Tetra­kis(μ3-2-{[1,1-bis­(hydroxy­meth­yl)-2-oxidoeth­yl]imino­meth­yl}-6-methoxy­phenol­ato)tetra­nickel(II) tetra­hydrate

Guo, Y.; Li, L.; Liu, Y.; Dong, J.; Wang, D.

doi:10.1107/S1600536808009872

metal-organic compounds

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ISSN: 2056-9890

Volume 64| Part 5| May 2008| Pages m675-m676

doi:10.1107/S1600536808009872

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Tetrakis(μ₃-2-{[1,1-bis(hydroxymethyl)-2-oxidoethyl]iminomethyl}-6-methoxyphenolato)tetranickel(II) tetrahydrate

Yujing Guo,^a Lianzhi Li,^a ^* Yan Liu,^a Jianfang Dong ^a and Daqi Wang ^a

^aSchool of Chemistry and Chemical Engineering, Liaocheng University, Shandong 252059, People's Republic of China
^*Correspondence e-mail: lilianzhi1963@yahoo.com.cn

(Received 4 April 2008; accepted 10 April 2008; online 16 April 2008)

The title complex, [Ni₄(C₁₂H₁₅NO₄)₄]·4H₂O, has crystallographic fourfold inversion symmetry, with each Ni^II ion coordinated in a slightly distorted square-pyramidal coordination environment and forming an Ni₄O₄ cubane-like core. In the crystal structure, intermolecular O—H⋯O hydrogen bonds connect complex and water molecules to form a three-dimensional network. The O atom of one of the unique hydroxymethyl groups is disordered over two sites, with the ratio of occupancies being approximately 0.79:0.21.

Related literature

For related literature, see: Dong, Li, Xu & Wang (2007 ); Dong, Li, Xu, Cui & Wang (2007 ); Koikawa et al. (2005 ); Mishtu et al. (2002 ); Nihei et al. (2003 ).

Experimental

Crystal data

[Ni₄(C₁₂H₁₅NO₄)₄]·4H₂O
M_r = 1319.90
Tetragonal, I 4₁ /a
a = 18.754 (2) Å
c = 15.4395 (15) Å
V = 5430.3 (10) Å³
Z = 4
Mo Kα radiation
μ = 1.45 mm⁻¹
T = 298 (2) K
0.30 × 0.29 × 0.28 mm

Data collection

Bruker SMART CCD area-detector diffractometer
Absorption correction: multi-scan (SADABS; Sheldrick, 1996 ) T_min = 0.670, T_max = 0.686
11110 measured reflections
2399 independent reflections
1840 reflections with I > 2σ(I)
R_int = 0.034

Refinement

R[F² > 2σ(F²)] = 0.066
wR(F²) = 0.194
S = 1.08
2399 reflections
186 parameters
H-atom parameters constrained
Δρ_max = 1.23 e Å⁻³
Δρ_min = −0.70 e Å⁻³

Table 1
Selected geometric parameters (Å, °)

Ni1—O1	1.912 (4)
Ni1—O3	1.941 (4)
Ni1—N1	1.949 (6)
Ni1—O3ⁱ	1.970 (4)
Ni1—O3ⁱⁱ	2.565 (5)

O1—Ni1—O3	172.2 (2)
O1—Ni1—N1	94.3 (2)
O3—Ni1—N1	84.1 (2)
O1—Ni1—O3ⁱ	94.57 (19)
O3—Ni1—O3ⁱ	88.47 (19)
N1—Ni1—O3ⁱ	166.1 (2)
O1—Ni1—O3ⁱⁱ	94.23 (17)
O3—Ni1—O3ⁱⁱ	79.80 (17)
N1—Ni1—O3ⁱⁱ	117.2 (2)
O3ⁱ—Ni1—O3ⁱⁱ	72.63 (17)
Symmetry codes: (i) $[y-{\script{1\over 4}}, -x+{\script{5\over 4}}, -z+{\script{9\over 4}}]$ ; (ii) $[-x+1, -y+{\script{3\over 2}}, z]$ .

