | 1.489 (8) |
C8—C9 | 1.541 (8) | Ni4—N8 | 1.934 (6) |
C9—C10 | 1.346 (9) | Ni4—N7 | 1.984 (6) |
C10—C11 | 1.424 (10) | Ni4—O27 | 2.121 (5) |
C10—H10 | 0.9500 | Ni4—O29 | 2.121 (7) |
C11—C12 | 1.380 (11) | Ni4—O31 | 2.156 (6) |
C11—H11 | 0.9500 | Ni4—O25 | 2.213 (6) |
C12—C13 | 1.365 (9) | O25—C43 | 1.214 (8) |
C12—H12 | 0.9500 | O26—C43 | 1.291 (9) |
C13—C14 | 1.497 (10) | O27—C49 | 1.288 (10) |
Ni2—N3 | 1.963 (6) | O28—C49 | 1.236 (10) |
Ni2—N4 | 1.995 (5) | O29—C56 | 1.263 (9) |
Ni2—O11 | 2.065 (5) | O30—C56 | 1.233 (9) |
Ni2—O13 | 2.075 (6) | O31—C50 | 1.228 (10) |
Ni2—O15 | 2.142 (6) | O32—C50 | 1.283 (10) |
Ni2—O9 | 2.166 (5) | N7—C44 | 1.309 (10) |
O9—C15 | 1.249 (9) | N7—C48 | 1.340 (9) |
O10—C15 | 1.301 (9) | N8—C55 | 1.330 (9) |
O10—H10A | 0.93 (5) | N8—C51 | 1.368 (9) |
O11—C21 | 1.292 (8) | C43—C44 | 1.511 (9) |
O12—C21 | 1.222 (9) | C44—C45 | 1.429 (10) |
O13—C28 | 1.273 (8) | C45—C46 | 1.394 (12) |
O14—C28 | 1.248 (9) | C45—H45 | 0.9500 |
O15—C22 | 1.271 (8) | C46—C47 | 1.359 (13) |
O16—C22 | 1.261 (9) | C46—H46 | 0.9500 |
O16—H16 | 0.93 (8) | C47—C48 | 1.416 (11) |
N3—C20 | 1.339 (10) | C47—H47 | 0.9500 |
N3—C16 | 1.351 (9) | C48—C49 | 1.510 (12) |
N4—C23 | 1.290 (9) | C50—C51 | 1.526 (11) |
N4—C27 | 1.337 (9) | C51—C52 | 1.369 (11) |
C15—C16 | 1.484 (11) | C52—C53 | 1.371 (12) |
C16—C17 | 1.374 (9) | C52—H52 | 0.9500 |
C17—C18 | 1.401 (11) | C53—C54 | 1.402 (12) |
C17—H17 | 0.9500 | C53—H53 | 0.9500 |
C18—C19 | 1.399 (12) | C54—C55 | 1.392 (10) |
C18—H18 | 0.9500 | C54—H54 | 0.9500 |
C19—C20 | 1.399 (10) | C55—C56 | 1.537 (10) |
C19—H19 | 0.9500 | O1W—H1A | 0.960 (14) |
C20—C21 | 1.487 (11) | O1W—H1B | 0.947 (14) |
C22—C23 | 1.499 (10) | O1W—H1C | 0.943 (14) |
C23—C24 | 1.391 (9) | O2W—H2A | 0.956 (14) |
C24—C25 | 1.394 (10) | O2W—H2B | 0.959 (14) |
C24—H24 | 0.9500 | O3W—H3A | 0.952 (14) |
C25—C26 | 1.388 (11) | O3W—H3B | 0.948 (14) |
C25—H25 | 0.9500 | O4W—H4A | 0.963 (15) |
C26—C27 | 1.388 (9) | O5W—H5A | 0.951 (14) |
C26—H26 | 0.9500 | O5W—H5B | 0.952 (14) |
C27—C28 | 1.497 (10) | O6W—H6A | 0.955 (14) |
Ni3—N5 | 1.936 (6) | O6W—H6B | 0.961 (14) |
Ni3—N6 | 1.992 (6) | O6W—H6C | 0.967 (14) |
Ni3—O17 | 2.134 (6) | O7W—H7A | 0.956 (14) |
Ni3—O23 | 2.135 (6) | O7W—H7B | 0.953 (14) |
Ni3—O21 | 2.177 (5) | O7W—H7C | 0.960 (14) |
Ni3—O19 | 2.179 (6) | O8W—H8A | 0.956 (14) |
O17—C29 | 1.265 (9) | O8W—H8B | 0.953 (14) |
O18—C29 | 1.250 (9) | ||
N2—Ni1—N1 | 176.0 (3) | O17—Ni3—O23 | 92.8 (2) |
N2—Ni1—O1 | 104.9 (2) | N5—Ni3—O21 | 103.1 (2) |
N1—Ni1—O1 | 78.8 (2) | N6—Ni3—O21 | 76.5 (2) |
