Tetra­kis[tris­(2,2′-bi-1H-benzimidazole)nickel(II)] bis­(phosphate) sulfate

Ling, C.-S.; Yan, L.

doi:10.1107/S1600536808032571

metal-organic compounds

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ISSN: 2056-9890

Volume 64| Part 11| November 2008| Page m1399

doi:10.1107/S1600536808032571

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Tetrakis[tris(2,2′-bi-1H-benzimidazole)nickel(II)] bis(phosphate) sulfate

Chun-Sheng Ling ^a and Lin Yan ^a ^*

^aInstitute of Pharmacy, Henan University, Kaifeng 475004, People's Republic of China
^*Correspondence e-mail: yanlin_online@163.com

(Received 28 September 2008; accepted 8 October 2008; online 15 October 2008)

The title compound, [Ni(C₁₄H₁₀N₄)₃]₄(PO₄)₂(SO₄), consists of [Ni(C₁₄H₁₀N₄)₃]²⁺ complex cations (.3. symmetry) and disordered anions ( $[{\overline 4}]$ symmetry) with occupancy factors of two-thirds for PO₄³⁻ and one-third for SO₄²⁻. The Ni²⁺ centre is chelated by three bidentate 2,2′-bi-1H-benzimidazole molecules in a distorted octahedral coordination. N—H⋯O hydrogen bonds consolidate the building units into a framework structure.

Related literature

For the potential applications of metal–organic coordination compounds in gas absorption and separation, catalysis, non-linear optics, luminescence and magnetism, see: Kitagawa & Matsuda (2007 ); Maspoch et al. (2007 ).

Experimental

Crystal data

[Ni(C₁₄H₁₀N₄)₃]₄(PO₄)₂(SO₄)
M_r = 3331.96
Cubic, $[I \overline 43d ]$
a = 24.964 (7) Å
V = 15558 (8) Å³
Z = 4
Mo Kα radiation
μ = 0.59 mm⁻¹
T = 296 (2) K
0.32 × 0.27 × 0.23 mm

Data collection

Bruker SMART CCD area-detector diffractometer
Absorption correction: multi-scan (SADABS; Sheldrick, 2001 ) T_min = 0.834, T_max = 0.876
20222 measured reflections
2551 independent reflections
1782 reflections with I > 2σ(I)
R_int = 0.066

Refinement

R[F² > 2σ(F²)] = 0.038
wR(F²) = 0.098
S = 1.01
2551 reflections
177 parameters
H-atom parameters constrained
Δρ_max = 0.61 e Å⁻³
Δρ_min = −0.20 e Å⁻³
Absolute structure: Flack (1983 ), 1182 Friedel pairs
Flack parameter: −0.02 (2)

Table 1
Hydrogen-bond geometry (Å, °)

D—H⋯A	D—H	H⋯A	D⋯A	D—H⋯A
N4—H4B⋯O1ⁱ	0.86	1.96	2.766 (4)	156
N2—H2B⋯O1ⁱⁱ	0.86	1.82	2.675 (4)	170
Symmetry codes: (i) $[x-{\script{1\over 4}}, -z+{\script{5\over 4}}, -y+{\script{3\over 4}}]$ ; (ii) x, y, z-1.

Data collection: SMART (Bruker, 2001 ); cell refinement: SAINT-Plus (Bruker, 2001); data reduction: SAINT-Plus; 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/S1600536808032571/at2642sup1.cif

Structure factors: contains datablock I. DOI: 10.1107/S1600536808032571/at2642Isup2.hkl

checkCIF report

Comment top

More attentions have been paid to metal-organic coordination compounds (MOCCs) because of their potential applications in gas absorption and separation, catalysis, nonlinear optics, luminescence and magnetism (Kitagawa & Matsuda 2007, Maspoch et al. 2007). In the field of coordination chemistry, the N,N-bidentate ligands, such as 2,2'-bipyridine, 1,10-phenanthroline and their derivatives act as versatile ligands owing to the stable coordination configuration in the bidentate N-donors chelating manner. Herein, we report the title compound (I).