Table 2
Hydrogen-bond geometry (Å, °)

D—H⋯A	D—H	H⋯A	D⋯A	D—H⋯A
O5—H5⋯N1	0.82	2.58	2.988 (9)	112
O4—H4⋯O6ⁱⁱⁱ	0.82	1.94	2.714 (8)	157
O4′—H4′⋯O6ⁱⁱⁱ	0.82	1.96	2.68 (3)	148
O6—H6A⋯O1^iv	0.85	1.95	2.803 (7)	180
O6—H6B⋯O4^v	0.85	2.04	2.892 (9)	180
Symmetry codes: (iii) $[y-{\script{1\over 4}}, -x+{\script{3\over 4}}, z+{\script{3\over 4}}]$ ; (iv) $[-y+{\script{5\over 4}}, x+{\script{1\over 4}}, -z+{\script{5\over 4}}]$ ; (v) x, y, z-1.

Data collection: SMART (Siemens, 1996 ); cell refinement: SAINT (Siemens, 1996); data reduction: SAINT; program(s) used to solve structure: SHELXS97 (Sheldrick, 2008 ); program(s) used to refine structure: SHELXL97 (Sheldrick, 2008); molecular graphics: SHELXTL (Sheldrick, 2008); software used to prepare material for publication: SHELXTL.

Supporting information

Crystal structure: contains datablocks global, I. DOI: 10.1107/S1600536808009872/lh2612sup1.cif

Structure factors: contains datablock I. DOI: 10.1107/S1600536808009872/lh2612Isup2.hkl

checkCIF report

Comment top

The chemistry of transition metal ion complexes of hydroxy (aryl-OH and alkyl-OH) rich molecules containing imine/amine group is important in the biomimetic studies of metalloproteins (Mishtu et al., 2002). Polynuclear metal complexes with tridentate ligand containing hydroxyl groups as terminal coordinating atoms have been reported and have attracted much attention (Nihei et al., 2003).

A few structurally characterized multinuclear complexes containing Schiff base ligands has been reported( e.g. Dong, Li, Xu & Wang (2007); Dong, Li, Xu, Cui & Wang (2007); Nihei et al., 2003). Herein, we report the synthesis and crystal structure of a novel tetranickel(II) complex with a tridentate Schiff base ligand derived from the condensation of o-vanillin and trihydroxymethylaminomethane.

The title compound contains a tetranuclear cubane core based on an approximately cubic array of alternating nickel and oxygen atoms (Fig.1). Each Ni^II ion is in a distorted square-pyramidal coordination environment with one nitrogen and two oxygen atoms from one Schiff base ligand and two oxygen atoms from the symmetry related units of the cubane core. The Ni atom deviates from the basal plane (formed by O1, N1, O3 and O3ⁱ, symmetry code (i) y - 7/4, -x + 3/4, -z + 7/4) by 0.1299 (33) Å, with a significantly longer Ni—O_apical bond distance (Table 1). In the molecular structure, the Ni—Ni distances (3.472 (4) Å, 3.182 (3) Å) are longer than some reported values (Koikawa et al., 2005). In addition, there are four H₂O solvent molecules, which are involved in intermolecular O-H···O hydrogen bonds (Fig. 2, Table 2) which stabilize the crystal atructure along with van der Waals forces.

Related literature top

For related literature, see: Dong, Li, Xu & Wang (2007); Dong, Li, Xu, Cui & Wang (2007); Koikawa et al. (2005); Mishtu et al. (2002); Nihei et al. (2003).

Experimental top

Trihydroxymethylaminomethane(1 mmol, 121.14 mg) was dissolved in hot methanol (10 ml) and added successively to a methanol solution(3 ml) of o-vanillin (1 mmol, 152.15 mg). The mixture was then stirred at 323 K for 2 h. Subsequently, an aqueous solution(2 ml) of nickel chlorate hexahydrate(1 mmol, 237.66 mg) was added dropwise and stirred for another 5 h. The solution was held at room temperature for ten days, whereupon green blocky crystals suitable for X-ray diffraction were obtained.