N2—Ni1—O5 | 78.3 (2) | O17—Ni3—O21 | 94.3 (2) |
N1—Ni1—O5 | 100.0 (2) | O23—Ni3—O21 | 154.6 (2) |
O1—Ni1—O5 | 92.3 (2) | N5—Ni3—O19 | 77.8 (2) |
N2—Ni1—O3 | 99.2 (2) | N6—Ni3—O19 | 98.1 (2) |
N1—Ni1—O3 | 77.2 (2) | O17—Ni3—O19 | 156.3 (2) |
O1—Ni1—O3 | 155.9 (2) | O23—Ni3—O19 | 93.0 (2) |
O5—Ni1—O3 | 92.9 (2) | O21—Ni3—O19 | 90.2 (2) |
N2—Ni1—O7 | 77.8 (2) | C29—O17—Ni3 | 112.1 (5) |
N1—Ni1—O7 | 103.9 (2) | C35—O19—Ni3 | 112.2 (5) |
O1—Ni1—O7 | 93.0 (2) | C42—O21—Ni3 | 111.9 (4) |
O5—Ni1—O7 | 156.11 (19) | C36—O23—Ni3 | 114.0 (5) |
O3—Ni1—O7 | 91.7 (2) | C30—N5—C34 | 117.9 (6) |
C1—O1—Ni1 | 115.6 (5) | C30—N5—Ni3 | 121.1 (5) |
C7—O3—Ni1 | 114.0 (4) | C34—N5—Ni3 | 120.8 (5) |
C8—O5—Ni1 | 115.2 (4) | C41—N6—C37 | 123.3 (6) |
C14—O7—Ni1 | 112.8 (4) | C41—N6—Ni3 | 120.3 (5) |
C14—O8—H6C | 114 (2) | C37—N6—Ni3 | 116.4 (5) |
C6—N1—C2 | 123.8 (6) | O18—C29—O17 | 125.1 (7) |
C6—N1—Ni1 | 119.4 (4) | O18—C29—C30 | 117.1 (6) |
C2—N1—Ni1 | 116.8 (5) | O17—C29—C30 | 117.8 (6) |
C9—N2—C13 | 120.2 (6) | N5—C30—C31 | 124.8 (7) |
C9—N2—Ni1 | 120.7 (4) | N5—C30—C29 | 110.0 (6) |
C13—N2—Ni1 | 119.1 (5) | C31—C30—C29 | 125.1 (7) |
O1—C1—O2 | 125.5 (7) | C30—C31—C32 | 115.5 (7) |
O1—C1—C2 | 115.2 (6) | C30—C31—H31 | 122.2 |
O2—C1—C2 | 119.2 (6) | C32—C31—H31 | 122.2 |
N1—C2—C3 | 118.4 (6) | C33—C32—C31 | 120.9 (7) |
N1—C2—C1 | 113.7 (5) | C33—C32—H32 | 119.6 |
C3—C2—C1 | 127.7 (6) | C31—C32—H32 | 119.6 |
C2—C3—C4 | 119.3 (6) | C34—C33—C32 | 119.5 (7) |
C2—C3—H3 | 120.3 | C34—C33—H33 | 120.2 |
C4—C3—H3 | 120.3 | C32—C33—H33 | 120.2 |
C3—C4—C5 | 120.1 (6) | C33—C34—N5 | 121.2 (7) |
C3—C4—H4 | 119.9 | C33—C34—C35 | 129.3 (7) |
C5—C4—H4 | 119.9 | N5—C34—C35 | 109.4 (6) |
C6—C5—C4 | 116.6 (6) | O19—C35—O20 | 126.4 (7) |
C6—C5—H5 | 121.7 | O19—C35—C34 | 119.5 (6) |
C4—C5—H5 | 121.7 | O20—C35—C34 | 114.1 (7) |
N1—C6—C5 | 121.6 (6) | O24—C36—O23 | 126.0 (9) |
N1—C6—C7 | 114.6 (5) | O24—C36—C37 | 117.4 (9) |
C5—C6—C7 | 123.8 (6) | O23—C36—C37 | 116.6 (6) |
O4—C7—O3 | 126.4 (6) | N6—C37—C38 | 116.6 (8) |
O4—C7—C6 | 118.8 (5) | N6—C37—C36 | 114.8 (7) |
O3—C7—C6 | 114.8 (6) | C38—C37—C36 | 128.7 (7) |
O6—C8—O5 | 126.4 (6) | C39—C38—C37 | 120.3 (7) |
O6—C8—C9 | 119.5 (6) | C39—C38—H38 | 119.9 |
O5—C8—C9 | 114.1 (6) | C37—C38—H38 | 119.9 |
N2—C9—C10 | 124.5 (6) | C38—C39—C40 | 122.0 (8) |
N2—C9—C8 | 111.7 (6) | C38—C39—H39 | 119.0 |
C10—C9—C8 | 123.8 (6) | C40—C39—H39 | 119.0 |
C9—C10—C11 | 116.4 (7) | C41—C40—C39 | 114.8 (9) |
C9—C10—H10 | 121.8 | C41—C40—H40 | 122.6 |
C11—C10—H10 | 121.8 | C39—C40—H40 | 122.6 |
