Hexaaqua­cobalt(II) bis­{[N-(4-meth­oxy-2-oxidobenzyl­idene)glycylglycinato]nickel(II)} hexa­hydrate

Jiang, J.; Lu, Y.; Yuan, L.; Liu, W.

doi:10.1107/S1600536809026750

metal-organic compounds

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ISSN: 2056-9890

Volume 65| Part 8| August 2009| Page m952

doi:10.1107/S1600536809026750

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Hexaaquacobalt(II) bis{[N-(4-methoxy-2-oxidobenzylidene)glycylglycinato]nickel(II)} hexahydrate

Jiaxun Jiang,^a Yao Lu,^a Limin Yuan ^a and Wenlong Liu ^a ^*

^aCollege of Chemistry and Chemical Engineering, Yangzhou Universitry, Yangzhou 225002, People's Republic of China
^*Correspondence e-mail: liuwl@yzu.edu.cn

(Received 5 June 2009; accepted 8 July 2009; online 18 July 2009)

In the title compound, [Co(H₂O)₆][Ni(C₁₂H₁₁N₂O₅)]₂·6H₂O, the Ni^II atom has a nearly square-planar coordination with two N and two O atoms of the N-(4-methoxy-2-oxidobenzylidene)glycylglycinate Schiff base ligand (L³⁻). The Co^II atom sits on an inversion center and is coordinated to six aqua ligands in a slightly distorted octahedral geometry. The [Co(H₂O)₆]²⁺ cations and [NiL]⁻ anions form columns along the a axis by O—H⋯O hydrogen bonds. Additional hydrogen bonds between the uncoordinated and coordinated water molecules help to consolidate the crystal packing.

Related literature

For the structures of the copper(II) analogues, see: Liu et al. (2006 ); Zou et al. (2004 ). For the magnetic properties of copper(II) heteronuclear complexes, see: Liu et al. (2004 ); Zou et al. (2003 ).

Experimental

Crystal data

[Co(H₂O)₆][Ni(C₁₂H₁₁N₂O₅)]₂·6H₂O
M_r = 919.00
Triclinic, $[P \overline 1]$
a = 7.9052 (8) Å
b = 10.7595 (10) Å
c = 11.5032 (11) Å
α = 76.325 (1)°
β = 76.654 (1)°
γ = 80.334 (1)°
V = 918.34 (15) Å³
Z = 1
Mo Kα radiation
μ = 1.55 mm⁻¹
T = 296 K
0.30 × 0.30 × 0.25 mm

Data collection

Bruker SMART APEX CCD diffractometer
Absorption correction: multi-scan (SADABS; Sheldrick, 2004 ) T_min = 0.633, T_max = 0.672
7254 measured reflections
3572 independent reflections
3300 reflections with I > 2σ(I)
R_int = 0.073

Refinement

R[F² > 2σ(F²)] = 0.035
wR(F²) = 0.091
S = 1.04
3572 reflections
272 parameters
18 restraints
H atoms treated by a mixture of independent and constrained refinement
Δρ_max = 0.67 e Å⁻³
Δρ_min = −0.88 e Å⁻³

Table 1
Hydrogen-bond geometry (Å, °)

D—H⋯A	D—H	H⋯A	D⋯A	D—H⋯A
O6—H6A⋯O9	0.831 (16)	1.973 (17)	2.796 (2)	171 (3)
O6—H6B⋯O2	0.848 (16)	1.964 (16)	2.809 (2)	175 (3)
O7—H7A⋯O3	0.854 (16)	1.890 (17)	2.721 (2)	164 (3)
O7—H7B⋯O4ⁱ	0.844 (16)	2.007 (17)	2.835 (2)	167 (3)
O8—H8C⋯O10ⁱⁱ	0.827 (16)	1.914 (17)	2.733 (2)	170 (3)
O8—H8D⋯O11ⁱⁱ	0.844 (16)	1.927 (17)	2.756 (2)	167 (3)
O9—H9A⋯O11ⁱⁱⁱ	0.850 (17)	2.030 (17)	2.871 (2)	170 (3)
O9—H9B⋯O4^iv	0.824 (17)	2.121 (18)	2.941 (2)	173 (3)
O10—H10C⋯O4^v	0.822 (16)	1.963 (17)	2.775 (2)	169 (3)
O10—H10D⋯O3^vi	0.831 (17)	2.025 (17)	2.840 (2)	167 (3)
O11—H11B⋯O1^vii	0.850 (17)	1.976 (17)	2.817 (2)	170 (3)
O11—H11A⋯O10^viii	0.841 (17)	1.999 (18)	2.778 (2)	154 (3)
Symmetry codes: (i) -x+1, -y+2, -z+2; (ii) x, y+1, z; (iii) -x, -y+1, -z+1; (iv) x, y, z-1; (v) -x, -y+1, -z+2; (vi) x, y-1, z; (vii) -x+1, -y+1, -z+1; (viii) -x, -y, -z+1.