The title compound (I) consists of four [Ni(C₁₄H₁₀N₄)₃]²⁺ complex cations, one [SO₄]^2- and two [PO₄]^3- anions. In the mlecular structure, the Ni²⁺ centre is coordinated by six N atoms from three bidentate 1H,1'H-2,2'-bi-1H-benzimidazole molecules (Fig.1). The 1H,1'H-2,2'-bi-1H-benzimidazole ligand was prepared in situ and coordinated to the Ni²⁺ cations in hydrothermal reaction. Additionally, the [SO₄]^2- and [PO₄]^3- anions statistically distribute in one position with 1/3 probability for S and 2/3 probability for P atoms. The environment of the Ni²⁺ caion is in a distorted octahedral geometry with the Ni—N distances ranging from 2.088 (3) to 2.122 (3) Å (Table 1).

In addition, the [Ni(C₁₄H₁₀N₄)₃]²⁺ complex cations, [SO₄]^2- and [PO₄]^3- anions in the complexes are linked together via many N—H···O hydrogen bonds resulting in a three-dimensional structural frameworks (Fig.2 and Table 2).

Related literature top

For the potential applications of metal–organic coordination compounds in gas absorption and separation, catalysis, nonlinear optics, luminescence and magnetism, see: Kitagawa & Matsuda (2007); Maspoch et al. (2007).

Experimental top

All reagents were commercially available and of analytical grade. The mixture of NiSO₄.6H₂O, H₃PO₄, oxalic acid, and 1,2-diaminobenzene in the mole ratio of 1: 1.5: 6: 6 was dissolved in 25 ml H₂O, which was heated in a Teflon-lined steel autoclave inside a programmable electric furnace at 393 K for five days. After cooling the autoclave to room temperature, green block crystals of (I) were obtained.

Computing details top

Data collection: SMART (Bruker, 2001); cell refinement: SAINT-Plus (Bruker, 2001); data reduction: SAINT-Plus (Bruker, 2001); 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 molecular structure of (I), showing the atom-labelling scheme. Displacement ellipsoids are drawn at the 50% probability level. H atoms are omitted for clarity.
	Fig. 2. Three-dimensional structure of (I). Displacement ellipsoids are drawn at the 50% probability level. For clarity, H atoms not involved in hydrogen bonds are omitted.

Tetrakis[tris(2,2'-bi-1H-benzimidazole)nickel(II)] bis(phosphate) sulfate top

Crystal data top

[Ni(C₁₄H₁₀N₄)₃]₄(PO₄)₂(SO₄)	D_x = 1.423 Mg m⁻³
M_r = 3331.96	Mo Kα radiation, λ = 0.71073 Å
Cubic, I43d	Cell parameters from 3375 reflections
Hall symbol: I -4bd 2c 3	θ = 2.3–19.2°
a = 24.964 (7) Å	µ = 0.59 mm⁻¹
V = 15558 (8) Å³	T = 296 K
Z = 4	Block, green
F(000) = 6872	0.32 × 0.27 × 0.23 mm

Data collection top

Bruker SMART CCD area-detector diffractometer	2551 independent reflections
Radiation source: fine-focus sealed tube	1782 reflections with I > 2σ(I)
Graphite monochromator	R_int = 0.066
ϕ and ω scans	θ_max = 26.0°, θ_min = 2.0°
Absorption correction: multi-scan (SADABS; Sheldrick, 2001)	h = −30→11
T_min = 0.834, T_max = 0.876	k = −30→29
20222 measured reflections	l = −21→20

