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The title nickel(II) coordination polymer, viz. poly[[bis­(1,10-phenanthroline)tris­(μ3-1,4-phenyl­enediacetato)trinickel(II)] dihydrate], {[Ni3(C10H8O4)3(C12H8N2)2]·2H2O}n, consists of linear trinuclear building blocks with two crystallographically unique Ni atoms. One NiII atom and the geometric centre of one 1,4-phenyl­enediacetate ligand in the trinuclear unit both lie on inversion centres, while the other unique NiII atom lies near the inversion centre, together with another 1,4-phenyl­enediacetate ligand. Each pair of adjacent trinuclear units is bridged by 1,4-phenyl­enediacetate ligands, forming two kinds of infinite chains along the a and b axes, respectively. These two kinds of chains crosslink to yield a two-dimensional network in the ab plane. The two-dimensional sheets further stack along the c axis via π–π stacking inter­actions and hydrogen bonds, forming a three-dimensional supramolecular structure.

Supporting information

cif

Crystallographic Information File (CIF) https://doi.org/10.1107/S0108270105042575/av1273sup1.cif
Contains datablocks global, I

hkl

Structure factor file (CIF format) https://doi.org/10.1107/S0108270105042575/av1273Isup2.hkl
Contains datablock I

CCDC reference: 299619

Comment top

The rational design of high-dimensional metal–organic frameworks has attracted much attention, owing to their fascinating framework structures and their potential applications as functional solid materials, such as gas storage, heterogeneous catalysis and magnetic materials (Kitaura et al., 2002; Seo et al., 2000; Pavlishchuk et al., 2001; Swiegers et al., 2000; Hagrman et al., 1999). Among the linker molecules, carboxylic acids with aromatic rings have been extensively studied because of their versatile properties. Such work has usually concentrated on rigid aromatic carboxylic acids, such as 1,4-dicarboxylic benzoic acid and 1,2,4-tricarboxylic benzoic acid (Stepanow et al., 2004; Rosi et al., 2003). The use of much more flexible aromatic carboxylic acids, such as 1,4-phenylenediacetic acids (H2PDA) (Lin et al., 2005; Babb et al., 2003), is rare. Metal–organic frameworks assembled with 1,4-phenylenediacetic acids may show much more interesting properties. It is also interesting to investigate the structural changes while such compounds are functioning as solid materials. In this work, we introduce an ancillary ligand of 1,10-phenanthroline (phen) to tune the structure. Therefore, we report here the synthesis and X-ray structure of the title complex, {[Ni3(phen)2(PDA)3]·2H2O}n, (I), which exhibits a two-dimensional network structure assembled from NiII cations and 1,4-phenylenediacetate anions via two kinds of cross-linked one-dimensional chains.

Single-crystal X-ray diffraction analysis reveals that compound (I) consists of trinuclear nickel building blocks, [Ni3(phen)2(PDA)3] (Fig. 1), in which atom Ni1 and the geometric centre of one PDA2− ligand both lie on inversion centres. Another crystallographically unique NiII atom (Ni2) and another PDA2− ligand are located near the inversion centre. Both crystallographically unique NiII atoms (Ni1 and Ni2) have distorted octahedral coordination environments. Atom Ni1 is coordinated to six carboxylate O atoms from six PDA2− ligands, with Ni—O bond lengths in the range 2.031 (2)–2.104 (2) Å and the O—Ni1—O bond angles varying from 85.27 (9) to 180.0° (Table 1). Atom Ni2 is coordinated to two N atoms from one phen molecule and four carboxylate O atoms from three carboxylate groups of PDA2− ligands, with the Ni—N and Ni—O bond lengths in the ranges 2.071 (3)–2.089 (3) and 1.990 (2)–2.268 (2) Å, respectively. The O—Ni2—O bond angles range from 60.31 (8) to 159.39 (9)°. These carboxylate groups of the 1,4-phenylenediacetate ligands show two types of coordination mode. One type of carboxylate group chelates to one NiII atom and, at the same time, affords one of the carboxylate O atoms to bridge another NiII atom. The other type of carboxylate group acts simply as a bidentate bridge connecting two NiII atoms. Therefore, two Ni2 atoms are bridged to one Ni1 atom via six bridging carboxylate groups, resulting in the formation of a linear trinuclear nickel unit with an Ni1···Ni2 separation of 3.4714 (7) Å.