Computing details top

Data collection: SMART (Siemens, 1996); cell refinement: SAINT (Siemens, 1996); data reduction: SAINT (Siemens, 1996); program(s) used to solve structure: SHELXS97 (Sheldrick, 2008); program(s) used to refine structure: SHELXL97 (Sheldrick, 2008); molecular graphics: SHELXTL (Sheldrick, 2008); software used to prepare material for publication: SHELXTL (Sheldrick, 2008).

Figures top

	Fig. 1. The structure of the title compound, showing 30% probability displacement ellipsoids and the atom-numbering scheme. The water solvent molecules are not shown. Open bonds indicate disordered atoms and only the assymetric unit is labelled.
	Fig. 2. Part of the crystal structure with hydrogen bonds shown as dashed lines. The disorder is not shown.

Tetrakis(µ₃-2-{[1,1-bis(hydroxymethyl)-2-oxidoethyl]iminomethyl}- 6-methoxyphenolato)tetranickel(II) tetrahydrate top

Crystal data top

[Ni₄(C₁₂H₁₅NO₄)₄]·4H₂O	D_x = 1.614 Mg m⁻³
M_r = 1319.90	Mo Kα radiation, λ = 0.71073 Å
Tetragonal, I4₁/a	Cell parameters from 3768 reflections
Hall symbol: -I 4ad	θ = 2.2–25.2°
a = 18.754 (2) Å	µ = 1.45 mm⁻¹
c = 15.4395 (15) Å	T = 298 K
V = 5430.3 (10) Å³	Block, green
Z = 4	0.30 × 0.29 × 0.28 mm
F(000) = 2752

Data collection top

Bruker SMART CCD area-detector diffractometer	2399 independent reflections
Radiation source: fine-focus sealed tube	1840 reflections with I > 2σ(I)
Graphite monochromator	R_int = 0.034
ϕ and ω scans	θ_max = 25.0°, θ_min = 1.7°
Absorption correction: multi-scan (SADABS; Sheldrick, 1996)	h = −22→22
T_min = 0.670, T_max = 0.686	k = −22→15
11110 measured reflections	l = −9→18

Refinement top

Refinement on F²	Primary atom site location: structure-invariant direct methods
Least-squares matrix: full	Secondary atom site location: difference Fourier map
R[F² > 2σ(F²)] = 0.066	Hydrogen site location: inferred from neighbouring sites
wR(F²) = 0.194	H-atom parameters constrained
S = 1.08	w = 1/[σ²(F_o²) + (0.0801P)² + 60.7787P] where P = (F_o² + 2F_c²)/3
2399 reflections	(Δ/σ)_max = 0.001
186 parameters	Δρ_max = 1.23 e Å⁻³
0 restraints	Δρ_min = −0.70 e Å⁻³

Crystal data top

[Ni₄(C₁₂H₁₅NO₄)₄]·4H₂O	Z = 4
M_r = 1319.90	Mo Kα radiation
Tetragonal, I4₁/a	µ = 1.45 mm⁻¹
a = 18.754 (2) Å	T = 298 K
c = 15.4395 (15) Å	0.30 × 0.29 × 0.28 mm
V = 5430.3 (10) Å³

Data collection top

Bruker SMART CCD area-detector diffractometer	2399 independent reflections
Absorption correction: multi-scan (SADABS; Sheldrick, 1996)	1840 reflections with I > 2σ(I)
T_min = 0.670, T_max = 0.686	R_int = 0.034
11110 measured reflections

Refinement top

R[F² > 2σ(F²)] = 0.066	0 restraints
wR(F²) = 0.194	H-atom parameters constrained
S = 1.08	w = 1/[σ²(F_o²) + (0.0801P)² + 60.7787P] where P = (F_o² + 2F_c²)/3
2399 reflections	Δρ_max = 1.23 e Å⁻³
186 parameters	Δρ_min = −0.70 e Å⁻³

