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The structure of Ni(Hpydc)2·3H2O (H2pydc = pyridine-2,6-di­carb­oxy­lic acid, also known as dipicolinic acid) has been reinvestigated at variable temperatures. At room temperature, it matches the known structure in the space group P21/c, but at 180 K it undergoes a phase transformation to a twinned structure in Cc. By 120 K, the structure is ordered and twinned with Z′ = 4, and shows interesting short hydrogen-bonding interactions that include the formation of hydroxonium species.

Supporting information

cif

Crystallographic Information File (CIF) https://doi.org/10.1107/S2052520617004334/eb5059sup1.cif
Contains datablocks mn2293, 180c, 298d, 280d, 260d, 240d, 220d, 200d, 160d, 140d, 120d, 100d, 150u, 200u, 250u, 298u

hkl

Structure factor file (CIF format) https://doi.org/10.1107/S2052520617004334/eb5059mn2293sup2.hkl
Contains datablock mn2293

hkl

Structure factor file (CIF format) https://doi.org/10.1107/S2052520617004334/eb5059180csup3.hkl
Contains datablock 180c

hkl

Structure factor file (CIF format) https://doi.org/10.1107/S2052520617004334/eb5059298dsup4.hkl
Contains datablock 298d

hkl

Structure factor file (CIF format) https://doi.org/10.1107/S2052520617004334/eb5059280dsup5.hkl
Contains datablock 280d

hkl

Structure factor file (CIF format) https://doi.org/10.1107/S2052520617004334/eb5059260dsup6.hkl
Contains datablock 260d

hkl

Structure factor file (CIF format) https://doi.org/10.1107/S2052520617004334/eb5059240dsup7.hkl
Contains datablock 240d

hkl

Structure factor file (CIF format) https://doi.org/10.1107/S2052520617004334/eb5059220dsup8.hkl
Contains datablock 220d

hkl

Structure factor file (CIF format) https://doi.org/10.1107/S2052520617004334/eb5059200dsup9.hkl
Contains datablock 200d

hkl

Structure factor file (CIF format) https://doi.org/10.1107/S2052520617004334/eb5059160dsup10.hkl
Contains datablock 160d

hkl

Structure factor file (CIF format) https://doi.org/10.1107/S2052520617004334/eb5059140dsup11.hkl
Contains datablock 140d

hkl

Structure factor file (CIF format) https://doi.org/10.1107/S2052520617004334/eb5059120dsup12.hkl
Contains datablock 120

hkl

Structure factor file (CIF format) https://doi.org/10.1107/S2052520617004334/eb5059100dsup13.hkl
Contains datablock 100

hkl

Structure factor file (CIF format) https://doi.org/10.1107/S2052520617004334/eb5059150usup14.hkl
Contains datablock 150

hkl

Structure factor file (CIF format) https://doi.org/10.1107/S2052520617004334/eb5059200usup15.hkl
Contains datablock 200u

hkl

Structure factor file (CIF format) https://doi.org/10.1107/S2052520617004334/eb5059250usup16.hkl
Contains datablock 250u

hkl

Structure factor file (CIF format) https://doi.org/10.1107/S2052520617004334/eb5059298usup17.hkl
Contains datablock 298u

pdf

Portable Document Format (PDF) file https://doi.org/10.1107/S2052520617004334/eb5059sup18.pdf
History of the structure reports at room temperature, transformations, hydrogen bond parameters

Computing details top

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).

(mn2293) top
Crystal data top
C14H12N2NiO10·2(C14H10N2NiO9)·C14H7N2NiO8·H3O·7(H2O)Z = 2
Mr = 1779.92F(000) = 1824
Triclinic, P1Dx = 1.777 Mg m3
a = 13.7266 (12) ÅMo Kα radiation, λ = 0.71073 Å
b = 16.9157 (15) ÅCell parameters from 9917 reflections
c = 16.9080 (14) Åθ = 2.5–28.3°
α = 69.7619 (11)°µ = 1.24 mm1
β = 69.3377 (11)°T = 90 K
γ = 69.3655 (11)°Block, blue-green
V = 3325.9 (5) Å30.41 × 0.25 × 0.17 mm
Data collection top
Bruker Apex II
diffractometer
16469 independent reflections
Radiation source: fine-focus sealed tube16170 reflections with I > 2σ(I)
Detector resolution: 8.3 pixels mm-1Rint = 0.018
ω scansθmax = 28.3°, θmin = 1.6°
Absorption correction: multi-scan
SADABS (Sheldrick, 2014)
h = 1818
Tmin = 0.655, Tmax = 0.746k = 2222
46008 measured reflectionsl = 2222
Refinement top
Refinement on F20 restraints
Least-squares matrix: fullHydrogen site location: mixed
R[F2 > 2σ(F2)] = 0.020H 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 reflectionsΔρmax = 0.50 e Å3
1138 parametersΔρmin = 0.59 e Å3
Special details top

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.

Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top
xyzUiso*/Ueq
Ni10.24678 (2)0.62448 (2)0.12902 (2)0.00918 (4)
O10.29354 (8)0.49888 (7)0.21576 (7)0.0124 (2)
O20.28983 (9)0.43838 (7)0.35757 (7)0.0142 (2)
O30.06519 (9)0.87063 (7)0.15950 (7)0.0186 (2)
O40.17118 (8)0.76087 (7)0.09594 (7)0.0132 (2)
O50.12593 (8)0.59332 (7)0.10481 (7)0.0127 (2)
O60.09988 (8)0.54432 (7)0.00856 (7)0.0138 (2)
O70.56025 (8)0.64301 (7)0.00611 (7)0.0147 (2)
O80.40549 (8)0.64381 (7)0.10108 (7)0.01242 (19)
N10.18288 (9)0.65059 (8)0.24453 (8)0.0097 (2)
N20.31990 (9)0.59977 (8)0.01385 (8)0.0097 (2)
C10.26525 (11)0.50131 (9)0.29390 (9)0.0110 (3)
C20.19698 (11)0.58628 (9)0.31601 (9)0.0105 (3)
C30.15309 (11)0.60120 (10)0.39871 (9)0.0137 (3)
H30.1620280.5551330.4494410.016*
C40.09540 (12)0.68612 (11)0.40484 (10)0.0149 (3)
H40.0651980.6985970.4605040.018*
C50.08173 (11)0.75267 (10)0.33013 (10)0.0131 (3)
H50.0423780.8106440.3337980.016*
C60.12737 (11)0.73185 (9)0.24992 (9)0.0114 (3)
C70.11944 (11)0.79473 (9)0.16172 (10)0.0125 (3)
C80.15468 (11)0.57093 (9)0.03416 (9)0.0110 (3)
C90.26670 (11)0.57688 (9)0.02345 (9)0.0103 (2)
C100.31350 (11)0.56102 (10)0.10590 (9)0.0125 (3)
H100.2753680.5447100.1323550.015*
C110.41804 (12)0.56972 (10)0.14869 (9)0.0131 (3)
H110.4518590.5595320.2051900.016*
C120.47295 (11)0.59332 (9)0.10876 (9)0.0116 (3)
H120.5442720.5992150.1369960.014*
C130.42023 (11)0.60788 (9)0.02665 (9)0.0103 (2)
C140.46563 (11)0.63352 (9)0.02710 (9)0.0109 (3)
Ni20.25329 (2)0.12175 (2)0.11808 (2)0.00967 (4)
O90.10055 (8)0.14844 (7)0.09529 (7)0.0135 (2)
O100.05740 (8)0.25189 (7)0.09740 (7)0.0161 (2)
O110.39904 (8)0.23826 (7)0.20297 (7)0.0142 (2)
O120.37077 (8)0.14356 (7)0.15385 (7)0.01317 (19)
O130.32874 (8)0.16257 (7)0.01668 (7)0.0136 (2)
O140.43321 (10)0.10624 (8)0.13125 (7)0.0208 (2)
O150.21858 (8)0.11661 (7)0.29451 (7)0.0148 (2)
H150.157 (2)0.099 (2)0.355 (2)0.067 (9)*
O160.21067 (8)0.02623 (7)0.24196 (7)0.0134 (2)
N30.17856 (10)0.23468 (8)0.14631 (8)0.0102 (2)
N40.31764 (9)0.00931 (8)0.08610 (8)0.0103 (2)
C150.03645 (11)0.22107 (9)0.10764 (9)0.0114 (3)
C160.07836 (11)0.27440 (9)0.13732 (9)0.0104 (3)
C170.02435 (11)0.35565 (9)0.15362 (9)0.0122 (3)
H170.0471960.3833520.1481290.015*
C180.07831 (12)0.39569 (9)0.17840 (9)0.0125 (3)
H180.0433610.4515570.1898670.015*
C190.18360 (12)0.35391 (9)0.18640 (9)0.0130 (3)
H190.2215930.3809340.2021790.016*
C200.23069 (11)0.27167 (9)0.17053 (9)0.0106 (3)
C210.34265 (11)0.21374 (9)0.17667 (9)0.0112 (3)
C220.37979 (11)0.09982 (10)0.05469 (9)0.0135 (3)
C230.37138 (10)0.01018 (10)0.00321 (9)0.0115 (2)
C240.41561 (11)0.06645 (10)0.02480 (10)0.0138 (3)
H240.4550100.0657780.0837580.017*
C250.40030 (12)0.14390 (10)0.03622 (10)0.0158 (3)
H250.4287280.1970560.0187820.019*
C260.34346 (11)0.14421 (10)0.12291 (10)0.0140 (3)
H260.3328480.1968370.1651940.017*
C270.30298 (11)0.06485 (9)0.14518 (9)0.0112 (3)
C280.23924 (11)0.04943 (10)0.23381 (9)0.0115 (3)
Ni30.75403 (2)0.35799 (2)0.37533 (2)0.00989 (4)
O170.69383 (8)0.30932 (7)0.50907 (7)0.0146 (2)
O180.60244 (9)0.35062 (8)0.63310 (7)0.0211 (2)
O190.76962 (9)0.60229 (7)0.20894 (7)0.0155 (2)
H19A0.824 (2)0.593 (2)0.151 (2)0.070 (9)*
O200.78817 (8)0.45783 (7)0.25591 (7)0.0138 (2)
O210.63035 (8)0.33731 (7)0.34342 (7)0.0139 (2)
O220.60517 (8)0.24845 (7)0.28405 (7)0.0142 (2)
O231.07128 (8)0.22781 (7)0.37710 (7)0.0147 (2)
O240.91384 (8)0.33175 (7)0.38746 (7)0.01260 (19)
N50.68758 (9)0.46617 (8)0.41561 (8)0.0119 (2)
N60.82746 (9)0.24807 (8)0.34004 (8)0.0100 (2)
C290.64462 (11)0.36635 (10)0.55327 (10)0.0140 (3)
C300.63951 (11)0.45993 (10)0.50049 (9)0.0121 (3)
C310.59124 (11)0.53454 (10)0.53213 (10)0.0157 (3)
H310.5557810.5304540.5923100.019*
C320.59646 (12)0.61485 (11)0.47330 (11)0.0178 (3)
H320.5644680.6665830.4933210.021*
C330.64838 (12)0.62033 (10)0.38477 (10)0.0157 (3)
H330.6527130.6750150.3440570.019*
C340.69332 (11)0.54319 (10)0.35848 (9)0.0117 (3)
C350.75446 (11)0.53242 (10)0.26776 (10)0.0122 (3)
C360.65997 (11)0.27090 (9)0.31431 (9)0.0111 (3)
C370.77287 (11)0.21314 (9)0.31602 (9)0.0106 (3)
C380.81827 (12)0.13204 (10)0.29755 (9)0.0136 (3)
H380.7789320.1069740.2808730.016*
C390.92377 (12)0.08822 (10)0.30420 (10)0.0138 (3)
H390.9569690.0325590.2920000.017*
C400.98012 (11)0.12612 (9)0.32868 (9)0.0122 (3)
H401.0519130.0973280.3331020.015*
C410.92815 (11)0.20720 (9)0.34639 (9)0.0104 (3)
C420.97505 (11)0.25954 (9)0.37279 (9)0.0111 (3)
Ni41.25272 (2)0.13793 (2)0.60421 (2)0.01043 (4)
O251.28403 (8)0.02147 (7)0.70974 (7)0.0139 (2)
O261.26696 (9)0.01781 (7)0.85421 (7)0.0174 (2)
H26A1.3133 (18)0.0767 (16)0.8458 (16)0.037 (6)*
O271.10148 (9)0.39723 (7)0.58434 (8)0.0198 (2)
O281.19134 (8)0.26965 (7)0.55008 (7)0.0142 (2)
O291.12944 (8)0.10217 (7)0.58858 (7)0.0138 (2)
O301.10129 (8)0.03963 (7)0.50430 (7)0.0141 (2)
O311.57283 (8)0.12944 (8)0.47660 (7)0.0164 (2)
H31A1.606 (2)0.143 (2)0.527 (2)0.070 (9)*
O321.41149 (8)0.15281 (7)0.57461 (7)0.0147 (2)
N71.18741 (10)0.18360 (8)0.70928 (8)0.0117 (2)
N81.32572 (9)0.09660 (8)0.49787 (8)0.0104 (2)
C431.25302 (11)0.03833 (10)0.78164 (10)0.0130 (3)
C441.19363 (11)0.13056 (10)0.78774 (10)0.0131 (3)
C451.14907 (12)0.16077 (10)0.86258 (10)0.0156 (3)
H451.1548810.1226580.9181520.019*
C461.09540 (12)0.24905 (11)0.85350 (10)0.0170 (3)
H461.0625530.2716890.9036620.020*
C471.08970 (11)0.30433 (10)0.77106 (10)0.0152 (3)
H471.0535170.3646360.7641620.018*
C481.13858 (11)0.26858 (10)0.69915 (10)0.0125 (3)
C491.14269 (11)0.31791 (9)0.60439 (10)0.0132 (3)
C501.15749 (11)0.07093 (9)0.52331 (9)0.0113 (3)
C511.27044 (11)0.07139 (9)0.46459 (9)0.0107 (3)
C521.31630 (12)0.04892 (9)0.38525 (9)0.0127 (3)
H521.2760760.0323030.3609320.015*
C531.42291 (12)0.05139 (10)0.34223 (10)0.0144 (3)
H531.4565310.0356490.2882000.017*
C541.48032 (11)0.07697 (9)0.37851 (9)0.0124 (3)
H541.5531810.0785800.3501900.015*
C551.42790 (11)0.09989 (9)0.45689 (9)0.0108 (3)
C561.47300 (11)0.13035 (9)0.50675 (9)0.0129 (3)
O1W1.15570 (9)0.32166 (8)0.39989 (7)0.0152 (2)
H1A1.115 (2)0.3733 (19)0.3887 (17)0.045 (7)*
H1B1.164 (2)0.293 (2)0.467 (2)0.068 (9)*
H1C1.117 (2)0.272 (2)0.395 (2)0.076 (10)*
O2W0.39736 (9)0.29718 (7)0.33030 (7)0.0141 (2)
H2A0.3820 (14)0.2799 (13)0.2956 (13)0.015 (4)*
H2B0.466 (2)0.2857 (19)0.3175 (19)0.057 (8)*
H2C0.350 (2)0.3660 (19)0.3413 (18)0.055 (8)*
O3W0.12798 (9)0.83936 (8)0.05238 (8)0.0193 (2)
H3A0.074 (2)0.8926 (17)0.0533 (16)0.042 (7)*
H3B0.1414 (17)0.8080 (15)0.0035 (15)0.030 (6)*
H3C0.099 (2)0.802 (2)0.0644 (19)0.065 (9)*
O4W1.64368 (9)0.15762 (8)0.57453 (8)0.0193 (2)
H4A1.6664 (16)0.2034 (14)0.5534 (13)0.017 (5)*
H4B1.602 (2)0.1615 (18)0.625 (2)0.051 (8)*
O5W0.64397 (9)0.68318 (8)0.07545 (7)0.0160 (2)
H5A0.6502 (19)0.7300 (17)0.0633 (16)0.035 (6)*
H5B0.613 (2)0.6642 (17)0.1335 (18)0.040 (7)*
H5C0.606 (2)0.661 (2)0.036 (2)0.081 (10)*
O6W1.38147 (9)0.16849 (8)0.83977 (8)0.0168 (2)
H6A1.443 (2)0.1814 (17)0.8323 (17)0.038 (7)*
H6B1.3679 (18)0.1971 (18)0.8134 (17)0.042 (7)*
O7W0.11206 (9)0.09167 (8)0.43920 (7)0.0156 (2)
H7A0.0435 (19)0.0760 (15)0.4491 (15)0.030 (6)*
H7B0.1287 (19)0.0526 (17)0.4504 (16)0.034 (6)*
O8W0.88656 (9)0.58139 (8)0.06530 (8)0.0164 (2)
H8A0.956 (2)0.5699 (16)0.0580 (16)0.033 (6)*
H8B0.8742 (17)0.5511 (15)0.0474 (15)0.023 (6)*
O9W0.52805 (9)0.60206 (8)0.22051 (8)0.0204 (2)
H9A0.4910 (19)0.6111 (17)0.2703 (18)0.046 (7)*
H9B0.4819 (18)0.6090 (16)0.1937 (16)0.035 (6)*
O10W1.01615 (9)0.46431 (8)0.34976 (8)0.0193 (2)
H10A0.9843 (19)0.5053 (18)0.3686 (17)0.042 (7)*
H10B0.970 (2)0.4394 (19)0.3590 (18)0.053 (8)*
O11W0.03939 (10)0.03378 (8)0.05294 (8)0.0244 (2)
H11A0.039 (3)0.017 (2)0.083 (2)0.075 (10)*
H11B0.0670 (19)0.0591 (17)0.0749 (17)0.044 (7)*
O12W1.50472 (12)0.20790 (10)0.71034 (9)0.0309 (3)
H12A1.477 (3)0.182 (2)0.766 (2)0.087 (11)*
H12B1.540 (3)0.251 (2)0.707 (2)0.103 (13)*
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
Ni10.00980 (8)0.01074 (9)0.00775 (8)0.00310 (7)0.00144 (7)0.00368 (6)
O10.0132 (5)0.0128 (5)0.0107 (5)0.0032 (4)0.0014 (4)0.0045 (4)
O20.0181 (5)0.0112 (5)0.0128 (5)0.0033 (4)0.0054 (4)0.0018 (4)
O30.0208 (5)0.0126 (5)0.0208 (6)0.0011 (4)0.0073 (4)0.0037 (4)