C12—C11—C10 | 119.3 (6) | N6—C41—C40 | 123.0 (7) |
C12—C11—H11 | 120.4 | N6—C41—C42 | 112.7 (6) |
C10—C11—H11 | 120.4 | C40—C41—C42 | 124.3 (7) |
C13—C12—C11 | 120.0 (6) | O21—C42—O22 | 124.6 (6) |
C13—C12—H12 | 120.0 | O21—C42—C41 | 118.6 (6) |
C11—C12—H12 | 120.0 | O22—C42—C41 | 116.7 (6) |
N2—C13—C12 | 119.7 (7) | N8—Ni4—N7 | 176.4 (3) |
N2—C13—C14 | 112.0 (5) | N8—Ni4—O27 | 100.8 (2) |
C12—C13—C14 | 128.3 (6) | N7—Ni4—O27 | 80.1 (3) |
O7—C14—O8 | 125.6 (7) | N8—Ni4—O29 | 78.6 (3) |
O7—C14—C13 | 118.1 (6) | N7—Ni4—O29 | 104.9 (3) |
O8—C14—C13 | 116.4 (6) | O27—Ni4—O29 | 92.4 (2) |
N3—Ni2—N4 | 175.9 (3) | N8—Ni4—O31 | 78.3 (3) |
N3—Ni2—O11 | 78.2 (2) | N7—Ni4—O31 | 98.2 (2) |
N4—Ni2—O11 | 99.3 (2) | O27—Ni4—O31 | 92.5 (2) |
N3—Ni2—O13 | 104.6 (2) | O29—Ni4—O31 | 156.9 (2) |
N4—Ni2—O13 | 78.7 (2) | N8—Ni4—O25 | 103.9 (2) |
O11—Ni2—O13 | 92.4 (2) | N7—Ni4—O25 | 75.3 (2) |
N3—Ni2—O15 | 99.4 (2) | O27—Ni4—O25 | 155.3 (2) |
N4—Ni2—O15 | 77.4 (2) | O29—Ni4—O25 | 92.9 (2) |
O11—Ni2—O15 | 92.8 (2) | O31—Ni4—O25 | 92.1 (2) |
O13—Ni2—O15 | 156.0 (2) | C43—O25—Ni4 | 113.7 (5) |
N3—Ni2—O9 | 77.2 (2) | C49—O27—Ni4 | 112.5 (5) |
N4—Ni2—O9 | 105.3 (2) | C56—O29—Ni4 | 113.1 (5) |
O11—Ni2—O9 | 155.4 (2) | C50—O31—Ni4 | 112.0 (5) |
O13—Ni2—O9 | 94.0 (2) | C44—N7—C48 | 122.4 (6) |
O15—Ni2—O9 | 90.8 (2) | C44—N7—Ni4 | 121.4 (5) |
C15—O9—Ni2 | 111.8 (5) | C48—N7—Ni4 | 116.3 (6) |
C15—O10—H10A | 113 (3) | C55—N8—C51 | 117.9 (6) |
C21—O11—Ni2 | 117.0 (5) | C55—N8—Ni4 | 120.9 (5) |
C28—O13—Ni2 | 116.5 (5) | C51—N8—Ni4 | 120.8 (5) |
C22—O15—Ni2 | 113.6 (5) | O25—C43—O26 | 125.6 (7) |
C22—O16—H16 | 105 (5) | O25—C43—C44 | 117.8 (7) |
C20—N3—C16 | 121.7 (7) | O26—C43—C44 | 116.6 (6) |
C20—N3—Ni2 | 117.5 (5) | N7—C44—C45 | 122.6 (7) |
C16—N3—Ni2 | 120.7 (5) | N7—C44—C43 | 111.9 (6) |
C23—N4—C27 | 125.8 (6) | C45—C44—C43 | 125.4 (7) |
C23—N4—Ni2 | 118.4 (5) | C46—C45—C44 | 114.7 (9) |
C27—N4—Ni2 | 115.8 (5) | C46—C45—H45 | 122.6 |
O9—C15—O10 | 124.6 (7) | C44—C45—H45 | 122.6 |
O9—C15—C16 | 120.2 (6) | C47—C46—C45 | 122.4 (7) |
O10—C15—C16 | 115.2 (7) | C47—C46—H46 | 118.8 |
N3—C16—C17 | 121.8 (7) | C45—C46—H46 | 118.8 |
N3—C16—C15 | 109.9 (6) | C46—C47—C48 | 119.1 (7) |
C17—C16—C15 | 128.2 (7) | C46—C47—H47 | 120.4 |
C16—C17—C18 | 118.6 (7) | C48—C47—H47 | 120.4 |
C16—C17—H17 | 120.7 | N7—C48—C47 | 118.7 (8) |
C18—C17—H17 | 120.7 | N7—C48—C49 | 114.5 (6) |
C19—C18—C17 | 118.3 (7) | C47—C48—C49 | 126.8 (7) |
C19—C18—H18 | 120.8 | O28—C49—O27 | 124.4 (9) |
C17—C18—H18 | 120.8 | O28—C49—C48 | 119.0 (8) |