Refinement top

Refinement on F²	Secondary atom site location: difference Fourier map
Least-squares matrix: full	Hydrogen site location: inferred from neighbouring sites
R[F² > 2σ(F²)] = 0.038	H-atom parameters constrained
wR(F²) = 0.098	w = 1/[σ²(F_o²) + (0.0528P)²] where P = (F_o² + 2F_c²)/3
S = 1.01	(Δ/σ)_max = 0.001
2551 reflections	Δρ_max = 0.61 e Å⁻³
177 parameters	Δρ_min = −0.20 e Å⁻³
0 restraints	Absolute structure: Flack (1983), 1182 Friedel pairs
Primary atom site location: structure-invariant direct methods	Absolute structure parameter: −0.02 (2)

Crystal data top

[Ni(C₁₄H₁₀N₄)₃]₄(PO₄)₂(SO₄)	Z = 4
M_r = 3331.96	Mo Kα radiation
Cubic, I43d	µ = 0.59 mm⁻¹
a = 24.964 (7) Å	T = 296 K
V = 15558 (8) Å³	0.32 × 0.27 × 0.23 mm

Data collection top

Bruker SMART CCD area-detector diffractometer	2551 independent reflections
Absorption correction: multi-scan (SADABS; Sheldrick, 2001)	1782 reflections with I > 2σ(I)
T_min = 0.834, T_max = 0.876	R_int = 0.066
20222 measured reflections

Refinement top

R[F² > 2σ(F²)] = 0.038	H-atom parameters constrained
wR(F²) = 0.098	Δρ_max = 0.61 e Å⁻³
S = 1.01	Δρ_min = −0.20 e Å⁻³
2551 reflections	Absolute structure: Flack (1983), 1182 Friedel pairs
177 parameters	Absolute structure parameter: −0.02 (2)
0 restraints

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	0.564621 (16)	0.435379 (16)	−0.064621 (16)	0.0428 (2)
P1	0.7500	0.6250	1.0000	0.0427 (4)	0.67
S1	0.7500	0.6250	1.0000	0.0427 (4)	0.33
N1	0.64773 (10)	0.44469 (11)	−0.06574 (11)	0.0443 (6)
N2	0.71668 (10)	0.50117 (12)	−0.06248 (11)	0.0498 (7)
H2B	0.7340	0.5309	−0.0604	0.060*
N3	0.56297 (10)	0.42828 (11)	0.02009 (10)	0.0444 (6)
N4	0.55652 (11)	0.37290 (12)	0.08942 (11)	0.0502 (7)
H4B	0.5538	0.3435	0.1072	0.060*
C1	0.69498 (13)	0.41559 (13)	−0.06917 (13)	0.0462 (8)
C2	0.70405 (15)	0.36114 (16)	−0.07434 (15)	0.0594 (9)
H2	0.6758	0.3370	−0.0763	0.071*
C3	0.75637 (17)	0.34409 (18)	−0.07642 (16)	0.0744 (13)
H3	0.7638	0.3077	−0.0797	0.089*
C4	0.79858 (16)	0.3808 (2)	−0.07359 (16)	0.0707 (12)
H4	0.8335	0.3679	−0.0750	0.085*
C5	0.79104 (13)	0.43383 (18)	−0.06895 (15)	0.0627 (10)
H5	0.8197	0.4576	−0.0670	0.075*
C6	0.73810 (12)	0.45147 (14)	−0.06724 (14)	0.0473 (8)
C7	0.66286 (13)	0.49523 (14)	−0.06164 (13)	0.0443 (8)
C8	0.56226 (15)	0.45873 (13)	0.06673 (14)	0.0487 (9)
C9	0.56566 (17)	0.51278 (15)	0.07424 (15)	0.0645 (11)
H9	0.5681	0.5363	0.0455	0.077*
C10	0.5653 (2)	0.53090 (18)	0.12671 (19)	0.0848 (13)
H10	0.5672	0.5675	0.1333	0.102*
C11	0.5623 (2)	0.49628 (19)	0.16920 (17)	0.0863 (14)
H11	0.5627	0.5102	0.2037	0.104*
C12	0.55859 (18)	0.44183 (18)	0.16272 (14)	0.0698 (11)
H12	0.5562	0.4186	0.1917	0.084*
C13	0.55865 (13)	0.42369 (14)	0.11042 (13)	0.0489 (8)
C14	0.55946 (13)	0.37792 (14)	0.03571 (13)	0.0443 (8)
O1	0.77314 (11)	0.59036 (9)	0.95604 (10)	0.0629 (7)

