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Acta Cryst. (2003). E59, m507-m509
https://doi.org/10.1107/S1600536803013448
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Aqua(4,4-bi­pyridine)­phthalatonickel(II) trihydrate

S.-Y. Yang, L.-S. Long, R.-B. Huang, L.-S. Zheng and S. W. Ng
The (H2O)(C10H8N2)Ni(C8H4O4) portion of the title compound, [Ni(C8H4O4)(C10H8N2)(H2O)]·3H2O, adopts a layer architecture in which the dianionic entity chelates to the Ni atom [Ni-O = 2.053 (5) and 2.056 (4) Å, and O-Ni-O = 91.5 (2)°]. The two chelating O atoms, a water mol­ecule [Ni-O = 2.083 (5) Å], the carboxyl O atom from an adjacent dianion, and the N atoms of two 4,4'-bi­pyridine heterocycles comprise the octahedron around the Ni atom. Adjacent layers are linked into a network motif by hydrogen bonds.
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Supporting information

cif

Crystallographic Information File (CIF) https://doi.org/10.1107/S1600536803013448/cv6200sup1.cif
Contains datablocks I, global

hkl

Structure factor file (CIF format) https://doi.org/10.1107/S1600536803013448/cv6200Isup2.hkl
Contains datablock I

CCDC reference: 217387

checkCIF report

Key indicators

  • Single-crystal X-ray study
  • T = 298 K
  • Mean [sigma](C-C) = 0.010 Å
  • R factor = 0.060
  • wR factor = 0.153
  • Data-to-parameter ratio = 11.2

checkCIF results

No syntax errors found

ADDSYM reports no extra symmetry


Amber Alert Alert Level B:



ABSTM_02  Alert B The ratio of expected to reported Tmax/Tmin(RR') is < 0.75
          Tmin and Tmax reported:      0.455     0.939
          Tmin' and Tmax expected:      0.703     0.938
          RR' =      0.646
          Please check that your absorption correction is appropriate.

PLAT_420  Alert B D-H Without Acceptor       O2W    -   H2W1   ...          ?

PLAT_420  Alert B D-H Without Acceptor       O3W    -   H3W2   ...          ?

PLAT_420  Alert B D-H Without Acceptor       O4W    -   H4W2   ...          ?

General Notes



REFLT_03
         From the CIF: _diffrn_reflns_theta_max           30.00
         From the CIF: _reflns_number_total               2936
         Count of symmetry unique reflns         2947
         Completeness (_total/calc)             99.63%
         TEST3: Check Friedels for noncentro structure
         Estimate of Friedel pairs measured         0
         Fraction of Friedel pairs measured     0.000
         Are heavy atom types Z>Si present          yes
          WARNING: Large fraction of Friedel related reflns may
                   be needed to determine absolute structure


 0 Alert Level A = Potentially serious problem

 4 Alert Level B = Potential problem

 0 Alert Level C = Please check
Comment top

In our studies on the complexes of transition metal benzenedicarboxylates, we have documented the 4,4'-bipyridine adduct of nickel(II) terephthalate (Yang et al., 2003). The use of phthalic anhydride as the reagent in place of terephthalic acid in the synthesis afforded the analogous nickel phthalate, but the compound crystallizes with four water molecules, one of which is coordinated to the Ni atom (Fig. 1 and Table 1). In the (H2O)(C10H8N2)Ni(C8H4O4) unit, the phthalate dianion chelates to the Ni atom [Ni—O = 2.053 (5) and 2.056 (4) Å, and O—Ni—O = 91.5 (2)°]. The two chelating O atoms, a water molecule [Ni—O = 2.083 (5) Å], the carboxyl O atom from an adjacent dianion, and the N atoms of two 4,4'-bipyridine heterocycles comprise the octahedron around the Ni atom. The dianion links adjacent Ni atoms into a chain, and adjacent chains are held together through the space heterocycle into layers (Fig. 2). Adjacent layers are linked into a network motif by hydrogen bonds (Table 2). The dianion is only monodentate in the 2,2'-bipyridine adduct of nickel phthalate, which exists as a triaqua monohydrate (Poleti et al., 1990).