Each pair of neighbouring trinuclear [Ni3(phen)2(PDA)3] units is connected by two PDA2− ligands to form an infinite coordination chain along the a axis. The shortest Ni1···Ni1 or Ni2···Ni2 separation in this chain is 10.708 (3) Å. Alternatively, another kind of one-dimensional coordination chain is constructed via the bridging of each pair of adjacent trinuclear [Ni3(phen)2(PDA)3] units by one PDA2− ligand along the b axis. The shortest Ni1···Ni1 or Ni2···Ni2 separation in this chain is 11.172 (3) Å. The two types of infinite chains cross-link in the ab plane to yield a two-dimensional network, as shown in Fig. 2. This differs from the reported structures of 1,4-phenylenediacetate complexes, which exhibit only one-dimensional infinite chains (Lin et al., 2005; Babb et al., 2003).

As shown in Fig. 3, 1,10-phenanthroline molecules from adjacent two-dimensional sheets are parallel to each other and partly overlap in a head-to-tail mode with a separation of 3.4296 Å, indicating significant ππ stacking effects. These ππ stacking interactions between 1,10-phenanthroline molecules lead to the formation of a three-dimensional supramolecular network by the stacking of two-dimensional sheets along the c axis. Free water molecules in the structure interact with adjacent two-dimensional sheets by formation of hydrogen bonds (Table 2), further stabilizing the three-dimensional supramolecular structure.

Experimental top

To a mixture of NiCl2·6H2O (0.0951 g, 0.4 mmol), 1,4-phenylenediacetic acid (0.1572 g, 0.8 mmol), NaOH (0.064 g, 1.6 mmol) and phen (0.0793 g, 0.4 mmol), placed in a 23 ml Teflon-lined autoclave, were added distilled water (8 ml) and ethanol (2 ml). The mixture was then heated at 433 K for 200 h. The autoclave was then cooled over a period of 48 h and the resulting green crystals of (I) were separated from the solution and dried. Elemental analysis for C54H44N4Ni3O14, calculated: C 56.45, H 3.86, N 4.88%; found: C 56.47, H 3.65, N 4.24%.

Refinement top

H atoms of water molecules were located in a difference Fourier map. During refinement, O—H and H···H distances were restrained to ensure a reasonable geometry for the water molecules. H atoms on C atoms were placed in calculated positions, with C—H = 0.93 Å in aromatic rings and 0.97 Å for others, and refined in riding mode with Uiso(H) = 1.2Ueq(C).

Computing details top

Data collection: SMART (Bruker, 1998); cell refinement: SMART; data reduction: SAINT (Bruker, 1998); program(s) used to solve structure: SHELXS97 (Sheldrick, 1997); program(s) used to refine structure: SHELXL97 (Sheldrick, 1997); molecular graphics: SHELXTL (Bruker, 1997); software used to prepare material for publication: SHELXTL.

