Aqua­[2,6-bis­(2-pyridylamino)pyridine]sulfatonickel(II) monohydrate

Lu, L.; Wang, J.; Xie, B.; Zou, L.-K.

doi:10.1107/S1600536808035101

metal-organic compounds

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ISSN: 2056-9890

Volume 64| Part 12| December 2008| Pages m1490-m1491

doi:10.1107/S1600536808035101

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Aqua[2,6-bis(2-pyridylamino)pyridine]sulfatonickel(II) monohydrate

Lu Lu,^a ^* Jun Wang,^a Bin Xie ^a and Li-Ke Zou ^a

^aDepartment of Chemistry and Pharmaceutical Engineering, Sichuan University of Science and Engineering, Zigong, Sichuan 643000, People's Republic of China
^*Correspondence e-mail: lulusczg@126.com

(Received 23 October 2008; accepted 28 October 2008; online 8 November 2008)

The Ni atom in the title complex, [Ni(SO₄)(C₁₅H₁₃N₅)(H₂O)]·H₂O, has a distorted trigonal-bipyramidal coordination formed by the tridentate 2,6-bis(2-pyridylamino)pyridine (tpdaH₂) ligand, one sulfate and one coordinated water molecule. The tpdaH₂ ligand is three-coordinated, with the N atom of the central pyridine ring in the equatorial position [Ni—N = 1.9961 (14) Å] and the N atoms of the peripheral pyridine rings in the axial positions [Ni—N = 1.9668 (15) and 1.9895 (15) Å]. The remaining equatorial positions are occupied by the O atoms of the sulfate ligand and the water molecule. The H atoms of both NH groups of the tpdaH₂ ligand are involved in hydrogen bonds with the O atoms of the uncoordinated water molecule and the sulfate group which link the complex molecules, forming an infinite three-dimensional network.

Related literature

For the properties of transition metal complexes with polypyridylamine ligands, see: Wang et al. (1999 ). For the tri-pyridyldiamine ligand, see: Jing et al. (2000 ). For metal–metal interactions, see: Cotton et al. (1998 ); Yang et al. (1997 ).

Experimental

Crystal data

[Ni(SO₄)(C₁₅H₁₃N₅)(H₂O)]·H₂O
M_r = 454.11
Monoclinic, P 2₁ /n
a = 7.3536 (8) Å
b = 18.026 (2) Å
c = 12.9125 (14) Å
β = 95.634 (2)°
V = 1703.3 (3) Å³
Z = 4
Mo Kα radiation
μ = 1.31 mm⁻¹
T = 298 (2) K
0.22 × 0.16 × 0.12 mm

Data collection

Bruker APEXII area-detector diffractometer
Absorption correction: multi-scan (SADABS; Bruker, 2004 ) T_min = 0.761, T_max = 0.859
8650 measured reflections
3068 independent reflections
2821 reflections with I > 2σ(I)
R_int = 0.014

Refinement

R[F² > 2σ(F²)] = 0.021
wR(F²) = 0.056
S = 1.06
3068 reflections
259 parameters
8 restraints
H atoms treated by a mixture of independent and constrained refinement
Δρ_max = 0.24 e Å⁻³
Δρ_min = −0.32 e Å⁻³

Table 1
Hydrogen-bond geometry (Å, °)

D—H⋯A	D—H	H⋯A	D⋯A	D—H⋯A
N2—H2B⋯O6ⁱ	0.866 (9)	2.079 (10)	2.9433 (19)	176 (2)
N4—H4B⋯O4ⁱⁱ	0.862 (9)	2.050 (10)	2.8967 (18)	167.1 (18)
O5—H5A⋯O6	0.86	2.08	2.9112 (18)	163
O5—H5B⋯O4ⁱⁱⁱ	0.85	1.98	2.8192 (19)	169
O6—H6A⋯O2^iv	0.85	1.91	2.7531 (18)	173
O6—H6B⋯O3ⁱⁱⁱ	0.85	1.97	2.785 (2)	162
Symmetry codes: (i) -x, -y, -z+1; (ii) -x+1, -y, -z; (iii) x-1, y, z; (iv) $[x-{\script{1\over 2}}, -y+{\script{1\over 2}}, z+{\script{1\over 2}}]$ .