Data collection: SMART (Bruker, 2002 ); cell refinement: SAINT-Plus (Bruker, 2003 ); data reduction: SAINT-Plus; program(s) used to solve structure: SHELXTL (Sheldrick, 2008 ); program(s) used to refine structure: SHELXTL; molecular graphics: SHELXTL; software used to prepare material for publication: SHELXTL.

Supporting information

Crystal structure: contains datablocks I, global. DOI: 10.1107/S1600536809026750/pk2168sup1.cif

Structure factors: contains datablock I. DOI: 10.1107/S1600536809026750/pk2168Isup2.hkl

checkCIF report

Comment top

We have reported a series of heteronuclear complexes of Schiff bases synthesized from small peptides. Recently, we reported the copper(II) heteronuclear complexes of Schiff base ligands resulting from the condensation of simple peptides with salicylaldehyde (Liu et al., 2006; Zou et al., 2004) and magnetic properties (Liu et al., 2004; Zou et al., 2003). Hydrogen bonds play an important role in these complexes. Now we report the synthesis and structure of Ni(II)—Co(II) Schiff base complex derived from glycylglycine and 4-methoxy-salicylaldehyde. The heteronuclear complex crystallizes in the triclinic space group P1. The asymmetric unit consists of one [NiL]^- anion (L is a Schiff base derived from glycylglycine and 4-methoxy-salicylaldehyde), half a Co(H₂O)₆²⁺ cation [Co(1), O(6), O(7), O(8)] and three uncoordinated water molecules [O(9), O(10), O(11)] (Fig. 1). [NiL]^- has an approximate square-planar geometry. The deprotonated Schiff base is a triple negatively charged tetradentate ONNO ligand, coordinating to the Ni(II) center by one phenolate O atom [O(1)], one imine N atom [N(1)], one deprotonated amide N atom [N(2)] and one carboxylate O atom [O(3)]. The benzene ring [C(1)–C(6)] and the O(1), C(1), C(6), C(7), N(1), Ni(1) chelate ring are almost coplanar with a dihedral angle of 0.55 (7)°, suggesting a large π-electron delocalization. The Cobalt(II) atom lies on an inversion center and the coordination by six aqua ligands is slightly distorted octahedral. The six Co—O bonds in the structure are in the range of 2.0518 (13) - 2.0711 (14) Å. O—H···O hydrogen bonds (Table 1) play an important role in the stabilization of the crystal structure. The anions and cations form hydrogen bonded columns along the a-axis (Fig. 2). These are well segregated from each other.

Related literature top

For the structures of the copper(II) analogues, see: Liu et al. (2006); Zou et al. (2004). For the magnetic properties of copper(II) heteronuclear complexes, see: Liu et al. (2004); Zou et al. (2003).

Experimental top

Glycylglycine (5 mmol), 4-methoxy-salicylaldehyde (5 mmol) and LiOH (10 mmol) were dissolved in MeOH/H₂O (30 ml, v:v = 1:1) and refluxed for 30 min. Then Ni(ClO₄)₂.6H₂O (5 mmol) was added to the solution and the resulting solution was adjusted to pH 9–11 by 5 mol/L NaOH solution. After stirring at room temperature for 1 h, CoCl₂.6H₂O (2.5 mmol) was added. A yellow precipitate formed immediately, and was stirred for another 30 min and then filtere. The precipitate was recrystallized from water. Yellow crystals suitable for X-ray diffraction were obtained after one week. (yield 30% based on Ni(ClO₄)₂.6H₂O).