Figures top
[Figure 1] Fig. 1. A view of the molecular structure of (I), with the atom-numbering scheme and 30% probability displacement ellipsoids. For clarity, H atoms have been omitted. Atoms labelled with the suffixes AC are at the symmetry positions (−x + 1, −y + 1, −z + 2), (x − 1, y, z) and (−x + 2, −y + 1, −z + 2), respectively.
[Figure 2] Fig. 2. The two-dimensional network in the structure of (I). For clarity, H atoms and 1,10-phenanthroline molecules have been omitted.
[Figure 3] Fig. 3. A packing diagram of the two-dimensional sheets along the c axis. Dashed lines indicate O—H···O hydrogen bonds.
poly[[bis(1,10-phenanthroline)tris(µ3-1,4-phenylenediacetato)trinickel(II)] dihydrate] top
Crystal data top
[Ni3(C10H8O4)3(C12H8N2)2]·2H2OZ = 1
Mr = 1149.06F(000) = 592
Triclinic, P1Dx = 1.604 Mg m3
Hall symbol: -P 1Mo Kα radiation, λ = 0.71073 Å
a = 10.708 (3) ÅCell parameters from 2429 reflections
b = 11.172 (3) Åθ = 2.2–27.8°
c = 12.448 (3) ŵ = 1.25 mm1
α = 107.126 (4)°T = 298 K
β = 101.059 (4)°Block, green
γ = 115.803 (3)°0.29 × 0.17 × 0.14 mm
V = 1189.3 (5) Å3
Data collection top
Bruker SMART CCD area-detector
diffractometer
4148 independent reflections
Radiation source: fine-focus sealed tube3102 reflections with I > 2σ(I)
Graphite monochromatorRint = 0.021
ϕ and ω scansθmax = 25.0°, θmin = 1.8°
Absorption correction: multi-scan
(SADABS; Bruker, 1998)
h = 1212
Tmin = 0.713, Tmax = 0.844k = 1313
6299 measured reflectionsl = 148
Refinement top
Refinement on F2Primary atom site location: structure-invariant direct methods
Least-squares matrix: fullSecondary atom site location: difference Fourier map
R[F2 > 2σ(F2)] = 0.036Hydrogen site location: inferred from neighbouring sites
wR(F2) = 0.084H-atom parameters constrained
S = 1.06 w = 1/[σ2(Fo2) + (0.0296P)2 + 0.6844P]
where P = (Fo2 + 2Fc2)/3
4148 reflections(Δ/σ)max = 0.004
346 parametersΔρmax = 0.60 e Å3
3 restraintsΔρmin = 0.33 e Å3
Crystal data top
[Ni3(C10H8O4)3(C12H8N2)2]·2H2Oγ = 115.803 (3)°
Mr = 1149.06V = 1189.3 (5) Å3
Triclinic, P1Z = 1
a = 10.708 (3) ÅMo Kα radiation
b = 11.172 (3) ŵ = 1.25 mm1
c = 12.448 (3) ÅT = 298 K
α = 107.126 (4)°0.29 × 0.17 × 0.14 mm
β = 101.059 (4)°
Data collection top
Bruker SMART CCD area-detector
diffractometer
4148 independent reflections
Absorption correction: multi-scan
(SADABS; Bruker, 1998)
3102 reflections with I > 2σ(I)
Tmin = 0.713, Tmax = 0.844Rint = 0.021
6299 measured reflections
Refinement top
R[F2 > 2σ(F2)] = 0.0363 restraints
wR(F2) = 0.084H-atom parameters constrained
S = 1.06Δρmax = 0.60 e Å3
4148 reflectionsΔρmin = 0.33 e Å3
346 parameters
Special details top

Geometry. All e.s.d.'s (except the e.s.d. in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell e.s.d.'s are taken into account individually in the estimation of e.s.d.'s in distances, angles and torsion angles; correlations between e.s.d.'s in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell e.s.d.'s is used for estimating e.s.d.'s involving l.s. planes.

Refinement. Refinement of F2 against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F2, conventional R-factors R are based on F, with F set to zero for negative F2. The threshold expression of F2 > σ(F2) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F2 are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger.

Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top
xyzUiso*/Ueq
Ni10.50000.50001.00000.02372 (15)
Ni20.26388 (4)0.42348 (4)0.72300 (3)0.02559 (13)
N10.1354 (3)0.5204 (3)0.7334 (2)0.0286 (6)
N20.0885 (3)0.2830 (3)0.5572 (2)0.0297 (6)
O10.4903 (2)0.3409 (2)0.85126 (19)0.0305 (5)
O20.3798 (2)0.3326 (2)0.67459 (19)0.0340 (5)
O31.2841 (2)0.3732 (2)0.97944 (19)0.0328 (5)
O41.1469 (2)0.2806 (2)0.7831 (2)0.0352 (6)
O50.4366 (2)0.5854 (2)0.88518 (18)0.0258 (5)
O60.4473 (2)0.6300 (2)0.7267 (2)0.0379 (6)
O70.3489 (4)0.3213 (6)0.4110 (4)0.1086 (14)
H280.421 (5)0.398 (4)0.417 (6)0.130*
H290.391 (6)0.309 (7)0.468 (4)0.130*
C10.6585 (3)0.2249 (4)0.7380 (3)0.0315 (8)
C20.7634 (4)0.3260 (4)0.8531 (3)0.0357 (8)
H20.75670.40530.89580.043*
C30.8782 (3)0.3099 (4)0.9051 (3)0.0352 (8)
H30.94740.37890.98260.042*
C40.8928 (3)0.1943 (4)0.8450 (3)0.0312 (8)
C50.7887 (4)0.0938 (4)0.7308 (3)0.0393 (9)
H50.79570.01460.68830.047*
C60.6738 (4)0.1090 (4)0.6784 (3)0.0405 (9)
H60.60480.03950.60100.049*
C70.4650 (3)0.3118 (3)0.7418 (3)0.0270 (7)
C80.5361 (4)0.2406 (5)0.6732 (3)0.0476 (10)
H8A0.45600.14270.61410.057*
H8B0.57550.29560.62790.057*
C91.1657 (3)0.2905 (3)0.8883 (3)0.0261 (7)
C101.0257 (3)0.1877 (4)0.9033 (3)0.0329 (8)
H10A1.00360.08770.86660.039*
H10B1.04420.21520.98880.039*
C110.5667 (3)0.9196 (3)0.9634 (3)0.0320 (8)
C120.5504 (4)1.0050 (3)0.9066 (3)0.0345 (8)
H120.58451.00910.84360.041*
C130.4844 (3)1.0839 (3)0.9425 (3)0.0352 (8)
H130.47411.14010.90310.042*
C140.5005 (3)0.6704 (3)0.8378 (3)0.0286 (7)
C150.6301 (4)0.8256 (4)0.9188 (3)0.0393 (9)
H15A0.69000.86340.87400.047*
H15B0.69320.82670.98690.047*
C160.1648 (4)0.6443 (4)0.8179 (3)0.0403 (9)
H160.25270.69750.88560.048*
C170.0699 (4)0.6986 (4)0.8098 (3)0.0451 (10)
H170.09610.78720.87030.054*
C180.0607 (4)0.6216 (4)0.7132 (3)0.0444 (10)
H180.12540.65620.70770.053*
C190.0970 (4)0.4901 (4)0.6223 (3)0.0350 (8)
C200.0062 (3)0.4446 (3)0.6356 (3)0.0287 (7)
C210.0216 (3)0.3136 (3)0.5427 (3)0.0298 (8)
C220.1574 (4)0.2247 (4)0.4439 (3)0.0400 (9)
C230.1807 (4)0.0941 (4)0.3606 (3)0.0518 (11)
H230.27000.03030.29390.062*
C240.0727 (4)0.0602 (4)0.3772 (3)0.0493 (10)
H240.08870.02780.32360.059*
C250.0622 (4)0.1596 (4)0.4758 (3)0.0405 (9)
H250.13700.13770.48440.049*