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

	x	y	z	U_iso*/U_eq	Occ. (<1)
Ni1	0.40964 (4)	0.72996 (4)	1.05945 (5)	0.0374 (3)
N1	0.3971 (4)	0.6819 (3)	0.9486 (4)	0.0575 (16)
O1	0.3327 (2)	0.7952 (2)	1.0412 (3)	0.0480 (11)
O2	0.2316 (3)	0.8868 (4)	1.0480 (5)	0.097 (2)
O3	0.4952 (2)	0.6720 (2)	1.0675 (3)	0.0435 (10)
O4	0.3704 (5)	0.5372 (4)	0.9346 (5)	0.079 (2)	0.791 (10)
H4	0.3533	0.5023	0.9103	0.119*	0.791 (10)
O4'	0.3587 (16)	0.5547 (15)	0.836 (2)	0.079 (2)	0.209 (10)
H4'	0.3562	0.5134	0.8190	0.119*	0.209 (10)
O5	0.4819 (5)	0.6865 (5)	0.7848 (5)	0.120 (3)
H5	0.4383	0.6853	0.7893	0.181*
O6	0.3380 (3)	0.6042 (3)	0.0986 (4)	0.0729 (16)
H6A	0.3733	0.5978	0.1322	0.088*
H6B	0.3472	0.5846	0.0503	0.088*
C1	0.3427 (4)	0.6889 (4)	0.9010 (5)	0.061 (2)
H1	0.3392	0.6586	0.8535	0.073*
C2	0.2852 (4)	0.7394 (4)	0.9132 (5)	0.0529 (18)
C3	0.2839 (3)	0.7900 (4)	0.9815 (4)	0.0476 (16)
C4	0.2269 (4)	0.8386 (5)	0.9823 (5)	0.067 (2)
C5	0.1712 (5)	0.8344 (6)	0.9218 (6)	0.078 (3)
H5A	0.1334	0.8664	0.9245	0.094*
C6	0.1727 (5)	0.7834 (6)	0.8595 (6)	0.078 (3)
H6	0.1354	0.7800	0.8201	0.094*
C7	0.2279 (4)	0.7377 (5)	0.8544 (6)	0.068 (2)
H7	0.2281	0.7038	0.8104	0.081*
C8	0.1829 (7)	0.9466 (7)	1.0493 (9)	0.130 (5)
H8A	0.1797	0.9668	0.9923	0.195*
H8B	0.2001	0.9820	1.0891	0.195*
H8C	0.1366	0.9306	1.0675	0.195*
C9	0.4572 (5)	0.6290 (5)	0.9262 (6)	0.075 (3)
C10	0.4932 (4)	0.6144 (4)	1.0099 (4)	0.0523 (17)
H10A	0.4691	0.5749	1.0380	0.063*
H10B	0.5418	0.5995	0.9981	0.063*
C11	0.4273 (5)	0.5654 (5)	0.8832 (6)	0.073 (2)
H11A	0.4096	0.5781	0.8262	0.088*	0.791 (10)
H11B	0.4642	0.5296	0.8762	0.088*	0.791 (10)
H11C	0.4635	0.5509	0.8420	0.088*	0.209 (10)
H11D	0.4276	0.5290	0.9279	0.088*	0.209 (10)
C12	0.5136 (5)	0.6631 (6)	0.8640 (6)	0.085 (3)
H12A	0.5359	0.7033	0.8927	0.101*
H12B	0.5504	0.6283	0.8514	0.101*

