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Acta Cryst. (2007). E63, m1921-m1922    [ doi:10.1107/S1600536807026359 ]

catena-Poly[[[tetra-[mu]2-aqua-heptaaqua([mu]2-benzene-1,3,5-tricarboxylato)-[mu]3-hydroxido-trinickel(II)sodium]-[mu]4-benzene-1,3,5-tricarboxylato] sesquihydrate]

Y. Yan, W.-H. Li and B.-R. Hou

Abstract top

The title coordination polymer, {[Ni3Na(OH)(C9H3O6)2(H2O)11]·1.5H2O}n, is built up from three independent NiII ions and one NaI cation bridged by benzene-2,4,6-tricarboxylate (BTC) ligands and water molecules. Three NiII ions are bridged by three bidentate carboxylate groups of three BTC ligands, two aqua ligands and one OH- unit, to form a trinuclear metal cluster. The NaI cation is bonded to the NiII cluster by two bridging water molecules. One of the three BTC ligands bridges neighbouring clusters into one-dimensional chains, which are further connected through a complex hydrogen-bonding scheme, forming a three-dimensional suprastructure. The title complex is isomorphous with the previously reported CoII complex.

Comment top

Benzenetricarboxylate (BTC) ligands are universal bridging ligands in the construction of a number of coordination networks (Yaghi et al., 1996; Wei & Han, 2005; Guo et al., 2006; Eddaoudi et al., 2001). In this paper, we present the synthesis and structural characterization of a new coordination polymer of trinuclear NiII units bridged by BTC ligands, {[Ni3Na(OH)(C9H3O6)2(H2O)11]·1.5H2O}n, (I), which was synthesized by the reaction of nickel(II) salt with H3BTC in basic conditions. The title compound is isomorphous with the CoII complex published by Cheng et al. (2004).

As shown in Fig. 1, the asymmetric unit contains three crystallographically independent NiII centers, which are all octahedrally coordinated by six O atoms, which are from two BTC carboxylate groups, one OH− unit and three aqua ligands (Table 2). The three NiII ions are bridged by three bidentate carboxylates of three BTC ligands, two aqua ligands and one OH− anion, to form a new trinuclear metal cluster. The NaI ion is coordinated by six water molecules, and the distorted octahedron is attached to the trinuclear unit though two bridging aqua ligands.

The BTC ligands exhibit two different coordination modes in (I). In the first one, the BTC ligand acts as a bidentate ligand bridging two NiII centers, while another one acts as a tetradentate ligand linking four NiII centers of neighboring trinuclear units to form a one-dimensional zigzag chain (Fig. 2). The chains are further connected into a three-dimensional framework through a complex hydrogen bonding scheme involving water molecules and carboxylate groups of BTC (Table 3 and Fig. 3). The hydrogen bonds D···A separations range from 2.597 to 3.437 Å.

Related literature top

For related literature, see: Guo et al. (2006) Yaghi et al. (1996); Wei & Han (2005); Eddaoudi et al. (2001); Cheng et al. (2004).

Experimental top

An aqueous solution (20 ml) of benzene-1,3,5-tricarboxylic acid (H3BTC) (0.96 g, 0.5 mmol) and NaOH (0.04 g, 1 mmol) was added into an aqueous solution (10 ml) of Ni(CH3CO2)2·2H2O (0.12 g, 0.5 mmol) under stirring. The resulting solution was filtered and a solution of 4,4'-bipy (0.05 g, 0.5 mmol in 15 ml e thanol) was added dropwise. After 15 days, green crystals suitable for X-ray single-crystal diffraction studies were collected by filtration and washed with ethanol. Yield: 68%.

Refinement top

A lattice water molecule with occupancy 1/2 is disordered over two sites, O13w and O14w, with 1/4 occupancy for each. The C-bonded H atoms were placed geometrically and refined with C—H bond lengths constrained to 0.93 Å and Uiso(H) = 1.2Ueq(carrier C). H atoms of water molecules and hydroxy group were clearly visible in a difference map, and were included in the refinement as riding atoms after regularizing some bond lengths [O—H in the range 0.82 to 0.97 Å] and with fixed isotropic displacement parameters: Uiso(H) = 1.2Ueq(carrier O).