Experimental top

The compound was synthesized hydrothermally from nickel nitrate hexahydrate (0.29 g, 1 mmol), phthalic anhydride (0.16 g, 1 mmol), 4,4'-bipyridine (0.16 g, 1 mmol) and sodium hydroxide (0.08 g, 2 mmol) in water (18 ml). The mixture was placed into a 20 ml Teflon-lined stainless-steel vessel, which was heated to 443 K for 120 h. The vessel was cooled to room temperature at 5 K h−1. The compound separated from the solution as fine crystals.

Refinement top

H atoms were generated geometrically (C—H = 0.93 Å) and were included in the subsequent refinement in the riding-model approximation with Uiso(H) = 1.2Ueq(C). The water H atoms were found by using the HYDROGEN (Nardelli, 1999) option in the WinGX suite (Farrugia, 1999). These were not refined; their displacement parameters were set at 0.05 Å2.

Computing details top

Data collection: CAD-4 Software (Enraf-Nonius, 1988); cell refinement: CAD-4 Software; data reduction: XCAD4 (Harms, 1997); program(s) used to solve structure: SHELXS97 (Sheldrick, 1997); program(s) used to refine structure: SHELXL97 (Sheldrick, 1997); molecular graphics: ORTEPII (Johnson, 1976); software used to prepare material for publication: SHELXL97.