Atomic displacement parameters (Å²) top

	U¹¹	U²²	U³³	U¹²	U¹³	U²³
Ni1	0.0427 (5)	0.0358 (5)	0.0337 (5)	0.0002 (3)	−0.0072 (3)	−0.0007 (3)
N1	0.080 (4)	0.046 (3)	0.046 (3)	0.015 (3)	−0.022 (3)	−0.009 (3)
O1	0.045 (3)	0.055 (3)	0.043 (2)	0.008 (2)	−0.009 (2)	−0.005 (2)
O2	0.070 (4)	0.125 (6)	0.095 (5)	0.048 (4)	−0.010 (4)	−0.019 (4)
O3	0.056 (3)	0.039 (2)	0.036 (2)	0.010 (2)	−0.008 (2)	−0.0013 (19)
O4	0.094 (6)	0.059 (4)	0.086 (5)	0.007 (4)	−0.005 (5)	−0.030 (4)
O4'	0.094 (6)	0.059 (4)	0.086 (5)	0.007 (4)	−0.005 (5)	−0.030 (4)
O5	0.111 (6)	0.189 (8)	0.061 (4)	0.038 (6)	0.005 (4)	0.011 (5)
O6	0.053 (3)	0.096 (4)	0.070 (4)	−0.001 (3)	0.011 (3)	−0.003 (3)
C1	0.079 (5)	0.056 (4)	0.048 (4)	0.006 (4)	−0.022 (4)	−0.007 (3)
C2	0.055 (4)	0.059 (4)	0.045 (4)	−0.010 (3)	−0.013 (3)	0.007 (3)
C3	0.039 (4)	0.059 (4)	0.044 (4)	−0.001 (3)	−0.002 (3)	0.014 (3)
C4	0.049 (4)	0.093 (6)	0.058 (5)	0.010 (4)	−0.001 (4)	0.002 (5)
C5	0.050 (5)	0.110 (8)	0.075 (6)	0.014 (5)	−0.004 (4)	0.010 (6)
C6	0.060 (5)	0.106 (7)	0.069 (6)	−0.008 (5)	−0.018 (4)	0.007 (5)
C7	0.064 (5)	0.081 (6)	0.058 (5)	−0.011 (4)	−0.025 (4)	0.005 (4)
C8	0.105 (9)	0.148 (12)	0.137 (12)	0.064 (9)	−0.013 (8)	−0.026 (9)
C9	0.088 (6)	0.076 (6)	0.061 (5)	0.035 (5)	−0.005 (5)	−0.016 (4)
C10	0.054 (4)	0.060 (4)	0.043 (4)	0.010 (3)	−0.001 (3)	−0.013 (3)
C11	0.081 (6)	0.076 (6)	0.061 (5)	0.016 (5)	−0.007 (5)	−0.031 (5)
C12	0.085 (7)	0.104 (8)	0.065 (6)	0.024 (6)	0.001 (5)	−0.002 (5)

Geometric parameters (Å, º) top

Ni1—O1	1.912 (4)	C2—C7	1.408 (10)
Ni1—O3	1.941 (4)	C2—C3	1.419 (10)
Ni1—N1	1.949 (6)	C3—C4	1.405 (11)
Ni1—O3ⁱ	1.970 (4)	C4—C5	1.403 (12)
Ni1—O3ⁱⁱ	2.565 (5)	C5—C6	1.357 (13)
N1—C1	1.265 (9)	C5—H5A	0.9300
N1—C9	1.541 (10)	C6—C7	1.345 (13)
O1—C3	1.303 (8)	C6—H6	0.9300
O2—C4	1.362 (11)	C7—H7	0.9300
O2—C8	1.446 (12)	C8—H8A	0.9600
O3—C10	1.400 (8)	C8—H8B	0.9600
O3—Ni1ⁱⁱⁱ	1.970 (4)	C8—H8C	0.9600
O4—C11	1.430 (12)	C9—C11	1.475 (13)
O4—H4	0.8200	C9—C10	1.484 (11)
O4—H11D	1.0883	C9—C12	1.565 (14)
O4'—C11	1.49 (3)	C10—H10A	0.9700
O4'—H4'	0.8200	C10—H10B	0.9700
O5—C12	1.429 (12)	C11—H11A	0.9700
O5—H5	0.8200	C11—H11B	0.9700
O6—H6A	0.8500	C11—H11C	0.9698
O6—H6B	0.8499	C11—H11D	0.9699
C1—C2	1.447 (11)	C12—H12A	0.9700
C1—H1	0.9300	C12—H12B	0.9700