Computing details top

Data collection: SMART (Siemens, 1994); cell refinement: SMART; data reduction: XPREP (Siemens, 1996); program(s) used to solve structure: SHELXS97 (Sheldrick, 1997); program(s) used to refine structure: SHELXL97 (Sheldrick, 1997); molecular graphics: SHELXTL (Siemens, 1996); software used to prepare material for publication: SHELXTL.

Figures top
[Figure 1] Fig. 1. ORTEPlike representation of the symmetry expanded local structure for (I) (25% probability ellipsoids).
[Figure 2] Fig. 2. The one-dimensional zigzag chain of the trinuclear NiII units bridged by the BTC ligands.
[Figure 3] Fig. 3. Crystal packing diagram of (I) viewed down the [100] axis, showing the complex hydrogen bonding.
catena-Poly[[[tetra-µ2-aqua-heptaaqua(µ2-benzene-1,3,5-tricarboxylato)- µ3-hydroxido-trinickel(II)sodium]-µ4-benzene-1,3,5-tricarboxylato] sesquihydrate] top
Crystal data top
[Ni3Na(OH)(C9H3O6)2(H2O)11]·1.5H2OF000 = 3472
Mr = 855.56Dx = 1.921 Mg m−3
Orthorhombic, PbcaMo Kα radiation
λ = 0.71073 Å
Hall symbol: -P 2ac 2abθ = 3.2–27.5º
a = 18.842 (5) ŵ = 2.03 mm−1
b = 14.557 (4) ÅT = 293 (2) K
c = 21.343 (6) ÅPrism, green
V = 5854 (3) Å30.18 × 0.12 × 0.10 mm
Z = 8
Data collection top
Siemens SMART CCD area-detector
diffractometer		6693 independent reflections
Radiation source: fine-focus sealed tube2994 reflections with I > 2σ(I)
Monochromator: graphiteRint = 0.133
T = 293(2) Kθmax = 27.5º
φ and ω scansθmin = 3.2º
Absorption correction: multi-scan
(SADABS; Sheldrick, 1995)		h = −24→17
Tmin = 0.712, Tmax = 0.820k = −18→18
43629 measured reflectionsl = −27→27
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)] = 0.057H-atom parameters constrained
wR(F2) = 0.127  w = 1/[σ2(Fo2) + (0.0069P)2]
where P = (Fo2 + 2Fc2)/3
S = 0.89(Δ/σ)max = 0.003
6693 reflectionsΔρmax = 0.67 e Å−3
442 parametersΔρmin = −0.64 e Å−3
Primary atom site location: structure-invariant direct methodsExtinction correction: none
Crystal data top
[Ni3Na(OH)(C9H3O6)2(H2O)11]·1.5H2OV = 5854 (3) Å3
Mr = 855.56Z = 8
Orthorhombic, PbcaMo Kα
a = 18.842 (5) ŵ = 2.03 mm−1
b = 14.557 (4) ÅT = 293 (2) K
c = 21.343 (6) Å0.18 × 0.12 × 0.10 mm
Data collection top
Siemens SMART CCD area-detector
diffractometer		6693 independent reflections
Absorption correction: multi-scan
(SADABS; Sheldrick, 1995)		2994 reflections with I > 2σ(I)
