[μ-10,21-Dimethyl-3,6,14,17-tetra­aza­tricyclo­[17.3.1.18,12]tetra­cosa-1(23),8(24),9,11,19,21-hexa­ene-23,24-diolato-κ8N3,N6,O23,O24:N14,N17,O23,O24]bis­[(nitrato-κ2O,O′)nickel(II)]

Li, Q.-J.; Ma, J.-F.; Liu, J.; Han, T.-T.

doi:10.1107/S1600536809010174

metal-organic compounds

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ISSN: 2056-9890

Volume 65| Part 5| May 2009| Page m522

doi:10.1107/S1600536809010174

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[μ-10,21-Dimethyl-3,6,14,17-tetraazatricyclo[17.3.1.1^8,12]tetracosa-1(23),8(24),9,11,19,21-hexaene-23,24-diolato-κ⁸N³,N⁶,O²³,O²⁴:N¹⁴,N¹⁷,O²³,O²⁴]bis[(nitrato-κ²O,O′)nickel(II)]

Quan-Jun Li,^a Jian-Fang Ma,^a ^* Jie Liu ^a and Ting-Ting Han ^a

^aDepartment of Chemistry, Northeast Normal University, Changchun 130024, People's Republic of China
^*Correspondence e-mail: majf247nenu@yahoo.com.cn

(Received 11 March 2009; accepted 19 March 2009; online 18 April 2009)

In the title centrosymmetric dinuclear nickel complex, [Ni₂(C₂₂H₃₀N₄O₂)(NO₃)₂], each of the two Ni^II atoms has a distorted octahedral geometry, defined by two N atoms and two O atoms from the macrocyclic ligand and two O atoms from a chelating nitrate anion. The two Ni atoms are bridged by two phenolate O atoms, forming a four-membered Ni₂O₂ ring.

Related literature

For general background, see: Caldwell & Crumbliss (1998 ); Rosa et al. (1998 ). For related structures, see: Aromi et al. (2002 ). For the ligand synthesis, see: Mandal & Nag (1986 ).

Experimental

Crystal data

[Ni₂(C₂₂H₃₀N₄O₂)(NO₃)₂]
M_r = 623.90
Trigonal, $[R \overline 3]$
a = 25.020 (5) Å
c = 10.616 (5) Å
V = 5755 (3) Å³
Z = 9
Mo Kα radiation
μ = 1.53 mm⁻¹
T = 293 K
0.40 × 0.30 × 0.25 mm

Data collection

Bruker APEX CCD diffractometer
Absorption correction: multi-scan (SADABS; Sheldrick, 1996 ) T_min = 0.495, T_max = 0.609 (expected range = 0.554–0.682)
9432 measured reflections
2213 independent reflections
1745 reflections with I > 2σ(I)
R_int = 0.107

Refinement

R[F² > 2σ(F²)] = 0.043
wR(F²) = 0.117
S = 1.03
2213 reflections
178 parameters
1 restraint
H atoms treated by a mixture of independent and constrained refinement
Δρ_max = 1.06 e Å⁻³
Δρ_min = −0.35 e Å⁻³

Table 1
Selected bond lengths (Å)

Ni1—O1	2.000 (2)
Ni1—O1ⁱ	2.006 (2)
Ni1—N2	2.038 (3)
Ni1—N1	2.054 (3)
Ni1—O3	2.134 (3)
Ni1—O2	2.183 (3)
Symmetry code: (i) $[-x+{\script{2\over 3}}, -y+{\script{1\over 3}}, -z+{\script{1\over 3}}]$ .

Data collection: SMART (Bruker, 2007 ); cell refinement: SAINT (Bruker, 2007); 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: SHELXL97.

Supporting information

Crystal structure: contains datablocks global, I. DOI: 10.1107/S1600536809010174/hy2188sup1.cif

Structure factors: contains datablock I. DOI: 10.1107/S1600536809010174/hy2188Isup2.hkl

checkCIF report

Comment top

Crown ether compounds have attracted much interest as a result of their significance in biological transport systems (Caldwell & Crumbliss, 1998). In addition, crown ether compounds are found to have functions in selective molecular recognition (Rosa et al., 1998). To further widen the scope of applications of crown ether, there is a need to prepare new series of crown ether compounds. In this work, a new dinuclear nickel(II) compound has been synthesized and its struture is reported here.