C260.2317 (4)0.4003 (4)0.5159 (3)0.0454 (10)
H260.29950.43060.50460.054*
C270.2613 (4)0.2733 (4)0.4327 (4)0.0478 (10)
H270.35120.21560.36640.057*
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
Ni10.0218 (3)0.0302 (3)0.0206 (3)0.0159 (3)0.0060 (2)0.0104 (3)
Ni20.0243 (2)0.0313 (2)0.0223 (2)0.01678 (19)0.00614 (18)0.01103 (19)
N10.0251 (14)0.0355 (16)0.0248 (15)0.0175 (13)0.0065 (12)0.0116 (13)
N20.0324 (15)0.0308 (15)0.0259 (15)0.0171 (13)0.0091 (12)0.0124 (13)
O10.0380 (13)0.0394 (13)0.0251 (13)0.0278 (11)0.0135 (10)0.0142 (11)
O20.0390 (13)0.0479 (14)0.0263 (12)0.0323 (12)0.0113 (11)0.0152 (11)
O30.0239 (12)0.0430 (14)0.0298 (13)0.0172 (11)0.0076 (11)0.0158 (11)
O40.0287 (12)0.0420 (14)0.0275 (13)0.0124 (11)0.0095 (11)0.0161 (11)
O50.0256 (11)0.0298 (12)0.0245 (12)0.0166 (10)0.0062 (10)0.0133 (10)
O60.0402 (14)0.0470 (15)0.0352 (14)0.0256 (12)0.0139 (12)0.0240 (12)
O70.076 (3)0.170 (4)0.109 (3)0.070 (3)0.045 (3)0.082 (3)
C10.0310 (18)0.046 (2)0.0283 (18)0.0265 (17)0.0146 (15)0.0162 (16)
C20.0344 (19)0.038 (2)0.038 (2)0.0234 (17)0.0144 (17)0.0120 (17)
C30.0267 (18)0.0323 (19)0.034 (2)0.0126 (16)0.0042 (15)0.0078 (16)
C40.0239 (17)0.038 (2)0.038 (2)0.0164 (16)0.0150 (16)0.0204 (17)
C50.039 (2)0.046 (2)0.038 (2)0.0300 (18)0.0139 (18)0.0117 (18)
C60.038 (2)0.055 (2)0.0263 (19)0.0301 (19)0.0091 (16)0.0082 (17)
C70.0261 (17)0.0268 (17)0.0278 (19)0.0146 (15)0.0099 (15)0.0105 (15)
C80.055 (2)0.082 (3)0.031 (2)0.055 (2)0.0195 (19)0.023 (2)
C90.0251 (17)0.0289 (18)0.034 (2)0.0202 (15)0.0126 (16)0.0151 (15)
C100.0259 (17)0.039 (2)0.040 (2)0.0170 (16)0.0139 (16)0.0230 (17)
C110.0258 (17)0.0221 (17)0.0333 (19)0.0082 (15)0.0005 (15)0.0073 (15)
C120.0356 (19)0.0293 (19)0.0319 (19)0.0123 (16)0.0094 (16)0.0142 (16)
C130.0346 (19)0.0290 (19)0.032 (2)0.0117 (16)0.0014 (16)0.0160 (16)
C140.0281 (18)0.0329 (18)0.032 (2)0.0224 (16)0.0075 (15)0.0150 (16)
C150.0241 (17)0.034 (2)0.051 (2)0.0108 (16)0.0070 (17)0.0183 (18)
C160.036 (2)0.047 (2)0.036 (2)0.0246 (18)0.0110 (17)0.0127 (18)
C170.054 (2)0.051 (2)0.042 (2)0.036 (2)0.024 (2)0.0164 (19)
C180.045 (2)0.061 (3)0.054 (3)0.040 (2)0.025 (2)0.033 (2)
C190.0311 (19)0.048 (2)0.042 (2)0.0240 (17)0.0172 (17)0.0307 (18)