Data collection: APEX2 (Bruker, 2004); cell refinement: APEX2 and SAINT (Bruker, 2004); data reduction: SAINT; program(s) used to solve structure: SHELXS97 (Sheldrick, 2008 ); program(s) used to refine structure: SHELXL97 (Sheldrick, 2008); molecular graphics: ORTEPIII (Burnett & Johnson, 1996 ) and ORTEP-3 for Windows (Farrugia, 1997 ); software used to prepare material for publication: SHELXL97.

Supporting information

Crystal structure: contains datablocks I, global. DOI: 10.1107/S1600536808035101/dn2397sup1.cif

Structure factors: contains datablock I. DOI: 10.1107/S1600536808035101/dn2397Isup2.hkl

checkCIF report

Comment top

Transition metal complexes with polypyridylamine ligands, possessing diverse structures and special optical and electromagnetic properties (Wang et al.,1999), have aroused great interest among researchers, Tri-pyridyldiamine ligand usually exhibits donor as well as acceptor properties and can be used as a popular chelating ligand (Jing et al., 2000). In recent years great efforts have been taken to synthesize and characterize metal chain complexes which can be used to study the metal-metal interactions (Yang et al., 1997; Cotton et al., 1998). Herein we report the synthesis and crystal structure of the title complex with tri-pyridyldiamine ligand.

The Ni1 atom in the title complex has a distorted trigonal-bipyramidal coordination formed by the tridentate tpdaH₂ ligand, one sulfate and one coordinated water molecule. (Fig. 1). The tpdaH₂ ligand is tri-coordinated, with the peripheral N1 and N5 atoms in the axial positions [Ni1—N1 = 1.9895 (15) Å, Ni1—N5 = 1.9668 (15) Å and N1—Ni1—N5 = 169.26 (6)°] and the central N3 atom in the equatorial plane of the bipyramid [Ni1—N3 = 1.9961 (14) Å]. The remaining equatorial positions are occupied by one sulfate and one coordinated water molecule. Selected geometric parameters have been listed in tabel 1.

The three pyridine rings of the tpdaH₂ ligand are not coplanar. The dihedral angles between the planes of the central pyridine ring and two peripheral rings are 15.0 (7) and 22.7 (3)° respectively. In the title complex the two H atoms of both NH groups of tpdaH₂ act as active H atoms in forming inter-molecular classical hydrogen bonds (Table 2). The inter-molecular hydrogen bonds function greatly in linking the complex to be a infinite three-dimensional network.

Related literature top

For the properties of transition metal complexes with polypyridylamine ligands, see: Wang et al. (1999). For the tri-pyridyldiamine ligand, see: Jing et al. (2000). For metal–metal

interactions, see: Cotton et al. (1998); Yang et al. (1997).

Experimental top

Tripyridyldiamine (0.031 g, 0.12 mmol), NiSO4 (0.26 g, 0.13 mmol), were added in a solvent of acetonitrile, the mixture was heated for six hours under reflux. during the process stirring and influx were required. The resultant was then filtered to give a pure solution which was infiltrated by diethyl ether freely in a closed vessel, three weeks later some single crystals of the size suitable for X-Ray diffraction analysis.

Computing details top

Data collection: APEX2 (Bruker, 2004); cell refinement: APEX2 (Bruker, 2004) and SAINT (Bruker, 2004); data reduction: SAINT (Bruker, 2004); program(s) used to solve structure: SHELXS97 (Sheldrick, 2008); program(s) used to refine structure: SHELXL97 (Sheldrick, 2008); molecular graphics: ORTEPIII (Burnett & Johnson, 1996) and ORTEP-3 for Windows (Farrugia, 1997);; software used to prepare material for publication: SHELXL97 (Sheldrick, 2008).