Computing details top

Data collection: SMART (Bruker, 2002); cell refinement: SAINT-Plus (Bruker, 2003); data reduction: SAINT-Plus (Bruker, 2003); program(s) used to solve structure: SHELXTL (Sheldrick, 2008); program(s) used to refine structure: SHELXTL (Sheldrick, 2008); molecular graphics: SHELXTL (Sheldrick, 2008); software used to prepare material for publication: SHELXTL (Sheldrick, 2008).

Figures top

	Fig. 1. The molecular structure with atom labels and 50% probability displacement ellipsoids. Unlabeled atoms are related to labeled atoms by the symmetry operation (-x + 1, -y + 2, -z + 1).
	Fig. 2. Crystal packing viewed down the a-axis, showing separated stacked columns connected by O—H···O hydrogen bonds (dashed lines).

Hexaaquacobalt(II) bis{[N-(4-methoxy-2-oxidobenzylidene)glycylglycinato]nickel(II)} hexahydrate top

Crystal data top

[Co(H₂O)₆][Ni(C₁₂H₁₁N₂O₅)]₂·6H₂O	Z = 1
M_r = 919.00	F(000) = 477
Triclinic, P1	D_x = 1.662 Mg m⁻³
Hall symbol: -P 1	Mo Kα radiation, λ = 0.71073 Å
a = 7.9052 (8) Å	Cell parameters from 6194 reflections
b = 10.7595 (10) Å	θ = 2.4–28.4°
c = 11.5032 (11) Å	µ = 1.55 mm⁻¹
α = 76.325 (1)°	T = 296 K
β = 76.654 (1)°	Block, yellow
γ = 80.334 (1)°	0.30 × 0.30 × 0.25 mm
V = 918.34 (15) Å³

Data collection top

Bruker SMART APEX CCD diffractometer	3572 independent reflections
Radiation source: sealed tube	3300 reflections with I > 2σ(I)
Graphite monochromator	R_int = 0.073
ϕ and ω scans	θ_max = 26.0°, θ_min = 1.9°
Absorption correction: multi-scan (SADABS; Sheldrick, 2004)	h = −9→9
T_min = 0.633, T_max = 0.672	k = −13→13
7254 measured reflections	l = −14→14

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)] = 0.035	Hydrogen site location: inferred from neighbouring sites
wR(F²) = 0.091	H atoms treated by a mixture of independent and constrained refinement
S = 1.04	w = 1/[σ²(F_o²) + (0.0608P)² + 0.0666P] where P = (F_o² + 2F_c²)/3
3572 reflections	(Δ/σ)_max = 0.002
272 parameters	Δρ_max = 0.67 e Å⁻³
18 restraints	Δρ_min = −0.88 e Å⁻³

Crystal data top

[Co(H₂O)₆][Ni(C₁₂H₁₁N₂O₅)]₂·6H₂O	γ = 80.334 (1)°
M_r = 919.00	V = 918.34 (15) Å³
Triclinic, P1	Z = 1
a = 7.9052 (8) Å	Mo Kα radiation
b = 10.7595 (10) Å	µ = 1.55 mm⁻¹
c = 11.5032 (11) Å	T = 296 K
α = 76.325 (1)°	0.30 × 0.30 × 0.25 mm
β = 76.654 (1)°

Data collection top

Bruker SMART APEX CCD diffractometer	3572 independent reflections
Absorption correction: multi-scan (SADABS; Sheldrick, 2004)	3300 reflections with I > 2σ(I)
T_min = 0.633, T_max = 0.672	R_int = 0.073
7254 measured reflections