O1—Ni1—O3	172.2 (2)	O2—C8—H8A	109.5
O1—Ni1—N1	94.3 (2)	O2—C8—H8B	109.5
O3—Ni1—N1	84.1 (2)	H8A—C8—H8B	109.5
O1—Ni1—O3ⁱ	94.57 (19)	O2—C8—H8C	109.5
O3—Ni1—O3ⁱ	88.47 (19)	H8A—C8—H8C	109.5
N1—Ni1—O3ⁱ	166.1 (2)	H8B—C8—H8C	109.5
O1—Ni1—O3ⁱⁱ	94.23 (17)	C11—C9—C10	114.6 (8)
O3—Ni1—O3ⁱⁱ	79.80 (17)	C11—C9—N1	110.2 (8)
N1—Ni1—O3ⁱⁱ	117.2 (2)	C10—C9—N1	104.9 (6)
O3ⁱ—Ni1—O3ⁱⁱ	72.63 (17)	C11—C9—C12	108.1 (8)
C1—N1—C9	121.7 (6)	C10—C9—C12	107.5 (8)
C1—N1—Ni1	124.1 (6)	N1—C9—C12	111.6 (7)
C9—N1—Ni1	114.0 (5)	O3—C10—C9	115.0 (6)
C3—O1—Ni1	125.9 (4)	O3—C10—H10A	108.5
C4—O2—C8	119.0 (8)	C9—C10—H10A	108.5
C10—O3—Ni1	111.7 (4)	O3—C10—H10B	108.5
C10—O3—Ni1ⁱⁱⁱ	121.9 (4)	C9—C10—H10B	108.5
Ni1—O3—Ni1ⁱⁱⁱ	108.9 (2)	H10A—C10—H10B	107.5
C11—O4—H4	109.5	O4—C11—C9	109.4 (7)
H4—O4—H11D	103.2	O4—C11—O4'	65.0 (13)
C11—O4'—H4'	109.5	C9—C11—O4'	130.9 (13)
C12—O5—H5	109.5	O4—C11—H11A	109.8
H6A—O6—H6B	108.4	C9—C11—H11A	109.8
N1—C1—C2	126.4 (7)	O4'—C11—H11A	45.3
N1—C1—H1	116.8	O4—C11—H11B	109.8
C2—C1—H1	116.8	C9—C11—H11B	109.8
C7—C2—C3	118.8 (7)	O4'—C11—H11B	117.9
C7—C2—C1	118.0 (7)	H11A—C11—H11B	108.2
C3—C2—C1	123.1 (6)	O4—C11—H11C	141.6
O1—C3—C4	118.7 (7)	C9—C11—H11C	104.8
O1—C3—C2	124.4 (6)	O4'—C11—H11C	104.3
C4—C3—C2	116.9 (7)	H11A—C11—H11C	73.3
O2—C4—C5	125.6 (8)	O4—C11—H11D	49.5
O2—C4—C3	112.8 (7)	C9—C11—H11D	104.3
C5—C4—C3	121.6 (9)	O4'—C11—H11D	104.9
C6—C5—C4	119.7 (9)	H11A—C11—H11D	145.1
C6—C5—H5A	120.1	H11B—C11—H11D	65.7
C4—C5—H5A	120.1	H11C—C11—H11D	105.4
C7—C6—C5	120.5 (8)	O5—C12—C9	111.7 (8)
C7—C6—H6	119.8	O5—C12—H12A	109.3
C5—C6—H6	119.8	C9—C12—H12A	109.3
C6—C7—C2	122.3 (9)	O5—C12—H12B	109.3
C6—C7—H7	118.9	C9—C12—H12B	109.3
C2—C7—H7	118.9	H12A—C12—H12B	107.9

C1—C2—C3—C4	176.2 (7)

Symmetry codes: (i) y−1/4, −x+5/4, −z+9/4; (ii) −x+1, −y+3/2, z; (iii) −y+5/4, x+1/4, −z+9/4.