Figures top

Fig. 1. View of compound (I) with the atom-labeling scheme. Displacement ellipsoids are drawn at the 30% probability level. Only H atoms attached to water have been represented as small spheres of arbitrary radii. H bond is shown as dashed line.

Aqua[2,6-bis(2-pyridylamino)pyridine]sulfatonickel(II) monohydrate top

Crystal data top

[Ni(SO₄)(C₁₅H₁₃N₅)(H₂O)]·H₂O	F(000) = 936
M_r = 454.11	D_x = 1.771 Mg m⁻³
Monoclinic, P2₁/n	Mo Kα radiation, λ = 0.71073 Å
Hall symbol: -P 2yn	Cell parameters from 3068 reflections
a = 7.3536 (8) Å	θ = 2.0–25.2°
b = 18.026 (2) Å	µ = 1.31 mm⁻¹
c = 12.9125 (14) Å	T = 298 K
β = 95.634 (2)°	Block, green
V = 1703.3 (3) Å³	0.22 × 0.16 × 0.12 mm
Z = 4

Data collection top

Bruker APEXII area-detector diffractometer	3068 independent reflections
Radiation source: fine-focus sealed tube	2821 reflections with I > 2σ(I)
Graphite monochromator	R_int = 0.014
ϕ and ω scans	θ_max = 25.2°, θ_min = 2.0°
Absorption correction: multi-scan (SADABS; Bruker, 2004)	h = −8→8
T_min = 0.762, T_max = 0.859	k = −20→21
8650 measured reflections	l = −15→13

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)] = 0.021	Hydrogen site location: inferred from neighbouring sites
wR(F²) = 0.056	H atoms treated by a mixture of independent and constrained refinement
S = 1.06	w = 1/[s²(F_o²) + (0.0291P)² + 0.6456P] where P = (F_o² + 2F_c²)/3
3068 reflections	(Δ/σ)_max < 0.001
259 parameters	Δρ_max = 0.24 e Å⁻³
8 restraints	Δρ_min = −0.32 e Å⁻³

Crystal data top

[Ni(SO₄)(C₁₅H₁₃N₅)(H₂O)]·H₂O	V = 1703.3 (3) Å³
M_r = 454.11	Z = 4
Monoclinic, P2₁/n	Mo Kα radiation
a = 7.3536 (8) Å	µ = 1.31 mm⁻¹
b = 18.026 (2) Å	T = 298 K
c = 12.9125 (14) Å	0.22 × 0.16 × 0.12 mm
β = 95.634 (2)°

Data collection top

Bruker APEXII area-detector diffractometer	3068 independent reflections
Absorption correction: multi-scan (SADABS; Bruker, 2004)	2821 reflections with I > 2σ(I)
T_min = 0.762, T_max = 0.859	R_int = 0.014
8650 measured reflections

Refinement top

R[F² > 2σ(F²)] = 0.021	8 restraints
wR(F²) = 0.056	H atoms treated by a mixture of independent and constrained refinement
S = 1.06	Δρ_max = 0.24 e Å⁻³
3068 reflections	Δρ_min = −0.32 e Å⁻³
259 parameters