C18—C19—C20 | 120.8 (7) | O27—C49—C48 | 116.6 (6) |
C18—C19—H19 | 119.6 | O31—C50—O32 | 126.1 (7) |
C20—C19—H19 | 119.6 | O31—C50—C51 | 120.2 (7) |
N3—C20—C19 | 118.7 (7) | O32—C50—C51 | 113.7 (7) |
N3—C20—C21 | 114.6 (6) | N8—C51—C52 | 121.3 (7) |
C19—C20—C21 | 126.7 (7) | N8—C51—C50 | 108.5 (6) |
O12—C21—O11 | 126.0 (8) | C52—C51—C50 | 130.2 (7) |
O12—C21—C20 | 121.3 (6) | C51—C52—C53 | 119.7 (7) |
O11—C21—C20 | 112.6 (6) | C51—C52—H52 | 120.1 |
O16—C22—O15 | 125.2 (7) | C53—C52—H52 | 120.1 |
O16—C22—C23 | 119.1 (6) | C52—C53—C54 | 120.8 (7) |
O15—C22—C23 | 115.7 (6) | C52—C53—H53 | 119.6 |
N4—C23—C24 | 120.7 (6) | C54—C53—H53 | 119.6 |
N4—C23—C22 | 114.7 (6) | C55—C54—C53 | 115.3 (8) |
C24—C23—C22 | 124.6 (6) | C55—C54—H54 | 122.3 |
C23—C24—C25 | 116.8 (7) | C53—C54—H54 | 122.3 |
C23—C24—H24 | 121.6 | N8—C55—C54 | 124.9 (7) |
C25—C24—H24 | 121.6 | N8—C55—C56 | 110.0 (6) |
C26—C25—C24 | 120.0 (6) | C54—C55—C56 | 125.1 (7) |
C26—C25—H25 | 120.0 | O30—C56—O29 | 125.1 (7) |
C24—C25—H25 | 120.0 | O30—C56—C55 | 117.8 (6) |
C25—C26—C27 | 120.2 (7) | O29—C56—C55 | 117.1 (6) |
C25—C26—H26 | 119.9 | H1A—O1W—H1B | 110 (3) |
C27—C26—H26 | 119.9 | H1A—O1W—H1C | 110 (3) |
N4—C27—C26 | 116.3 (7) | H1B—O1W—H1C | 108 (3) |
N4—C27—C28 | 115.3 (6) | H2A—O2W—H2B | 104 (3) |
C26—C27—C28 | 128.3 (7) | H3A—O3W—H3B | 110 (3) |
O14—C28—O13 | 126.7 (7) | H5A—O5W—H5B | 106 (3) |
O14—C28—C27 | 119.5 (6) | H6A—O6W—H6B | 105 (3) |
O13—C28—C27 | 113.7 (6) | H6A—O6W—H6C | 106 (3) |
N5—Ni3—N6 | 175.8 (3) | H6B—O6W—H6C | 103 (3) |
N5—Ni3—O17 | 78.6 (2) | H7A—O7W—H7B | 108 (3) |
N6—Ni3—O17 | 105.6 (2) | H7A—O7W—H7C | 106 (3) |
N5—Ni3—O23 | 102.2 (3) | H7B—O7W—H7C | 106 (3) |
N6—Ni3—O23 | 78.1 (3) | H8A—O8W—H8B | 105 (3) |
D—H···A | D—H | H···A | D···A | D—H···A |
O1W—H1A···O5 | 0.96 (1) | 1.70 (2) | 2.637 (7) | 164 (6) |
O1W—H1B···O4i | 0.95 (1) | 1.56 (2) | 2.461 (7) | 158 (5) |
O1W—H1C···O11Wi | 0.94 (1) | 1.67 (4) | 2.472 (12) | 141 (6) |
O1W—H1C···O14Wi | 0.94 (1) | 1.72 (2) | 2.659 (18) | 177 (7) |
O2W—H2B···O30i | 0.96 (1) | 1.78 (3) | 2.713 (9) | 163 (6) |
O3W—H3A···O2ii | 0.95 (1) | 1.84 (4) | 2.697 (7) | 148 (5) |
O3W—H3B···O18iii | 0.95 (1) | 1.72 (2) | 2.648 (8) | 166 (6) |
O4W—H4A···O15W | 0.96 (2) | 1.68 (3) | 2.623 (17) | 165 (7) |
O5W—H5A···O2 | 0.95 (1) | 1.76 (3) | 2.682 (9) | 164 (7) |
O5W—H5B···O18iv | 0.95 (1) | 1.91 (4) | 2.782 (8) | 151 (6) |
O6W—H6A···O30iv | 0.96 (1) | 1.81 (3) | 2.716 (8) | 158 (5) |
O6W—H6C···O7 | 0.97 (1) | 2.65 (5) | 3.362 (8) | 131 (5) |