Refinement top

R[F² > 2σ(F²)] = 0.035	18 restraints
wR(F²) = 0.091	H atoms treated by a mixture of independent and constrained refinement
S = 1.04	Δρ_max = 0.67 e Å⁻³
3572 reflections	Δρ_min = −0.88 e Å⁻³
272 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

	x	y	z	U_iso*/U_eq
Ni1	0.53859 (3)	0.70463 (2)	0.993860 (18)	0.02321 (10)
Co1	0.5000	1.0000	0.5000	0.02262 (11)
C1	0.7940 (2)	0.51644 (17)	0.89989 (17)	0.0253 (4)
C2	0.9034 (2)	0.46971 (18)	0.79967 (18)	0.0292 (4)
H2	0.9018	0.5164	0.7207	0.035*
C3	1.0127 (2)	0.35529 (19)	0.81779 (19)	0.0302 (4)
C4	1.0201 (3)	0.28302 (19)	0.9361 (2)	0.0349 (4)
H4	1.0962	0.2073	0.9477	0.042*
C5	0.9134 (3)	0.32634 (18)	1.03332 (19)	0.0329 (4)
H5	0.9168	0.2780	1.1115	0.039*
C6	0.7977 (2)	0.44218 (17)	1.01975 (17)	0.0273 (4)
C7	0.6938 (2)	0.48078 (18)	1.12730 (18)	0.0295 (4)
H7	0.7051	0.4269	1.2020	0.035*
C8	0.4866 (2)	0.6148 (2)	1.24644 (17)	0.0337 (4)
H8A	0.5669	0.6223	1.2960	0.040*
H8B	0.4162	0.5464	1.2908	0.040*
C9	0.3700 (2)	0.74026 (19)	1.22086 (16)	0.0268 (4)
C10	0.2913 (2)	0.90964 (18)	1.05217 (17)	0.0290 (4)
H10A	0.3237	0.9817	1.0760	0.035*
H10B	0.1664	0.9068	1.0811	0.035*
C11	0.3377 (2)	0.92460 (18)	0.91472 (17)	0.0282 (4)
C12	1.1187 (3)	0.3666 (2)	0.6024 (2)	0.0459 (5)
H12A	1.0029	0.3720	0.5875	0.069*
H12B	1.2000	0.3187	0.5483	0.069*
H12C	1.1511	0.4518	0.5884	0.069*
N1	0.58553 (19)	0.58460 (15)	1.12880 (14)	0.0268 (3)
N2	0.3876 (2)	0.79006 (16)	1.10386 (14)	0.0273 (3)
O1	0.69326 (16)	0.62706 (13)	0.87706 (12)	0.028
O2	0.45819 (18)	0.84079 (13)	0.87239 (11)	0.0307 (3)
O3	0.26077 (19)	1.01400 (14)	0.84986 (12)	0.0393 (3)
O4	0.27210 (18)	0.78848 (15)	1.30738 (12)	0.0342 (3)
O5	1.12210 (19)	0.30305 (15)	0.72600 (14)	0.0408 (3)
O6	0.4645 (2)	0.83132 (15)	0.62941 (13)	0.0392 (3)
H6A	0.387 (3)	0.794 (3)	0.618 (2)	0.059*
H6B	0.457 (4)	0.831 (3)	0.7041 (17)	0.059*
O7	0.46103 (19)	1.10891 (15)	0.63028 (12)	0.0339 (3)
H7A	0.386 (3)	1.093 (3)	0.6968 (19)	0.051*
H7B	0.551 (2)	1.129 (3)	0.645 (2)	0.051*
O8	0.23876 (17)	1.02599 (15)	0.49286 (13)	0.0361 (3)
H8C	0.162 (3)	1.018 (3)	0.5560 (17)	0.054*
H8D	0.208 (3)	1.089 (2)	0.4394 (19)	0.054*
O9	0.2328 (2)	0.69532 (17)	0.57292 (15)	0.0458 (4)
H9A	0.127 (3)	0.722 (3)	0.601 (2)	0.069*
H9B	0.251 (4)	0.717 (3)	0.4978 (15)	0.069*
O10	0.00613 (19)	0.01756 (16)	0.71029 (14)	0.0415 (4)
H10C	−0.067 (3)	0.081 (2)	0.699 (3)	0.062*
H10D	0.073 (3)	0.029 (3)	0.752 (3)	0.062*
O11	0.1080 (2)	0.20515 (16)	0.31073 (15)	0.0446 (4)
H11B	0.178 (3)	0.248 (3)	0.254 (2)	0.067*
H11A	0.080 (4)	0.150 (2)	0.280 (3)	0.067*