O40.0154 (5)0.0137 (5)0.0108 (5)0.0039 (4)0.0043 (4)0.0023 (4)
O50.0112 (5)0.0163 (5)0.0120 (5)0.0048 (4)0.0008 (4)0.0064 (4)
O60.0138 (5)0.0165 (5)0.0146 (5)0.0062 (4)0.0043 (4)0.0050 (4)
O70.0127 (5)0.0195 (5)0.0140 (5)0.0076 (4)0.0023 (4)0.0044 (4)
O80.0127 (5)0.0154 (5)0.0116 (5)0.0050 (4)0.0029 (4)0.0052 (4)
N10.0089 (5)0.0108 (6)0.0110 (6)0.0030 (4)0.0017 (4)0.0050 (4)
N20.0109 (5)0.0103 (5)0.0082 (5)0.0033 (4)0.0020 (4)0.0026 (4)
C10.0089 (6)0.0118 (6)0.0141 (6)0.0035 (5)0.0026 (5)0.0050 (5)
C20.0103 (6)0.0129 (6)0.0100 (6)0.0043 (5)0.0025 (5)0.0037 (5)
C30.0137 (6)0.0184 (7)0.0101 (6)0.0052 (5)0.0024 (5)0.0046 (5)
C40.0139 (6)0.0211 (8)0.0123 (7)0.0052 (6)0.0010 (5)0.0091 (6)
C50.0107 (6)0.0143 (7)0.0164 (7)0.0023 (5)0.0023 (5)0.0086 (5)
C60.0106 (6)0.0129 (7)0.0127 (6)0.0048 (5)0.0037 (5)0.0033 (5)
C70.0115 (6)0.0132 (7)0.0143 (6)0.0042 (5)0.0042 (5)0.0036 (5)
C80.0111 (6)0.0102 (6)0.0115 (6)0.0031 (5)0.0032 (5)0.0020 (5)
C90.0112 (6)0.0090 (6)0.0106 (6)0.0032 (5)0.0025 (5)0.0022 (5)
C100.0149 (7)0.0140 (7)0.0105 (6)0.0050 (5)0.0039 (5)0.0037 (5)
C110.0165 (7)0.0125 (7)0.0093 (6)0.0037 (5)0.0016 (5)0.0035 (5)
C120.0117 (6)0.0107 (6)0.0096 (6)0.0030 (5)0.0008 (5)0.0013 (5)
C130.0111 (6)0.0091 (6)0.0105 (6)0.0027 (5)0.0033 (5)0.0017 (5)
C140.0116 (6)0.0099 (6)0.0109 (6)0.0031 (5)0.0038 (5)0.0013 (5)
Ni20.01035 (8)0.00905 (9)0.01057 (10)0.00238 (7)0.00243 (7)0.00412 (7)
O90.0130 (5)0.0133 (5)0.0171 (5)0.0030 (4)0.0053 (4)0.0065 (4)
O100.0136 (5)0.0171 (5)0.0203 (5)0.0034 (4)0.0080 (4)0.0051 (4)
O110.0130 (5)0.0172 (5)0.0160 (5)0.0050 (4)0.0051 (4)0.0061 (4)
O120.0118 (4)0.0143 (5)0.0150 (5)0.0018 (4)0.0041 (4)0.0067 (4)
O130.0162 (5)0.0125 (5)0.0123 (5)0.0058 (4)0.0027 (4)0.0025 (4)
O140.0274 (6)0.0223 (6)0.0112 (5)0.0114 (5)0.0013 (4)0.0039 (4)
O150.0172 (5)0.0140 (5)0.0121 (5)0.0066 (4)0.0010 (4)0.0024 (4)
O160.0148 (5)0.0127 (5)0.0125 (5)0.0033 (4)0.0017 (4)0.0051 (4)
N30.0112 (5)0.0100 (6)0.0094 (5)0.0034 (4)0.0026 (4)0.0022 (4)
N40.0095 (5)0.0115 (6)0.0111 (5)0.0032 (4)0.0018 (4)0.0048 (4)
C150.0147 (6)0.0124 (6)0.0080 (6)0.0060 (5)0.0025 (5)0.0016 (5)
C160.0109 (6)0.0113 (6)0.0079 (6)0.0032 (5)0.0021 (5)0.0013 (5)
C170.0128 (6)0.0131 (7)0.0099 (6)0.0036 (5)0.0026 (5)0.0021 (5)
C180.0164 (7)0.0091 (6)0.0101 (6)0.0020 (5)0.0020 (5)0.0030 (5)
C190.0176 (7)0.0131 (7)0.0107 (6)0.0065 (5)0.0043 (5)0.0028 (5)
C200.0116 (6)0.0109 (6)0.0085 (6)0.0041 (5)0.0016 (5)0.0016 (5)
C210.0113 (6)0.0122 (6)0.0087 (6)0.0042 (5)0.0011 (5)0.0013 (5)
C220.0141 (6)0.0168 (7)0.0120 (6)0.0068 (5)0.0041 (5)0.0033 (5)
C230.0098 (5)0.0162 (7)0.0104 (6)0.0049 (5)0.0017 (5)0.0051 (5)
C240.0119 (6)0.0181 (7)0.0135 (6)0.0034 (5)0.0017 (5)0.0087 (6)
C250.0144 (6)0.0148 (7)0.0209 (8)0.0018 (5)0.0036 (6)0.0108 (6)
C260.0133 (6)0.0123 (7)0.0170 (7)0.0036 (5)0.0033 (5)0.0050 (5)
C270.0086 (6)0.0142 (7)0.0121 (6)0.0036 (5)0.0025 (5)0.0045 (5)
C280.0092 (6)0.0143 (7)0.0123 (6)0.0026 (5)0.0038 (5)0.0044 (5)
Ni30.00954 (8)0.01104 (9)0.01006 (9)0.00251 (7)0.00174 (7)0.00488 (7)
O170.0159 (5)0.0160 (5)0.0124 (5)0.0064 (4)0.0002 (4)0.0057 (4)
O180.0250 (6)0.0264 (6)0.0125 (5)0.0116 (5)0.0015 (4)0.0074 (4)
O190.0168 (5)0.0151 (5)0.0148 (5)0.0053 (4)0.0035 (4)0.0035 (4)
O200.0147 (5)0.0144 (5)0.0126 (5)0.0034 (4)0.0025 (4)0.0051 (4)
O210.0112 (4)0.0158 (5)0.0158 (5)0.0018 (4)0.0040 (4)0.0067 (4)
O220.0120 (4)0.0175 (5)0.0165 (5)0.0050 (4)0.0050 (4)0.0060 (4)
O230.0119 (5)0.0147 (5)0.0195 (5)0.0038 (4)0.0069 (4)0.0036 (4)
O240.0121 (4)0.0148 (5)0.0133 (5)0.0038 (4)0.0036 (4)0.0059 (4)
N50.0095 (5)0.0157 (6)0.0132 (6)0.0038 (4)0.0028 (4)0.0063 (5)
N60.0110 (5)0.0101 (6)0.0079 (5)0.0034 (4)0.0011 (4)0.0017 (4)
C290.0113 (6)0.0190 (7)0.0144 (7)0.0060 (5)0.0019 (5)0.0069 (5)
C300.0090 (6)0.0173 (7)0.0131 (6)0.0036 (5)0.0026 (5)0.0075 (5)
C310.0117 (6)0.0218 (8)0.0177 (7)0.0023 (6)0.0034 (5)0.0123 (6)
C320.0152 (7)0.0188 (8)0.0231 (8)0.0006 (6)0.0053 (6)0.0136 (6)
C330.0154 (6)0.0139 (7)0.0194 (7)0.0023 (5)0.0067 (6)0.0057 (5)
C340.0093 (6)0.0144 (7)0.0137 (6)0.0029 (5)0.0039 (5)0.0058 (5)
C350.0094 (6)0.0154 (7)0.0146 (7)0.0035 (5)0.0049 (5)0.0050 (5)
C360.0110 (6)0.0136 (6)0.0089 (6)0.0049 (5)0.0020 (5)0.0021 (5)
C370.0102 (6)0.0134 (6)0.0084 (6)0.0045 (5)0.0013 (5)0.0025 (5)
C380.0159 (7)0.0126 (7)0.0140 (7)0.0051 (5)0.0041 (5)0.0041 (5)
C390.0159 (7)0.0102 (7)0.0144 (7)0.0033 (5)0.0026 (5)0.0034 (5)
C400.0106 (6)0.0119 (6)0.0116 (6)0.0024 (5)0.0016 (5)0.0018 (5)
C410.0099 (6)0.0129 (6)0.0088 (6)0.0047 (5)0.0022 (5)0.0019 (5)
C420.0127 (6)0.0134 (6)0.0075 (6)0.0056 (5)0.0019 (5)0.0015 (5)
Ni40.00982 (8)0.01123 (9)0.01129 (8)0.00219 (7)0.00173 (7)0.00573 (6)
O250.0140 (5)0.0132 (5)0.0141 (5)0.0017 (4)0.0025 (4)0.0063 (4)
O260.0214 (5)0.0154 (5)0.0144 (5)0.0022 (4)0.0059 (4)0.0039 (4)
O270.0217 (5)0.0132 (5)0.0242 (6)0.0002 (4)0.0072 (4)0.0078 (4)
O280.0157 (5)0.0130 (5)0.0148 (5)0.0014 (4)0.0049 (4)0.0064 (4)
O290.0110 (5)0.0168 (5)0.0158 (5)0.0040 (4)0.0011 (4)0.0086 (4)
O300.0129 (5)0.0174 (5)0.0148 (5)0.0062 (4)0.0030 (4)0.0057 (4)
O310.0128 (5)0.0218 (6)0.0156 (5)0.0082 (4)0.0037 (4)0.0022 (4)
O320.0127 (5)0.0169 (5)0.0164 (5)0.0041 (4)0.0035 (4)0.0067 (4)
N70.0094 (5)0.0145 (6)0.0134 (6)0.0039 (4)0.0027 (4)0.0057 (5)
N80.0092 (5)0.0107 (6)0.0107 (5)0.0021 (4)0.0022 (4)0.0031 (4)
C430.0100 (6)0.0151 (7)0.0155 (7)0.0047 (5)0.0025 (5)0.0050 (5)
C440.0110 (6)0.0133 (7)0.0170 (7)0.0031 (5)0.0034 (5)0.0066 (5)
C450.0159 (7)0.0188 (7)0.0140 (7)0.0057 (6)0.0022 (5)0.0071 (6)
C460.0155 (6)0.0211 (8)0.0168 (7)0.0042 (6)0.0011 (6)0.0117 (6)
C470.0125 (6)0.0174 (7)0.0196 (7)0.0044 (5)0.0026 (5)0.0108 (6)
C480.0098 (6)0.0140 (7)0.0172 (7)0.0034 (5)0.0041 (5)0.0071 (5)
C490.0113 (6)0.0130 (7)0.0180 (7)0.0026 (5)0.0055 (5)0.0059 (5)
C500.0096 (6)0.0105 (6)0.0126 (6)0.0018 (5)0.0023 (5)0.0030 (5)
C510.0107 (6)0.0097 (6)0.0111 (6)0.0023 (5)0.0023 (5)0.0030 (5)
C520.0146 (6)0.0130 (7)0.0108 (6)0.0033 (5)0.0042 (5)0.0028 (5)
C530.0168 (7)0.0144 (7)0.0094 (6)0.0025 (5)0.0015 (5)0.0035 (5)
C540.0103 (6)0.0113 (6)0.0109 (6)0.0020 (5)0.0005 (5)0.0002 (5)
C550.0101 (6)0.0093 (6)0.0118 (6)0.0027 (5)0.0030 (5)0.0008 (5)
C560.0121 (6)0.0110 (6)0.0145 (7)0.0038 (5)0.0043 (5)0.0001 (5)
O1W0.0151 (5)0.0160 (5)0.0171 (5)0.0050 (4)0.0062 (4)0.0042 (4)
O2W0.0115 (5)0.0141 (5)0.0183 (5)0.0014 (4)0.0053 (4)0.0065 (4)
O3W0.0225 (6)0.0212 (6)0.0180 (5)0.0101 (5)0.0100 (4)0.0002 (4)
O4W0.0193 (5)0.0210 (6)0.0192 (6)0.0092 (5)0.0077 (5)0.0002 (5)
O5W0.0187 (5)0.0161 (6)0.0153 (5)0.0080 (4)0.0063 (4)0.0008 (4)
O6W0.0129 (5)0.0178 (6)0.0215 (6)0.0006 (4)0.0057 (4)0.0094 (4)
O7W0.0122 (5)0.0206 (6)0.0144 (5)0.0060 (4)0.0001 (4)0.0068 (4)
O8W0.0131 (5)0.0206 (6)0.0178 (5)0.0063 (4)0.0016 (4)0.0079 (4)
O9W0.0181 (5)0.0318 (7)0.0149 (5)0.0085 (5)0.0015 (4)0.0111 (5)
O10W0.0214 (6)0.0165 (6)0.0217 (6)0.0048 (5)0.0047 (4)0.0081 (4)
O11W0.0339 (6)0.0161 (6)0.0292 (6)0.0081 (5)0.0182 (5)0.0010 (5)
O12W0.0404 (8)0.0301 (7)0.0207 (6)0.0179 (6)0.0044 (6)0.0005 (5)
Geometric parameters (Å, º) top
Ni1—N21.9652 (12)N5—C341.3359 (19)
Ni1—N11.9732 (12)N6—C371.3298 (18)
Ni1—O52.1076 (11)N6—C411.3340 (18)
Ni1—O42.1312 (11)C29—C301.515 (2)
Ni1—O12.1504 (11)C30—C311.3947 (19)
Ni1—O82.1782 (10)C31—C321.387 (2)
O1—C11.2500 (17)C31—H310.9500
O2—C11.2714 (18)C32—C331.398 (2)
O2—H2C1.27 (3)C32—H320.9500
O3—C71.2316 (18)C33—C341.386 (2)
O4—C71.2908 (17)C33—H330.9500
O5—C81.2654 (17)C34—C351.5058 (19)
O6—C81.2486 (17)C36—C371.5173 (19)
O7—C141.2641 (17)C37—C381.387 (2)
O7—H5C1.27 (3)C38—C391.400 (2)
O8—C141.2636 (17)C38—H380.9500
N1—C61.3333 (18)C39—C401.393 (2)
N1—C21.3374 (18)C39—H390.9500
N2—C91.3320 (18)C40—C411.3870 (19)
N2—C131.3368 (18)C40—H400.9500
C1—C21.5029 (19)C41—C421.5085 (19)
C2—C31.3873 (19)Ni4—N81.9572 (12)
C3—C41.395 (2)Ni4—N71.9732 (12)
C3—H30.9500Ni4—O282.0789 (11)
C4—C51.390 (2)Ni4—O292.1087 (11)
C4—H40.9500Ni4—O322.1433 (10)
C5—C61.390 (2)Ni4—O252.1822 (11)
C5—H50.9500O25—C431.2367 (18)
C6—C71.517 (2)O26—C431.2944 (18)
C8—C91.5190 (19)O26—H26A1.00 (2)
C9—C101.3905 (19)O27—C491.2333 (18)
C10—C111.395 (2)O28—C491.2873 (17)
C10—H100.9500O28—H1B1.47 (3)