C200.0256 (17)0.0360 (19)0.0285 (18)0.0162 (15)0.0094 (15)0.0191 (16)
C210.0253 (17)0.0365 (19)0.0260 (18)0.0139 (15)0.0060 (14)0.0174 (16)
C220.034 (2)0.044 (2)0.031 (2)0.0124 (17)0.0035 (16)0.0192 (18)
C230.046 (2)0.047 (2)0.030 (2)0.010 (2)0.0059 (18)0.0112 (19)
C240.057 (3)0.038 (2)0.030 (2)0.018 (2)0.0043 (19)0.0065 (18)
C250.050 (2)0.041 (2)0.034 (2)0.0264 (19)0.0149 (18)0.0163 (18)
C260.031 (2)0.066 (3)0.051 (2)0.028 (2)0.0133 (18)0.037 (2)
C270.028 (2)0.061 (3)0.042 (2)0.0156 (19)0.0010 (17)0.029 (2)
Geometric parameters (Å, º) top
Ni1—O3i2.031 (2)C6—H60.9300
Ni1—O3ii2.031 (2)C7—C81.523 (4)
Ni1—O52.099 (2)C8—H8A0.9700
Ni1—O5iii2.099 (2)C8—H8B0.9700
Ni1—O12.104 (2)C9—C101.528 (4)
Ni1—O1iii2.104 (2)C10—H10A0.9700
Ni2—O21.990 (2)C10—H10B0.9700
Ni2—O4i1.999 (2)C11—C13v1.389 (5)
Ni2—O52.067 (2)C11—C121.392 (4)
Ni2—N22.071 (3)C11—C151.515 (5)
Ni2—N12.089 (3)C12—C131.381 (5)
Ni2—O62.268 (2)C12—H120.9300
N1—C161.326 (4)C13—C11v1.389 (5)
N1—C201.357 (4)C13—H130.9300
N2—C251.319 (4)C14—C151.513 (4)
N2—C211.357 (4)C15—H15A0.9700
O1—C71.248 (4)C15—H15B0.9700
O2—C71.262 (4)C16—C171.393 (5)
O3—C91.248 (4)C16—H160.9300
O3—Ni1iv2.031 (2)C17—C181.357 (5)
O4—C91.250 (4)C17—H170.9300
O4—Ni2iv1.999 (2)C18—C191.395 (5)
O5—C141.279 (4)C18—H180.9300
O6—C141.244 (4)C19—C201.406 (4)
O7—H280.84 (5)C19—C261.437 (5)
O7—H290.85 (6)C20—C211.435 (4)
C1—C21.384 (4)C21—C221.397 (4)
C1—C61.385 (4)C22—C231.399 (5)
C1—C81.509 (4)C22—C271.437 (5)
C2—C31.386 (4)C23—C241.364 (5)
C2—H20.9300C23—H230.9300
C3—C41.379 (4)C24—C251.395 (5)
C3—H30.9300C24—H240.9300
C4—C51.373 (5)C25—H250.9300
C4—C101.511 (4)C26—C271.342 (5)
C5—C61.381 (5)C26—H260.9300
C5—H50.9300C27—H270.9300
O3i—Ni1—O3ii180C7—C8—H8A106.9
O3i—Ni1—O590.90 (8)C1—C8—H8B106.9
O3ii—Ni1—O589.10 (8)C7—C8—H8B106.9
O3i—Ni1—O5iii89.10 (8)H8A—C8—H8B106.7
O3ii—Ni1—O5iii90.90 (8)O3—C9—O4127.3 (3)
O5—Ni1—O5iii180O3—C9—C10118.1 (3)
O3i—Ni1—O194.73 (9)O4—C9—C10114.6 (3)
O3ii—Ni1—O185.27 (8)C4—C10—C9111.4 (3)
O5—Ni1—O189.45 (8)C4—C10—H10A109.3
O5iii—Ni1—O190.55 (8)C9—C10—H10A109.3
O3i—Ni1—O1iii85.27 (9)C4—C10—H10B109.3
O3ii—Ni1—O1iii94.73 (9)C9—C10—H10B109.3
O5—Ni1—O1iii90.55 (8)H10A—C10—H10B108.0
O5iii—Ni1—O1iii89.45 (8)C13v—C11—C12118.4 (3)
O1—Ni1—O1iii180C13v—C11—C15120.7 (3)