Atomic displacement parameters (Å²) top

	U¹¹	U²²	U³³	U¹²	U¹³	U²³
Ni1	0.02687 (14)	0.02163 (15)	0.01832 (14)	0.00209 (10)	−0.00428 (10)	−0.00239 (10)
Co1	0.02615 (18)	0.0238 (2)	0.01660 (18)	−0.00234 (14)	−0.00260 (13)	−0.00383 (13)
C1	0.0255 (8)	0.0193 (8)	0.0313 (9)	−0.0020 (6)	−0.0082 (7)	−0.0040 (7)
C2	0.0315 (9)	0.0232 (9)	0.0317 (10)	−0.0001 (7)	−0.0080 (7)	−0.0042 (7)
C3	0.0282 (8)	0.0240 (9)	0.0398 (11)	−0.0004 (7)	−0.0075 (8)	−0.0108 (8)
C4	0.0354 (9)	0.0230 (9)	0.0459 (12)	0.0035 (7)	−0.0143 (9)	−0.0048 (8)
C5	0.0369 (9)	0.0228 (10)	0.0387 (10)	−0.0010 (8)	−0.0158 (8)	0.0002 (8)
C6	0.0285 (8)	0.0198 (9)	0.0336 (10)	−0.0019 (7)	−0.0106 (7)	−0.0019 (7)
C7	0.0316 (8)	0.0253 (9)	0.0292 (9)	−0.0038 (7)	−0.0102 (7)	0.0036 (7)
C8	0.0333 (9)	0.0425 (11)	0.0222 (9)	−0.0015 (8)	−0.0066 (7)	−0.0020 (8)
C9	0.0269 (8)	0.0333 (10)	0.0215 (8)	−0.0059 (7)	−0.0044 (7)	−0.0067 (7)
C10	0.0351 (9)	0.0254 (9)	0.0244 (9)	0.0011 (7)	−0.0031 (7)	−0.0067 (7)
C11	0.0328 (9)	0.0238 (9)	0.0249 (9)	0.0013 (7)	−0.0026 (7)	−0.0053 (7)
C12	0.0519 (12)	0.0402 (13)	0.0409 (12)	0.0061 (10)	−0.0034 (10)	−0.0130 (10)
N1	0.0278 (7)	0.0279 (8)	0.0227 (7)	−0.0017 (6)	−0.0065 (6)	−0.0012 (6)
N2	0.0324 (7)	0.0260 (8)	0.0220 (7)	0.0015 (6)	−0.0053 (6)	−0.0053 (6)
O1	0.031	0.023	0.024	0.006	−0.004	−0.001
O2	0.0386 (7)	0.0272 (7)	0.0203 (6)	0.0076 (5)	−0.0038 (5)	−0.0035 (5)
O3	0.0491 (8)	0.0322 (8)	0.0258 (7)	0.0151 (6)	−0.0042 (6)	−0.0019 (6)
O4	0.0367 (7)	0.0427 (8)	0.0218 (7)	−0.0003 (6)	−0.0036 (5)	−0.0091 (6)
O5	0.0438 (8)	0.0324 (8)	0.0418 (8)	0.0109 (6)	−0.0068 (7)	−0.0116 (7)
O6	0.0556 (9)	0.0372 (8)	0.0253 (7)	−0.0144 (7)	−0.0108 (6)	0.0014 (6)
O7	0.0368 (7)	0.0401 (8)	0.0258 (7)	−0.0076 (6)	0.0001 (5)	−0.0129 (6)
O8	0.0303 (7)	0.0435 (9)	0.0288 (7)	0.0000 (6)	−0.0052 (5)	−0.0005 (6)
O9	0.0518 (9)	0.0448 (10)	0.0398 (9)	−0.0103 (8)	−0.0107 (7)	−0.0022 (7)
O10	0.0363 (7)	0.0485 (10)	0.0365 (8)	0.0039 (7)	−0.0028 (6)	−0.0128 (7)
O11	0.0486 (9)	0.0420 (9)	0.0361 (8)	−0.0067 (7)	−0.0053 (7)	0.0037 (7)