As shown in Fig. 1, the title compound is a centrosymmetric dinuclear nickel complex. The coordination environment around each Ni^II atom is distorted octahedral, with one N atom and one O atom from the macrocyclic ligand and two O atoms from the nitrate anion occupying the equatorial plane, and the other N atom and O atom from the ligand occupying the axial positions. In the complex molecule, two Ni atoms are bridged by two phenolate O atoms, generating a four-membered Ni₂O₂ ring, with a Ni···Ni distance of 2.9737 (10) Å. The Ni—O and Ni—N distances are normal (Aromi et al., 2002).

Related literature top

For general background, see: Caldwell & Crumbliss (1998); Rosa et al. (1998). For related structures, see: Aromi et al. (2002). For the ligand synthesis, see: Mandal & Nag (1986).

Experimental top

The macrocyclic ligand, C₂₂H₃₂N₄O₂ (H₂L), was prepared by the reported procedure (Mandal & Nag, 1986). A mixture of H₂L (0.10 g, 0.26 mmol) and Ni(NO₃)₂.6H₂O (0.15 g, 0.52 mmol) in methanol (20 ml) was stirred for 10 min. The resulting solution was filtered. Green single crystals were obtained by slow evaporation of the filtrate at room temperature (yield 56%).

Computing details top

Data collection: SMART (Bruker, 2007); cell refinement: SAINT (Bruker, 2007); data reduction: SAINT (Bruker, 2007); 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: SHELXL97 (Sheldrick, 2008).

Figures top

Fig. 1. Molecular structure of the title compound. Displacement ellipsoids are draw at the 30% probability level. H atoms have been omitted for clarity. [Symmetry code: (i) -x + 2/3, -y + 1/3, -z + 1/3.]

[µ-10,21-Dimethyl-3,6,14,17-tetraazatricyclo[17.3.1.1^8,12]tetracosa- 1(23),8(24),9,11,19,21-hexaene-23,24-diolato- κ⁸N³,N⁶,O²³,O²⁴:N¹⁴, N¹⁷,O²³,O²⁴]bis[(nitrato- κ²O,O')nickel(II)] top

Crystal data top

[Ni₂(C₂₂H₃₀N₄O₂)(NO₃)₂]	D_x = 1.620 Mg m⁻³
M_r = 623.90	Mo Kα radiation, λ = 0.71069 Å
Trigonal, R3	Cell parameters from 3000 reflections
Hall symbol: -R 3	θ = 2.4–28.4°
a = 25.020 (5) Å	µ = 1.53 mm⁻¹
c = 10.616 (5) Å	T = 293 K
V = 5755 (3) Å³	Block, green
Z = 9	0.40 × 0.30 × 0.25 mm
F(000) = 2916

Data collection top

Bruker APEX CCD diffractometer	2213 independent reflections
Radiation source: fine-focus sealed tube	1745 reflections with I > 2σ(I)
Graphite monochromator	R_int = 0.107
ϕ and ω scans	θ_max = 24.9°, θ_min = 1.6°
Absorption correction: multi-scan (SADABS; Sheldrick, 1996)	h = −15→29
T_min = 0.495, T_max = 0.609	k = −29→23
9432 measured reflections	l = −12→12

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)] = 0.043	Hydrogen site location: inferred from neighbouring sites
wR(F²) = 0.117	H atoms treated by a mixture of independent and constrained refinement
S = 1.03	w = 1/[σ²(F_o²) + (0.066P)²] where P = (F_o² + 2F_c²)/3
2213 reflections	(Δ/σ)_max = 0.007
178 parameters	Δρ_max = 1.06 e Å⁻³
1 restraint	Δρ_min = −0.35 e Å⁻³

Crystal data top

[Ni₂(C₂₂H₃₀N₄O₂)(NO₃)₂]	Z = 9
M_r = 623.90	Mo Kα radiation
Trigonal, R3	µ = 1.53 mm⁻¹
a = 25.020 (5) Å	T = 293 K
c = 10.616 (5) Å	0.40 × 0.30 × 0.25 mm
V = 5755 (3) Å³

Data collection top

Bruker APEX CCD diffractometer	2213 independent reflections
Absorption correction: multi-scan (SADABS; Sheldrick, 1996)	1745 reflections with I > 2σ(I)
T_min = 0.495, T_max = 0.609	R_int = 0.107
9432 measured reflections

Refinement top

R[F² > 2σ(F²)] = 0.043	1 restraint
wR(F²) = 0.117	H atoms treated by a mixture of independent and constrained refinement
S = 1.03	Δρ_max = 1.06 e Å⁻³
2213 reflections	Δρ_min = −0.35 e Å⁻³
178 parameters

Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å²) top

	x	y	z	U_iso*/U_eq
Ni1	0.355561 (19)	0.13534 (2)	0.25357 (4)	0.03150 (19)
C1	0.04882 (19)	−0.0620 (2)	0.3314 (4)	0.0658 (13)
H1A	0.0488	−0.0770	0.4147	0.099*
H1B	0.0372	−0.0948	0.2717	0.099*
H1C	0.0199	−0.0475	0.3276	0.099*
C2	0.11262 (17)	−0.00973 (17)	0.3005 (3)	0.0431 (9)
C3	0.12561 (16)	0.01995 (17)	0.1862 (3)	0.0410 (9)
H3	0.0947	0.0056	0.1255	0.049*
C4	0.18315 (15)	0.07079 (16)	0.1570 (3)	0.0353 (8)
C5	0.22847 (15)	0.09460 (15)	0.2510 (3)	0.0347 (8)
C6	0.16018 (17)	0.01062 (17)	0.3868 (3)	0.0446 (9)
H6	0.1536	−0.0111	0.4617	0.054*
C7	0.21738 (16)	0.06230 (16)	0.3656 (3)	0.0374 (8)
C8	0.26663 (17)	0.08766 (18)	0.4652 (3)	0.0443 (9)
H8A	0.2746	0.1284	0.4892	0.053*
H8B	0.2515	0.0614	0.5391	0.053*
C9	0.37778 (18)	0.13034 (17)	0.5104 (3)	0.0430 (9)
H9A	0.4112	0.1221	0.4949	0.052*
H9B	0.3646	0.1196	0.5972	0.052*
C10	0.40046 (18)	0.19842 (17)	0.4892 (3)	0.0421 (9)
H10A	0.3704	0.2085	0.5224	0.050*
H10B	0.4390	0.2230	0.5342	0.050*
C11	0.47350 (15)	0.23666 (16)	0.3077 (3)	0.0383 (8)
H11A	0.4824	0.2031	0.3091	0.046*
H11B	0.5022	0.2685	0.3644	0.046*
N1	0.32528 (14)	0.09201 (14)	0.4244 (3)	0.0377 (7)
N2	0.41009 (14)	0.21377 (13)	0.3532 (2)	0.0355 (7)
N3	0.37310 (14)	0.05216 (15)	0.1596 (3)	0.0479 (8)
O1	0.28230 (10)	0.14687 (10)	0.23716 (19)	0.0342 (5)
O2	0.41509 (12)	0.09599 (12)	0.2220 (2)	0.0455 (6)
O3	0.32302 (12)	0.05220 (12)	0.1480 (2)	0.0459 (6)
O4	0.38022 (15)	0.01126 (15)	0.1141 (4)	0.0853 (11)
HN1	0.320 (3)	0.055 (3)	0.423 (6)	0.128*
HN2	0.401 (3)	0.242 (2)	0.336 (6)	0.128*

Atomic displacement parameters (Å²) top

	U¹¹	U²²	U³³	U¹²	U¹³	U²³
Ni1	0.0299 (3)	0.0299 (3)	0.0353 (3)	0.0154 (2)	−0.00202 (16)	0.00065 (16)
C1	0.041 (3)	0.060 (3)	0.081 (3)	0.014 (2)	0.014 (2)	0.004 (2)
C2	0.037 (2)	0.035 (2)	0.052 (2)	0.0137 (17)	0.0119 (16)	−0.0027 (16)
C3	0.033 (2)	0.038 (2)	0.055 (2)	0.0200 (18)	−0.0023 (16)	−0.0069 (16)
C4	0.0299 (19)	0.0322 (19)	0.0451 (18)	0.0165 (16)	0.0011 (14)	−0.0002 (14)
C5	0.0322 (19)	0.033 (2)	0.0424 (18)	0.0193 (17)	0.0038 (14)	−0.0001 (14)
C6	0.044 (2)	0.042 (2)	0.049 (2)	0.022 (2)	0.0114 (17)	0.0067 (16)
C7	0.037 (2)	0.037 (2)	0.0402 (18)	0.0193 (17)	0.0053 (15)	0.0017 (14)
C8	0.043 (2)	0.051 (2)	0.0380 (18)	0.024 (2)	0.0040 (15)	0.0054 (16)
C9	0.047 (2)	0.045 (2)	0.0366 (18)	0.0226 (19)	−0.0053 (15)	0.0029 (15)
C10	0.048 (2)	0.043 (2)	0.0359 (18)	0.0227 (19)	−0.0046 (15)	−0.0049 (15)
C11	0.033 (2)	0.034 (2)	0.049 (2)	0.0181 (17)	−0.0105 (15)	−0.0059 (15)
N1	0.0404 (18)	0.0370 (18)	0.0381 (14)	0.0211 (16)	−0.0010 (12)	0.0024 (13)
N2	0.0366 (17)	0.0327 (17)	0.0383 (15)	0.0182 (15)	−0.0035 (12)	−0.0001 (12)
N3	0.0349 (19)	0.040 (2)	0.067 (2)	0.0180 (16)	−0.0012 (15)	−0.0111 (16)
O1	0.0289 (13)	0.0311 (13)	0.0408 (12)	0.0137 (11)	−0.0007 (10)	0.0025 (10)
O2	0.0341 (14)	0.0377 (15)	0.0634 (16)	0.0171 (13)	−0.0070 (12)	−0.0076 (12)
O3	0.0329 (15)	0.0434 (16)	0.0570 (15)	0.0159 (13)	−0.0059 (11)	−0.0075 (11)
O4	0.058 (2)	0.062 (2)	0.139 (3)	0.0324 (18)	−0.0003 (19)	−0.048 (2)