Tmin = 0.712, Tmax = 0.820Rint = 0.133
43629 measured reflections
Refinement top
R[F2 > 2σ(F2)] = 0.057442 parameters
wR(F2) = 0.127H-atom parameters constrained
S = 0.89Δρmax = 0.67 e Å−3
6693 reflectionsΔρmin = −0.64 e Å−3
Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top
xyzUiso*/UeqOcc. (<1)
Ni10.30004 (5)0.96049 (7)0.12261 (4)0.0209 (2)
Ni20.46166 (5)0.96371 (7)0.21056 (4)0.0221 (2)
Ni30.43621 (5)0.85216 (7)0.09272 (4)0.0203 (2)
Na10.4108 (2)1.2046 (2)0.12750 (16)0.0479 (10)
O10.4066 (2)0.9715 (3)0.1299 (2)0.0177 (11)
H1A0.42401.02270.10430.021*
O1W0.4691 (3)0.8171 (3)0.1864 (2)0.0231 (12)
H1WA0.51680.79240.18900.028*
H1WB0.43560.77850.20880.028*
O2W0.5213 (3)0.9412 (4)0.2905 (2)0.0386 (16)
H2WB0.54440.98740.29870.046*
H2WA0.49470.92920.31980.046*
O3W0.4550 (3)0.7222 (3)0.0684 (2)0.0298 (13)
H3WB0.41900.69160.07370.036*
H3WA0.49610.71690.05630.036*
O4W0.2878 (3)1.1036 (3)0.1260 (2)0.0302 (14)
H4B0.26421.11760.15680.036*
H4A0.26851.12790.10190.036*
O5W0.4611 (3)1.1076 (3)0.2207 (2)0.0246 (13)
H5WA0.50161.12580.22710.030*
H5WB0.43391.12250.25790.030*
O6W0.3608 (4)1.2973 (5)0.2047 (3)0.072 (2)
H6WA0.34231.34230.18830.087*
H6WB0.38461.29410.23680.087*
O7W0.3552 (3)1.2859 (4)0.0450 (2)0.0418 (16)
H7WA0.37981.28270.01340.050*
H7WB0.31611.26300.03830.050*
O8W0.4635 (3)1.1087 (4)0.0522 (2)0.0359 (15)
H8WB0.43961.10930.02010.043*
H8WA0.50371.12680.04450.043*
O9W0.5163 (4)1.2981 (5)0.1248 (3)0.087 (3)
H9WA0.54341.28180.15270.105*
H9WB0.53591.29260.09070.105*
O10W0.9046 (4)0.5735 (5)0.3553 (3)0.081 (3)
H10A0.87380.55720.38000.097*
H10B0.87990.61140.33550.097*
O110.4002 (3)0.8816 (4)0.0019 (2)0.0244 (13)
O11W0.3286 (3)0.8147 (3)0.1170 (2)0.0216 (12)
H11A0.32480.78250.15670.026*
H11B0.30400.78170.08410.026*
O120.3000 (3)0.9568 (4)0.0280 (2)0.0255 (12)
O12W0.1917 (3)0.9377 (4)0.1137 (2)0.0382 (15)
H12B0.17800.90510.14260.046*
H12C0.18260.90740.07460.046*
O130.0850 (3)0.8013 (4)−0.1728 (2)0.0396 (16)
O140.0847 (3)0.8387 (4)−0.0716 (2)0.0366 (15)
O150.3123 (3)0.7961 (4)−0.2849 (2)0.0501 (19)
O160.4126 (3)0.7897 (4)−0.2299 (2)0.0346 (15)
O210.5430 (3)0.8863 (3)0.0806 (2)0.0200 (11)
O220.5552 (3)0.9755 (3)0.1659 (2)0.0225 (12)
O230.8758 (3)0.8365 (4)0.0208 (2)0.0412 (17)
O240.7754 (3)0.7999 (3)−0.0298 (2)0.0241 (13)
O250.8776 (3)0.9416 (4)0.2330 (2)0.0346 (15)