O6W—H6C···O8 | 0.97 (1) | 1.47 (2) | 2.429 (8) | 170 (6) |
O7W—H7A···O20 | 0.96 (1) | 1.53 (2) | 2.470 (8) | 168 (6) |
O7W—H7C···O27v | 0.96 (1) | 1.66 (4) | 2.526 (8) | 149 (6) |
O8W—H8A···O23 | 0.96 (1) | 1.72 (4) | 2.531 (9) | 141 (6) |
O8W—H8B···O32 | 0.95 (1) | 1.84 (7) | 2.495 (9) | 123 (7) |
Symmetry codes: (i) x, −y+2, z+1/2; (ii) x+1/2, y−1/2, z; (iii) x, −y+1, z+1/2; (iv) x−1/2, −y+3/2, z+1/2; (v) x, y, z+1. |
C14H7N2NiO8·H3O·H2O·O | F(000) = 904 |
Mr = 442.97 | Dx = 1.716 Mg m−3 |
Monoclinic, P21/c | Mo Kα radiation, λ = 0.71073 Å |
a = 13.6716 (8) Å | Cell parameters from 9943 reflections |
b = 10.0554 (6) Å | θ = 2.6–31.5° |
c = 13.7813 (8) Å | µ = 1.20 mm−1 |
β = 115.185 (3)° | T = 298 K |
V = 1714.46 (18) Å3 | Block, blue-green |
Z = 4 | 0.47 × 0.40 × 0.34 mm |
Bruker Kappa DUO with Photon 100 detector diffractometer | 5701 independent reflections |
Radiation source: microsource | 4751 reflections with I > 2σ(I) |
Detector resolution: 10.42 pixels mm-1 | Rint = 0.025 |
ω and φ scans | θmax = 31.6°, θmin = 2.6° |
Absorption correction: multi-scan SADABS (Shedrick, 2014) | h = −20→20 |
Tmin = 0.653, Tmax = 0.746 | k = −14→11 |
18349 measured reflections | l = −16→20 |
Refinement on F2 | Secondary atom site location: difference Fourier map |
Least-squares matrix: full | Hydrogen site location: mixed |
R[F2 > 2σ(F2)] = 0.038 | H atoms treated by a mixture of independent and constrained refinement |
wR(F2) = 0.110 | w = 1/[σ2(Fo2) + (0.0564P)2 + 0.8461P] where P = (Fo2 + 2Fc2)/3 |
S = 1.04 | (Δ/σ)max = 0.001 |
5701 reflections | Δρmax = 0.80 e Å−3 |
277 parameters | Δρmin = −0.73 e Å−3 |
4 restraints | Extinction correction: SHELXL-2016/6 (Sheldrick 2016), Fc*=kFc[1+0.001xFc2λ3/sin(2θ)]-1/4 |
Primary atom site location: structure-invariant direct methods | Extinction coefficient: 0.0236 (14) |
Geometry. All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. |
Refinement. One of the three solvate waters is disordered into 3 sites and hydrogen atoms could not be reliably added. |
x | y | z | Uiso*/Ueq | Occ. (<1) | |
Ni1 | 0.24988 (2) | 0.49365 (2) | 0.24789 (2) | 0.02873 (8) | |
N1 | 0.10554 (10) | 0.41406 (12) | 0.17530 (10) | 0.0278 (2) | |
N2 | 0.39697 (9) | 0.56861 (14) | 0.31362 (10) | 0.0299 (2) | |
O1 | 0.19345 (10) | 0.51023 (12) | 0.36687 (10) | 0.0367 (3) | |
O2 | 0.04743 (11) | 0.46980 (15) | 0.39573 (10) | 0.0427 (3) | |
O3 | 0.12913 (12) | 0.34632 (14) | −0.06306 (10) | 0.0467 (3) | |
O4 | 0.24047 (9) | 0.44477 (13) | 0.09067 (10) | 0.0379 (3) | |