Geometric parameters (Å, º) top

Ni1—O1	2.000 (2)	C7—C8	1.502 (5)
Ni1—O1ⁱ	2.006 (2)	C8—N1	1.481 (5)
Ni1—N2	2.038 (3)	C8—H8A	0.9700
Ni1—N1	2.054 (3)	C8—H8B	0.9700
Ni1—O3	2.134 (3)	C9—N1	1.489 (4)
Ni1—O2	2.183 (3)	C9—C10	1.519 (5)
Ni1—Ni1ⁱ	2.9737 (10)	C9—H9A	0.9700
C1—C2	1.510 (5)	C9—H9B	0.9700
C1—H1A	0.9600	C10—N2	1.483 (4)
C1—H1B	0.9600	C10—H10A	0.9700
C1—H1C	0.9600	C10—H10B	0.9700
C2—C3	1.374 (5)	C11—N2	1.473 (4)
C2—C6	1.382 (5)	C11—C4ⁱ	1.505 (5)
C3—C4	1.398 (5)	C11—H11A	0.9700
C3—H3	0.9300	C11—H11B	0.9700
C4—C5	1.400 (5)	N1—HN1	0.87 (6)
C4—C11ⁱ	1.505 (5)	N2—HN2	0.86 (6)
C5—O1	1.336 (4)	N3—O4	1.223 (4)
C5—C7	1.408 (5)	N3—O3	1.260 (4)
C6—C7	1.386 (5)	N3—O2	1.262 (4)
C6—H6	0.9300