O2—Ni2—O4i96.62 (10)C12—C11—C15120.8 (3)
O2—Ni2—O593.60 (9)C13—C12—C11120.9 (3)
O4i—Ni2—O599.08 (9)C13—C12—H12119.6
O2—Ni2—N291.37 (10)C11—C12—H12119.6
O4i—Ni2—N285.83 (10)C12—C13—C11v120.7 (3)
O5—Ni2—N2172.56 (9)C12—C13—H13119.6
O2—Ni2—N1166.22 (9)C11v—C13—H13119.6
O4i—Ni2—N193.07 (10)O6—C14—O5119.9 (3)
O5—Ni2—N194.51 (9)O6—C14—C15120.2 (3)
N2—Ni2—N179.57 (10)O5—C14—C15119.6 (3)
O2—Ni2—O685.80 (9)C14—C15—C11107.9 (3)
O4i—Ni2—O6159.39 (9)C14—C15—H15A110.1
O5—Ni2—O660.31 (8)C11—C15—H15A110.1
N2—Ni2—O6114.64 (10)C14—C15—H15B110.1
N1—Ni2—O688.57 (10)C11—C15—H15B110.1
C16—N1—C20117.4 (3)H15A—C15—H15B108.4
C16—N1—Ni2129.6 (2)N1—C16—C17123.1 (3)
C20—N1—Ni2113.0 (2)N1—C16—H16118.5
C25—N2—C21117.7 (3)C17—C16—H16118.5
C25—N2—Ni2128.0 (2)C18—C17—C16119.7 (3)
C21—N2—Ni2113.4 (2)C18—C17—H17120.1
C7—O1—Ni1136.1 (2)C16—C17—H17120.1
C7—O2—Ni2126.9 (2)C17—C18—C19119.4 (3)
C9—O3—Ni1iv132.4 (2)C17—C18—H18120.3
C9—O4—Ni2iv130.7 (2)C19—C18—H18120.3
C14—O5—Ni293.97 (18)C18—C19—C20117.5 (3)
C14—O5—Ni1136.82 (19)C18—C19—C26124.0 (3)
Ni2—O5—Ni1112.86 (10)C20—C19—C26118.5 (3)
C14—O6—Ni285.8 (2)N1—C20—C19123.0 (3)
H28—O7—H29100 (5)N1—C20—C21116.8 (3)
C2—C1—C6117.3 (3)C19—C20—C21120.2 (3)
C2—C1—C8123.2 (3)N2—C21—C22123.5 (3)
C6—C1—C8119.4 (3)N2—C21—C20116.8 (3)
C1—C2—C3120.5 (3)C22—C21—C20119.7 (3)
C1—C2—H2119.8C21—C22—C23116.6 (3)
C3—C2—H2119.8C21—C22—C27118.8 (3)
C4—C3—C2121.8 (3)C23—C22—C27124.5 (3)
C4—C3—H3119.1C24—C23—C22120.0 (3)
C2—C3—H3119.1C24—C23—H23120.0
C5—C4—C3117.8 (3)C22—C23—H23120.0
C5—C4—C10122.7 (3)C23—C24—C25119.0 (3)
C3—C4—C10119.4 (3)C23—C24—H24120.5
C4—C5—C6120.7 (3)C25—C24—H24120.5
C4—C5—H5119.6N2—C25—C24123.0 (3)
C6—C5—H5119.6N2—C25—H25118.5
C5—C6—C1121.9 (3)C24—C25—H25118.5
C5—C6—H6119.1C27—C26—C19121.1 (3)
C1—C6—H6119.1C27—C26—H26119.4
O1—C7—O2126.7 (3)C19—C26—H26119.4
O1—C7—C8121.2 (3)C26—C27—C22121.5 (3)
O2—C7—C8112.1 (3)C26—C27—H27119.3
C1—C8—C7121.5 (3)C22—C27—H27119.3
C1—C8—H8A106.9
Symmetry codes: (i) x1, y, z; (ii) x+2, y+1, z+2; (iii) x+1, y+1, z+2; (iv) x+1, y, z; (v) x+1, y+2, z+2.
Hydrogen-bond geometry (Å, º) top
D—H···AD—HH···AD···AD—H···A
O7—H28···O6vi0.84 (5)2.51 (6)2.990 (5)117 (5)
O7—H29···O20.85 (6)2.54 (5)3.193 (5)135 (6)
Symmetry code: (vi) x+1, y+1, z+1.