Special details top

Geometry. All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds 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	0.26748 (3)	0.067232 (10)	0.233759 (14)	0.02550 (8)
N1	0.3089 (2)	0.06540 (7)	0.38831 (11)	0.0315 (3)
N2	0.2360 (2)	−0.06140 (8)	0.39796 (11)	0.0372 (4)
H2B	0.215 (3)	−0.0957 (9)	0.4422 (13)	0.045*
N3	0.28575 (18)	−0.04276 (7)	0.22027 (10)	0.0263 (3)
N4	0.3172 (2)	−0.03370 (8)	0.03833 (10)	0.0308 (3)
H4B	0.348 (3)	−0.0593 (9)	−0.0137 (11)	0.037*
N5	0.1828 (2)	0.07800 (7)	0.08526 (11)	0.0302 (3)
C1	0.3337 (3)	0.13148 (10)	0.43903 (14)	0.0397 (4)
H1	0.3680	0.1724	0.4015	0.048*
C2	0.3110 (3)	0.14091 (11)	0.54147 (15)	0.0464 (5)
H2	0.3247	0.1874	0.5725	0.056*
C3	0.2670 (3)	0.07959 (13)	0.59813 (15)	0.0525 (5)
H3	0.2530	0.0842	0.6687	0.063*
C4	0.2442 (3)	0.01220 (12)	0.55020 (14)	0.0468 (5)
H4	0.2156	−0.0295	0.5878	0.056*
C5	0.2643 (2)	0.00678 (9)	0.44353 (13)	0.0314 (4)
C6	0.2794 (2)	−0.08911 (9)	0.30303 (12)	0.0288 (3)
C7	0.3110 (3)	−0.16439 (9)	0.29762 (13)	0.0355 (4)
H7	0.2963	−0.1949	0.3543	0.043*
C8	0.3645 (3)	−0.19360 (9)	0.20725 (14)	0.0362 (4)
H8	0.3949	−0.2436	0.2037	0.043*
C9	0.3728 (2)	−0.14842 (9)	0.12190 (13)	0.0327 (4)
H9	0.4099	−0.1672	0.0603	0.039*
C10	0.3249 (2)	−0.07446 (8)	0.12950 (12)	0.0268 (3)
C11	0.2342 (2)	0.03302 (9)	0.01132 (12)	0.0274 (3)
C12	0.2087 (3)	0.05246 (10)	−0.09421 (13)	0.0353 (4)
H12	0.2458	0.0206	−0.1448	0.042*
C13	0.1283 (3)	0.11901 (10)	−0.12178 (14)	0.0389 (4)
H13	0.1129	0.1334	−0.1913	0.047*
C14	0.0701 (2)	0.16493 (10)	−0.04534 (14)	0.0370 (4)
H14	0.0126	0.2098	−0.0628	0.044*
C15	0.0987 (2)	0.14286 (9)	0.05574 (14)	0.0351 (4)
H15	0.0590	0.1735	0.1069	0.042*
S1	0.55296 (6)	0.18214 (2)	0.18169 (3)	0.02779 (10)
O1	0.37943 (18)	0.16682 (6)	0.22894 (10)	0.0409 (3)
O2	0.5111 (2)	0.22657 (8)	0.08910 (10)	0.0496 (4)
O3	0.6762 (2)	0.22117 (8)	0.25801 (11)	0.0553 (4)
O4	0.63271 (18)	0.11012 (7)	0.15417 (10)	0.0417 (3)
O5	−0.02550 (18)	0.09435 (8)	0.27157 (10)	0.0466 (3)
H5A	−0.0394	0.1213	0.3252	0.070*
H5B	−0.1208	0.1008	0.2292	0.070*
O6	−0.1511 (2)	0.17329 (7)	0.44790 (10)	0.0473 (3)
H6A	−0.0976	0.2059	0.4872	0.071*
H6B	−0.2151	0.1947	0.3983	0.071*