O1—Ni1—O1ⁱ	84.17 (9)	N1—C8—C7	113.5 (3)
O1—Ni1—N2	97.29 (10)	N1—C8—H8A	108.9
O1ⁱ—Ni1—N2	87.95 (10)	C7—C8—H8A	108.9
O1—Ni1—N1	91.74 (10)	N1—C8—H8B	108.9
O1ⁱ—Ni1—N1	172.81 (10)	C7—C8—H8B	108.9
N2—Ni1—N1	86.72 (12)	H8A—C8—H8B	107.7
O1—Ni1—O3	99.46 (9)	N1—C9—C10	110.3 (3)
O1ⁱ—Ni1—O3	91.39 (10)	N1—C9—H9A	109.6
N2—Ni1—O3	163.09 (11)	C10—C9—H9A	109.6
N1—Ni1—O3	95.11 (11)	N1—C9—H9B	109.6
O1—Ni1—O2	158.83 (9)	C10—C9—H9B	109.6
O1ⁱ—Ni1—O2	92.93 (9)	H9A—C9—H9B	108.1
N2—Ni1—O2	103.57 (11)	N2—C10—C9	110.8 (3)
N1—Ni1—O2	92.99 (11)	N2—C10—H10A	109.5
O3—Ni1—O2	59.57 (10)	C9—C10—H10A	109.5
O1—Ni1—Ni1ⁱ	42.16 (6)	N2—C10—H10B	109.5
O1ⁱ—Ni1—Ni1ⁱ	42.01 (6)	C9—C10—H10B	109.5
N2—Ni1—Ni1ⁱ	93.51 (8)	H10A—C10—H10B	108.1
N1—Ni1—Ni1ⁱ	133.62 (9)	N2—C11—C4ⁱ	112.7 (3)
O3—Ni1—Ni1ⁱ	97.29 (7)	N2—C11—H11A	109.0
O2—Ni1—Ni1ⁱ	131.44 (7)	C4ⁱ—C11—H11A	109.0
C2—C1—H1A	109.5	N2—C11—H11B	109.0
C2—C1—H1B	109.5	C4ⁱ—C11—H11B	109.0
H1A—C1—H1B	109.5	H11A—C11—H11B	107.8
C2—C1—H1C	109.5	C8—N1—C9	113.0 (3)
H1A—C1—H1C	109.5	C8—N1—Ni1	112.8 (2)
H1B—C1—H1C	109.5	C9—N1—Ni1	103.2 (2)
C3—C2—C6	117.3 (3)	C8—N1—HN1	108 (4)
C3—C2—C1	121.5 (4)	C9—N1—HN1	108 (4)
C6—C2—C1	121.2 (4)	Ni1—N1—HN1	112 (4)
C2—C3—C4	123.0 (3)	C11—N2—C10	115.1 (3)
C2—C3—H3	118.5	C11—N2—Ni1	106.0 (2)
C4—C3—H3	118.5	C10—N2—Ni1	108.2 (2)
C3—C4—C5	118.4 (3)	C11—N2—HN2	107 (4)
C3—C4—C11ⁱ	118.1 (3)	C10—N2—HN2	110 (4)
C5—C4—C11ⁱ	123.5 (3)	Ni1—N2—HN2	110 (4)
O1—C5—C4	122.9 (3)	O4—N3—O3	121.5 (3)
O1—C5—C7	118.0 (3)	O4—N3—O2	121.9 (3)
C4—C5—C7	119.1 (3)	O3—N3—O2	116.6 (3)
C2—C6—C7	122.2 (3)	C5—O1—Ni1	113.40 (19)
C2—C6—H6	118.9	C5—O1—Ni1ⁱ	125.52 (19)
C7—C6—H6	118.9	Ni1—O1—Ni1ⁱ	95.83 (9)
C6—C7—C5	119.4 (3)	N3—O2—Ni1	90.8 (2)
C6—C7—C8	121.7 (3)	N3—O3—Ni1	93.11 (19)
C5—C7—C8	118.7 (3)