O260.7764 (3)0.9579 (4)0.2863 (2)0.0328 (14)
C110.3022 (4)0.8840 (5)−0.0699 (3)0.0214 (17)
C120.2288 (4)0.8807 (5)−0.0723 (3)0.0202 (17)
H12A0.20270.9008−0.03790.024*
C130.1934 (4)0.8482 (5)−0.1249 (3)0.0220 (17)
C140.2331 (4)0.8259 (5)−0.1778 (3)0.0243 (18)
H14A0.21000.8074−0.21420.029*
C150.3057 (5)0.8311 (5)−0.1770 (3)0.0244 (18)
C160.3418 (4)0.8565 (5)−0.1224 (3)0.0231 (17)
H16A0.39110.8552−0.12090.028*
C170.3378 (5)0.9104 (5)−0.0088 (3)0.0238 (18)
C180.1150 (5)0.8302 (6)−0.1236 (4)0.030 (2)
C190.3468 (5)0.8048 (5)−0.2348 (4)0.032 (2)
C210.6585 (4)0.9124 (4)0.1226 (3)0.0140 (15)
C220.6952 (4)0.8773 (5)0.0710 (3)0.0198 (17)
H22A0.67010.85920.03560.024*
C230.7686 (4)0.8689 (5)0.0717 (3)0.0173 (16)
C240.8055 (4)0.8929 (4)0.1251 (3)0.0170 (16)
H24A0.85470.88840.12550.020*
C250.7701 (4)0.9238 (5)0.1788 (3)0.0188 (17)
C260.6972 (4)0.9336 (5)0.1762 (3)0.0182 (16)
H26A0.67330.95500.21140.022*
C270.5799 (4)0.9255 (5)0.1228 (3)0.0183 (16)
C280.8090 (5)0.8336 (5)0.0160 (3)0.0253 (19)
C290.8120 (4)0.9432 (5)0.2376 (3)0.0231 (18)
O13W0.5621 (14)0.9796 (16)0.4849 (11)0.071 (7)0.25
H13A0.56280.93790.51080.086*0.25
H13B0.58500.97120.45740.086*0.25
O14W0.4786 (16)0.975 (2)0.4410 (12)0.088 (9)0.25
H14B0.47820.92930.41870.105*0.25
H14C0.51060.99970.41060.105*0.25
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
Ni10.0187 (6)0.0275 (5)0.0165 (5)0.0014 (5)0.0001 (4)−0.0005 (4)
Ni20.0183 (6)0.0295 (6)0.0186 (5)−0.0004 (5)0.0007 (4)−0.0014 (4)
Ni30.0170 (5)0.0255 (5)0.0184 (5)−0.0001 (5)−0.0008 (4)−0.0022 (4)
Na10.049 (3)0.055 (2)0.040 (2)0.015 (2)−0.0016 (19)−0.0046 (18)
O10.015 (3)0.023 (3)0.016 (2)−0.002 (2)−0.005 (2)0.000 (2)
O1W0.018 (3)0.025 (3)0.026 (3)−0.002 (2)0.000 (2)0.007 (2)
O2W0.040 (4)0.053 (4)0.022 (3)−0.008 (3)−0.006 (3)0.000 (3)
O3W0.016 (3)0.033 (3)0.041 (3)−0.004 (3)−0.002 (3)−0.008 (2)
O4W0.038 (4)0.027 (3)0.026 (3)0.016 (3)0.001 (3)−0.001 (2)
O5W0.018 (3)0.030 (3)0.026 (3)−0.004 (3)0.004 (2)−0.011 (2)
O6W0.100 (7)0.070 (5)0.047 (4)0.024 (5)0.022 (4)0.013 (4)
O7W0.035 (4)0.055 (4)0.035 (3)0.002 (3)0.003 (3)−0.008 (3)
O8W0.027 (4)0.053 (4)0.027 (3)−0.008 (3)0.003 (3)0.007 (3)
O9W0.066 (6)0.111 (7)0.085 (5)−0.013 (5)0.012 (5)−0.043 (5)
O10W0.092 (7)0.067 (5)0.083 (6)−0.010 (5)0.021 (5)−0.011 (4)
O110.017 (3)0.041 (3)0.015 (3)0.001 (3)−0.004 (2)−0.003 (2)