C11—C121.393 (2)O29—C501.2671 (17)
C11—H110.9500O30—C501.2486 (17)
C12—C131.3833 (19)O31—C561.2789 (17)
C12—H120.9500O31—H31A1.20 (3)
C13—C141.5050 (19)O32—C561.2512 (18)
Ni2—N31.9579 (12)N7—C441.3322 (19)
Ni2—N41.9698 (12)N7—C481.3328 (19)
Ni2—O122.0891 (10)N8—C511.3302 (18)
Ni2—O132.1193 (10)N8—C551.3390 (18)
Ni2—O92.1286 (10)C43—C441.505 (2)
Ni2—O162.1909 (11)C44—C451.385 (2)
O9—C151.2701 (17)C45—C461.394 (2)
O10—C151.2581 (18)C45—H450.9500
O11—C211.2512 (17)C46—C471.395 (2)
O12—C211.2634 (17)C46—H460.9500
O13—C221.2887 (18)C47—C481.393 (2)
O14—C221.2304 (18)C47—H470.9500
O15—C281.2807 (18)C48—C491.520 (2)
O15—H151.13 (3)C50—C511.5187 (19)
O16—C281.2414 (18)C51—C521.3887 (19)
N3—C201.3308 (18)C52—C531.394 (2)
N3—C161.3386 (18)C52—H520.9500
N4—C231.3313 (18)C53—C541.396 (2)
N4—C271.3346 (19)C53—H530.9500
C15—C161.5099 (19)C54—C551.3820 (19)
C16—C171.3835 (19)C54—H540.9500
C17—C181.397 (2)C55—C561.501 (2)
C17—H170.9500O1W—H1A0.85 (3)
C18—C191.399 (2)O1W—H1B1.10 (3)
C18—H180.9500O1W—H1C1.18 (3)
C19—C201.3883 (19)O2W—H2A0.852 (19)
C19—H190.9500O2W—H2B0.85 (3)
C20—C211.5210 (19)O2W—H2C1.16 (3)
C22—C231.512 (2)O3W—H3A0.94 (3)
C23—C241.3928 (19)O3W—H3B0.96 (2)
C24—C251.390 (2)O3W—H3C0.96 (3)
C24—H240.9500O4W—H31A1.23 (3)
C25—C261.396 (2)O4W—H4A0.85 (2)
C25—H250.9500O4W—H4B0.85 (3)
C26—C271.3889 (19)O5W—H5A0.77 (3)
C26—H260.9500O5W—H5B0.91 (3)
C27—C281.5044 (19)O5W—H5C1.19 (3)
Ni3—N61.9625 (12)O6W—H6A0.76 (2)
Ni3—N51.9728 (12)O6W—H6B0.86 (2)
Ni3—O172.0849 (11)O7W—H151.37 (3)
Ni3—O212.1193 (10)O7W—H7A0.85 (2)
Ni3—O242.1494 (10)O7W—H7B0.87 (2)
Ni3—O202.1632 (11)O8W—H19A1.44 (3)
O17—C291.2762 (18)O8W—H8A0.88 (2)
O18—C291.2396 (18)O8W—H8B0.77 (2)
O19—C351.2820 (18)O9W—H9A0.85 (3)
O19—H19A1.03 (3)O9W—H9B0.86 (2)
O20—C351.2427 (18)O10W—H10A0.78 (3)
O21—C361.2604 (17)O10W—H10B0.82 (3)
O22—C361.2567 (17)O11W—H11A0.83 (4)
O23—C421.2568 (18)O11W—H11B0.89 (2)
O23—H1C1.29 (3)O12W—H12A0.90 (4)
O24—C421.2644 (17)O12W—H12B0.99 (4)
N5—C301.3350 (18)
N2—Ni1—N1175.96 (5)C29—O17—Ni3115.70 (10)
N2—Ni1—O578.59 (5)C35—O19—H19A115.3 (18)
N1—Ni1—O5105.44 (4)C35—O20—Ni3112.78 (9)
N2—Ni1—O4102.50 (5)C36—O21—Ni3113.77 (9)
N1—Ni1—O477.74 (5)C42—O23—H1C119.6 (14)
O5—Ni1—O492.16 (4)C42—O24—Ni3113.39 (9)
N2—Ni1—O1101.91 (5)C30—N5—C34121.61 (13)
N1—Ni1—O177.80 (5)C30—N5—Ni3118.53 (10)
O5—Ni1—O194.30 (4)C34—N5—Ni3119.84 (10)
O4—Ni1—O1155.54 (4)C37—N6—C41121.51 (12)
N2—Ni1—O877.20 (4)C37—N6—Ni3118.95 (10)
N1—Ni1—O898.77 (4)C41—N6—Ni3119.38 (10)
O5—Ni1—O8155.78 (4)O18—C29—O17125.43 (15)
O4—Ni1—O893.56 (4)O18—C29—C30119.72 (13)
O1—Ni1—O890.16 (4)O17—C29—C30114.85 (13)
C1—O1—Ni1112.98 (9)N5—C30—C31120.67 (14)
C1—O2—H2C117.9 (13)N5—C30—C29112.56 (12)
C7—O4—Ni1114.92 (9)C31—C30—C29126.76 (13)
C8—O5—Ni1114.26 (9)C32—C31—C30118.15 (14)
C14—O7—H5C120.7 (14)C32—C31—H31120.9
C14—O8—Ni1113.14 (9)C30—C31—H31120.9
C6—N1—C2121.25 (12)C31—C32—C33120.57 (14)
C6—N1—Ni1119.59 (10)C31—C32—H32119.7
C2—N1—Ni1119.15 (10)C33—C32—H32119.7
C9—N2—C13121.06 (12)C34—C33—C32117.68 (14)
C9—N2—Ni1118.72 (9)C34—C33—H33121.2
C13—N2—Ni1120.21 (10)C32—C33—H33121.2
O1—C1—O2126.12 (13)N5—C34—C33121.30 (13)
O1—C1—C2117.95 (13)N5—C34—C35111.33 (12)
O2—C1—C2115.92 (12)C33—C34—C35127.37 (14)
N1—C2—C3121.33 (13)O20—C35—O19125.29 (14)
N1—C2—C1111.91 (12)O20—C35—C34118.58 (13)
C3—C2—C1126.75 (13)O19—C35—C34116.11 (13)
C2—C3—C4117.74 (14)O22—C36—O21126.25 (13)
C2—C3—H3121.1O22—C36—C37117.36 (12)
C4—C3—H3121.1O21—C36—C37116.39 (12)
C5—C4—C3120.51 (13)N6—C37—C38121.09 (13)
C5—C4—H4119.7N6—C37—C36112.09 (12)
C3—C4—H4119.7C38—C37—C36126.80 (13)
C6—C5—C4118.01 (13)C37—C38—C39118.05 (13)
C6—C5—H5121.0C37—C38—H38121.0
C4—C5—H5121.0C39—C38—H38121.0
N1—C6—C5121.14 (13)C40—C39—C38120.10 (13)
N1—C6—C7113.06 (12)C40—C39—H39120.0
C5—C6—C7125.78 (13)C38—C39—H39120.0
O3—C7—O4126.89 (14)C41—C40—C39117.92 (13)
O3—C7—C6118.49 (13)C41—C40—H40121.0
O4—C7—C6114.61 (12)C39—C40—H40121.0
O6—C8—O5125.96 (13)N6—C41—C40121.32 (13)
O6—C8—C9118.01 (12)N6—C41—C42112.44 (12)
O5—C8—C9116.02 (12)C40—C41—C42126.23 (13)
N2—C9—C10121.11 (13)O23—C42—O24126.32 (13)
N2—C9—C8112.25 (12)O23—C42—C41117.04 (13)
C10—C9—C8126.65 (12)O24—C42—C41116.63 (12)
C9—C10—C11118.13 (13)N8—Ni4—N7175.93 (5)
C9—C10—H10120.9N8—Ni4—O28100.13 (5)
C11—C10—H10120.9N7—Ni4—O2878.71 (5)
C12—C11—C10120.17 (13)N8—Ni4—O2978.45 (5)
C12—C11—H11119.9N7—Ni4—O29105.45 (5)
C10—C11—H11119.9O28—Ni4—O2992.83 (4)
C13—C12—C11117.84 (13)N8—Ni4—O3278.11 (5)
C13—C12—H12121.1N7—Ni4—O3298.01 (4)
C11—C12—H12121.1O28—Ni4—O3292.59 (4)
N2—C13—C12121.70 (13)O29—Ni4—O32156.52 (4)
N2—C13—C14112.42 (12)N8—Ni4—O25104.23 (5)
C12—C13—C14125.88 (12)N7—Ni4—O2576.94 (5)
O8—C14—O7126.11 (13)O28—Ni4—O25155.63 (4)
O8—C14—C13116.97 (12)O29—Ni4—O2592.77 (4)
O7—C14—C13116.93 (12)O32—Ni4—O2591.65 (4)
N3—Ni2—N4174.99 (5)C43—O25—Ni4112.36 (9)
N3—Ni2—O1278.65 (5)C43—O26—H26A112.8 (14)
N4—Ni2—O12106.32 (4)C49—O28—Ni4115.84 (10)
N3—Ni2—O13100.77 (5)C49—O28—H1B121.2 (12)
N4—Ni2—O1378.72 (5)Ni4—O28—H1B117.5 (12)
O12—Ni2—O1391.92 (4)C50—O29—Ni4114.20 (9)
N3—Ni2—O978.08 (4)C56—O31—H31A111.8 (14)
N4—Ni2—O996.95 (4)C56—O32—Ni4112.73 (9)
O12—Ni2—O9156.72 (4)C44—N7—C48121.40 (13)
O13—Ni2—O992.92 (4)C44—N7—Ni4120.41 (10)
N3—Ni2—O16103.97 (5)C48—N7—Ni4118.18 (10)
N4—Ni2—O1676.58 (5)C51—N8—C55121.30 (12)
O12—Ni2—O1693.39 (4)C51—N8—Ni4119.18 (9)
O13—Ni2—O16155.25 (4)C55—N8—Ni4119.35 (10)
O9—Ni2—O1691.68 (4)O25—C43—O26125.10 (14)
C15—O9—Ni2114.13 (9)O25—C43—C44119.01 (13)
C21—O12—Ni2114.83 (9)O26—C43—C44115.89 (13)
C22—O13—Ni2114.33 (9)N7—C44—C45121.74 (14)
C28—O15—H15112.4 (16)N7—C44—C43111.12 (13)
C28—O16—Ni2112.90 (9)C45—C44—C43127.14 (14)
C20—N3—C16121.65 (12)C44—C45—C46117.66 (14)
C20—N3—Ni2118.88 (10)C44—C45—H45121.2
C16—N3—Ni2119.41 (10)C46—C45—H45121.2
C23—N4—C27121.23 (12)C45—C46—C47120.29 (14)
C23—N4—Ni2118.06 (10)C45—C46—H46119.9
C27—N4—Ni2120.63 (10)C47—C46—H46119.9
O10—C15—O9126.10 (13)C48—C47—C46118.12 (14)
O10—C15—C16117.88 (13)C48—C47—H47120.9
O9—C15—C16116.03 (12)C46—C47—H47120.9
N3—C16—C17121.14 (13)N7—C48—C47120.76 (14)
N3—C16—C15112.32 (12)N7—C48—C49113.16 (12)
C17—C16—C15126.54 (13)C47—C48—C49126.08 (13)
C16—C17—C18117.92 (13)O27—C49—O28124.99 (14)
C16—C17—H17121.0O27—C49—C48120.90 (13)
C18—C17—H17121.0O28—C49—C48114.11 (12)
C17—C18—C19120.34 (13)O30—C50—O29125.87 (13)
C17—C18—H18119.8O30—C50—C51118.23 (12)
C19—C18—H18119.8O29—C50—C51115.90 (12)
C20—C19—C18117.79 (13)N8—C51—C52121.03 (13)
C20—C19—H19121.1N8—C51—C50111.90 (12)
C18—C19—H19121.1C52—C51—C50127.08 (13)
N3—C20—C19121.15 (13)C51—C52—C53118.25 (13)
N3—C20—C21111.84 (12)C51—C52—H52120.9
C19—C20—C21127.01 (13)C53—C52—H52120.9
O11—C21—O12125.39 (13)C52—C53—C54120.03 (13)
O11—C21—C20118.92 (12)C52—C53—H53120.0
O12—C21—C20115.69 (12)C54—C53—H53120.0
O14—C22—O13126.70 (14)C55—C54—C53117.97 (13)
O14—C22—C23118.61 (13)C55—C54—H54121.0
O13—C22—C23114.69 (12)C53—C54—H54121.0
N4—C23—C24121.22 (14)N8—C55—C54121.39 (13)
N4—C23—C22114.10 (12)N8—C55—C56111.55 (12)
C24—C23—C22124.67 (13)C54—C55—C56127.06 (13)
C25—C24—C23117.91 (13)O32—C56—O31125.36 (14)
C25—C24—H24121.0O32—C56—C55118.11 (12)
C23—C24—H24121.0O31—C56—C55116.51 (13)
C24—C25—C26120.51 (13)H1A—O1W—H1B117 (2)
C24—C25—H25119.7H1A—O1W—H1C110 (2)
C26—C25—H25119.7H1B—O1W—H1C100 (2)
C27—C26—C25117.65 (14)H2A—O2W—H2B107 (2)
C27—C26—H26121.2H2A—O2W—H2C118.3 (18)
C25—C26—H26121.2H2B—O2W—H2C116 (2)
N4—C27—C26121.47 (13)H3A—O3W—H3B115.1 (19)
N4—C27—C28111.60 (12)H3A—O3W—H3C106 (2)
C26—C27—C28126.93 (13)H3B—O3W—H3C103 (2)
O16—C28—O15125.72 (13)H31A—O4W—H4A115 (2)
O16—C28—C27118.07 (13)H31A—O4W—H4B116 (2)
O15—C28—C27116.20 (13)H4A—O4W—H4B105 (2)
N6—Ni3—N5175.97 (5)H5A—O5W—H5B112 (2)
N6—Ni3—O1799.97 (5)H5A—O5W—H5C123 (2)
N5—Ni3—O1778.36 (5)H5B—O5W—H5C107 (2)
N6—Ni3—O2178.43 (4)H6A—O6W—H6B107 (2)
N5—Ni3—O21105.25 (4)H15—O7W—H7A109.3 (19)
O17—Ni3—O2193.27 (4)H15—O7W—H7B114 (2)
N6—Ni3—O2477.82 (4)H7A—O7W—H7B106 (2)
N5—Ni3—O2498.54 (4)H19A—O8W—H8A113.0 (19)
O17—Ni3—O2492.63 (4)H19A—O8W—H8B118 (2)
O21—Ni3—O24156.18 (4)H8A—O8W—H8B111 (2)
N6—Ni3—O20104.14 (4)H9A—O9W—H9B105 (2)
N5—Ni3—O2077.42 (5)H10A—O10W—H10B104 (2)
O17—Ni3—O20155.76 (4)H11A—O11W—H11B111 (3)