Atomic displacement parameters (Å²) top

	U¹¹	U²²	U³³	U¹²	U¹³	U²³
Ni1	0.03692 (13)	0.01854 (12)	0.02107 (12)	0.00086 (8)	0.00302 (8)	−0.00001 (7)
N1	0.0354 (8)	0.0303 (8)	0.0283 (7)	0.0020 (6)	−0.0002 (6)	−0.0009 (6)
N2	0.0549 (10)	0.0298 (8)	0.0288 (8)	−0.0026 (7)	0.0136 (7)	0.0031 (6)
N3	0.0305 (7)	0.0233 (7)	0.0256 (7)	−0.0004 (5)	0.0051 (5)	0.0005 (5)
N4	0.0429 (9)	0.0260 (7)	0.0247 (7)	0.0043 (6)	0.0097 (6)	0.0005 (6)
N5	0.0371 (8)	0.0250 (7)	0.0289 (7)	0.0033 (6)	0.0048 (6)	0.0019 (6)
C1	0.0503 (11)	0.0323 (9)	0.0346 (9)	0.0003 (8)	−0.0053 (8)	−0.0044 (7)
C2	0.0556 (13)	0.0447 (11)	0.0373 (10)	0.0055 (9)	−0.0041 (9)	−0.0141 (9)
C3	0.0634 (14)	0.0641 (14)	0.0313 (10)	0.0005 (11)	0.0108 (9)	−0.0123 (10)
C4	0.0602 (13)	0.0507 (12)	0.0314 (10)	−0.0041 (10)	0.0140 (9)	0.0006 (8)
C5	0.0315 (9)	0.0335 (9)	0.0294 (8)	0.0029 (7)	0.0039 (7)	0.0002 (7)
C6	0.0316 (9)	0.0278 (8)	0.0275 (8)	−0.0018 (7)	0.0054 (6)	0.0018 (7)
C7	0.0469 (11)	0.0272 (9)	0.0327 (9)	−0.0019 (7)	0.0051 (8)	0.0063 (7)
C8	0.0451 (11)	0.0221 (8)	0.0413 (10)	0.0027 (7)	0.0032 (8)	0.0010 (7)
C9	0.0392 (10)	0.0270 (8)	0.0327 (9)	0.0022 (7)	0.0071 (7)	−0.0024 (7)
C10	0.0266 (8)	0.0259 (8)	0.0280 (8)	−0.0010 (6)	0.0039 (6)	0.0002 (6)
C11	0.0285 (8)	0.0256 (8)	0.0283 (8)	−0.0029 (6)	0.0041 (6)	0.0014 (6)
C12	0.0443 (11)	0.0342 (9)	0.0278 (8)	0.0003 (8)	0.0057 (7)	0.0002 (7)
C13	0.0459 (11)	0.0401 (10)	0.0299 (9)	0.0004 (8)	−0.0001 (8)	0.0079 (8)
C14	0.0385 (10)	0.0299 (9)	0.0414 (10)	0.0032 (7)	−0.0016 (8)	0.0071 (8)
C15	0.0401 (10)	0.0286 (9)	0.0366 (9)	0.0049 (7)	0.0037 (7)	0.0005 (7)
S1	0.0340 (2)	0.0242 (2)	0.02483 (19)	0.00013 (16)	0.00140 (16)	−0.00106 (15)
O1	0.0525 (8)	0.0268 (6)	0.0467 (7)	−0.0059 (5)	0.0217 (6)	−0.0056 (5)
O2	0.0642 (9)	0.0480 (8)	0.0378 (7)	0.0110 (7)	0.0114 (6)	0.0162 (6)
O3	0.0541 (9)	0.0483 (9)	0.0593 (9)	−0.0030 (7)	−0.0153 (7)	−0.0187 (7)
O4	0.0489 (8)	0.0356 (7)	0.0401 (7)	0.0116 (6)	0.0020 (6)	−0.0076 (5)
O5	0.0364 (7)	0.0672 (9)	0.0361 (7)	0.0131 (7)	0.0035 (5)	−0.0052 (6)
O6	0.0628 (9)	0.0392 (7)	0.0391 (7)	−0.0064 (6)	0.0004 (6)	−0.0034 (6)