Atomic displacement parameters (Å²) top

	U¹¹	U²²	U³³	U¹²	U¹³	U²³
Ni1	0.0428 (2)	0.0428 (2)	0.0428 (2)	−0.00140 (19)	−0.00140 (19)	0.00140 (19)
P1	0.0469 (6)	0.0341 (9)	0.0469 (6)	0.000	0.000	0.000
S1	0.0469 (6)	0.0341 (9)	0.0469 (6)	0.000	0.000	0.000
N1	0.0386 (14)	0.0485 (17)	0.0458 (16)	0.0000 (13)	−0.0006 (13)	0.0019 (15)
N2	0.0447 (17)	0.0543 (18)	0.0503 (17)	−0.0083 (14)	−0.0009 (14)	−0.0019 (15)
N3	0.0432 (16)	0.0445 (16)	0.0456 (15)	0.0006 (15)	−0.0046 (13)	−0.0007 (13)
N4	0.0552 (19)	0.0518 (18)	0.0436 (17)	−0.0046 (14)	−0.0034 (14)	0.0093 (14)
C1	0.049 (2)	0.0486 (19)	0.0411 (18)	0.0030 (16)	−0.0031 (17)	−0.0036 (15)
C2	0.054 (2)	0.060 (2)	0.065 (2)	0.0073 (18)	−0.0023 (19)	−0.0042 (19)
C3	0.064 (3)	0.076 (3)	0.084 (3)	0.024 (2)	−0.003 (2)	−0.009 (2)
C4	0.045 (2)	0.097 (4)	0.070 (3)	0.021 (2)	−0.002 (2)	−0.014 (2)
C5	0.0439 (19)	0.083 (3)	0.061 (3)	0.000 (2)	−0.0050 (18)	−0.016 (3)
C6	0.0417 (19)	0.064 (2)	0.0366 (18)	0.0018 (16)	−0.0048 (16)	−0.0077 (17)
C7	0.044 (2)	0.048 (2)	0.0410 (19)	−0.0065 (15)	−0.0027 (15)	−0.0012 (16)
C8	0.049 (2)	0.052 (2)	0.0449 (19)	0.0051 (16)	−0.0042 (18)	−0.0057 (16)
C9	0.092 (3)	0.050 (2)	0.051 (2)	−0.002 (2)	−0.009 (2)	−0.0036 (17)
C10	0.124 (4)	0.065 (3)	0.066 (3)	0.006 (3)	−0.010 (3)	−0.013 (2)
C11	0.133 (4)	0.077 (3)	0.049 (3)	0.001 (3)	−0.013 (3)	−0.017 (2)
C12	0.093 (3)	0.074 (3)	0.042 (2)	−0.006 (3)	−0.005 (2)	0.001 (2)
C13	0.050 (2)	0.055 (2)	0.0423 (19)	−0.0009 (18)	−0.0050 (16)	−0.0006 (16)
C14	0.0315 (18)	0.053 (2)	0.049 (2)	−0.0032 (16)	−0.0021 (15)	0.0045 (17)
O1	0.0818 (18)	0.0455 (15)	0.0616 (17)	−0.0077 (13)	0.0150 (14)	−0.0033 (12)