O21—Ni3—O2093.95 (4)H12A—O12W—H12B111 (3)
O24—Ni3—O2090.03 (4)
Ni1—O1—C1—O2173.90 (11)Ni3—O17—C29—O18179.31 (12)
Ni1—O1—C1—C25.19 (15)Ni3—O17—C29—C300.54 (15)
C6—N1—C2—C31.0 (2)C34—N5—C30—C311.4 (2)
Ni1—N1—C2—C3179.58 (10)Ni3—N5—C30—C31179.90 (10)
C6—N1—C2—C1177.94 (12)C34—N5—C30—C29178.78 (12)
Ni1—N1—C2—C11.50 (15)Ni3—N5—C30—C290.12 (15)
O1—C1—C2—N14.64 (18)O18—C29—C30—N5179.42 (13)
O2—C1—C2—N1174.55 (12)O17—C29—C30—N50.45 (18)
O1—C1—C2—C3176.52 (13)O18—C29—C30—C310.4 (2)
O2—C1—C2—C34.3 (2)O17—C29—C30—C31179.79 (13)
N1—C2—C3—C41.3 (2)N5—C30—C31—C321.2 (2)
C1—C2—C3—C4177.47 (13)C29—C30—C31—C32179.06 (13)
C2—C3—C4—C50.9 (2)C30—C31—C32—C330.3 (2)
C3—C4—C5—C60.2 (2)C31—C32—C33—C340.4 (2)
C2—N1—C6—C50.2 (2)C30—N5—C34—C330.7 (2)
Ni1—N1—C6—C5179.67 (10)Ni3—N5—C34—C33179.39 (10)
C2—N1—C6—C7179.25 (12)C30—N5—C34—C35178.13 (12)
Ni1—N1—C6—C71.31 (16)Ni3—N5—C34—C350.51 (16)
C4—C5—C6—N10.2 (2)C32—C33—C34—N50.2 (2)
C4—C5—C6—C7178.72 (13)C32—C33—C34—C35178.84 (13)
Ni1—O4—C7—O3176.11 (12)Ni3—O20—C35—O19175.72 (11)
Ni1—O4—C7—C63.11 (15)Ni3—O20—C35—C342.42 (15)
N1—C6—C7—O3176.34 (12)N5—C34—C35—O202.05 (18)
C5—C6—C7—O32.6 (2)C33—C34—C35—O20179.16 (14)
N1—C6—C7—O42.96 (17)N5—C34—C35—O19176.26 (12)
C5—C6—C7—O4178.08 (13)C33—C34—C35—O192.5 (2)
Ni1—O5—C8—O6175.14 (12)Ni3—O21—C36—O22173.69 (11)
Ni1—O5—C8—C94.40 (16)Ni3—O21—C36—C376.12 (15)
C13—N2—C9—C100.3 (2)C41—N6—C37—C380.8 (2)
Ni1—N2—C9—C10178.21 (11)Ni3—N6—C37—C38174.57 (11)
C13—N2—C9—C8179.57 (12)C41—N6—C37—C36179.43 (12)
Ni1—N2—C9—C81.93 (16)Ni3—N6—C37—C364.09 (15)
O6—C8—C9—N2175.31 (13)O22—C36—C37—N6172.99 (12)
O5—C8—C9—N24.27 (18)O21—C36—C37—N66.84 (18)
O6—C8—C9—C104.5 (2)O22—C36—C37—C388.4 (2)
O5—C8—C9—C10175.88 (14)O21—C36—C37—C38171.73 (14)
N2—C9—C10—C110.0 (2)N6—C37—C38—C390.5 (2)
C8—C9—C10—C11179.82 (13)C36—C37—C38—C39178.99 (13)
C9—C10—C11—C120.3 (2)C37—C38—C39—C400.1 (2)
C10—C11—C12—C130.3 (2)C38—C39—C40—C410.4 (2)
C9—N2—C13—C120.3 (2)C37—N6—C41—C400.4 (2)
Ni1—N2—C13—C12178.21 (10)Ni3—N6—C41—C40174.93 (10)
C9—N2—C13—C14179.56 (12)C37—N6—C41—C42178.81 (12)
Ni1—N2—C13—C141.96 (16)Ni3—N6—C41—C425.86 (15)
C11—C12—C13—N20.0 (2)C39—C40—C41—N60.2 (2)
C11—C12—C13—C14179.83 (13)C39—C40—C41—C42179.29 (13)
Ni1—O8—C14—O7178.10 (12)Ni3—O24—C42—O23178.53 (12)
Ni1—O8—C14—C131.68 (15)Ni3—O24—C42—C412.35 (15)
N2—C13—C14—O80.01 (18)N6—C41—C42—O23177.26 (12)
C12—C13—C14—O8179.81 (13)C40—C41—C42—O231.9 (2)
N2—C13—C14—O7179.79 (12)N6—C41—C42—O241.94 (18)
C12—C13—C14—O70.4 (2)C40—C41—C42—O24178.90 (13)
Ni2—O9—C15—O10179.01 (12)Ni4—O25—C43—O26176.02 (11)
Ni2—O9—C15—C160.96 (15)Ni4—O25—C43—C444.34 (15)
C20—N3—C16—C170.5 (2)C48—N7—C44—C450.5 (2)
Ni2—N3—C16—C17177.67 (10)Ni4—N7—C44—C45179.68 (11)
C20—N3—C16—C15178.85 (12)C48—N7—C44—C43179.64 (12)
Ni2—N3—C16—C151.70 (15)Ni4—N7—C44—C430.51 (16)
O10—C15—C16—N3179.65 (12)O25—C43—C44—N72.83 (19)
O9—C15—C16—N30.38 (18)O26—C43—C44—N7177.50 (12)
O10—C15—C16—C171.0 (2)O25—C43—C44—C45176.97 (14)
O9—C15—C16—C17178.96 (13)O26—C43—C44—C452.7 (2)
N3—C16—C17—C181.0 (2)N7—C44—C45—C461.0 (2)
C15—C16—C17—C18178.25 (13)C43—C44—C45—C46178.77 (13)
C16—C17—C18—C190.2 (2)C44—C45—C46—C471.3 (2)
C17—C18—C19—C201.1 (2)C45—C46—C47—C480.2 (2)
C16—N3—C20—C190.9 (2)C44—N7—C48—C471.8 (2)
Ni2—N3—C20—C19176.28 (10)Ni4—N7—C48—C47179.10 (10)
C16—N3—C20—C21179.64 (12)C44—N7—C48—C49178.58 (12)
Ni2—N3—C20—C213.19 (15)Ni4—N7—C48—C490.57 (15)
C18—C19—C20—N31.7 (2)C46—C47—C48—N71.4 (2)
C18—C19—C20—C21178.92 (13)C46—C47—C48—C49179.03 (13)
Ni2—O12—C21—O11177.73 (11)Ni4—O28—C49—O27179.86 (11)
Ni2—O12—C21—C202.48 (15)Ni4—O28—C49—C480.46 (15)
N3—C20—C21—O11176.50 (12)N7—C48—C49—O27179.64 (13)
C19—C20—C21—O114.1 (2)C47—C48—C49—O270.7 (2)
N3—C20—C21—O123.70 (18)N7—C48—C49—O280.67 (18)
C19—C20—C21—O12175.74 (14)C47—C48—C49—O28178.98 (13)
Ni2—O13—C22—O14177.02 (12)Ni4—O29—C50—O30174.62 (12)
Ni2—O13—C22—C232.74 (15)Ni4—O29—C50—C514.61 (16)
C27—N4—C23—C240.9 (2)C55—N8—C51—C521.1 (2)
Ni2—N4—C23—C24177.63 (10)Ni4—N8—C51—C52174.30 (11)
C27—N4—C23—C22179.73 (12)C55—N8—C51—C50178.74 (12)
Ni2—N4—C23—C222.95 (15)Ni4—N8—C51—C505.88 (16)
O14—C22—C23—N4176.02 (13)O30—C50—C51—N8172.44 (13)
O13—C22—C23—N43.76 (17)O29—C50—C51—N86.85 (18)
O14—C22—C23—C243.4 (2)O30—C50—C51—C527.4 (2)
O13—C22—C23—C24176.85 (13)O29—C50—C51—C52173.35 (14)
N4—C23—C24—C251.1 (2)N8—C51—C52—C531.5 (2)
C22—C23—C24—C25179.53 (13)C50—C51—C52—C53178.24 (13)
C23—C24—C25—C260.8 (2)C51—C52—C53—C540.8 (2)
C24—C25—C26—C270.3 (2)C52—C53—C54—C550.5 (2)
C23—N4—C27—C260.3 (2)C51—N8—C55—C540.2 (2)
Ni2—N4—C27—C26176.98 (10)Ni4—N8—C55—C54175.59 (11)
C23—N4—C27—C28179.45 (12)C51—N8—C55—C56179.85 (13)
Ni2—N4—C27—C282.76 (16)Ni4—N8—C55—C564.48 (16)
C25—C26—C27—N40.0 (2)C53—C54—C55—N81.0 (2)
C25—C26—C27—C28179.68 (13)C53—C54—C55—C56179.11 (14)
Ni2—O16—C28—O15175.40 (11)Ni4—O32—C56—O31177.03 (12)
Ni2—O16—C28—C274.02 (15)Ni4—O32—C56—C551.53 (16)
N4—C27—C28—O161.23 (18)N8—C55—C56—O323.86 (19)
C26—C27—C28—O16179.06 (14)C54—C55—C56—O32176.22 (14)
N4—C27—C28—O15178.24 (12)N8—C55—C56—O31174.83 (13)
C26—C27—C28—O151.5 (2)C54—C55—C56—O315.1 (2)
Hydrogen-bond geometry (Å, º) top
D—H···AD—HH···AD···AD—H···A
O15—H15···O7W1.13 (3)1.37 (3)2.4609 (15)161 (3)
O19—H19A···O8W1.03 (3)1.44 (3)2.4581 (16)171 (3)
O26—H26A···O6W1.00 (2)1.52 (2)2.5224 (16)176 (2)
O31—H31A···O4W1.20 (3)1.23 (3)2.4339 (16)177 (3)
O1W—H1A···O10W0.85 (3)1.76 (3)2.5852 (17)162 (2)
O1W—H1B···O281.10 (3)1.47 (3)2.5475 (15)167 (3)
O1W—H1C···O231.18 (3)1.29 (3)2.4590 (15)170 (3)
O2W—H2A···O110.852 (19)1.84 (2)2.6575 (15)160.1 (17)
O2W—H2B···O220.85 (3)1.74 (3)2.5772 (15)170 (3)
O2W—H2C···O21.16 (3)1.27 (3)2.4275 (15)174 (2)
O3W—H3A···O11Wi0.94 (3)1.62 (3)2.5317 (18)163 (2)
O3W—H3B···O40.96 (2)1.61 (2)2.5679 (16)175 (2)
O3W—H3C···O10i0.96 (3)1.55 (3)2.5076 (16)172 (3)
O4W—H4A···O17ii0.85 (2)1.81 (2)2.6507 (16)171.4 (19)
O4W—H4B···O12W0.85 (3)1.78 (3)2.5983 (19)160 (3)
O5W—H5A···O13iii0.77 (3)1.80 (3)2.5628 (16)170 (3)
O5W—H5B···O9W0.91 (3)1.79 (3)2.6242 (17)151 (2)
O5W—H5C···O71.19 (3)1.27 (3)2.4499 (15)176 (3)
O6W—H6A···O11iv0.76 (2)2.00 (2)2.7459 (15)164 (2)
O6W—H6B···O22iv0.86 (2)1.99 (2)2.7856 (15)154 (2)
O7W—H7A···O30v0.85 (2)1.82 (2)2.6560 (15)166 (2)
O7W—H7B···O30vi0.87 (2)1.93 (2)2.7408 (16)155 (2)
O8W—H8A···O6ii0.88 (2)1.81 (2)2.6509 (15)161 (2)
O8W—H8B···O6iii0.77 (2)2.01 (2)2.7405 (16)159 (2)
O9W—H9A···O18vii0.85 (3)1.84 (3)2.6846 (16)170 (3)
O9W—H9B···O80.86 (2)2.00 (2)2.8250 (16)162 (2)
O10W—H10A···O27viii0.78 (3)1.90 (3)2.6842 (16)176 (2)
O10W—H10B···O240.82 (3)2.07 (3)2.8293 (16)155 (3)
O11W—H11A···O3ix0.83 (4)1.89 (4)2.7037 (17)166 (3)
O11W—H11B···O90.89 (2)1.89 (3)2.7406 (16)159 (2)
O12W—H12A···O14x0.90 (4)1.81 (4)2.6912 (17)166 (3)
O12W—H12B···O18ii0.99 (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) x1, y, z; (vii) x+1, y+1, z+1; (viii) x+2, y+1, z+1; (ix) x, y1, z; (x) x+1, y, z+1.
(180c) [Ni(pydcH)2](H2O)3 top
Crystal data top
3(C14H6N2NiO8)·C14H8N2NiO8·3(H3O)·4(H2O)·HO·4(O)F(000) = 3600
Mr = 1767.75Dx = 1.745 Mg m3
Monoclinic, CcMo Kα radiation, λ = 0.71073 Å
a = 27.5303 (18) ÅCell parameters from 9820 reflections
b = 19.6477 (13) Åθ = 2.7–27.5°
c = 13.7534 (9) ŵ = 1.22 mm1
β = 115.261 (2)°T = 180 K
V = 6727.9 (8) Å3Block, blue-green
Z = 40.47 × 0.40 × 0.34 mm
Data collection top
Bruker Kappa DUO with Photon 100 detector
diffractometer
14609 independent reflections
Radiation source: microsource13325 reflections with I > 2σ(I)
Detector resolution: 10.42 pixels mm-1Rint = 0.022
ω and φ scansθmax = 27.6°, θmin = 2.4°
Absorption correction: multi-scan
SADABS (Sheldrick, 2015)
h = 3535
Tmin = 0.667, Tmax = 0.746k = 2523
30960 measured reflectionsl = 1715
Refinement top
Refinement on F2Secondary atom site location: difference Fourier map
Least-squares matrix: fullHydrogen site location: mixed
R[F2 > 2σ(F2)] = 0.041H 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 reflectionsΔρmax = 0.89 e Å3
1069 parametersΔρmin = 0.72 e Å3
33 restraintsAbsolute structure: Refined as an inversion twin.
Primary atom site location: structure-invariant direct methodsAbsolute structure parameter: 0.50 (2)
Special details top