Figures top
[Figure 1] Fig. 1. ORTEPII (Johnson, 1976) plot of a fragment of the structure of the title compound at the 50% probability level. H atoms are drawn as spheres of arbitrary radii. [Symmetry codes: (i) x, 1 − y, z; (ii) x, y, 1 + z.]
[Figure 2] Fig. 2. Layer structure of the title compound. The lattice water molecules are not shown.
Aqua(4,4-bipyridine)phthalatonickel(II) trihydrate top
Crystal data top
[Ni(C8H4O4)(C10H8N2)(H2O)]·3H2OF(000) = 468
Mr = 451.07Dx = 1.578 Mg m−3
Monoclinic, P21Mo Kα radiation, λ = 0.71073 Å
a = 11.134 (2) ÅCell parameters from 25 reflections
b = 8.379 (2) Åθ = 12.0–14.0°
c = 11.265 (2) ŵ = 1.07 mm−1
β = 115.39 (3)°T = 298 K
V = 949.4 (3) Å3Plate, green
Z = 20.32 × 0.29 × 0.06 mm
Data collection top
Enraf-Nonius CAD-4
diffractometer		2171 reflections with I > 2σ(I)
Radiation source: fine-focus sealed tubeRint = 0.059
Graphite monochromatorθmax = 30.0°, θmin = 2.0°
ω scansh = 0→15
Absorption correction: empirical (using intensity measurements)
via ψ scan (North et al., 1968)		k = 0→11
Tmin = 0.455, Tmax = 0.939l = −15→14
3070 measured reflections2 standard reflections every 60 min
2936 independent reflections intensity decay: none
Refinement top
Refinement on F2Secondary atom site location: difference Fourier map
Least-squares matrix: fullHydrogen site location: inferred from neighbouring sites
R[F2 > 2σ(F2)] = 0.060H-atom parameters constrained
wR(F2) = 0.153 w = 1/[σ2(Fo2) + (0.0777P)2]
where P = (Fo2 + 2Fc2)/3
S = 1.03(Δ/σ)max = 0.03
2936 reflectionsΔρmax = 0.62 e Å−3
262 parametersΔρmin = −0.64 e Å−3
1 restraintAbsolute structure: Flack & Schwarzenbach (1988)
Primary atom site location: structure-invariant direct methodsAbsolute structure parameter: 0.00 (3)
Crystal data top
[Ni(C8H4O4)(C10H8N2)(H2O)]·3H2OV = 949.4 (3) Å3
Mr = 451.07Z = 2
Monoclinic, P21Mo Kα radiation
a = 11.134 (2) ŵ = 1.07 mm−1
b = 8.379 (2) ÅT = 298 K
c = 11.265 (2) Å0.32 × 0.29 × 0.06 mm
β = 115.39 (3)°
Data collection top
Enraf-Nonius CAD-4
diffractometer		2171 reflections with I > 2σ(I)
Absorption correction: empirical (using intensity measurements)
via ψ scan (North et al., 1968)		Rint = 0.059
Tmin = 0.455, Tmax = 0.9392 standard reflections every 60 min
3070 measured reflections intensity decay: none
2936 independent reflections
Refinement top
R[F2 > 2σ(F2)] = 0.060H-atom parameters constrained
wR(F2) = 0.153Δρmax = 0.62 e Å−3
S = 1.03Δρmin = −0.64 e Å−3
2936 reflectionsAbsolute structure: Flack & Schwarzenbach (1988)
262 parametersAbsolute structure parameter: 0.00 (3)
1 restraint
Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top
xyzUiso*/Ueq
Ni10.85558 (7)0.50005 (9)0.91180 (6)0.0200 (2)
O10.8954 (5)0.7404 (6)0.9307 (4)0.026 (1)
O20.9420 (4)0.9772 (6)1.0274 (4)0.025 (1)
O30.5322 (6)0.7523 (8)0.7245 (5)0.056 (2)
O40.6542 (4)0.5418 (5)0.8217 (4)0.027 (1)
O1w0.8144 (5)0.2564 (6)0.8959 (4)0.034 (1)
O2w0.6123 (8)0.0756 (9)0.7096 (7)0.079 (2)
O3w0.633 (1)0.049 (2)0.475 (1)0.146 (5)
O4w0.412 (1)0.240 (2)0.516 (1)0.165 (5)
N10.8702 (5)0.4862 (9)1.1030 (4)0.025 (1)
N20.8460 (4)0.512 (1)1.7206 (4)0.026 (1)
C10.8712 (6)0.8514 (8)0.9919 (5)0.021 (1)
C20.7571 (6)0.8385 (8)1.0286 (6)0.026 (1)
C30.7726 (7)0.909 (1)1.1465 (7)0.036 (2)
C40.6773 (8)0.889 (1)1.1949 (7)0.042 (2)
C50.5662 (8)0.805 (1)1.1237 (7)0.045 (2)
C60.5455 (6)0.7411 (9)1.0045 (7)0.035 (2)
C70.6413 (6)0.7576 (8)0.9560 (6)0.027 (1)
C80.6107 (6)0.6764 (9)0.8250 (6)0.027 (1)
C90.7668 (7)0.432 (1)1.1187 (6)0.033 (2)
C100.7576 (6)0.435 (1)1.2374 (6)0.034 (2)
C110.8640 (5)0.496 (1)1.3483 (5)0.026 (1)
C120.9754 (6)0.5424 (9)1.3329 (6)0.034 (2)
C130.9739 (6)0.5369 (7)1.2110 (5)0.027 (2)
C140.7780 (7)0.404 (1)1.6307 (6)0.039 (2)
C150.7801 (8)0.395 (1)1.5076 (7)0.040 (2)
C160.8569 (5)0.504 (1)1.4766 (5)0.027 (1)
C170.9257 (7)0.615 (1)1.5707 (6)0.033 (2)
C180.9177 (7)0.6158 (9)1.6887 (6)0.031 (2)
H1w10.85470.18880.95730.050*
H1w20.74150.21510.84150.050*
H2w10.55700.11830.73970.050*
H2w20.6176−0.02260.73480.050*
H3w10.6102−0.05250.45570.050*
H3w20.71710.04220.52870.050*
H4w10.49170.23200.51520.050*
H4w20.36600.16180.46280.050*
H30.84770.97011.19370.043*
H40.69020.93281.27530.050*
H50.50290.78941.15600.054*
H60.46700.68660.95530.042*
H90.69590.39011.04590.039*
H100.68190.39681.24330.041*
H121.05090.57711.40490.041*
H131.04950.57031.20260.033*
H140.72680.33001.65050.047*
H150.73050.31801.44710.048*
H170.97810.69021.55430.040*
H180.96500.69341.74990.037*
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
Ni10.0263 (3)0.0231 (3)0.0141 (3)−0.0001 (4)0.0122 (2)0.0004 (4)
O10.036 (2)0.021 (2)0.028 (2)−0.001 (2)0.022 (2)−0.004 (2)
O20.027 (2)0.024 (3)0.026 (2)−0.001 (2)0.013 (2)−0.004 (2)
O30.064 (4)0.046 (3)0.036 (3)0.014 (3)0.002 (3)−0.001 (3)
O40.027 (2)0.029 (3)0.028 (2)0.003 (2)0.014 (2)−0.001 (2)
O1w0.037 (2)0.028 (3)0.031 (2)0.000 (2)0.010 (2)0.005 (2)
O2w0.088 (5)0.052 (4)0.074 (5)−0.015 (4)0.014 (4)0.006 (4)
O3w0.18 (1)0.13 (1)0.105 (7)−0.055 (9)0.037 (7)0.008 (7)
O4w0.16 (1)0.14 (1)0.19 (1)−0.03 (1)0.073 (9)0.01 (1)
N10.031 (2)0.030 (3)0.020 (2)0.001 (3)0.016 (2)0.001 (3)
N20.028 (2)0.034 (3)0.018 (2)−0.001 (3)0.013 (2)−0.002 (3)