Geometric parameters (Å, º) top

Ni1—N1	2.088 (3)	C1—C6	1.401 (5)
Ni1—N1ⁱ	2.088 (3)	C2—C3	1.375 (5)
Ni1—N1ⁱⁱ	2.088 (3)	C2—H2	0.9300
Ni1—N3ⁱⁱ	2.122 (3)	C3—C4	1.398 (6)
Ni1—N3	2.122 (3)	C3—H3	0.9300
Ni1—N3ⁱ	2.122 (3)	C4—C5	1.342 (6)
P1—O1ⁱⁱⁱ	1.512 (3)	C4—H4	0.9300
P1—O1^iv	1.512 (3)	C5—C6	1.394 (4)
P1—O1	1.512 (3)	C5—H5	0.9300
P1—O1^v	1.512 (3)	C7—C14ⁱⁱ	1.435 (5)
N1—C7	1.321 (4)	C8—C9	1.365 (5)
N1—C1	1.388 (4)	C8—C13	1.401 (5)
N2—C7	1.352 (4)	C9—C10	1.386 (6)
N2—C6	1.356 (4)	C9—H9	0.9300
N2—H2B	0.8600	C10—C11	1.370 (6)
N3—C14	1.319 (4)	C10—H10	0.9300
N3—C8	1.391 (4)	C11—C12	1.372 (6)
N4—C14	1.349 (4)	C11—H11	0.9300
N4—C13	1.373 (4)	C12—C13	1.382 (5)
N4—H4B	0.8600	C12—H12	0.9300
C1—C2	1.384 (5)	C14—C7ⁱ	1.435 (5)

N1—Ni1—N1ⁱ	95.67 (10)	C1—C2—H2	121.2
N1—Ni1—N1ⁱⁱ	95.67 (10)	C2—C3—C4	120.7 (4)
N1ⁱ—Ni1—N1ⁱⁱ	95.67 (10)	C2—C3—H3	119.6
N1—Ni1—N3ⁱⁱ	78.84 (10)	C4—C3—H3	119.6
N1ⁱ—Ni1—N3ⁱⁱ	170.67 (9)	C5—C4—C3	123.0 (4)
N1ⁱⁱ—Ni1—N3ⁱⁱ	92.40 (9)	C5—C4—H4	118.5
N1—Ni1—N3	92.40 (9)	C3—C4—H4	118.5
N1ⁱ—Ni1—N3	78.84 (10)	C4—C5—C6	116.6 (4)
N1ⁱⁱ—Ni1—N3	170.67 (9)	C4—C5—H5	121.7
N3ⁱⁱ—Ni1—N3	93.75 (9)	C6—C5—H5	121.7
N1—Ni1—N3ⁱ	170.67 (9)	N2—C6—C5	131.7 (3)
N1ⁱ—Ni1—N3ⁱ	92.40 (9)	N2—C6—C1	106.6 (3)
N1ⁱⁱ—Ni1—N3ⁱ	78.84 (10)	C5—C6—C1	121.7 (3)
N3ⁱⁱ—Ni1—N3ⁱ	93.75 (9)	N1—C7—N2	112.8 (3)
N3—Ni1—N3ⁱ	93.75 (9)	N1—C7—C14ⁱⁱ	118.2 (3)
O1ⁱⁱⁱ—P1—O1^iv	110.22 (17)	N2—C7—C14ⁱⁱ	128.9 (3)
O1ⁱⁱⁱ—P1—O1	109.10 (9)	C9—C8—N3	130.9 (3)
O1^iv—P1—O1	109.10 (9)	C9—C8—C13	121.0 (3)
O1ⁱⁱⁱ—P1—O1^v	109.10 (9)	N3—C8—C13	108.1 (3)
O1^iv—P1—O1^v	109.10 (9)	C8—C9—C10	116.9 (4)
O1—P1—O1^v	110.22 (17)	C8—C9—H9	121.6
C7—N1—C1	105.2 (3)	C10—C9—H9	121.6
C7—N1—Ni1	112.9 (2)	C11—C10—C9	121.7 (4)
C1—N1—Ni1	141.9 (2)	C11—C10—H10	119.1
C7—N2—C6	107.0 (3)	C9—C10—H10	119.1
C7—N2—H2B	126.5	C10—C11—C12	122.5 (4)
C6—N2—H2B	126.5	C10—C11—H11	118.7
C14—N3—C8	105.8 (3)	C12—C11—H11	118.7
C14—N3—Ni1	112.0 (2)	C11—C12—C13	115.8 (4)
C8—N3—Ni1	142.1 (2)	C11—C12—H12	122.1
C14—N4—C13	107.0 (3)	C13—C12—H12	122.1
C14—N4—H4B	126.5	N4—C13—C12	131.5 (3)
C13—N4—H4B	126.5	N4—C13—C8	106.4 (3)
C2—C1—N1	131.2 (3)	C12—C13—C8	122.1 (3)
C2—C1—C6	120.4 (3)	N3—C14—N4	112.7 (3)
N1—C1—C6	108.4 (3)	N3—C14—C7ⁱ	117.7 (3)
C3—C2—C1	117.6 (4)	N4—C14—C7ⁱ	129.5 (3)
C3—C2—H2	121.2