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.

Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top
xyzUiso*/UeqOcc. (<1)
Ni10.38091 (3)0.87394 (4)0.75039 (7)0.01359 (18)
O10.3526 (2)0.8674 (2)0.8677 (5)0.0185 (11)
O20.2807 (2)0.8891 (3)0.8993 (5)0.0213 (11)
O30.37738 (18)0.8992 (3)0.5944 (4)0.0200 (10)
O40.32294 (19)0.9516 (3)0.4388 (4)0.0202 (10)
O50.42857 (17)0.9584 (2)0.8239 (4)0.0158 (9)
O60.5150 (2)0.9870 (3)0.9272 (5)0.0358 (12)
O70.3643 (2)0.7676 (3)0.7063 (5)0.0230 (11)
O80.4077 (2)0.6685 (2)0.7153 (5)0.0295 (12)
N10.3101 (2)0.9185 (3)0.6775 (5)0.0155 (12)
N20.4530 (2)0.8333 (3)0.8163 (4)0.0155 (11)
C10.3065 (3)0.8919 (4)0.8426 (6)0.0165 (13)
C20.2803 (2)0.9226 (3)0.7323 (6)0.0150 (13)
C30.2317 (2)0.9575 (3)0.6862 (6)0.0124 (12)
H30.2110680.9646240.7258590.015*
C40.2135 (3)0.9819 (4)0.5810 (6)0.0186 (14)
H40.1792281.0029890.5471460.022*
C50.2456 (2)0.9751 (3)0.5253 (6)0.0143 (12)
H50.2343960.9919330.4542280.017*
C60.2950 (2)0.9425 (3)0.5798 (6)0.0129 (12)
C70.3343 (2)0.9304 (3)0.5324 (6)0.0146 (12)
C80.4800 (2)0.9459 (3)0.8755 (5)0.0191 (13)
C90.4954 (3)0.8711 (3)0.8701 (6)0.0194 (14)
C100.5461 (3)0.8475 (4)0.9164 (6)0.0249 (14)
H100.5757480.8765990.9548260.030*
C110.5530 (3)0.7766 (4)0.9048 (7)0.0306 (17)
H110.5877160.7566570.9374460.037*
C120.5087 (3)0.7372 (4)0.8455 (6)0.0266 (15)
H120.5129400.6902430.8345860.032*
C130.4587 (3)0.7657 (3)0.8026 (6)0.0190 (13)
C140.4060 (3)0.7324 (3)0.7354 (6)0.0225 (14)
Ni20.37233 (3)0.38450 (5)0.74654 (6)0.0178 (2)
O90.3642 (2)0.2766 (3)0.7109 (5)0.0240 (11)
O100.4157 (2)0.1837 (3)0.7289 (5)0.0315 (12)
H10A0.384 (2)0.161 (3)0.688 (4)0.002 (12)*
O110.41370 (19)0.4734 (3)0.8103 (4)0.0275 (12)
O120.4961 (2)0.5161 (3)0.9043 (5)0.0414 (13)
O130.3458 (2)0.3767 (3)0.8665 (5)0.0213 (11)
O140.2726 (2)0.3897 (3)0.8986 (5)0.0222 (11)
O150.36589 (19)0.4067 (3)0.5890 (4)0.0219 (10)
O160.3085 (2)0.4518 (3)0.4315 (4)0.0246 (11)
H160.338 (3)0.442 (4)0.418 (6)0.04 (2)*
N30.4469 (2)0.3523 (3)0.8141 (5)0.0202 (12)
N40.2982 (2)0.4223 (3)0.6724 (5)0.0150 (11)
C150.4088 (3)0.2477 (4)0.7442 (6)0.0274 (16)
C160.4587 (3)0.2862 (4)0.8073 (6)0.0256 (15)
C170.5107 (3)0.2628 (4)0.8516 (6)0.0258 (15)
H170.5183010.2162080.8453820.031*
C180.5523 (3)0.3089 (5)0.9062 (7)0.039 (2)
H180.5887060.2944130.9378620.047*
C190.5389 (3)0.3769 (4)0.9128 (6)0.0300 (16)
H190.5663750.4087050.9511790.036*
C200.4854 (3)0.3985 (4)0.8635 (6)0.0274 (16)
C210.4654 (3)0.4692 (4)0.8603 (6)0.0271 (15)
C220.3213 (3)0.4334 (3)0.5272 (6)0.0179 (13)
C230.2822 (3)0.4442 (3)0.5752 (6)0.0162 (13)
C240.2316 (3)0.4732 (3)0.5213 (6)0.0198 (14)
H240.2189430.4886140.4491610.024*
C250.2002 (3)0.4785 (4)0.5781 (6)0.0228 (15)
H250.1652960.4978870.5447730.027*
C260.2200 (3)0.4555 (3)0.6835 (6)0.0223 (15)
H260.1993540.4613430.7233390.027*
C270.2698 (3)0.4240 (3)0.7307 (6)0.0188 (14)
C280.2978 (3)0.3955 (4)0.8420 (6)0.0199 (14)
Ni30.63070 (4)0.62559 (5)0.75260 (7)0.0185 (2)
O170.6581 (2)0.6201 (3)0.6292 (5)0.0222 (12)
O180.7319 (2)0.6420 (3)0.6057 (5)0.0230 (11)
O190.6359 (2)0.6483 (3)0.9118 (4)0.0217 (10)
O200.6910 (3)0.6999 (3)1.0636 (5)0.0328 (13)
O210.64563 (19)0.5184 (2)0.7952 (4)0.0190 (10)
O220.6004 (2)0.4226 (3)0.7801 (5)0.0249 (11)
O230.5813 (3)0.7121 (3)0.6816 (5)0.0395 (15)
O240.4956 (3)0.7396 (4)0.5817 (6)0.069 (2)
N50.7014 (2)0.6659 (3)0.8237 (5)0.0148 (11)
N60.5575 (2)0.5846 (3)0.6895 (5)0.0219 (13)
C290.7056 (3)0.6420 (3)0.6606 (6)0.0166 (13)
C300.7322 (3)0.6743 (3)0.7724 (6)0.0166 (13)
C310.7821 (3)0.7050 (4)0.8155 (7)0.0267 (16)
H310.8041200.7069090.7780010.032*
C320.7979 (3)0.7329 (4)0.9175 (7)0.0263 (17)
H320.8310530.7566750.9500310.032*
C330.7664 (3)0.7264 (3)0.9718 (6)0.0246 (15)
H330.7774990.7457141.0413590.030*
C340.7191 (3)0.6923 (4)0.9254 (6)0.0192 (14)
C350.6776 (3)0.6786 (4)0.9684 (6)0.0226 (14)
C360.5318 (4)0.6985 (5)0.6320 (7)0.038 (2)
C370.5162 (3)0.6274 (4)0.6350 (6)0.0258 (17)
C380.4634 (3)0.5979 (7)0.5886 (6)0.047 (3)
H380.4330050.6257200.5495640.056*
C390.4569 (3)0.5328 (6)0.5998 (7)0.051 (3)
H390.4215830.5145350.5703590.061*
C400.5012 (3)0.4886 (5)0.6548 (7)0.040 (2)
H400.4969960.4410030.6608970.047*
C410.5514 (2)0.5206 (4)0.6991 (6)0.0216 (14)
C420.6032 (2)0.4848 (3)0.7615 (5)0.0152 (12)
Ni40.62611 (4)0.86765 (5)0.25176 (7)0.0205 (2)
O250.63616 (19)0.9776 (3)0.2900 (5)0.0218 (11)
O260.5890 (2)1.0725 (3)0.2741 (5)0.0302 (12)
O270.5823 (2)0.7780 (3)0.1813 (5)0.0340 (13)
O280.4979 (3)0.7446 (4)0.0831 (6)0.066 (2)
O290.6543 (2)0.8772 (3)0.1309 (5)0.0250 (12)
O300.7273 (2)0.8577 (3)0.1056 (5)0.0257 (12)
O310.6298 (2)0.8428 (3)0.4075 (4)0.0262 (11)
O320.6865 (3)0.7959 (3)0.5630 (5)0.0413 (16)
N70.5522 (2)0.9052 (4)0.1859 (5)0.0244 (13)
N80.6981 (2)0.8314 (3)0.3246 (5)0.0169 (12)
C430.5941 (2)1.0088 (4)0.2569 (6)0.0203 (14)
C440.5429 (3)0.9696 (4)0.1951 (6)0.0223 (15)
C450.4901 (3)0.9982 (5)0.1482 (7)0.039 (2)
H450.4833821.0450480.1540660.047*
C460.4492 (3)0.9518 (5)0.0931 (7)0.038 (2)
H460.4131670.9674590.0609710.045*
C470.4591 (3)0.8849 (6)0.0836 (6)0.046 (3)
H470.4304270.8546130.0448870.055*
C480.5127 (3)0.8609 (4)0.1323 (6)0.0232 (15)
C490.5314 (3)0.7887 (4)0.1317 (7)0.037 (2)
C500.6727 (3)0.8160 (4)0.4661 (6)0.0247 (15)
C510.7161 (3)0.8054 (4)0.4264 (6)0.0225 (15)
C520.7651 (3)0.7741 (4)0.4750 (7)0.0292 (18)
H520.7770810.7565610.5458060.035*
C530.7968 (3)0.7681 (4)0.4209 (7)0.0294 (18)
H530.8302350.7451530.4538710.035*
C540.7803 (3)0.7955 (4)0.3176 (7)0.0290 (17)
H540.8024390.7944260.2802460.035*
C550.7293 (3)0.8245 (3)0.2735 (6)0.0170 (13)
C560.7020 (3)0.8565 (3)0.1610 (6)0.0174 (13)
O1W0.3860 (2)1.0707 (3)0.8587 (5)0.0334 (12)
H1A0.403 (2)1.035 (2)0.838 (5)0.040*
H1B0.3599 (19)1.053 (3)0.879 (5)0.040*
H1C0.4119 (17)1.094 (3)0.918 (3)0.040*
O2W0.6725 (2)1.1360 (3)0.3886 (5)0.0302 (13)
H2A0.7040 (16)1.137 (4)0.376 (5)0.036*
H2B0.686 (2)1.143 (4)0.4647 (16)0.036*
O3W0.6833 (2)0.3622 (3)0.8930 (5)0.0234 (11)
H3A0.7120 (17)0.362 (3)0.872 (4)0.028*
H3B0.697 (2)0.355 (3)0.9682 (16)0.028*
O4W0.3677 (2)0.5796 (3)0.1507 (5)0.0316 (12)
H4A0.4040 (12)0.592 (4)0.104 (5)0.038*
O5W0.3335 (2)0.8788 (3)1.1137 (5)0.0274 (13)
H5A0.319 (2)0.875 (3)1.0375 (14)0.033*
H5B0.3060 (19)0.865 (3)1.134 (5)0.033*
O6W0.3238 (3)0.6107 (3)0.6076 (5)0.0321 (13)
H6A0.2953 (16)0.630 (3)0.620 (5)0.039*
H6B0.316 (2)0.623 (3)0.5345 (18)0.039*
H6C0.3551 (15)0.638 (3)0.648 (4)0.039*
O7W0.6311 (3)0.6769 (3)1.1516 (5)0.0363 (14)
H7A0.651 (2)0.683 (3)1.110 (5)0.044*
H7B0.609 (2)0.6374 (19)1.126 (5)0.044*
H7C0.607 (2)0.715 (2)1.136 (5)0.044*
O8W0.6206 (3)0.8186 (3)0.6397 (6)0.0447 (16)
H8A0.622 (3)0.776 (2)0.675 (6)0.054*
H8B0.6566 (12)0.828 (4)0.651 (7)0.054*
O9W0.5921 (2)0.5689 (3)1.0253 (5)0.0429 (13)
O10W0.5579 (5)0.8895 (6)0.4803 (9)0.059 (3)*0.6
O11W0.4232 (4)0.8299 (5)0.4777 (8)0.050 (2)*0.6
O12W0.4150 (4)0.6721 (5)0.0202 (8)0.048 (2)*0.6
O13W0.5350 (6)0.8825 (8)0.5059 (13)0.055 (4)*0.4
O14W0.4577 (7)0.8597 (8)0.5232 (14)0.060 (4)*0.4
O15W0.4593 (7)0.6283 (8)0.0091 (13)0.059 (4)*0.4
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
Ni10.0087 (4)0.0159 (3)0.0158 (4)0.0071 (2)0.0049 (3)0.0019 (3)
O10.014 (2)0.025 (2)0.017 (3)0.0061 (16)0.007 (2)0.0023 (18)
O20.017 (2)0.027 (2)0.022 (3)0.0004 (18)0.010 (2)0.003 (2)
O30.0132 (19)0.026 (2)0.023 (2)0.0076 (17)0.0103 (18)0.0051 (18)
O40.020 (2)0.026 (2)0.017 (2)0.0049 (17)0.0105 (18)0.0055 (18)
O50.0119 (18)0.0165 (19)0.020 (2)0.0056 (14)0.0079 (16)0.0003 (16)
O60.027 (2)0.031 (2)0.046 (3)0.007 (2)0.012 (2)0.008 (2)
O70.015 (2)0.026 (2)0.021 (3)0.0006 (18)0.0018 (18)0.0054 (19)
O80.042 (3)0.015 (2)0.034 (3)0.0076 (19)0.018 (2)0.0070 (19)
N10.012 (2)0.019 (3)0.020 (3)0.0022 (19)0.011 (2)0.001 (2)
N20.017 (2)0.021 (3)0.007 (2)0.0070 (19)0.0026 (18)0.0004 (19)
C10.015 (3)0.020 (3)0.014 (3)0.004 (2)0.006 (2)0.001 (3)
C20.007 (2)0.020 (3)0.018 (3)0.002 (2)0.006 (2)0.000 (2)
C30.007 (2)0.015 (2)0.020 (3)0.0017 (19)0.011 (2)0.000 (2)
C40.010 (2)0.025 (3)0.023 (4)0.007 (2)0.009 (2)0.004 (3)
C50.012 (2)0.018 (3)0.016 (3)0.006 (2)0.009 (2)0.002 (2)
C60.007 (2)0.009 (2)0.018 (3)0.0019 (19)0.000 (2)0.004 (2)
C70.013 (2)0.011 (2)0.023 (3)0.002 (2)0.011 (2)0.001 (2)
C80.015 (3)0.027 (3)0.016 (3)0.001 (2)0.008 (2)0.003 (2)
C90.022 (3)0.022 (3)0.018 (3)0.006 (2)0.012 (3)0.000 (2)
C100.020 (3)0.035 (4)0.019 (3)0.006 (3)0.008 (3)0.001 (3)
C110.021 (3)0.039 (4)0.031 (4)0.023 (3)0.010 (3)0.002 (3)
C120.023 (3)0.033 (3)0.019 (3)0.017 (3)0.005 (2)0.002 (3)
C130.028 (3)0.015 (3)0.016 (3)0.014 (2)0.012 (2)0.004 (2)
C140.041 (4)0.014 (3)0.014 (3)0.007 (2)0.013 (3)0.000 (2)
Ni20.0117 (4)0.0255 (4)0.0149 (4)0.0002 (3)0.0046 (3)0.0005 (4)
O90.016 (2)0.026 (2)0.025 (3)0.0019 (17)0.0042 (19)0.0064 (19)
O100.033 (3)0.025 (2)0.039 (3)0.006 (2)0.017 (2)0.006 (2)
O110.0126 (19)0.046 (3)0.022 (2)0.0129 (19)0.0059 (17)0.009 (2)
O120.023 (2)0.054 (3)0.043 (3)0.018 (2)0.010 (2)0.014 (3)
O130.014 (2)0.032 (3)0.015 (3)0.0021 (18)0.002 (2)0.0032 (19)
O140.021 (2)0.029 (2)0.020 (3)0.0049 (19)0.012 (2)0.004 (2)
O150.015 (2)0.032 (2)0.020 (2)0.0032 (18)0.0080 (18)0.0025 (19)
O160.036 (3)0.025 (2)0.014 (2)0.007 (2)0.011 (2)0.0061 (19)
N30.021 (2)0.028 (3)0.014 (3)0.001 (2)0.010 (2)0.002 (2)
N40.010 (2)0.016 (2)0.016 (3)0.0050 (17)0.0030 (19)0.001 (2)
C150.039 (4)0.022 (3)0.022 (3)0.006 (3)0.014 (3)0.007 (3)
C160.032 (3)0.030 (4)0.015 (3)0.008 (3)0.010 (3)0.000 (3)
C170.016 (3)0.042 (4)0.023 (3)0.011 (3)0.010 (2)0.008 (3)
C180.024 (3)0.063 (6)0.029 (4)0.012 (3)0.009 (3)0.004 (4)
C190.020 (3)0.053 (4)0.018 (3)0.002 (3)0.010 (2)0.002 (3)
C200.020 (3)0.047 (4)0.014 (3)0.000 (3)0.006 (2)0.001 (3)
C210.015 (3)0.049 (4)0.021 (3)0.012 (3)0.011 (2)0.011 (3)
C220.021 (3)0.008 (2)0.019 (3)0.004 (2)0.003 (2)0.002 (2)
C230.022 (3)0.011 (2)0.015 (3)0.004 (2)0.007 (2)0.007 (2)
C240.023 (3)0.017 (3)0.012 (3)0.002 (2)0.000 (2)0.002 (2)
C250.017 (3)0.025 (3)0.024 (4)0.001 (2)0.006 (3)0.002 (3)
C260.025 (3)0.020 (3)0.021 (4)0.008 (3)0.010 (3)0.000 (3)
C270.015 (3)0.022 (3)0.022 (3)0.004 (2)0.011 (2)0.003 (3)
C280.023 (3)0.020 (3)0.014 (3)0.002 (2)0.006 (3)0.002 (3)
Ni30.0203 (4)0.0218 (4)0.0148 (4)0.0061 (3)0.0087 (3)0.0009 (3)
O170.023 (3)0.030 (3)0.017 (3)0.0018 (18)0.012 (2)0.0041 (18)
O180.030 (2)0.030 (2)0.016 (3)0.007 (2)0.017 (2)0.004 (2)
O190.030 (2)0.023 (2)0.017 (2)0.0024 (18)0.0136 (19)0.0009 (18)
O200.055 (3)0.032 (3)0.021 (3)0.010 (2)0.025 (2)0.008 (2)
O210.015 (2)0.018 (2)0.022 (2)0.0010 (16)0.0066 (18)0.0059 (18)
O220.021 (2)0.028 (2)0.029 (3)0.0034 (18)0.0134 (19)0.0077 (19)
O230.062 (4)0.030 (3)0.040 (3)0.023 (3)0.035 (3)0.015 (2)
O240.084 (5)0.078 (5)0.062 (4)0.067 (4)0.047 (4)0.050 (4)
N50.022 (2)0.012 (2)0.010 (2)0.0010 (19)0.006 (2)0.0033 (19)
N60.011 (2)0.043 (3)0.013 (3)0.013 (2)0.0066 (19)0.002 (2)
C290.020 (3)0.014 (3)0.020 (3)0.005 (2)0.012 (3)0.000 (3)
C300.029 (3)0.011 (3)0.011 (3)0.000 (2)0.010 (2)0.001 (2)
C310.027 (3)0.031 (4)0.027 (4)0.001 (3)0.016 (3)0.000 (3)
C320.031 (4)0.016 (3)0.025 (4)0.008 (3)0.006 (3)0.002 (3)
C330.037 (4)0.016 (3)0.017 (3)0.001 (3)0.008 (3)0.001 (2)
C340.027 (3)0.020 (3)0.013 (3)0.003 (2)0.010 (3)0.003 (2)
C350.038 (4)0.023 (3)0.014 (3)0.004 (3)0.018 (3)0.001 (3)
C360.046 (4)0.050 (5)0.032 (4)0.036 (4)0.028 (4)0.021 (3)
C370.014 (3)0.056 (5)0.011 (3)0.018 (3)0.008 (2)0.006 (3)
C380.014 (3)0.111 (8)0.016 (3)0.024 (4)0.008 (3)0.013 (5)
C390.010 (3)0.122 (10)0.019 (4)0.001 (4)0.004 (3)0.000 (4)
C400.028 (4)0.069 (6)0.026 (4)0.004 (4)0.016 (3)0.008 (4)
C410.007 (2)0.046 (4)0.013 (3)0.002 (2)0.006 (2)0.002 (3)
C420.008 (2)0.031 (3)0.010 (3)0.002 (2)0.007 (2)0.004 (2)
Ni40.0194 (4)0.0276 (5)0.0148 (4)0.0058 (4)0.0077 (3)0.0002 (4)
O250.012 (2)0.030 (2)0.023 (3)0.0019 (17)0.0069 (18)0.0097 (19)
O260.027 (2)0.033 (3)0.029 (3)0.004 (2)0.010 (2)0.005 (2)
O270.053 (3)0.021 (2)0.037 (3)0.017 (2)0.029 (3)0.011 (2)
O280.071 (4)0.082 (5)0.063 (4)0.062 (4)0.044 (4)0.049 (4)
O290.020 (2)0.038 (3)0.015 (3)0.003 (2)0.006 (2)0.006 (2)
O300.031 (3)0.035 (3)0.017 (3)0.004 (2)0.016 (2)0.005 (2)