Geometric parameters (Å, º) top

Ni1—N2	1.8318 (15)	C8—H8A	0.9700
Ni1—N1	1.8364 (15)	C8—H8B	0.9700
Ni1—O1	1.8510 (13)	C9—O4	1.270 (2)
Ni1—O2	1.9058 (13)	C9—N2	1.310 (2)
Co1—O7ⁱ	2.0518 (13)	C10—N2	1.451 (2)
Co1—O7	2.0518 (13)	C10—C11	1.514 (3)
Co1—O8	2.0551 (13)	C10—H10A	0.9700
Co1—O8ⁱ	2.0551 (13)	C10—H10B	0.9700
Co1—O6	2.0711 (14)	C11—O3	1.235 (2)
Co1—O6ⁱ	2.0711 (14)	C11—O2	1.289 (2)
C1—O1	1.323 (2)	C12—O5	1.429 (3)
C1—C2	1.413 (3)	C12—H12A	0.9600
C1—C6	1.425 (3)	C12—H12B	0.9600
C2—C3	1.382 (3)	C12—H12C	0.9600
C2—H2	0.9300	O6—H6A	0.831 (16)
C3—O5	1.369 (2)	O6—H6B	0.848 (16)
C3—C4	1.408 (3)	O7—H7A	0.854 (16)
C4—C5	1.363 (3)	O7—H7B	0.844 (16)
C4—H4	0.9300	O8—H8C	0.827 (16)
C5—C6	1.416 (3)	O8—H8D	0.844 (16)
C5—H5	0.9300	O9—H9A	0.850 (17)
C6—C7	1.427 (3)	O9—H9B	0.824 (17)
C7—N1	1.289 (2)	O10—H10C	0.822 (16)
C7—H7	0.9300	O10—H10D	0.831 (17)
C8—N1	1.477 (2)	O11—H11B	0.850 (17)
C8—C9	1.509 (3)	O11—H11A	0.841 (17)

N2—Ni1—N1	85.19 (7)	C9—C8—H8A	110.0
N2—Ni1—O1	176.83 (6)	N1—C8—H8B	110.0
N1—Ni1—O1	97.51 (6)	C9—C8—H8B	110.0
N2—Ni1—O2	85.41 (6)	H8A—C8—H8B	108.4
N1—Ni1—O2	170.42 (6)	O4—C9—N2	126.66 (18)
O1—Ni1—O2	91.94 (5)	O4—C9—C8	121.02 (16)
O7ⁱ—Co1—O7	180.000 (1)	N2—C9—C8	112.30 (16)
O7ⁱ—Co1—O8	87.11 (6)	N2—C10—C11	107.22 (14)
O7—Co1—O8	92.89 (6)	N2—C10—H10A	110.3
O7ⁱ—Co1—O8ⁱ	92.89 (6)	C11—C10—H10A	110.3
O7—Co1—O8ⁱ	87.11 (6)	N2—C10—H10B	110.3
O8—Co1—O8ⁱ	180.000 (1)	C11—C10—H10B	110.3
O7ⁱ—Co1—O6	87.25 (6)	H10A—C10—H10B	108.5
O7—Co1—O6	92.75 (6)	O3—C11—O2	123.75 (17)
O8—Co1—O6	90.07 (6)	O3—C11—C10	119.65 (16)
O8ⁱ—Co1—O6	89.93 (6)	O2—C11—C10	116.61 (15)
O7ⁱ—Co1—O6ⁱ	92.75 (6)	O5—C12—H12A	109.5
O7—Co1—O6ⁱ	87.25 (6)	O5—C12—H12B	109.5
O8—Co1—O6ⁱ	89.93 (6)	H12A—C12—H12B	109.5
O8ⁱ—Co1—O6ⁱ	90.07 (6)	O5—C12—H12C	109.5
O6—Co1—O6ⁱ	180.00 (6)	H12A—C12—H12C	109.5
O1—C1—C2	118.00 (16)	H12B—C12—H12C	109.5
O1—C1—C6	123.54 (17)	C7—N1—C8	119.95 (16)
C2—C1—C6	118.46 (17)	C7—N1—Ni1	125.62 (13)
C3—C2—C1	120.68 (18)	C8—N1—Ni1	114.43 (12)
C3—C2—H2	119.7	C9—N2—C10	124.56 (16)
C1—C2—H2	119.7	C9—N2—Ni1	119.54 (13)
O5—C3—C2	124.42 (18)	C10—N2—Ni1	115.88 (12)
O5—C3—C4	114.44 (17)	C1—O1—Ni1	125.20 (11)
C2—C3—C4	121.15 (18)	C11—O2—Ni1	114.57 (11)
C5—C4—C3	118.64 (18)	C3—O5—C12	118.60 (16)
C5—C4—H4	120.7	Co1—O6—H6A	111 (2)
C3—C4—H4	120.7	Co1—O6—H6B	120 (2)
C4—C5—C6	122.47 (18)	H6A—O6—H6B	113 (2)
C4—C5—H5	118.8	Co1—O7—H7A	121.4 (18)
C6—C5—H5	118.8	Co1—O7—H7B	117.0 (18)
C5—C6—C1	118.58 (17)	H7A—O7—H7B	109 (2)
C5—C6—C7	118.28 (17)	Co1—O8—H8C	121.2 (18)
C1—C6—C7	123.11 (17)	Co1—O8—H8D	115.3 (19)
N1—C7—C6	124.99 (17)	H8C—O8—H8D	111 (2)
N1—C7—H7	117.5	H9A—O9—H9B	109 (2)
C6—C7—H7	117.5	H10C—O10—H10D	111 (2)
N1—C8—C9	108.53 (15)	H11B—O11—H11A	107 (2)
N1—C8—H8A	110.0