C10.023 (3)0.025 (3)0.013 (2)0.001 (2)0.006 (2)0.005 (2)
C20.027 (3)0.029 (3)0.026 (3)0.004 (3)0.015 (2)−0.002 (3)
C30.035 (3)0.047 (4)0.034 (3)0.003 (3)0.023 (3)−0.006 (3)
C40.049 (4)0.054 (5)0.036 (4)0.006 (4)0.031 (3)−0.008 (3)
C50.044 (4)0.061 (5)0.049 (4)0.012 (4)0.037 (3)0.010 (4)
C60.029 (3)0.036 (4)0.049 (4)−0.005 (3)0.026 (3)0.001 (3)
C70.026 (3)0.027 (3)0.033 (3)0.005 (3)0.018 (2)0.003 (3)
C80.023 (3)0.035 (4)0.026 (3)−0.002 (3)0.012 (2)−0.001 (3)
C90.039 (4)0.044 (4)0.019 (3)−0.004 (3)0.017 (3)−0.005 (3)
C100.030 (3)0.057 (4)0.021 (3)−0.011 (3)0.017 (3)−0.002 (3)
C110.038 (3)0.030 (3)0.016 (2)0.003 (4)0.018 (2)0.002 (4)
C120.033 (3)0.054 (5)0.017 (2)−0.010 (3)0.014 (2)−0.008 (3)
C130.033 (3)0.032 (4)0.021 (2)−0.005 (3)0.015 (2)0.004 (2)
C140.054 (4)0.048 (4)0.018 (3)−0.022 (4)0.019 (3)−0.002 (3)
C150.063 (5)0.044 (4)0.024 (3)−0.022 (4)0.029 (3)−0.012 (3)
C160.032 (3)0.036 (3)0.019 (2)−0.006 (4)0.017 (2)−0.004 (4)
C170.044 (4)0.039 (4)0.025 (3)−0.014 (3)0.022 (3)−0.003 (3)
C180.043 (4)0.039 (4)0.016 (3)−0.012 (3)0.017 (3)−0.007 (3)
Geometric parameters (Å, º) top
Ni1—O12.053 (5)C12—C131.367 (8)
Ni1—O2i2.065 (4)C14—C151.398 (9)
Ni1—O42.056 (4)C15—C161.39 (1)
Ni1—O1w2.083 (5)C16—C171.37 (1)
Ni1—N12.093 (4)C17—C181.370 (8)
Ni1—N2ii2.112 (4)O1w—H1w10.86
O1—C11.254 (8)O1w—H1w20.85
O2—C11.273 (8)O2w—H2w10.90
O3—C81.266 (8)O2w—H2w20.87
N1—C91.317 (8)O3w—H3w10.88
N1—C131.337 (8)O3w—H3w20.87
N2—C141.328 (9)O4w—H4w10.89
N2—C181.332 (9)O4w—H4w20.89
C1—C21.499 (8)C3—H30.93
C2—C71.374 (9)C4—H40.93
C2—C31.394 (9)C5—H50.93
C3—C41.40 (1)C6—H60.93
O4—C81.234 (8)C9—H90.93
C4—C51.35 (1)C10—H100.93
C5—C61.37 (1)C12—H120.93
C7—C81.525 (9)C13—H130.93
C9—C101.384 (8)C14—H140.93
C10—C111.399 (9)C15—H150.93
C11—C121.380 (8)C17—H170.93
C11—C161.482 (6)C18—H180.93
O1—Ni1—O2i84.3 (2)C12—C11—C10117.0 (5)
O1—Ni1—O491.5 (2)C12—C11—C16122.5 (5)
O1—Ni1—O1w178.9 (2)C10—C11—C16120.5 (5)
O1—Ni1—N191.7 (2)C13—C12—C11119.5 (6)
O1—Ni1—N2ii88.5 (3)N1—C13—C12123.9 (6)
O2i—Ni1—O4169.7 (2)N2—C14—C15123.0 (6)
O2i—Ni1—O1w96.1 (2)C16—C15—C14119.3 (6)
O2i—Ni1—N193.6 (2)C17—C16—C15116.7 (5)
O2i—Ni1—N2ii85.0 (2)C17—C16—C11122.5 (6)
O4—Ni1—O1w88.4 (2)C15—C16—C11120.9 (6)
O4—Ni1—N196.0 (2)C18—C17—C16120.4 (6)
O4—Ni1—N2ii85.5 (2)N2—C18—C17123.7 (6)
O1w—Ni1—N187.2 (2)Ni1—O1w—H1w1124
O1w—Ni1—N2ii92.6 (3)Ni1—O1w—H1w2124
N1—Ni1—N2ii178.5 (2)H1w1—O1w—H1w2109
C1—O1—Ni1134.2 (4)H2w1—O2w—H2w2103
C1—O2—Ni1iii128.4 (4)H3w1—O3w—H3w2103
C8—O4—Ni1120.0 (4)H4w1—O4w—H4w2103
C9—N1—C13116.8 (5)C2—C3—H3119.4
C9—N1—Ni1118.1 (4)C4—C3—H3119.4
C13—N1—Ni1125.0 (4)C5—C4—H4120.4