O310.036 (3)0.029 (2)0.020 (2)0.006 (2)0.018 (2)0.001 (2)
O320.074 (4)0.035 (3)0.024 (3)0.007 (3)0.029 (3)0.006 (2)
N70.009 (2)0.048 (3)0.019 (3)0.005 (2)0.009 (2)0.002 (2)
N80.023 (3)0.013 (2)0.011 (3)0.002 (2)0.003 (2)0.0013 (19)
C430.010 (2)0.039 (4)0.012 (3)0.002 (2)0.006 (2)0.002 (3)
C440.014 (3)0.042 (4)0.010 (3)0.004 (2)0.005 (2)0.001 (3)
C450.018 (3)0.075 (6)0.025 (4)0.006 (3)0.010 (3)0.007 (4)
C460.009 (3)0.077 (6)0.022 (4)0.001 (3)0.003 (2)0.011 (4)
C470.013 (3)0.107 (8)0.016 (3)0.022 (4)0.004 (3)0.004 (4)
C480.014 (3)0.049 (4)0.009 (3)0.013 (3)0.007 (2)0.008 (2)
C490.041 (4)0.051 (5)0.029 (4)0.025 (3)0.025 (3)0.016 (3)
C500.042 (4)0.023 (3)0.015 (3)0.008 (3)0.018 (3)0.005 (3)
C510.037 (4)0.019 (3)0.012 (3)0.000 (3)0.010 (3)0.003 (2)
C520.045 (4)0.015 (3)0.019 (4)0.001 (3)0.006 (3)0.004 (3)
C530.035 (4)0.018 (3)0.023 (4)0.008 (3)0.002 (3)0.002 (3)
C540.030 (4)0.025 (3)0.030 (4)0.002 (3)0.010 (3)0.001 (3)
C550.027 (3)0.010 (3)0.013 (3)0.001 (2)0.008 (2)0.002 (2)
C560.021 (3)0.017 (3)0.016 (3)0.006 (2)0.009 (3)0.000 (3)
O1W0.046 (3)0.028 (3)0.040 (3)0.001 (2)0.032 (3)0.001 (2)
O2W0.030 (3)0.034 (3)0.025 (3)0.003 (2)0.010 (2)0.004 (2)
O3W0.023 (2)0.029 (2)0.022 (3)0.0031 (19)0.012 (2)0.003 (2)
O4W0.045 (3)0.026 (2)0.031 (3)0.002 (2)0.023 (2)0.003 (2)
O5W0.029 (3)0.038 (3)0.018 (3)0.0070 (19)0.013 (2)0.0034 (19)
O6W0.040 (3)0.039 (3)0.018 (3)0.003 (2)0.013 (2)0.007 (2)
O7W0.054 (3)0.035 (3)0.025 (3)0.023 (2)0.021 (2)0.003 (2)
O8W0.075 (4)0.030 (3)0.043 (4)0.002 (3)0.037 (3)0.007 (2)
O9W0.033 (2)0.043 (3)0.048 (3)0.017 (2)0.013 (2)0.009 (2)
Geometric parameters (Å, º) top
Ni1—N21.965 (5)O19—C351.232 (9)
Ni1—N11.976 (6)O20—C351.270 (10)
Ni1—O12.075 (6)O21—C421.248 (8)
Ni1—O52.089 (5)O22—C421.258 (9)
Ni1—O32.163 (6)O23—C361.265 (11)
Ni1—O72.169 (5)O24—C361.239 (9)
O1—C11.259 (8)N5—C301.325 (9)
O2—C11.261 (9)N5—C341.371 (9)
O3—C71.284 (8)N6—C411.284 (10)
O4—C71.259 (9)N6—C371.355 (8)
O5—C81.308 (7)C29—C301.530 (10)
O6—C81.225 (8)C30—C311.380 (10)
O7—C141.253 (9)C31—C321.392 (12)
O8—C141.290 (8)C31—H310.9500
O8—H6C1.471 (18)C32—C331.372 (11)
N1—C61.313 (9)C32—H320.9500
N1—C21.332 (9)C33—C341.358 (10)
N2—C91.314 (9)C33—H330.9500
N2—C131.361 (8)C34—C351.517 (10)
C1—C21.500 (10)C36—C371.467 (12)
C2—C31.393 (8)C37—C381.438 (12)
C3—C41.399 (10)C38—C391.309 (15)
C3—H30.9500C38—H380.9500
C4—C51.402 (9)C39—C401.424 (13)
C4—H40.9500C39—H390.9500
C5—C61.398 (8)C40—C411.399 (10)
C5—H50.9500C40—H400.9500
C6—C71.500 (9)C41—C421.489 (8)
C8—C91.541 (8)Ni4—N81.934 (6)
C9—C101.346 (9)Ni4—N71.984 (6)
C10—C111.424 (10)Ni4—O272.121 (5)
C10—H100.9500Ni4—O292.121 (7)
C11—C121.380 (11)Ni4—O312.156 (6)
C11—H110.9500Ni4—O252.213 (6)
C12—C131.365 (9)O25—C431.214 (8)
C12—H120.9500O26—C431.291 (9)
C13—C141.497 (10)O27—C491.288 (10)
Ni2—N31.963 (6)O28—C491.236 (10)
Ni2—N41.995 (5)O29—C561.263 (9)
Ni2—O112.065 (5)O30—C561.233 (9)
Ni2—O132.075 (6)O31—C501.228 (10)
Ni2—O152.142 (6)O32—C501.283 (10)
Ni2—O92.166 (5)N7—C441.309 (10)
O9—C151.249 (9)N7—C481.340 (9)
O10—C151.301 (9)N8—C551.330 (9)
O10—H10A0.93 (5)N8—C511.368 (9)
O11—C211.292 (8)C43—C441.511 (9)
O12—C211.222 (9)C44—C451.429 (10)
O13—C281.273 (8)C45—C461.394 (12)
O14—C281.248 (9)C45—H450.9500
O15—C221.271 (8)C46—C471.359 (13)
O16—C221.261 (9)C46—H460.9500
O16—H160.93 (8)C47—C481.416 (11)
N3—C201.339 (10)C47—H470.9500
N3—C161.351 (9)C48—C491.510 (12)
N4—C231.290 (9)C50—C511.526 (11)
N4—C271.337 (9)C51—C521.369 (11)
C15—C161.484 (11)C52—C531.371 (12)
C16—C171.374 (9)C52—H520.9500
C17—C181.401 (11)C53—C541.402 (12)
C17—H170.9500C53—H530.9500
C18—C191.399 (12)C54—C551.392 (10)
C18—H180.9500C54—H540.9500
C19—C201.399 (10)C55—C561.537 (10)
C19—H190.9500O1W—H1A0.960 (14)
C20—C211.487 (11)O1W—H1B0.947 (14)
C22—C231.499 (10)O1W—H1C0.943 (14)
C23—C241.391 (9)O2W—H2A0.956 (14)
C24—C251.394 (10)O2W—H2B0.959 (14)
C24—H240.9500O3W—H3A0.952 (14)
C25—C261.388 (11)O3W—H3B0.948 (14)
C25—H250.9500O4W—H4A0.963 (15)
C26—C271.388 (9)O5W—H5A0.951 (14)
C26—H260.9500O5W—H5B0.952 (14)
C27—C281.497 (10)O6W—H6A0.955 (14)
Ni3—N51.936 (6)O6W—H6B0.961 (14)
Ni3—N61.992 (6)O6W—H6C0.967 (14)
Ni3—O172.134 (6)O7W—H7A0.956 (14)
Ni3—O232.135 (6)O7W—H7B0.953 (14)
Ni3—O212.177 (5)O7W—H7C0.960 (14)
Ni3—O192.179 (6)O8W—H8A0.956 (14)
O17—C291.265 (9)O8W—H8B0.953 (14)
O18—C291.250 (9)
N2—Ni1—N1176.0 (3)O17—Ni3—O2392.8 (2)
N2—Ni1—O1104.9 (2)N5—Ni3—O21103.1 (2)
N1—Ni1—O178.8 (2)N6—Ni3—O2176.5 (2)
N2—Ni1—O578.3 (2)O17—Ni3—O2194.3 (2)
N1—Ni1—O5100.0 (2)O23—Ni3—O21154.6 (2)
O1—Ni1—O592.3 (2)N5—Ni3—O1977.8 (2)
N2—Ni1—O399.2 (2)N6—Ni3—O1998.1 (2)
N1—Ni1—O377.2 (2)O17—Ni3—O19156.3 (2)
O1—Ni1—O3155.9 (2)O23—Ni3—O1993.0 (2)
O5—Ni1—O392.9 (2)O21—Ni3—O1990.2 (2)
N2—Ni1—O777.8 (2)C29—O17—Ni3112.1 (5)
N1—Ni1—O7103.9 (2)C35—O19—Ni3112.2 (5)
O1—Ni1—O793.0 (2)C42—O21—Ni3111.9 (4)
O5—Ni1—O7156.11 (19)C36—O23—Ni3114.0 (5)
O3—Ni1—O791.7 (2)C30—N5—C34117.9 (6)
C1—O1—Ni1115.6 (5)C30—N5—Ni3121.1 (5)
C7—O3—Ni1114.0 (4)C34—N5—Ni3120.8 (5)
C8—O5—Ni1115.2 (4)C41—N6—C37123.3 (6)
C14—O7—Ni1112.8 (4)C41—N6—Ni3120.3 (5)
C14—O8—H6C114 (2)C37—N6—Ni3116.4 (5)
C6—N1—C2123.8 (6)O18—C29—O17125.1 (7)
C6—N1—Ni1119.4 (4)O18—C29—C30117.1 (6)
C2—N1—Ni1116.8 (5)O17—C29—C30117.8 (6)
C9—N2—C13120.2 (6)N5—C30—C31124.8 (7)
C9—N2—Ni1120.7 (4)N5—C30—C29110.0 (6)
C13—N2—Ni1119.1 (5)C31—C30—C29125.1 (7)
O1—C1—O2125.5 (7)C30—C31—C32115.5 (7)
O1—C1—C2115.2 (6)C30—C31—H31122.2
O2—C1—C2119.2 (6)C32—C31—H31122.2
N1—C2—C3118.4 (6)C33—C32—C31120.9 (7)
N1—C2—C1113.7 (5)C33—C32—H32119.6
C3—C2—C1127.7 (6)C31—C32—H32119.6
C2—C3—C4119.3 (6)C34—C33—C32119.5 (7)
C2—C3—H3120.3C34—C33—H33120.2
C4—C3—H3120.3C32—C33—H33120.2
C3—C4—C5120.1 (6)C33—C34—N5121.2 (7)
C3—C4—H4119.9C33—C34—C35129.3 (7)
C5—C4—H4119.9N5—C34—C35109.4 (6)
C6—C5—C4116.6 (6)O19—C35—O20126.4 (7)
C6—C5—H5121.7O19—C35—C34119.5 (6)
C4—C5—H5121.7O20—C35—C34114.1 (7)
N1—C6—C5121.6 (6)O24—C36—O23126.0 (9)
N1—C6—C7114.6 (5)O24—C36—C37117.4 (9)
C5—C6—C7123.8 (6)O23—C36—C37116.6 (6)
O4—C7—O3126.4 (6)N6—C37—C38116.6 (8)
O4—C7—C6118.8 (5)N6—C37—C36114.8 (7)
O3—C7—C6114.8 (6)C38—C37—C36128.7 (7)
O6—C8—O5126.4 (6)C39—C38—C37120.3 (7)
O6—C8—C9119.5 (6)C39—C38—H38119.9
O5—C8—C9114.1 (6)C37—C38—H38119.9
N2—C9—C10124.5 (6)C38—C39—C40122.0 (8)
N2—C9—C8111.7 (6)C38—C39—H39119.0
C10—C9—C8123.8 (6)C40—C39—H39119.0
C9—C10—C11116.4 (7)C41—C40—C39114.8 (9)
C9—C10—H10121.8C41—C40—H40122.6
C11—C10—H10121.8C39—C40—H40122.6
C12—C11—C10119.3 (6)N6—C41—C40123.0 (7)
C12—C11—H11120.4N6—C41—C42112.7 (6)
C10—C11—H11120.4C40—C41—C42124.3 (7)
C13—C12—C11120.0 (6)O21—C42—O22124.6 (6)
C13—C12—H12120.0O21—C42—C41118.6 (6)
C11—C12—H12120.0O22—C42—C41116.7 (6)
N2—C13—C12119.7 (7)N8—Ni4—N7176.4 (3)
N2—C13—C14112.0 (5)N8—Ni4—O27100.8 (2)
C12—C13—C14128.3 (6)N7—Ni4—O2780.1 (3)
O7—C14—O8125.6 (7)N8—Ni4—O2978.6 (3)
O7—C14—C13118.1 (6)N7—Ni4—O29104.9 (3)
O8—C14—C13116.4 (6)O27—Ni4—O2992.4 (2)
N3—Ni2—N4175.9 (3)N8—Ni4—O3178.3 (3)
N3—Ni2—O1178.2 (2)N7—Ni4—O3198.2 (2)
N4—Ni2—O1199.3 (2)O27—Ni4—O3192.5 (2)
N3—Ni2—O13104.6 (2)O29—Ni4—O31156.9 (2)
N4—Ni2—O1378.7 (2)N8—Ni4—O25103.9 (2)
O11—Ni2—O1392.4 (2)N7—Ni4—O2575.3 (2)
N3—Ni2—O1599.4 (2)O27—Ni4—O25155.3 (2)
N4—Ni2—O1577.4 (2)O29—Ni4—O2592.9 (2)
O11—Ni2—O1592.8 (2)O31—Ni4—O2592.1 (2)
O13—Ni2—O15156.0 (2)C43—O25—Ni4113.7 (5)
N3—Ni2—O977.2 (2)C49—O27—Ni4112.5 (5)
N4—Ni2—O9105.3 (2)C56—O29—Ni4113.1 (5)
O11—Ni2—O9155.4 (2)C50—O31—Ni4112.0 (5)
O13—Ni2—O994.0 (2)C44—N7—C48122.4 (6)
O15—Ni2—O990.8 (2)C44—N7—Ni4121.4 (5)
C15—O9—Ni2111.8 (5)C48—N7—Ni4116.3 (6)
C15—O10—H10A113 (3)C55—N8—C51117.9 (6)
C21—O11—Ni2117.0 (5)C55—N8—Ni4120.9 (5)
C28—O13—Ni2116.5 (5)C51—N8—Ni4120.8 (5)
C22—O15—Ni2113.6 (5)O25—C43—O26125.6 (7)
C22—O16—H16105 (5)O25—C43—C44117.8 (7)
C20—N3—C16121.7 (7)O26—C43—C44116.6 (6)
C20—N3—Ni2117.5 (5)N7—C44—C45122.6 (7)
C16—N3—Ni2120.7 (5)N7—C44—C43111.9 (6)
C23—N4—C27125.8 (6)C45—C44—C43125.4 (7)
C23—N4—Ni2118.4 (5)C46—C45—C44114.7 (9)
C27—N4—Ni2115.8 (5)C46—C45—H45122.6
O9—C15—O10124.6 (7)C44—C45—H45122.6
O9—C15—C16120.2 (6)C47—C46—C45122.4 (7)
O10—C15—C16115.2 (7)C47—C46—H46118.8
N3—C16—C17121.8 (7)C45—C46—H46118.8
N3—C16—C15109.9 (6)C46—C47—C48119.1 (7)
C17—C16—C15128.2 (7)C46—C47—H47120.4
C16—C17—C18118.6 (7)C48—C47—H47120.4
C16—C17—H17120.7N7—C48—C47118.7 (8)
C18—C17—H17120.7N7—C48—C49114.5 (6)
C19—C18—C17118.3 (7)C47—C48—C49126.8 (7)
C19—C18—H18120.8O28—C49—O27124.4 (9)
C17—C18—H18120.8O28—C49—C48119.0 (8)
C18—C19—C20120.8 (7)O27—C49—C48116.6 (6)
C18—C19—H19119.6O31—C50—O32126.1 (7)
C20—C19—H19119.6O31—C50—C51120.2 (7)
N3—C20—C19118.7 (7)O32—C50—C51113.7 (7)
N3—C20—C21114.6 (6)N8—C51—C52121.3 (7)
C19—C20—C21126.7 (7)N8—C51—C50108.5 (6)
O12—C21—O11126.0 (8)C52—C51—C50130.2 (7)
O12—C21—C20121.3 (6)C51—C52—C53119.7 (7)
O11—C21—C20112.6 (6)C51—C52—H52120.1
O16—C22—O15125.2 (7)C53—C52—H52120.1
O16—C22—C23119.1 (6)C52—C53—C54120.8 (7)
O15—C22—C23115.7 (6)C52—C53—H53119.6
N4—C23—C24120.7 (6)C54—C53—H53119.6
N4—C23—C22114.7 (6)C55—C54—C53115.3 (8)
C24—C23—C22124.6 (6)C55—C54—H54122.3
C23—C24—C25116.8 (7)C53—C54—H54122.3
C23—C24—H24121.6N8—C55—C54124.9 (7)
C25—C24—H24121.6N8—C55—C56110.0 (6)
C26—C25—C24120.0 (6)C54—C55—C56125.1 (7)
C26—C25—H25120.0O30—C56—O29125.1 (7)
C24—C25—H25120.0O30—C56—C55117.8 (6)
C25—C26—C27120.2 (7)O29—C56—C55117.1 (6)
C25—C26—H26119.9H1A—O1W—H1B110 (3)
C27—C26—H26119.9H1A—O1W—H1C110 (3)
N4—C27—C26116.3 (7)H1B—O1W—H1C108 (3)
N4—C27—C28115.3 (6)H2A—O2W—H2B104 (3)
C26—C27—C28128.3 (7)H3A—O3W—H3B110 (3)
O14—C28—O13126.7 (7)H5A—O5W—H5B106 (3)
O14—C28—C27119.5 (6)H6A—O6W—H6B105 (3)
O13—C28—C27113.7 (6)H6A—O6W—H6C106 (3)
N5—Ni3—N6175.8 (3)H6B—O6W—H6C103 (3)
N5—Ni3—O1778.6 (2)H7A—O7W—H7B108 (3)
N6—Ni3—O17105.6 (2)H7A—O7W—H7C106 (3)
N5—Ni3—O23102.2 (3)H7B—O7W—H7C106 (3)
N6—Ni3—O2378.1 (3)H8A—O8W—H8B105 (3)
Hydrogen-bond geometry (Å, º) top
D—H···AD—HH···AD···AD—H···A
O1W—H1A···O50.96 (1)1.70 (2)2.637 (7)164 (6)
O1W—H1B···O4i0.95 (1)1.56 (2)2.461 (7)158 (5)
O1W—H1C···O11Wi0.94 (1)1.67 (4)2.472 (12)141 (6)
O1W—H1C···O14Wi0.94 (1)1.72 (2)2.659 (18)177 (7)
O2W—H2B···O30i0.96 (1)1.78 (3)2.713 (9)163 (6)
O3W—H3A···O2ii0.95 (1)1.84 (4)2.697 (7)148 (5)
O3W—H3B···O18iii0.95 (1)1.72 (2)2.648 (8)166 (6)
O4W—H4A···O15W0.96 (2)1.68 (3)2.623 (17)165 (7)
O5W—H5A···O20.95 (1)1.76 (3)2.682 (9)164 (7)
O5W—H5B···O18iv0.95 (1)1.91 (4)2.782 (8)151 (6)
O6W—H6A···O30iv0.96 (1)1.81 (3)2.716 (8)158 (5)
O6W—H6C···O70.97 (1)2.65 (5)3.362 (8)131 (5)
O6W—H6C···O80.97 (1)1.47 (2)2.429 (8)170 (6)
O7W—H7A···O200.96 (1)1.53 (2)2.470 (8)168 (6)
O7W—H7C···O27v0.96 (1)1.66 (4)2.526 (8)149 (6)
O8W—H8A···O230.96 (1)1.72 (4)2.531 (9)141 (6)
O8W—H8B···O320.95 (1)1.84 (7)2.495 (9)123 (7)
Symmetry codes: (i) x, y+2, z+1/2; (ii) x+1/2, y1/2, z; (iii) x, y+1, z+1/2; (iv) x1/2, y+3/2, z+1/2; (v) x, y, z+1.
(298d) [Ni(pydcH)(pydc)](H3O)(H2O)2] top
Crystal data top
C14H7N2NiO8·H3O·H2O·OF(000) = 904
Mr = 442.97Dx = 1.716 Mg m3
Monoclinic, P21/cMo Kα radiation, λ = 0.71073 Å
a = 13.6716 (8) ÅCell parameters from 9943 reflections
b = 10.0554 (6) Åθ = 2.6–31.5°
c = 13.7813 (8) ŵ = 1.20 mm1
β = 115.185 (3)°T = 298 K
V = 1714.46 (18) Å3Block, blue-green
Z = 40.47 × 0.40 × 0.34 mm
Data collection top
Bruker Kappa DUO with Photon 100 detector
diffractometer
5701 independent reflections
Radiation source: microsource4751 reflections with I > 2σ(I)
Detector resolution: 10.42 pixels mm-1Rint = 0.025
ω and φ scansθmax = 31.6°, θmin = 2.6°
Absorption correction: multi-scan
SADABS (Shedrick, 2014)
h = 2020
Tmin = 0.653, Tmax = 0.746k = 1411
18349 measured reflectionsl = 1620
Refinement top
Refinement on F2Secondary atom site location: difference Fourier map
Least-squares matrix: fullHydrogen site location: mixed
R[F2 > 2σ(F2)] = 0.038H 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 reflectionsΔρmax = 0.80 e Å3
277 parametersΔρmin = 0.73 e Å3
4 restraintsExtinction correction: SHELXL-2016/6 (Sheldrick 2016), Fc*=kFc[1+0.001xFc2λ3/sin(2θ)]-1/4
Primary atom site location: structure-invariant direct methodsExtinction coefficient: 0.0236 (14)
Special details top