O5 | 0.22437 (9) | 0.70592 (12) | 0.20649 (10) | 0.0378 (3) | |
O6 | 0.31886 (12) | 0.89359 (13) | 0.22388 (12) | 0.0471 (3) | |
H6A | 0.248 (3) | 0.932 (4) | 0.176 (3) | 0.113 (12)* | |
O7 | 0.51307 (15) | 0.26162 (19) | 0.41839 (16) | 0.0712 (5) | |
O8 | 0.34227 (11) | 0.32402 (12) | 0.31883 (11) | 0.0423 (3) | |
O9 | 0.25429 (16) | 0.38941 (17) | −0.14492 (14) | 0.0564 (4) | |
H9A | 0.286 (3) | 0.317 (4) | −0.160 (3) | 0.092 (11)* | |
H9B | 0.304 (3) | 0.450 (3) | −0.104 (3) | 0.071 (8)* | |
H9C | 0.197 (3) | 0.369 (4) | −0.104 (3) | 0.127 (14)* | |
O10 | 0.15270 (13) | 1.01524 (14) | 0.10944 (13) | 0.0479 (3)* | |
H10A | 0.136 (3) | 0.993 (3) | 0.039 (3) | 0.098 (13)* | |
H10B | 0.097 (2) | 1.000 (3) | 0.126 (3) | 0.070 (9)* | |
O11A | 0.3833 (6) | 0.5365 (7) | 0.0113 (5) | 0.0686 (8)* | 0.334 (5) |
O11B | 0.3355 (4) | 0.5895 (5) | −0.0250 (4) | 0.0686 (8)* | 0.405 (4) |
O11C | 0.4353 (7) | 0.5198 (7) | −0.0066 (7) | 0.0686 (8)* | 0.262 (4) |
C1 | 0.09889 (12) | 0.46620 (16) | 0.33977 (12) | 0.0317 (3) | |
C2 | 0.04525 (11) | 0.40407 (15) | 0.22931 (12) | 0.0293 (3) | |
C3 | −0.05401 (13) | 0.34062 (17) | 0.18468 (14) | 0.0375 (3) | |
H3 | −0.096019 | 0.332531 | 0.222592 | 0.045* | |
C4 | −0.08916 (14) | 0.28935 (18) | 0.08166 (15) | 0.0409 (4) | |
H4 | −0.155873 | 0.247053 | 0.049723 | 0.049* | |
C5 | −0.02547 (13) | 0.30081 (16) | 0.02613 (13) | 0.0362 (3) | |
H5 | −0.048238 | 0.266603 | −0.042755 | 0.043* | |
C6 | 0.07287 (12) | 0.36467 (14) | 0.07649 (11) | 0.0292 (3) | |
C7 | 0.15440 (13) | 0.38726 (15) | 0.03162 (12) | 0.0327 (3) | |
C8 | 0.30988 (12) | 0.76907 (16) | 0.23960 (12) | 0.0326 (3) | |
C9 | 0.41358 (12) | 0.69734 (17) | 0.30348 (12) | 0.0322 (3) | |
C10 | 0.51644 (14) | 0.7516 (2) | 0.34797 (15) | 0.0439 (4) | |
H10 | 0.527663 | 0.841477 | 0.340325 | 0.053* | |
C11 | 0.60226 (14) | 0.6669 (2) | 0.40446 (16) | 0.0511 (5) | |
H11 | 0.672359 | 0.700262 | 0.435576 | 0.061* | |
C12 | 0.58434 (13) | 0.5341 (2) | 0.41470 (14) | 0.0460 (4) | |
H12 | 0.641579 | 0.477222 | 0.452648 | 0.055* | |
C13 | 0.47867 (13) | 0.48674 (18) | 0.36704 (13) | 0.0348 (3) | |
C14 | 0.44425 (15) | 0.34478 (19) | 0.36934 (15) | 0.0418 (4) |
U11 | U22 | U33 | U12 | U13 | U23 | |
Ni1 | 0.02366 (11) | 0.03313 (12) | 0.02836 (12) | −0.00153 (6) | 0.01008 (8) | −0.00108 (7) |
N1 | 0.0278 (5) | 0.0285 (5) | 0.0270 (5) | −0.0016 (4) | 0.0117 (4) | −0.0010 (4) |
N2 | 0.0230 (5) | 0.0401 (7) | 0.0260 (5) | 0.0010 (5) | 0.0099 (4) | 0.0014 (5) |
O1 | 0.0291 (5) | 0.0498 (7) | 0.0305 (5) | −0.0044 (4) | 0.0120 (4) | −0.0081 (4) |