N1ⁱ—Ni1—N1—C7	−168.5 (2)	C2—C1—C6—N2	179.6 (3)
N1ⁱⁱ—Ni1—N1—C7	95.2 (3)	N1—C1—C6—N2	0.3 (4)
N3ⁱⁱ—Ni1—N1—C7	3.9 (2)	C2—C1—C6—C5	−1.8 (5)
N3—Ni1—N1—C7	−89.5 (3)	N1—C1—C6—C5	178.9 (3)
N3ⁱ—Ni1—N1—C7	41.7 (7)	C1—N1—C7—N2	0.4 (4)
N1ⁱ—Ni1—N1—C1	11.1 (4)	Ni1—N1—C7—N2	−179.9 (2)
N1ⁱⁱ—Ni1—N1—C1	−85.2 (3)	C1—N1—C7—C14ⁱⁱ	177.6 (3)
N3ⁱⁱ—Ni1—N1—C1	−176.5 (4)	Ni1—N1—C7—C14ⁱⁱ	−2.6 (4)
N3—Ni1—N1—C1	90.1 (4)	C6—N2—C7—N1	−0.2 (4)
N3ⁱ—Ni1—N1—C1	−138.6 (6)	C6—N2—C7—C14ⁱⁱ	−177.1 (3)
N1—Ni1—N3—C14	−100.0 (2)	C14—N3—C8—C9	178.8 (4)
N1ⁱ—Ni1—N3—C14	−4.7 (2)	Ni1—N3—C8—C9	−4.5 (7)
N1ⁱⁱ—Ni1—N3—C14	49.9 (7)	C14—N3—C8—C13	0.5 (4)
N3ⁱⁱ—Ni1—N3—C14	−178.9 (2)	Ni1—N3—C8—C13	177.2 (3)
N3ⁱ—Ni1—N3—C14	87.1 (3)	N3—C8—C9—C10	−178.2 (4)
N1—Ni1—N3—C8	83.5 (4)	C13—C8—C9—C10	0.0 (6)
N1ⁱ—Ni1—N3—C8	178.8 (4)	C8—C9—C10—C11	0.7 (7)
N1ⁱⁱ—Ni1—N3—C8	−126.7 (6)	C9—C10—C11—C12	−1.0 (8)
N3ⁱⁱ—Ni1—N3—C8	4.5 (4)	C10—C11—C12—C13	0.6 (8)
N3ⁱ—Ni1—N3—C8	−89.5 (3)	C14—N4—C13—C12	−178.1 (4)
C7—N1—C1—C2	−179.6 (4)	C14—N4—C13—C8	0.8 (4)
Ni1—N1—C1—C2	0.7 (7)	C11—C12—C13—N4	178.7 (4)
C7—N1—C1—C6	−0.4 (4)	C11—C12—C13—C8	0.0 (6)
Ni1—N1—C1—C6	180.0 (3)	C9—C8—C13—N4	−179.3 (3)
N1—C1—C2—C3	−179.6 (3)	N3—C8—C13—N4	−0.8 (4)
C6—C1—C2—C3	1.2 (5)	C9—C8—C13—C12	−0.3 (6)
C1—C2—C3—C4	−0.3 (6)	N3—C8—C13—C12	178.2 (4)
C2—C3—C4—C5	−0.2 (6)	C8—N3—C14—N4	0.0 (4)
C3—C4—C5—C6	−0.3 (6)	Ni1—N3—C14—N4	−177.9 (2)
C7—N2—C6—C5	−178.5 (4)	C8—N3—C14—C7ⁱ	−177.4 (3)
C7—N2—C6—C1	0.0 (4)	Ni1—N3—C14—C7ⁱ	4.8 (3)
C4—C5—C6—N2	179.5 (4)	C13—N4—C14—N3	−0.5 (4)
C4—C5—C6—C1	1.3 (6)	C13—N4—C14—C7ⁱ	176.5 (3)