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.

Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top
xyzUiso*/UeqOcc. (<1)
Ni10.24988 (2)0.49365 (2)0.24789 (2)0.02873 (8)
N10.10554 (10)0.41406 (12)0.17530 (10)0.0278 (2)
N20.39697 (9)0.56861 (14)0.31362 (10)0.0299 (2)
O10.19345 (10)0.51023 (12)0.36687 (10)0.0367 (3)
O20.04743 (11)0.46980 (15)0.39573 (10)0.0427 (3)
O30.12913 (12)0.34632 (14)0.06306 (10)0.0467 (3)
O40.24047 (9)0.44477 (13)0.09067 (10)0.0379 (3)
O50.22437 (9)0.70592 (12)0.20649 (10)0.0378 (3)
O60.31886 (12)0.89359 (13)0.22388 (12)0.0471 (3)
H6A0.248 (3)0.932 (4)0.176 (3)0.113 (12)*
O70.51307 (15)0.26162 (19)0.41839 (16)0.0712 (5)
O80.34227 (11)0.32402 (12)0.31883 (11)0.0423 (3)
O90.25429 (16)0.38941 (17)0.14492 (14)0.0564 (4)
H9A0.286 (3)0.317 (4)0.160 (3)0.092 (11)*
H9B0.304 (3)0.450 (3)0.104 (3)0.071 (8)*
H9C0.197 (3)0.369 (4)0.104 (3)0.127 (14)*
O100.15270 (13)1.01524 (14)0.10944 (13)0.0479 (3)*
H10A0.136 (3)0.993 (3)0.039 (3)0.098 (13)*
H10B0.097 (2)1.000 (3)0.126 (3)0.070 (9)*
O11A0.3833 (6)0.5365 (7)0.0113 (5)0.0686 (8)*0.334 (5)
O11B0.3355 (4)0.5895 (5)0.0250 (4)0.0686 (8)*0.405 (4)
O11C0.4353 (7)0.5198 (7)0.0066 (7)0.0686 (8)*0.262 (4)
C10.09889 (12)0.46620 (16)0.33977 (12)0.0317 (3)
C20.04525 (11)0.40407 (15)0.22931 (12)0.0293 (3)
C30.05401 (13)0.34062 (17)0.18468 (14)0.0375 (3)
H30.0960190.3325310.2225920.045*
C40.08916 (14)0.28935 (18)0.08166 (15)0.0409 (4)
H40.1558730.2470530.0497230.049*
C50.02547 (13)0.30081 (16)0.02613 (13)0.0362 (3)
H50.0482380.2666030.0427550.043*
C60.07287 (12)0.36467 (14)0.07649 (11)0.0292 (3)
C70.15440 (13)0.38726 (15)0.03162 (12)0.0327 (3)
C80.30988 (12)0.76907 (16)0.23960 (12)0.0326 (3)
C90.41358 (12)0.69734 (17)0.30348 (12)0.0322 (3)
C100.51644 (14)0.7516 (2)0.34797 (15)0.0439 (4)
H100.5276630.8414770.3403250.053*
C110.60226 (14)0.6669 (2)0.40446 (16)0.0511 (5)
H110.6723590.7002620.4355760.061*
C120.58434 (13)0.5341 (2)0.41470 (14)0.0460 (4)
H120.6415790.4772220.4526480.055*
C130.47867 (13)0.48674 (18)0.36704 (13)0.0348 (3)
C140.44425 (15)0.34478 (19)0.36934 (15)0.0418 (4)
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
Ni10.02366 (11)0.03313 (12)0.02836 (12)0.00153 (6)0.01008 (8)0.00108 (7)
N10.0278 (5)0.0285 (5)0.0270 (5)0.0016 (4)0.0117 (4)0.0010 (4)
N20.0230 (5)0.0401 (7)0.0260 (5)0.0010 (5)0.0099 (4)0.0014 (5)
O10.0291 (5)0.0498 (7)0.0305 (5)0.0044 (4)0.0120 (4)0.0081 (4)
O20.0403 (6)0.0588 (8)0.0353 (6)0.0049 (6)0.0222 (5)0.0074 (6)
O30.0609 (8)0.0504 (7)0.0345 (6)0.0080 (6)0.0259 (6)0.0100 (5)
O40.0365 (6)0.0455 (6)0.0363 (6)0.0035 (5)0.0198 (5)0.0031 (5)
O50.0270 (5)0.0379 (6)0.0411 (6)0.0006 (4)0.0073 (4)0.0016 (5)
O60.0467 (7)0.0371 (6)0.0552 (8)0.0024 (5)0.0196 (6)0.0064 (6)
O70.0666 (10)0.0665 (10)0.0808 (12)0.0355 (9)0.0316 (9)0.0314 (9)
O80.0460 (7)0.0371 (6)0.0471 (7)0.0052 (5)0.0228 (6)0.0072 (5)
O90.0776 (11)0.0467 (8)0.0595 (9)0.0027 (8)0.0432 (9)0.0014 (7)
C10.0309 (7)0.0357 (7)0.0291 (7)0.0010 (6)0.0132 (5)0.0005 (6)
C20.0282 (6)0.0310 (6)0.0293 (6)0.0016 (5)0.0129 (5)0.0007 (5)
C30.0321 (7)0.0405 (8)0.0420 (8)0.0074 (6)0.0179 (6)0.0022 (7)
C40.0329 (7)0.0396 (8)0.0444 (9)0.0108 (6)0.0107 (7)0.0045 (7)
C50.0376 (8)0.0327 (7)0.0314 (7)0.0050 (6)0.0081 (6)0.0047 (6)
C60.0327 (6)0.0264 (6)0.0271 (6)0.0003 (5)0.0114 (5)0.0006 (5)
C70.0402 (8)0.0299 (7)0.0302 (7)0.0022 (6)0.0170 (6)0.0005 (5)
C80.0331 (7)0.0358 (7)0.0293 (6)0.0012 (6)0.0135 (5)0.0002 (6)
C90.0272 (6)0.0420 (8)0.0275 (6)0.0036 (6)0.0117 (5)0.0013 (6)
C100.0343 (8)0.0557 (10)0.0416 (9)0.0131 (7)0.0160 (7)0.0056 (8)
C110.0250 (7)0.0790 (15)0.0445 (10)0.0098 (8)0.0101 (7)0.0063 (9)
C120.0253 (7)0.0769 (13)0.0332 (8)0.0099 (8)0.0098 (6)0.0007 (8)
C130.0272 (7)0.0517 (9)0.0263 (7)0.0079 (6)0.0121 (5)0.0040 (6)
C140.0453 (9)0.0464 (9)0.0392 (8)0.0163 (7)0.0232 (7)0.0108 (7)
Geometric parameters (Å, º) top
Ni1—N11.9634 (12)O9—H9C1.16 (4)
Ni1—N21.9703 (12)O10—H10A0.93 (3)
Ni1—O12.0948 (12)O10—H10B0.89 (2)
Ni1—O82.1000 (12)O11C—O11Ci1.746 (18)
Ni1—O42.1716 (12)C1—C21.515 (2)
Ni1—O52.1986 (12)C2—C31.384 (2)
N1—C21.3289 (18)C3—C41.390 (2)
N1—C61.3352 (18)C3—H30.9300
N2—C131.329 (2)C4—C51.387 (3)
N2—C91.332 (2)C4—H40.9300
O1—C11.2634 (19)C5—C61.381 (2)
O2—C11.2460 (19)C5—H50.9300
O3—C71.2678 (19)C6—C71.504 (2)
O3—H9C1.30 (4)C8—C91.498 (2)
O4—C71.251 (2)C9—C101.385 (2)
O5—C81.2344 (19)C10—C111.390 (3)
O6—C81.286 (2)C10—H100.9300
O6—H6A0.99 (4)C11—C121.376 (3)
O7—C141.225 (2)C11—H110.9300
O8—C141.283 (2)C12—C131.392 (2)
O9—H9A0.91 (4)C12—H120.9300
O9—H9B0.91 (4)C13—C141.508 (3)
N1—Ni1—N2176.37 (5)C2—C3—C4118.18 (15)
N1—Ni1—O178.83 (5)C2—C3—H3120.9
N2—Ni1—O1104.68 (5)C4—C3—H3120.9
N1—Ni1—O8100.43 (5)C5—C4—C3120.49 (15)
N2—Ni1—O878.62 (5)C5—C4—H4119.8
O1—Ni1—O892.82 (5)C3—C4—H4119.8
N1—Ni1—O477.25 (5)C6—C5—C4117.82 (15)
N2—Ni1—O499.26 (5)C6—C5—H5121.1
O1—Ni1—O4156.04 (5)C4—C5—H5121.1
O8—Ni1—O492.82 (5)N1—C6—C5121.14 (14)
N1—Ni1—O5104.45 (5)N1—C6—C7112.22 (12)
N2—Ni1—O576.47 (5)C5—C6—C7126.63 (14)
O1—Ni1—O593.17 (5)O4—C7—O3126.03 (15)
O8—Ni1—O5155.09 (5)O4—C7—C6117.29 (13)
O4—Ni1—O591.45 (5)O3—C7—C6116.67 (14)
C2—N1—C6121.67 (13)O5—C8—O6125.60 (15)
C2—N1—Ni1118.29 (10)O5—C8—C9118.70 (14)
C6—N1—Ni1119.92 (10)O6—C8—C9115.70 (14)
C13—N2—C9121.28 (14)N2—C9—C10121.54 (16)
C13—N2—Ni1118.06 (12)N2—C9—C8111.63 (13)
C9—N2—Ni1120.65 (10)C10—C9—C8126.83 (16)
C1—O1—Ni1114.34 (10)C9—C10—C11117.57 (18)
C7—O3—H9C117.5 (18)C9—C10—H10121.2
C7—O4—Ni1113.17 (10)C11—C10—H10121.2
C8—O5—Ni1112.50 (10)C12—C11—C10120.50 (16)
C8—O6—H6A111 (2)C12—C11—H11119.7
C14—O8—Ni1114.83 (11)C10—C11—H11119.7
H9A—O9—H9B112 (3)C11—C12—C13118.57 (17)
H9A—O9—H9C116 (3)C11—C12—H12120.7
H9B—O9—H9C107 (3)C13—C12—H12120.7
H10A—O10—H10B112 (3)N2—C13—C12120.54 (17)
O2—C1—O1125.67 (15)N2—C13—C14113.68 (14)
O2—C1—C2118.33 (14)C12—C13—C14125.78 (16)
O1—C1—C2116.00 (13)O7—C14—O8126.2 (2)
N1—C2—C3120.69 (14)O7—C14—C13118.99 (19)
N1—C2—C1112.41 (12)O8—C14—C13114.80 (14)
C3—C2—C1126.89 (14)
Symmetry code: (i) x+1, y+1, z.
Hydrogen-bond geometry (Å, º) top
D—H···AD—HH···AD···AD—H···A
O9—H9C···O31.16 (4)1.30 (4)2.456 (2)178 (4)
O6—H6A···O100.99 (4)1.49 (4)2.469 (2)169 (4)
O9—H9A···O8ii0.91 (4)1.70 (4)2.610 (2)176 (3)
O10—H10A···O2iii0.93 (3)1.86 (3)2.676 (2)145 (3)
O10—H10B···O2iv0.89 (2)1.90 (3)2.745 (2)159 (3)
Symmetry codes: (ii) x, y+1/2, z1/2; (iii) x, y+3/2, z1/2; (iv) x, y+1/2, z+1/2.
 

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