Symmetry code: (i) −x+1, −y+2, −z+1.

Hydrogen-bond geometry (Å, º) top

D—H···A	D—H	H···A	D···A	D—H···A
O6—H6A···O9	0.83 (2)	1.97 (2)	2.796 (2)	171 (3)
O6—H6B···O2	0.85 (2)	1.96 (2)	2.809 (2)	175 (3)
O7—H7A···O3	0.85 (2)	1.89 (2)	2.721 (2)	164 (3)
O7—H7B···O4ⁱⁱ	0.84 (2)	2.01 (2)	2.835 (2)	167 (3)
O8—H8C···O10ⁱⁱⁱ	0.83 (2)	1.91 (2)	2.733 (2)	170 (3)
O8—H8D···O11ⁱⁱⁱ	0.84 (2)	1.93 (2)	2.756 (2)	167 (3)
O9—H9A···O11^iv	0.85 (2)	2.03 (2)	2.871 (2)	170 (3)
O9—H9B···O4^v	0.82 (2)	2.12 (2)	2.941 (2)	173 (3)
O10—H10C···O4^vi	0.82 (2)	1.96 (2)	2.775 (2)	169 (3)
O10—H10D···O3^vii	0.83 (2)	2.03 (2)	2.840 (2)	167 (3)
O11—H11B···O1^viii	0.85 (2)	1.98 (2)	2.817 (2)	170 (3)
O11—H11A···O10^ix	0.84 (2)	2.00 (2)	2.778 (2)	154 (3)

Symmetry codes: (ii) −x+1, −y+2, −z+2; (iii) x, y+1, z; (iv) −x, −y+1, −z+1; (v) x, y, z−1; (vi) −x, −y+1, −z+2; (vii) x, y−1, z; (viii) −x+1, −y+1, −z+1; (ix) −x, −y, −z+1.

Experimental details

Crystal data
Chemical formula	[Co(H₂O)₆][Ni(C₁₂H₁₁N₂O₅)]₂·6H₂O
M_r	919.00
Crystal system, space group	Triclinic, P1
Temperature (K)	296
a, b, c (Å)	7.9052 (8), 10.7595 (10), 11.5032 (11)
α, β, γ (°)	76.325 (1), 76.654 (1), 80.334 (1)
V (Å³)	918.34 (15)
Z	1
Radiation type	Mo Kα
µ (mm⁻¹)	1.55
Crystal size (mm)	0.30 × 0.30 × 0.25

Data collection
Diffractometer	Bruker SMART APEX CCD diffractometer
Absorption correction	Multi-scan (SADABS; Sheldrick, 2004)
T_min, T_max	0.633, 0.672
No. of measured, independent and observed [I > 2σ(I)] reflections	7254, 3572, 3300
R_int	0.073
(sin θ/λ)_max (Å⁻¹)	0.617

Refinement
R[F² > 2σ(F²)], wR(F²), S	0.035, 0.091, 1.04
No. of reflections	3572
No. of parameters	272
No. of restraints	18
H-atom treatment	H atoms treated by a mixture of independent and constrained refinement
Δρ_max, Δρ_min (e Å⁻³)	0.67, −0.88

Computer programs: SMART (Bruker, 2002), SAINT-Plus (Bruker, 2003), SHELXTL (Sheldrick, 2008).