C6—C2—C3—C4	−3.1 (5)	O2—Ni1—N2—C11	32.8 (2)
C1—C2—C3—C4	176.2 (4)	Ni1ⁱ—Ni1—N2—C11	−101.34 (19)
C2—C3—C4—C5	−3.7 (5)	O1—Ni1—N2—C10	92.5 (2)
C2—C3—C4—C11ⁱ	175.9 (3)	O1ⁱ—Ni1—N2—C10	176.3 (2)
C3—C4—C5—O1	−172.4 (3)	N1—Ni1—N2—C10	1.1 (2)
C11ⁱ—C4—C5—O1	8.1 (5)	O3—Ni1—N2—C10	−95.6 (4)
C3—C4—C5—C7	7.8 (5)	O2—Ni1—N2—C10	−91.1 (2)
C11ⁱ—C4—C5—C7	−171.7 (3)	Ni1ⁱ—Ni1—N2—C10	134.7 (2)
C3—C2—C6—C7	5.8 (5)	C4—C5—O1—Ni1	−120.4 (3)
C1—C2—C6—C7	−173.5 (4)	C7—C5—O1—Ni1	59.4 (3)
C2—C6—C7—C5	−1.7 (5)	C4—C5—O1—Ni1ⁱ	−4.0 (4)
C2—C6—C7—C8	173.8 (3)	C7—C5—O1—Ni1ⁱ	175.8 (2)
O1—C5—C7—C6	174.9 (3)	O1ⁱ—Ni1—O1—C5	132.9 (2)
C4—C5—C7—C6	−5.2 (5)	N2—Ni1—O1—C5	−139.9 (2)
O1—C5—C7—C8	−0.7 (5)	N1—Ni1—O1—C5	−53.0 (2)
C4—C5—C7—C8	179.1 (3)	O3—Ni1—O1—C5	42.4 (2)
C6—C7—C8—N1	123.4 (4)	O2—Ni1—O1—C5	49.8 (3)
C5—C7—C8—N1	−61.0 (4)	Ni1ⁱ—Ni1—O1—C5	132.9 (2)
N1—C9—C10—N2	−48.9 (4)	O1ⁱ—Ni1—O1—Ni1ⁱ	0.0
C7—C8—N1—C9	166.4 (3)	N2—Ni1—O1—Ni1ⁱ	87.17 (11)
C7—C8—N1—Ni1	49.9 (4)	N1—Ni1—O1—Ni1ⁱ	174.08 (11)
C10—C9—N1—C8	−76.0 (4)	O3—Ni1—O1—Ni1ⁱ	−90.44 (10)
C10—C9—N1—Ni1	46.1 (3)	O2—Ni1—O1—Ni1ⁱ	−83.0 (3)
N2—Ni1—N1—C8	96.4 (2)	O4—N3—O2—Ni1	−179.5 (4)
O3—Ni1—N1—C8	−100.4 (2)	O3—N3—O2—Ni1	−0.4 (3)
O2—Ni1—N1—C8	−160.1 (2)	O1—Ni1—O2—N3	−8.2 (4)
Ni1ⁱ—Ni1—N1—C8	4.7 (3)	O1ⁱ—Ni1—O2—N3	−89.6 (2)
N2—Ni1—N1—C9	−25.8 (2)	N2—Ni1—O2—N3	−178.2 (2)
O3—Ni1—N1—C9	137.3 (2)	N1—Ni1—O2—N3	94.4 (2)
O2—Ni1—N1—C9	77.6 (2)	O3—Ni1—O2—N3	0.24 (19)
Ni1ⁱ—Ni1—N1—C9	−117.5 (2)	Ni1ⁱ—Ni1—O2—N3	−71.0 (2)
C4ⁱ—C11—N2—C10	−169.3 (3)	O4—N3—O3—Ni1	179.5 (4)
C4ⁱ—C11—N2—Ni1	71.2 (3)	O2—N3—O3—Ni1	0.4 (3)
C9—C10—N2—C11	−94.0 (4)	O1—Ni1—O3—N3	176.7 (2)
C9—C10—N2—Ni1	24.3 (4)	O1ⁱ—Ni1—O3—N3	92.3 (2)
O1—Ni1—N2—C11	−143.54 (19)	N2—Ni1—O3—N3	4.8 (5)
O1ⁱ—Ni1—N2—C11	−59.7 (2)	N1—Ni1—O3—N3	−90.7 (2)
N1—Ni1—N2—C11	125.1 (2)	O2—Ni1—O3—N3	−0.24 (19)
O3—Ni1—N2—C11	28.3 (5)	Ni1ⁱ—Ni1—O3—N3	134.08 (19)

Symmetry code: (i) −x+2/3, −y+1/3, −z+1/3.

Experimental details

Crystal data
Chemical formula	[Ni₂(C₂₂H₃₀N₄O₂)(NO₃)₂]
M_r	623.90
Crystal system, space group	Trigonal, R3
Temperature (K)	293
a, c (Å)	25.020 (5), 10.616 (5)
V (Å³)	5755 (3)
Z	9
Radiation type	Mo Kα
µ (mm⁻¹)	1.53
Crystal size (mm)	0.40 × 0.30 × 0.25

Data collection
Diffractometer	Bruker APEX CCD diffractometer
Absorption correction	Multi-scan (SADABS; Sheldrick, 1996)
T_min, T_max	0.495, 0.609
No. of measured, independent and observed [I > 2σ(I)] reflections	9432, 2213, 1745
R_int	0.107
(sin θ/λ)_max (Å⁻¹)	0.593

Refinement
R[F² > 2σ(F²)], wR(F²), S	0.043, 0.117, 1.03
No. of reflections	2213
No. of parameters	178
No. of restraints	1
H-atom treatment	H atoms treated by a mixture of independent and constrained refinement
Δρ_max, Δρ_min (e Å⁻³)	1.06, −0.35

Computer programs: SMART (Bruker, 2007), SAINT (Bruker, 2007), SHELXS97 (Sheldrick, 2008), SHELXL97 (Sheldrick, 2008), SHELXTL (Sheldrick, 2008).

Selected bond lengths (Å) top

Ni1—O1	2.000 (2)	Ni1—N1	2.054 (3)
Ni1—O1ⁱ	2.006 (2)	Ni1—O3	2.134 (3)
Ni1—N2	2.038 (3)	Ni1—O2	2.183 (3)

Symmetry code: (i) −x+2/3, −y+1/3, −z+1/3.

Acknowledgements

We thank the National Natural Science Foundation of China (grant No. 20471014), the Program for New Century Excellent Talents in Chinese Universities (grant No. NCET-05-0320), the Fok Ying Tung Education Foundation and the Analysis and Testing Foundation of Northeast Normal University for support.

References

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