O11W0.025 (3)0.020 (3)0.021 (3)−0.002 (2)−0.002 (2)−0.001 (2)
O120.027 (3)0.031 (3)0.018 (3)0.009 (3)−0.003 (2)−0.003 (2)
O12W0.025 (4)0.056 (4)0.034 (3)−0.004 (3)0.001 (3)−0.009 (3)
O130.026 (4)0.066 (4)0.027 (3)−0.011 (3)−0.008 (3)0.014 (3)
O140.021 (3)0.050 (4)0.039 (3)−0.004 (3)0.003 (3)−0.002 (3)
O150.048 (5)0.081 (5)0.021 (3)0.018 (4)−0.012 (3)−0.014 (3)
O160.030 (4)0.045 (4)0.029 (3)0.006 (3)0.005 (3)−0.013 (3)
O210.012 (3)0.027 (3)0.021 (3)−0.003 (2)0.000 (2)−0.004 (2)
O220.017 (3)0.029 (3)0.021 (3)−0.002 (2)0.006 (2)−0.007 (2)
O230.019 (3)0.068 (5)0.037 (3)−0.001 (3)0.007 (3)−0.024 (3)
O240.027 (3)0.029 (3)0.017 (3)0.003 (3)−0.002 (2)−0.007 (2)
O250.020 (3)0.064 (4)0.020 (3)0.000 (3)−0.005 (3)−0.004 (3)
O260.023 (3)0.059 (4)0.017 (3)0.009 (3)0.002 (2)−0.003 (3)
C110.019 (4)0.027 (4)0.018 (4)−0.007 (4)0.001 (3)0.005 (3)
C120.020 (5)0.027 (4)0.014 (3)0.000 (3)0.001 (3)0.000 (3)
C130.019 (4)0.023 (4)0.024 (4)0.005 (4)0.000 (4)0.004 (3)
C140.025 (5)0.022 (4)0.025 (4)−0.003 (4)−0.010 (4)0.001 (3)
C150.032 (5)0.026 (4)0.015 (4)−0.004 (4)−0.002 (4)−0.004 (3)
C160.020 (5)0.026 (4)0.023 (4)0.000 (4)−0.006 (3)−0.001 (3)
C170.030 (5)0.021 (4)0.021 (4)−0.007 (4)0.003 (4)0.001 (3)
C180.024 (5)0.041 (5)0.024 (4)−0.004 (4)0.002 (4)0.008 (4)
C190.042 (6)0.026 (5)0.027 (4)0.006 (4)0.006 (4)−0.003 (4)
C210.011 (4)0.016 (4)0.015 (3)0.005 (3)0.000 (3)−0.002 (3)
C220.016 (4)0.024 (4)0.019 (4)0.003 (3)−0.002 (3)−0.003 (3)
C230.012 (4)0.023 (4)0.017 (3)−0.004 (3)0.000 (3)0.005 (3)
C240.015 (4)0.020 (4)0.015 (3)0.003 (3)−0.005 (3)−0.004 (3)
C250.025 (5)0.019 (4)0.012 (3)0.000 (3)0.000 (3)0.000 (3)
C260.015 (4)0.026 (4)0.013 (3)−0.004 (3)0.008 (3)−0.001 (3)
C270.017 (4)0.025 (4)0.013 (3)−0.006 (3)0.004 (3)0.004 (3)
C280.026 (5)0.031 (5)0.019 (4)−0.001 (4)0.011 (4)−0.001 (3)
C290.021 (5)0.022 (4)0.027 (4)0.000 (4)−0.006 (4)0.001 (3)
O13W0.127 (19)0.028 (17)0.059 (16)−0.004 (15)0.020 (15)0.029 (13)
O14W0.08 (3)0.03 (2)0.16 (2)−0.005 (19)0.038 (18)0.035 (17)
Geometric parameters (Å, °) top
Ni1—O26i1.995 (5)O11W—H11A0.9700
Ni1—O122.021 (4)O11W—H11B0.9700
Ni1—O12.021 (5)O12—C171.257 (8)
Ni1—O12W2.077 (5)O12W—H12B0.8200
Ni1—O4W2.098 (5)O12W—H12C0.9595
Ni1—O11W2.193 (5)O13—C181.265 (9)
Ni2—O222.011 (5)O14—C181.253 (8)
Ni2—O12.013 (4)O15—C191.260 (9)
Ni2—O25i2.016 (5)O16—C191.263 (10)
Ni2—O2W2.069 (5)O21—C271.273 (8)