Hydrogen-bond geometry (Å, º) top

D—H···A	D—H	H···A	D···A	D—H···A
O6—H6A···O9	0.831 (16)	1.973 (17)	2.796 (2)	171 (3)
O6—H6B···O2	0.848 (16)	1.964 (16)	2.809 (2)	175 (3)
O7—H7A···O3	0.854 (16)	1.890 (17)	2.721 (2)	164 (3)
O7—H7B···O4ⁱ	0.844 (16)	2.007 (17)	2.835 (2)	167 (3)
O8—H8C···O10ⁱⁱ	0.827 (16)	1.914 (17)	2.733 (2)	170 (3)
O8—H8D···O11ⁱⁱ	0.844 (16)	1.927 (17)	2.756 (2)	167 (3)
O9—H9A···O11ⁱⁱⁱ	0.850 (17)	2.030 (17)	2.871 (2)	170 (3)
O9—H9B···O4^iv	0.824 (17)	2.121 (18)	2.941 (2)	173 (3)
O10—H10C···O4^v	0.822 (16)	1.963 (17)	2.775 (2)	169 (3)
O10—H10D···O3^vi	0.831 (17)	2.025 (17)	2.840 (2)	167 (3)
O11—H11B···O1^vii	0.850 (17)	1.976 (17)	2.817 (2)	170 (3)
O11—H11A···O10^viii	0.841 (17)	1.999 (18)	2.778 (2)	154 (3)

Symmetry codes: (i) −x+1, −y+2, −z+2; (ii) x, y+1, z; (iii) −x, −y+1, −z+1; (iv) x, y, z−1; (v) −x, −y+1, −z+2; (vi) x, y−1, z; (vii) −x+1, −y+1, −z+1; (viii) −x, −y, −z+1.

Acknowledgements

This work was supported by SRF for ROCS, SEM and Yangzhou University.

References

Bruker (2002). SMART. Bruker AXS Inc., Madison, Wisconsin, USA. Google Scholar
Bruker (2003). SAINT-Plus. Bruker AXS Inc, Madison, Wisconsin, USA. Google Scholar
Liu, W. L., Liu, X. F., Lu, Y. & Hu, X. Y. (2006). J. Coord. Chem. pp. 721–728. Web of Science CSD CrossRef Google Scholar
Liu, W. L., Song, Y., Li, Y. Z., Zou, Y., Dang, D. B., Ni, C. L. & Meng, Q. J. (2004). Chem. Commun. pp. 2946–2947. Google Scholar
Sheldrick, G. M. (2004). SADABS. University of Göttingen, Germany. Google Scholar
Sheldrick, G. M. (2008). Acta Cryst. A64, 112–122. Web of Science CrossRef CAS IUCr Journals Google Scholar
Zou, Y., Liu, W. L., Gao, S., Xi, J. L. & Meng, Q. J. (2003). Chem. Commun. pp. 2946–2947. CSD CrossRef Google Scholar
Zou, Y., Liu, W. L., Lu, C. S., Wen, L. L. & Meng, Q. J. (2004). Inorg. Chem. Commun. pp. 985–987. Web of Science CSD CrossRef Google Scholar

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Volume 65| Part 8| August 2009| Page m952

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metal-organic compounds\(\def\hfill{\hskip 5em}\def\hfil{\hskip 3em}\def\eqno#1{\hfil {#1}}\)

Hexa­aqua­cobalt(II) bis­­{[N-(4-meth­­oxy-2-oxido­benzyl­­idene)glycylglycinato]nickel(II)} hexa­hydrate

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Experimental

Crystal data

Data collection

Refinement

Supporting information

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References

metal-organic compounds

Hexaaquacobalt(II) bis{[N-(4-methoxy-2-oxidobenzylidene)glycylglycinato]nickel(II)} hexahydrate