Experimental details

Crystal data
Chemical formula[Ni3(C10H8O4)3(C12H8N2)2]·2H2O
Mr1149.06
Crystal system, space groupTriclinic, P1
Temperature (K)298
a, b, c (Å)10.708 (3), 11.172 (3), 12.448 (3)
α, β, γ (°)107.126 (4), 101.059 (4), 115.803 (3)
V3)1189.3 (5)
Z1
Radiation typeMo Kα
µ (mm1)1.25
Crystal size (mm)0.29 × 0.17 × 0.14
Data collection
DiffractometerBruker SMART CCD area-detector
diffractometer
Absorption correctionMulti-scan
(SADABS; Bruker, 1998)
Tmin, Tmax0.713, 0.844
No. of measured, independent and
observed [I > 2σ(I)] reflections
6299, 4148, 3102
Rint0.021
(sin θ/λ)max1)0.595
Refinement
R[F2 > 2σ(F2)], wR(F2), S 0.036, 0.084, 1.06
No. of reflections4148
No. of parameters346
No. of restraints3
H-atom treatmentH-atom parameters constrained
Δρmax, Δρmin (e Å3)0.60, 0.33

Computer programs: SMART (Bruker, 1998), SMART, SAINT (Bruker, 1998), SHELXS97 (Sheldrick, 1997), SHELXL97 (Sheldrick, 1997), SHELXTL (Bruker, 1997), SHELXTL.

Selected geometric parameters (Å, º) top
Ni1—O3i2.031 (2)Ni2—O21.990 (2)
Ni1—O3ii2.031 (2)Ni2—O4i1.999 (2)
Ni1—O52.099 (2)Ni2—O52.067 (2)
Ni1—O5iii2.099 (2)Ni2—N22.071 (3)
Ni1—O12.104 (2)Ni2—N12.089 (3)
Ni1—O1iii2.104 (2)Ni2—O62.268 (2)
O3i—Ni1—O3ii180O4i—Ni2—N285.83 (10)
O3i—Ni1—O590.90 (8)O5—Ni2—N2172.56 (9)
O5—Ni1—O5iii180O2—Ni2—N1166.22 (9)
O3i—Ni1—O1iii85.27 (9)O4i—Ni2—N193.07 (10)
O3ii—Ni1—O1iii94.73 (9)O5—Ni2—N194.51 (9)
O5—Ni1—O1iii90.55 (8)N2—Ni2—N179.57 (10)
O5iii—Ni1—O1iii89.45 (8)O2—Ni2—O685.80 (9)
O1—Ni1—O1iii180O4i—Ni2—O6159.39 (9)
O2—Ni2—O4i96.62 (10)O5—Ni2—O660.31 (8)
O2—Ni2—O593.60 (9)N2—Ni2—O6114.64 (10)
O4i—Ni2—O599.08 (9)N1—Ni2—O688.57 (10)
O2—Ni2—N291.37 (10)
Symmetry codes: (i) x1, y, z; (ii) x+2, y+1, z+2; (iii) x+1, y+1, z+2.
Hydrogen-bond geometry (Å, º) top
D—H···AD—HH···AD···AD—H···A
O7—H28···O6iv0.84 (5)2.51 (6)2.990 (5)117 (5)
O7—H29···O20.85 (6)2.54 (5)3.193 (5)135 (6)
Symmetry code: (iv) x+1, y+1, z+1.
 

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