Ni2—O5W2.106 (5)O22—C271.262 (8)
Ni2—O1W2.200 (5)O23—C281.262 (9)
Ni3—O11.989 (5)O24—C281.265 (8)
Ni3—O3W1.993 (5)O25—C291.241 (9)
Ni3—O212.088 (5)O25—Ni2ii2.016 (5)
Ni3—O112.099 (5)O26—C291.255 (8)
Ni3—O1W2.155 (4)O26—Ni1ii1.995 (5)
Ni3—O11W2.162 (5)C11—C121.385 (10)
Na1—O6W2.329 (7)C11—C161.403 (10)
Na1—O8W2.348 (6)C11—C171.516 (10)
Na1—O7W2.367 (6)C12—C131.388 (9)
Na1—O9W2.410 (8)C12—H12A0.9300
Na1—O5W2.616 (6)C13—C141.394 (10)
Na1—O4W2.744 (7)C13—C181.500 (10)
O1—H1A0.9800C14—C151.370 (11)
O1W—H1WA0.9700C14—H14A0.9300
O1W—H1WB0.9700C15—C161.401 (9)
O2W—H2WB0.8200C15—C191.505 (10)
O2W—H2WA0.8201C16—H16A0.9300
O3W—H3WB0.8200C21—C261.392 (9)
O3W—H3WA0.8201C21—C221.397 (9)
O4W—H4B0.8200C21—C271.494 (10)
O4W—H4A0.7223C22—C231.389 (10)
O5W—H5WA0.8200C22—H22A0.9300
O5W—H5WB0.9699C23—C241.379 (9)
O6W—H6WA0.8200C23—C281.502 (9)
O6W—H6WB0.8194C24—C251.400 (9)
O7W—H7WA0.8200C24—H24A0.9300
O7W—H7WB0.8199C25—C261.382 (10)
O8W—H8WB0.8200C25—C291.510 (9)
O8W—H8WA0.8200C26—H26A0.9300
O9W—H9WA0.8200O13W—O14W1.83 (4)
O9W—H9WB0.8197O13W—H13A0.8200
O10W—H10A0.8200O13W—H13B0.7389
O10W—H10B0.8363O14W—H14B0.8200
O11—C171.267 (9)O14W—H14C0.9557
O26i—Ni1—O12166.8 (2)H5WA—O5W—H5WB106.5
O26i—Ni1—O198.6 (2)Na1—O6W—H6WA108.9
O12—Ni1—O194.5 (2)Na1—O6W—H6WB109.6
O26i—Ni1—O12W82.3 (2)H6WA—O6W—H6WB129.8
O12—Ni1—O12W84.5 (2)Na1—O7W—H7WA109.4
O1—Ni1—O12W175.3 (2)Na1—O7W—H7WB108.9
O26i—Ni1—O4W87.7 (2)H7WA—O7W—H7WB109.9
O12—Ni1—O4W93.5 (2)Na1—O8W—H8WB109.5
O1—Ni1—O4W91.6 (2)Na1—O8W—H8WA109.7
O12W—Ni1—O4W93.1 (2)H8WB—O8W—H8WA109.6
O26i—Ni1—O11W95.1 (2)Na1—O9W—H9WA109.5
O12—Ni1—O11W85.39 (19)Na1—O9W—H9WB109.8
O1—Ni1—O11W80.59 (18)H9WA—O9W—H9WB109.7
O12W—Ni1—O11W94.7 (2)H10A—O10W—H10B97.0
O4W—Ni1—O11W172.0 (2)C17—O11—Ni3122.3 (5)
O22—Ni2—O192.37 (19)Ni3—O11W—Ni189.96 (17)
O22—Ni2—O25i170.2 (2)Ni3—O11W—H11A113.7
O1—Ni2—O25i96.6 (2)Ni1—O11W—H11A113.7
O22—Ni2—O2W85.9 (2)Ni3—O11W—H11B113.6
O1—Ni2—O2W173.7 (2)Ni1—O11W—H11B113.6
O25i—Ni2—O2W84.7 (2)H11A—O11W—H11B110.9
O22—Ni2—O5W88.2 (2)C17—O12—Ni1129.7 (5)
O1—Ni2—O5W91.67 (19)Ni1—O12W—H12B109.4
O25i—Ni2—O5W95.4 (2)Ni1—O12W—H12C109.2
O2W—Ni2—O5W94.4 (2)H12B—O12W—H12C109.4
O22—Ni2—O1W85.17 (19)C27—O21—Ni3123.1 (4)
O1—Ni2—O1W83.52 (18)C27—O22—Ni2128.3 (5)
O25i—Ni2—O1W92.0 (2)C29—O25—Ni2ii137.1 (5)
O2W—Ni2—O1W90.26 (19)C29—O26—Ni1ii133.7 (5)
O5W—Ni2—O1W171.62 (18)C12—C11—C16119.5 (7)