O2 | 0.0403 (6) | 0.0588 (8) | 0.0353 (6) | −0.0049 (6) | 0.0222 (5) | −0.0074 (6) |
O3 | 0.0609 (8) | 0.0504 (7) | 0.0345 (6) | −0.0080 (6) | 0.0259 (6) | −0.0100 (5) |
O4 | 0.0365 (6) | 0.0455 (6) | 0.0363 (6) | −0.0035 (5) | 0.0198 (5) | −0.0031 (5) |
O5 | 0.0270 (5) | 0.0379 (6) | 0.0411 (6) | 0.0006 (4) | 0.0073 (4) | 0.0016 (5) |
O6 | 0.0467 (7) | 0.0371 (6) | 0.0552 (8) | −0.0024 (5) | 0.0196 (6) | 0.0064 (6) |
O7 | 0.0666 (10) | 0.0665 (10) | 0.0808 (12) | 0.0355 (9) | 0.0316 (9) | 0.0314 (9) |
O8 | 0.0460 (7) | 0.0371 (6) | 0.0471 (7) | 0.0052 (5) | 0.0228 (6) | 0.0072 (5) |
O9 | 0.0776 (11) | 0.0467 (8) | 0.0595 (9) | −0.0027 (8) | 0.0432 (9) | −0.0014 (7) |
C1 | 0.0309 (7) | 0.0357 (7) | 0.0291 (7) | 0.0010 (6) | 0.0132 (5) | −0.0005 (6) |
C2 | 0.0282 (6) | 0.0310 (6) | 0.0293 (6) | −0.0016 (5) | 0.0129 (5) | −0.0007 (5) |
C3 | 0.0321 (7) | 0.0405 (8) | 0.0420 (8) | −0.0074 (6) | 0.0179 (6) | −0.0022 (7) |
C4 | 0.0329 (7) | 0.0396 (8) | 0.0444 (9) | −0.0108 (6) | 0.0107 (7) | −0.0045 (7) |
C5 | 0.0376 (8) | 0.0327 (7) | 0.0314 (7) | −0.0050 (6) | 0.0081 (6) | −0.0047 (6) |
C6 | 0.0327 (6) | 0.0264 (6) | 0.0271 (6) | −0.0003 (5) | 0.0114 (5) | −0.0006 (5) |
C7 | 0.0402 (8) | 0.0299 (7) | 0.0302 (7) | 0.0022 (6) | 0.0170 (6) | 0.0005 (5) |
C8 | 0.0331 (7) | 0.0358 (7) | 0.0293 (6) | −0.0012 (6) | 0.0135 (5) | −0.0002 (6) |
C9 | 0.0272 (6) | 0.0420 (8) | 0.0275 (6) | −0.0036 (6) | 0.0117 (5) | −0.0013 (6) |
C10 | 0.0343 (8) | 0.0557 (10) | 0.0416 (9) | −0.0131 (7) | 0.0160 (7) | −0.0056 (8) |
C11 | 0.0250 (7) | 0.0790 (15) | 0.0445 (10) | −0.0098 (8) | 0.0101 (7) | −0.0063 (9) |
C12 | 0.0253 (7) | 0.0769 (13) | 0.0332 (8) | 0.0099 (8) | 0.0098 (6) | 0.0007 (8) |
C13 | 0.0272 (7) | 0.0517 (9) | 0.0263 (7) | 0.0079 (6) | 0.0121 (5) | 0.0040 (6) |
C14 | 0.0453 (9) | 0.0464 (9) | 0.0392 (8) | 0.0163 (7) | 0.0232 (7) | 0.0108 (7) |
Ni1—N1 | 1.9634 (12) | O9—H9C | 1.16 (4) |
Ni1—N2 | 1.9703 (12) | O10—H10A | 0.93 (3) |
Ni1—O1 | 2.0948 (12) | O10—H10B | 0.89 (2) |
Ni1—O8 | 2.1000 (12) | O11C—O11Ci | 1.746 (18) |
Ni1—O4 | 2.1716 (12) | C1—C2 | 1.515 (2) |
Ni1—O5 | 2.1986 (12) | C2—C3 | 1.384 (2) |
N1—C2 | 1.3289 (18) | C3—C4 | 1.390 (2) |
N1—C6 | 1.3352 (18) | C3—H3 | 0.9300 |
N2—C13 | 1.329 (2) | C4—C5 | 1.387 (3) |
N2—C9 | 1.332 (2) | C4—H4 | 0.9300 |
O1—C1 | 1.2634 (19) | C5—C6 | 1.381 (2) |
O2—C1 | 1.2460 (19) | C5—H5 | 0.9300 |
O3—C7 | 1.2678 (19) | C6—C7 | 1.504 (2) |
O3—H9C | 1.30 (4) | C8—C9 | 1.498 (2) |
O4—C7 | 1.251 (2) | C9—C10 | 1.385 (2) |