C14—N2—C18116.8 (5)C3—C4—H4120.4
C14—N2—Ni1iv120.6 (5)C4—C5—H5119.6
C18—N2—Ni1iv122.1 (4)C6—C5—H5119.6
O1—C1—O2122.5 (5)C5—C6—H6119.7
O1—C1—C2120.3 (6)C7—C6—H6119.7
O2—C1—C2117.1 (5)N1—C9—H9118.2
C7—C2—C3118.4 (6)C10—C9—H9118.2
C7—C2—C1124.2 (5)C9—C10—H10120.5
C3—C2—C1117.3 (6)C11—C10—H10120.5
C2—C3—C4121.2 (7)C13—C12—H12120.3
C5—C4—C3119.2 (7)C11—C12—H12120.3
C4—C5—C6120.7 (7)N1—C13—H13118.0
C5—C6—C7120.7 (7)C12—C13—H13118.0
C2—C7—C6119.6 (6)N2—C14—H14118.5
C2—C7—C8124.0 (5)C15—C14—H14118.5
C6—C7—C8116.3 (6)C16—C15—H15120.3
O4—C8—O3124.2 (6)C14—C15—H15120.3
O4—C8—C7120.6 (6)C18—C17—H17119.8
O3—C8—C7115.1 (6)C16—C17—H17119.8
N1—C9—C10123.7 (6)N2—C18—H18118.1
C9—C10—C11118.9 (6)C17—C18—H18118.1
O4—Ni1—O1—C163.6 (6)C1—C2—C7—C8−3 (1)
O2i—Ni1—O1—C1−125.8 (6)C5—C6—C7—C20 (1)
N1—Ni1—O1—C1−32.4 (6)C5—C6—C7—C8177.5 (7)
N2ii—Ni1—O1—C1149.1 (6)Ni1—O4—C8—O3127.4 (6)
O1—Ni1—O4—C8−13.5 (5)Ni1—O4—C8—C7−57.6 (7)
O2i—Ni1—O4—C8−79 (1)C2—C7—C8—O482.2 (9)
O1w—Ni1—O4—C8165.3 (5)C6—C7—C8—O4−95.3 (7)
N1—Ni1—O4—C878.3 (5)C2—C7—C8—O3−102.3 (8)
N2ii—Ni1—O4—C8−102.0 (5)C6—C7—C8—O380.2 (8)
O1—Ni1—N1—C9122.3 (6)C13—N1—C9—C104 (1)
O4—Ni1—N1—C930.6 (6)Ni1—N1—C9—C10−172.1 (6)
O2i—Ni1—N1—C9−153.4 (6)N1—C9—C10—C11−1 (1)
O1w—Ni1—N1—C9−57.4 (6)C9—C10—C11—C12−3 (1)
O1—Ni1—N1—C13−53.6 (6)C9—C10—C11—C16178.9 (7)
O4—Ni1—N1—C13−145.2 (6)C10—C11—C12—C134 (1)
O2i—Ni1—N1—C1330.8 (6)C16—C11—C12—C13−178.1 (7)
O1w—Ni1—N1—C13126.8 (6)C9—N1—C13—C12−3 (1)
Ni1—O1—C1—O2154.7 (4)Ni1—N1—C13—C12172.7 (5)
Ni1—O1—C1—C2−24.0 (8)C11—C12—C13—N1−1 (1)
Ni1iii—O2—C1—O1−34.6 (8)C18—N2—C14—C150 (1)
Ni1iii—O2—C1—C2144.2 (4)Ni1iv—N2—C14—C15−172.8 (6)
O1—C1—C2—C7−31.5 (9)N2—C14—C15—C161 (1)
O2—C1—C2—C7149.7 (6)C14—C15—C16—C17−1 (1)
O1—C1—C2—C3146.2 (6)C14—C15—C16—C11178.6 (7)
O2—C1—C2—C3−32.6 (8)C12—C11—C16—C1730 (1)
C7—C2—C3—C44 (1)C10—C11—C16—C17−152.4 (9)
C1—C2—C3—C4−173.4 (7)C12—C11—C16—C15−149.4 (9)
C2—C3—C4—C5−2 (1)C10—C11—C16—C1528 (1)
C3—C4—C5—C6−1 (1)C15—C16—C17—C180 (1)
C4—C5—C6—C72 (1)C11—C16—C17—C18−179.0 (7)
C3—C2—C7—C6−3 (1)C14—N2—C18—C17−1 (1)
C1—C2—C7—C6174.6 (6)Ni1iv—N2—C18—C17172.2 (6)
C3—C2—C7—C8179.5 (7)C16—C17—C18—N21 (1)
Symmetry codes: (i) −x+2, y−1/2, −z+2; (ii) x, y, z−1; (iii) −x+2, y+1/2, −z+2; (iv) x, y, z+1.
Hydrogen-bond geometry (Å, º) top
D—H···AD—HH···AD···AD—H···A
O1w—H1w2···O2w0.851.952.778 (9)162
O1w—H1w1···O2v0.862.012.807 (7)154
O2w—H2w2···O3v0.872.092.88 (1)151
O3w—H3w1···O4wvi0.881.802.64 (2)158
O4w—H4w1···O2w0.892.402.73 (2)102
O4w—H4w1···O3w0.892.383.14 (2)142
Symmetry codes: (v) x, y−1, z; (vi) −x+1, y−1/2, −z+1.