O1—Ni3—O3W169.2 (2)C12—C11—C17118.8 (7)
O1—Ni3—O2196.40 (19)C16—C11—C17121.5 (7)
O3W—Ni3—O2191.3 (2)C11—C12—C13121.4 (7)
O1—Ni3—O1195.68 (19)C11—C12—H12A119.3
O3W—Ni3—O1190.6 (2)C13—C12—H12A119.3
O21—Ni3—O1198.54 (19)C12—C13—C14118.5 (7)
O1—Ni3—O1W85.27 (18)C12—C13—C18121.2 (7)
O3W—Ni3—O1W88.06 (18)C14—C13—C18120.1 (7)
O21—Ni3—O1W83.95 (19)C15—C14—C13120.8 (7)
O11—Ni3—O1W177.2 (2)C15—C14—H14A119.6
O1—Ni3—O11W82.07 (18)C13—C14—H14A119.6
O3W—Ni3—O11W89.4 (2)C14—C15—C16120.7 (7)
O21—Ni3—O11W173.16 (18)C14—C15—C19119.3 (7)
O11—Ni3—O11W88.26 (19)C16—C15—C19119.9 (8)
O1W—Ni3—O11W89.27 (18)C15—C16—C11118.8 (7)
O6W—Na1—O8W178.1 (3)C15—C16—H16A120.6
O6W—Na1—O7W93.3 (2)C11—C16—H16A120.6
O8W—Na1—O7W88.6 (2)O12—C17—O11126.2 (7)
O6W—Na1—O9W91.3 (3)O12—C17—C11115.0 (7)
O8W—Na1—O9W88.3 (2)O11—C17—C11118.8 (7)
O7W—Na1—O9W93.7 (3)O14—C18—O13124.3 (8)
O6W—Na1—O5W85.5 (2)O14—C18—C13116.6 (7)
O8W—Na1—O5W92.6 (2)O13—C18—C13118.9 (7)
O7W—Na1—O5W174.8 (3)O15—C19—O16124.0 (8)
O9W—Na1—O5W91.4 (3)O15—C19—C15117.1 (8)
O6W—Na1—O4W88.7 (2)O16—C19—C15118.8 (7)
O8W—Na1—O4W91.7 (2)C26—C21—C22118.1 (7)
O7W—Na1—O4W83.4 (2)C26—C21—C27119.3 (6)
O9W—Na1—O4W177.1 (3)C22—C21—C27122.6 (6)
O5W—Na1—O4W91.47 (19)C23—C22—C21121.1 (7)
Ni3—O1—Ni298.5 (2)C23—C22—H22A119.5
Ni3—O1—Ni1100.3 (2)C21—C22—H22A119.5
Ni2—O1—Ni1125.0 (2)C24—C23—C22119.3 (7)
Ni3—O1—H1A110.4C24—C23—C28119.0 (7)
Ni2—O1—H1A110.4C22—C23—C28121.7 (6)
Ni1—O1—H1A110.4C23—C24—C25121.2 (7)
Ni3—O1W—Ni288.23 (17)C23—C24—H24A119.4
Ni3—O1W—H1WA114.0C25—C24—H24A119.4
Ni2—O1W—H1WA114.0C26—C25—C24118.3 (6)
Ni3—O1W—H1WB113.9C26—C25—C29122.2 (6)
Ni2—O1W—H1WB113.9C24—C25—C29119.5 (7)
H1WA—O1W—H1WB111.1C25—C26—C21122.0 (6)
Ni2—O2W—H2WB109.5C25—C26—H26A119.0
Ni2—O2W—H2WA109.3C21—C26—H26A119.0
H2WB—O2W—H2WA109.7O22—C27—O21124.9 (7)
Ni3—O3W—H3WB109.5O22—C27—C21116.1 (6)
Ni3—O3W—H3WA109.8O21—C27—C21118.9 (6)
H3WB—O3W—H3WA140.7O23—C28—O24125.0 (7)
Ni1—O4W—Na1116.1 (2)O23—C28—C23115.5 (7)
Ni1—O4W—H4B109.4O24—C28—C23119.4 (7)
Na1—O4W—H4B108.5O25—C29—O26127.0 (7)
Ni1—O4W—H4A121.1O25—C29—C25116.8 (7)
Na1—O4W—H4A99.9O26—C29—C25116.2 (7)
H4B—O4W—H4A100.2O14W—O13W—H13A108.6
Ni2—O5W—Na1117.4 (2)O14W—O13W—H13B95.1
Ni2—O5W—H5WA109.5H13A—O13W—H13B114.0
Na1—O5W—H5WA106.9O13W—O14W—H14B109.5
Ni2—O5W—H5WB108.0O13W—O14W—H14C78.0
Na1—O5W—H5WB108.0H14B—O14W—H14C85.1