O5—C8 | 1.2344 (19) | C10—C11 | 1.390 (3) |
O6—C8 | 1.286 (2) | C10—H10 | 0.9300 |
O6—H6A | 0.99 (4) | C11—C12 | 1.376 (3) |
O7—C14 | 1.225 (2) | C11—H11 | 0.9300 |
O8—C14 | 1.283 (2) | C12—C13 | 1.392 (2) |
O9—H9A | 0.91 (4) | C12—H12 | 0.9300 |
O9—H9B | 0.91 (4) | C13—C14 | 1.508 (3) |
N1—Ni1—N2 | 176.37 (5) | C2—C3—C4 | 118.18 (15) |
N1—Ni1—O1 | 78.83 (5) | C2—C3—H3 | 120.9 |
N2—Ni1—O1 | 104.68 (5) | C4—C3—H3 | 120.9 |
N1—Ni1—O8 | 100.43 (5) | C5—C4—C3 | 120.49 (15) |
N2—Ni1—O8 | 78.62 (5) | C5—C4—H4 | 119.8 |
O1—Ni1—O8 | 92.82 (5) | C3—C4—H4 | 119.8 |
N1—Ni1—O4 | 77.25 (5) | C6—C5—C4 | 117.82 (15) |
N2—Ni1—O4 | 99.26 (5) | C6—C5—H5 | 121.1 |
O1—Ni1—O4 | 156.04 (5) | C4—C5—H5 | 121.1 |
O8—Ni1—O4 | 92.82 (5) | N1—C6—C5 | 121.14 (14) |
N1—Ni1—O5 | 104.45 (5) | N1—C6—C7 | 112.22 (12) |
N2—Ni1—O5 | 76.47 (5) | C5—C6—C7 | 126.63 (14) |
O1—Ni1—O5 | 93.17 (5) | O4—C7—O3 | 126.03 (15) |
O8—Ni1—O5 | 155.09 (5) | O4—C7—C6 | 117.29 (13) |
O4—Ni1—O5 | 91.45 (5) | O3—C7—C6 | 116.67 (14) |
C2—N1—C6 | 121.67 (13) | O5—C8—O6 | 125.60 (15) |
C2—N1—Ni1 | 118.29 (10) | O5—C8—C9 | 118.70 (14) |
C6—N1—Ni1 | 119.92 (10) | O6—C8—C9 | 115.70 (14) |
C13—N2—C9 | 121.28 (14) | N2—C9—C10 | 121.54 (16) |
C13—N2—Ni1 | 118.06 (12) | N2—C9—C8 | 111.63 (13) |
C9—N2—Ni1 | 120.65 (10) | C10—C9—C8 | 126.83 (16) |
C1—O1—Ni1 | 114.34 (10) | C9—C10—C11 | 117.57 (18) |
C7—O3—H9C | 117.5 (18) | C9—C10—H10 | 121.2 |
C7—O4—Ni1 | 113.17 (10) | C11—C10—H10 | 121.2 |
C8—O5—Ni1 | 112.50 (10) | C12—C11—C10 | 120.50 (16) |
C8—O6—H6A | 111 (2) | C12—C11—H11 | 119.7 |
C14—O8—Ni1 | 114.83 (11) | C10—C11—H11 | 119.7 |
H9A—O9—H9B | 112 (3) | C11—C12—C13 | 118.57 (17) |
H9A—O9—H9C | 116 (3) | C11—C12—H12 | 120.7 |
H9B—O9—H9C | 107 (3) | C13—C12—H12 | 120.7 |
H10A—O10—H10B | 112 (3) | N2—C13—C12 | 120.54 (17) |
O2—C1—O1 | 125.67 (15) | N2—C13—C14 | 113.68 (14) |
O2—C1—C2 | 118.33 (14) | C12—C13—C14 | 125.78 (16) |
O1—C1—C2 | 116.00 (13) | O7—C14—O8 | 126.2 (2) |
N1—C2—C3 | 120.69 (14) | O7—C14—C13 | 118.99 (19) |
N1—C2—C1 | 112.41 (12) | O8—C14—C13 | 114.80 (14) |
C3—C2—C1 | 126.89 (14) |
Symmetry code: (i) −x+1, −y+1, −z. |
D—H···A | D—H | H···A | D···A | D—H···A |
O9—H9C···O3 | 1.16 (4) | 1.30 (4) | 2.456 (2) | 178 (4) |
O6—H6A···O10 | 0.99 (4) | 1.49 (4) | 2.469 (2) | 169 (4) |
O9—H9A···O8ii | 0.91 (4) | 1.70 (4) | 2.610 (2) | 176 (3) |
O10—H10A···O2iii | 0.93 (3) | 1.86 (3) | 2.676 (2) | 145 (3) |
O10—H10B···O2iv | 0.89 (2) | 1.90 (3) | 2.745 (2) | 159 (3) |
Symmetry codes: (ii) x, −y+1/2, z−1/2; (iii) x, −y+3/2, z−1/2; (iv) −x, y+1/2, −z+1/2. |