Experimental details

Crystal data
Chemical formula[Ni(C8H4O4)(C10H8N2)(H2O)]·3H2O
Mr451.07
Crystal system, space groupMonoclinic, P21
Temperature (K)298
a, b, c (Å)11.134 (2), 8.379 (2), 11.265 (2)
β (°) 115.39 (3)
V (Å3)949.4 (3)
Z2
Radiation typeMo Kα
µ (mm−1)1.07
Crystal size (mm)0.32 × 0.29 × 0.06
Data collection
DiffractometerEnraf-Nonius CAD-4
diffractometer
Absorption correctionEmpirical (using intensity measurements)
via ψ scan (North et al., 1968)
Tmin, Tmax0.455, 0.939
No. of measured, independent and
observed [I > 2σ(I)] reflections		3070, 2936, 2171
Rint0.059
(sin θ/λ)max (Å−1)0.703
Refinement
R[F2 > 2σ(F2)], wR(F2), S 0.060, 0.153, 1.03
No. of reflections2936
No. of parameters262
No. of restraints1
H-atom treatmentH-atom parameters constrained
Δρmax, Δρmin (e Å−3)0.62, −0.64
Absolute structureFlack & Schwarzenbach (1988)
Absolute structure parameter0.00 (3)

Computer programs: CAD-4 Software (Enraf-Nonius, 1988), CAD-4 Software, XCAD4 (Harms, 1997), SHELXS97 (Sheldrick, 1997), SHELXL97 (Sheldrick, 1997), ORTEPII (Johnson, 1976), SHELXL97.

Selected geometric parameters (Å, º) top
Ni1—O12.053 (5)Ni1—O1w2.083 (5)
Ni1—O2i2.065 (4)Ni1—N12.093 (4)
Ni1—O42.056 (4)Ni1—N2ii2.112 (4)
O1—Ni1—O2i84.3 (2)O2i—Ni1—N2ii85.0 (2)
O1—Ni1—O491.5 (2)O4—Ni1—O1w88.4 (2)
O1—Ni1—O1w178.9 (2)O4—Ni1—N196.0 (2)
O1—Ni1—N191.7 (2)O4—Ni1—N2ii85.5 (2)
O1—Ni1—N2ii88.5 (3)O1w—Ni1—N187.2 (2)
O2i—Ni1—O4169.7 (2)O1w—Ni1—N2ii92.6 (3)
O2i—Ni1—O1w96.1 (2)N1—Ni1—N2ii178.5 (2)
O2i—Ni1—N193.6 (2)
Symmetry codes: (i) −x+2, y−1/2, −z+2; (ii) x, y, z−1.
Hydrogen-bond geometry (Å, º) top
D—H···AD—HH···AD···AD—H···A
O1w—H1w2···O2w0.851.952.778 (9)162
O1w—H1w1···O2iii0.862.012.807 (7)154
O2w—H2w2···O3iii0.872.092.88 (1)151
O3w—H3w1···O4wiv0.881.802.64 (2)158
O4w—H4w1···O2w0.892.402.73 (2)102
O4w—H4w1···O3w0.892.383.14 (2)142
Symmetry codes: (iii) x, y−1, z; (iv) −x+1, y−1/2, −z+1.
 

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