Symmetry codes: (i) x−1/2, y, −z+1/2; (ii) x+1/2, y, −z+1/2.
Hydrogen-bond geometry (Å, °) top
D—H···AD—HH···AD···AD—H···A
O1—H1A···O8W0.981.832.807 (7)173
O1W—H1WA···O13iii0.971.902.797 (8)152
O1W—H1WB···O16iv0.971.702.596 (7)152
O1W—H1WB···O15iv0.972.573.438 (8)149
O2W—H2WB···O10Wv0.821.992.752 (9)155
O2W—H2WA···O9Wvi0.822.262.848 (8)130
O3W—H3WB···O10Wi0.822.312.872 (8)126
O3W—H3WA···O14iii0.821.882.601 (8)145
O4W—H4B···O15vii0.822.283.049 (8)157
O4W—H4A···O24viii0.722.042.757 (7)174
O5W—H5WA···O16viii0.822.032.818 (8)160
O5W—H5WB···O13vii0.971.882.772 (7)151
O6W—H6WB···O13vii0.822.453.153 (9)145
O7W—H7WA···O14ix0.822.102.841 (8)150
O7W—H7WB···O24viii0.821.962.778 (8)174
O8W—H8WB···O21viii0.822.172.838 (7)138
O8W—H8WA···O11viii0.822.072.821 (8)153
O9W—H9WA···O16viii0.822.122.909 (10)162
O9W—H9WB···O23v0.822.323.062 (9)150
O10W—H10A···O12Wvi0.822.142.764 (9)133
O10W—H10B···O15iii0.842.142.981 (10)177
O11W—H11A···O15iv0.971.712.659 (7)166
O11W—H11B···O24x0.971.742.693 (6)165
O12W—H12C···O7Wxi0.962.012.795 (7)138
O13W—H13A···O14ii0.821.992.79 (2)168
Symmetry codes: (iii) x+1/2, −y+3/2, −z; (iv) x, −y+3/2, z+1/2; (v) −x+3/2, y+1/2, z; (vi) −x+1, y−1/2, −z+1/2; (i) x−1/2, y, −z+1/2; (vii) −x+1/2, −y+2, z+1/2; (viii) −x+1, −y+2, −z; (ix) −x+1/2, y+1/2, z; (x) x−1/2, −y+3/2, −z; (xi) −x+1/2, y−1/2, z; (ii) x+1/2, y, −z+1/2.
Table 1
Hydrogen-bond geometry (Å, °) top
D—H···AD—HH···AD···AD—H···A
O1—H1A···O8W0.981.832.807 (7)173
O1W—H1WA···O13i0.971.902.797 (8)152
O1W—H1WB···O16ii0.971.702.596 (7)152
O2W—H2WB···O10Wiii0.821.992.752 (9)155
O4W—H4B···O15iv0.822.283.049 (8)157
O4W—H4A···O24v0.722.042.757 (7)174
O5W—H5WA···O16v0.822.032.818 (8)160
O5W—H5WB···O13iv0.971.882.772 (7)151
O7W—H7WA···O14vi0.822.102.841 (8)150
O7W—H7WB···O24v0.821.962.778 (8)174
O8W—H8WA···O11v0.822.072.821 (8)153
O9W—H9WA···O16v0.822.122.909 (10)162
O9W—H9WB···O23iii0.822.323.062 (9)150
O10W—H10B···O15i0.842.142.981 (10)177
O11W—H11A···O15ii0.971.712.659 (7)166
O11W—H11B···O24vii0.971.742.693 (6)165
O13W—H13A···O14viii0.821.992.79 (2)168
Symmetry codes: (i) x+1/2, −y+3/2, −z; (ii) x, −y+3/2, z+1/2; (iii) −x+3/2, y+1/2, z; (iv) −x+1/2, −y+2, z+1/2; (v) −x+1, −y+2, −z; (vi) −x+1/2, y+1/2, z; (vii) x−1/2, −y+3/2, −z; (viii) x+1/2, y, −z+1/2.
references
References top

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