Geometric parameters (Å, º) top

Ni1—N5	1.9665 (14)	C4—H4	0.9300
Ni1—O1	1.9784 (12)	C6—C7	1.380 (2)
Ni1—N1	1.9892 (14)	C7—C8	1.373 (3)
Ni1—N3	1.9961 (14)	C7—H7	0.9300
Ni1—O5	2.3077 (13)	C8—C9	1.377 (2)
N1—C5	1.334 (2)	C8—H8	0.9300
N1—C1	1.363 (2)	C9—C10	1.385 (2)
N2—C5	1.370 (2)	C9—H9	0.9300
N2—C6	1.389 (2)	C11—C12	1.402 (2)
N2—H2B	0.866 (9)	C12—C13	1.369 (2)
N3—C10	1.360 (2)	C12—H12	0.9300
N3—C6	1.361 (2)	C13—C14	1.388 (3)
N4—C11	1.378 (2)	C13—H13	0.9300
N4—C10	1.384 (2)	C14—C15	1.361 (2)
N4—H4B	0.862 (9)	C14—H14	0.9300
N5—C11	1.335 (2)	C15—H15	0.9300
N5—C15	1.360 (2)	S1—O2	1.4467 (13)
C1—C2	1.360 (3)	S1—O3	1.4531 (14)
C1—H1	0.9300	S1—O4	1.4821 (12)
C2—C3	1.381 (3)	S1—O1	1.4932 (13)
C2—H2	0.9300	O5—H5A	0.8598
C3—C4	1.366 (3)	O5—H5B	0.8532
C3—H3	0.9300	O6—H6A	0.8477
C4—C5	1.403 (2)	O6—H6B	0.8488

N5—Ni1—O1	88.43 (6)	N3—C6—N2	120.04 (15)
N5—Ni1—N1	169.25 (6)	C7—C6—N2	116.92 (15)
O1—Ni1—N1	91.34 (6)	C8—C7—C6	118.96 (16)
N5—Ni1—N3	91.75 (5)	C8—C7—H7	120.5
O1—Ni1—N3	150.08 (5)	C6—C7—H7	120.5
N1—Ni1—N3	93.79 (5)	C7—C8—C9	119.51 (16)
N5—Ni1—O5	88.44 (5)	C7—C8—H8	120.2
O1—Ni1—O5	102.39 (5)	C9—C8—H8	120.2
N1—Ni1—O5	81.11 (5)	C8—C9—C10	118.76 (16)
N3—Ni1—O5	107.52 (5)	C8—C9—H9	120.6
C5—N1—C1	117.63 (15)	C10—C9—H9	120.6
C5—N1—Ni1	121.88 (11)	N3—C10—N4	121.05 (14)
C1—N1—Ni1	117.88 (11)	N3—C10—C9	122.84 (15)
C5—N2—C6	131.54 (15)	N4—C10—C9	116.11 (14)
C5—N2—H2B	112.7 (14)	N5—C11—N4	119.90 (14)
C6—N2—H2B	113.3 (14)	N5—C11—C12	121.54 (15)
C10—N3—C6	116.45 (14)	N4—C11—C12	118.55 (15)
C10—N3—Ni1	120.95 (10)	C13—C12—C11	119.02 (16)
C6—N3—Ni1	122.24 (11)	C13—C12—H12	120.5
C11—N4—C10	131.19 (14)	C11—C12—H12	120.5
C11—N4—H4B	114.3 (13)	C12—C13—C14	119.56 (16)
C10—N4—H4B	112.8 (12)	C12—C13—H13	120.2
C11—N5—C15	118.33 (14)	C14—C13—H13	120.2
C11—N5—Ni1	123.55 (11)	C15—C14—C13	118.56 (16)
C15—N5—Ni1	116.74 (11)	C15—C14—H14	120.7
C2—C1—N1	123.59 (18)	C13—C14—H14	120.7
C2—C1—H1	118.2	N5—C15—C14	122.94 (16)
N1—C1—H1	118.2	N5—C15—H15	118.5
C1—C2—C3	118.20 (18)	C14—C15—H15	118.5
C1—C2—H2	120.9	O2—S1—O3	111.12 (9)
C3—C2—H2	120.9	O2—S1—O4	110.11 (8)
C4—C3—C2	119.76 (18)	O3—S1—O4	110.59 (8)
C4—C3—H3	120.1	O2—S1—O1	108.60 (8)
C2—C3—H3	120.1	O3—S1—O1	108.26 (9)
C3—C4—C5	119.10 (19)	O4—S1—O1	108.06 (7)
C3—C4—H4	120.4	S1—O1—Ni1	123.76 (7)
C5—C4—H4	120.4	Ni1—O5—H5A	118.5
N1—C5—N2	121.08 (15)	Ni1—O5—H5B	128.2
N1—C5—C4	121.67 (16)	H5A—O5—H5B	106.5
N2—C5—C4	117.25 (16)	H6A—O6—H6B	109.1
N3—C6—C7	123.03 (15)