Hydrogen-bond geometry (Å, º) top

D—H···A	D—H	H···A	D···A	D—H···A
O5—H5···N1	0.82	2.58	2.988 (9)	112
O4—H4···O6^iv	0.82	1.94	2.714 (8)	157
O4′—H4′···O6^iv	0.82	1.96	2.68 (3)	148
O6—H6A···O1^v	0.85	1.95	2.803 (7)	180
O6—H6B···O4^vi	0.85	2.04	2.892 (9)	180

Symmetry codes: (iv) y−1/4, −x+3/4, z+3/4; (v) −y+5/4, x+1/4, −z+5/4; (vi) x, y, z−1.

Experimental details

Crystal data
Chemical formula	[Ni₄(C₁₂H₁₅NO₄)₄]·4H₂O
M_r	1319.90
Crystal system, space group	Tetragonal, I4₁/a
Temperature (K)	298
a, c (Å)	18.754 (2), 15.4395 (15)
V (Å³)	5430.3 (10)
Z	4
Radiation type	Mo Kα
µ (mm⁻¹)	1.45
Crystal size (mm)	0.30 × 0.29 × 0.28

Data collection
Diffractometer	Bruker SMART CCD area-detector diffractometer
Absorption correction	Multi-scan (SADABS; Sheldrick, 1996)
T_min, T_max	0.670, 0.686
No. of measured, independent and observed [I > 2σ(I)] reflections	11110, 2399, 1840
R_int	0.034
(sin θ/λ)_max (Å⁻¹)	0.595

Refinement
R[F² > 2σ(F²)], wR(F²), S	0.066, 0.194, 1.08
No. of reflections	2399
No. of parameters	186
H-atom treatment	H-atom parameters constrained
	w = 1/[σ²(F_o²) + (0.0801P)² + 60.7787P] where P = (F_o² + 2F_c²)/3
Δρ_max, Δρ_min (e Å⁻³)	1.23, −0.70

Computer programs: SMART (Siemens, 1996), SAINT (Siemens, 1996), SHELXS97 (Sheldrick, 2008), SHELXL97 (Sheldrick, 2008), SHELXTL (Sheldrick, 2008).

Selected geometric parameters (Å, º) top

Ni1—O1	1.912 (4)	Ni1—O3ⁱ	1.970 (4)
Ni1—O3	1.941 (4)	Ni1—O3ⁱⁱ	2.565 (5)
Ni1—N1	1.949 (6)

O1—Ni1—O3	172.2 (2)	N1—Ni1—O3ⁱ	166.1 (2)
O1—Ni1—N1	94.3 (2)	O1—Ni1—O3ⁱⁱ	94.23 (17)
O3—Ni1—N1	84.1 (2)	O3—Ni1—O3ⁱⁱ	79.80 (17)
O1—Ni1—O3ⁱ	94.57 (19)	N1—Ni1—O3ⁱⁱ	117.2 (2)
O3—Ni1—O3ⁱ	88.47 (19)	O3ⁱ—Ni1—O3ⁱⁱ	72.63 (17)

Symmetry codes: (i) y−1/4, −x+5/4, −z+9/4; (ii) −x+1, −y+3/2, z.

Hydrogen-bond geometry (Å, º) top

D—H···A	D—H	H···A	D···A	D—H···A
O5—H5···N1	0.82	2.58	2.988 (9)	112.3
O4—H4···O6ⁱⁱⁱ	0.82	1.94	2.714 (8)	156.5
O4'—H4'···O6ⁱⁱⁱ	0.82	1.96	2.68 (3)	147.6
O6—H6A···O1^iv	0.85	1.95	2.803 (7)	179.6
O6—H6B···O4^v	0.85	2.04	2.892 (9)	179.5

Symmetry codes: (iii) y−1/4, −x+3/4, z+3/4; (iv) −y+5/4, x+1/4, −z+5/4; (v) x, y, z−1.

Acknowledgements

The authors thank the Natural Science Foundation of Shandong Province (grant No. Y2004B02) for a research grant.

References

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