Symmetry codes: (i) −z+1/2, −x+1, y−1/2; (ii) −y+1, z+1/2, −x+1/2; (iii) −z+7/4, −y+5/4, x+1/4; (iv) z−1/4, −y+5/4, −x+7/4; (v) −x+3/2, y, −z+2.

Hydrogen-bond geometry (Å, º) top

D—H···A	D—H	H···A	D···A	D—H···A
N4—H4B···O1^vi	0.86	1.96	2.766 (4)	156
N2—H2B···O1^vii	0.86	1.82	2.675 (4)	170

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

Experimental details

Crystal data
Chemical formula	[Ni(C₁₄H₁₀N₄)₃]₄(PO₄)₂(SO₄)
M_r	3331.96
Crystal system, space group	Cubic, I43d
Temperature (K)	296
a (Å)	24.964 (7)
V (Å³)	15558 (8)
Z	4
Radiation type	Mo Kα
µ (mm⁻¹)	0.59
Crystal size (mm)	0.32 × 0.27 × 0.23

Data collection
Diffractometer	Bruker SMART CCD area-detector diffractometer
Absorption correction	Multi-scan (SADABS; Sheldrick, 2001)
T_min, T_max	0.834, 0.876
No. of measured, independent and observed [I > 2σ(I)] reflections	20222, 2551, 1782
R_int	0.066
(sin θ/λ)_max (Å⁻¹)	0.617

Refinement
R[F² > 2σ(F²)], wR(F²), S	0.038, 0.098, 1.01
No. of reflections	2551
No. of parameters	177
H-atom treatment	H-atom parameters constrained
Δρ_max, Δρ_min (e Å⁻³)	0.61, −0.20
Absolute structure	Flack (1983), 1182 Friedel pairs
Absolute structure parameter	−0.02 (2)

Computer programs: SMART (Bruker, 2001), SAINT-Plus (Bruker, 2001), SHELXS97 (Sheldrick, 2008), SHELXL97 (Sheldrick, 2008), SHELXTL (Sheldrick, 2008).

Hydrogen-bond geometry (Å, º) top

D—H···A	D—H	H···A	D···A	D—H···A
N4—H4B···O1ⁱ	0.86	1.96	2.766 (4)	156.1
N2—H2B···O1ⁱⁱ	0.86	1.82	2.675 (4)	170.0

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

Acknowledgements

This work was supported by the Basic Research Foundation for Natural Science of Henan University.

References

Bruker (2001). SMART and SAINT-Plus. Bruker AXS Inc., Madison, Wisconsin, USA. Google Scholar
Flack, H. D. (1983). Acta Cryst. A39, 876–881. CrossRef CAS Web of Science IUCr Journals Google Scholar
Kitagawa, S. & Matsuda, R. (2007). Coord. Chem. Rev. 251, 2490–2509. Web of Science CrossRef CAS Google Scholar
Maspoch, D., Ruiz-Molina, D. & Veciana, J. (2007). Chem. Soc. Rev. 36, 770–818. Web of Science CrossRef PubMed CAS Google Scholar
Sheldrick, G. M. (2001). 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