Hydrogen-bond geometry (Å, º) top

D—H···A	D—H	H···A	D···A	D—H···A
N2—H2B···O6ⁱ	0.87 (1)	2.08 (1)	2.9433 (19)	176 (2)
N4—H4B···O4ⁱⁱ	0.86 (1)	2.05 (1)	2.8967 (18)	167 (2)
O5—H5A···O6	0.86	2.08	2.9112 (18)	163
O5—H5B···O4ⁱⁱⁱ	0.85	1.98	2.8192 (19)	169
O6—H6A···O2^iv	0.85	1.91	2.7531 (18)	173
O6—H6B···O3ⁱⁱⁱ	0.85	1.97	2.785 (2)	162

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

Experimental details

Crystal data
Chemical formula	[Ni(SO₄)(C₁₅H₁₃N₅)(H₂O)]·H₂O
M_r	454.11
Crystal system, space group	Monoclinic, P2₁/n
Temperature (K)	298
a, b, c (Å)	7.3536 (8), 18.026 (2), 12.9125 (14)
β (°)	95.634 (2)
V (Å³)	1703.3 (3)
Z	4
Radiation type	Mo Kα
µ (mm⁻¹)	1.31
Crystal size (mm)	0.22 × 0.16 × 0.12

Data collection
Diffractometer	Bruker APEXII area-detector diffractometer
Absorption correction	Multi-scan (SADABS; Bruker, 2004)
T_min, T_max	0.762, 0.859
No. of measured, independent and observed [I > 2σ(I)] reflections	8650, 3068, 2821
R_int	0.014
(sin θ/λ)_max (Å⁻¹)	0.599

Refinement
R[F² > 2σ(F²)], wR(F²), S	0.021, 0.056, 1.06
No. of reflections	3068
No. of parameters	259
No. of restraints	8
H-atom treatment	H atoms treated by a mixture of independent and constrained refinement
Δρ_max, Δρ_min (e Å⁻³)	0.24, −0.32

Computer programs: , APEX2 (Bruker, 2004) and SAINT (Bruker, 2004), SAINT (Bruker, 2004), SHELXS97 (Sheldrick, 2008), SHELXL97 (Sheldrick, 2008), ORTEPIII (Burnett & Johnson, 1996) and ORTEP-3 for Windows (Farrugia, 1997);.

Hydrogen-bond geometry (Å, º) top

D—H···A	D—H	H···A	D···A	D—H···A
N2—H2B···O6ⁱ	0.866 (9)	2.079 (10)	2.9433 (19)	176 (2)
N4—H4B···O4ⁱⁱ	0.862 (9)	2.050 (10)	2.8967 (18)	167.1 (18)
O5—H5A···O6	0.86	2.08	2.9112 (18)	162.9
O5—H5B···O4ⁱⁱⁱ	0.85	1.98	2.8192 (19)	168.9
O6—H6A···O2^iv	0.85	1.91	2.7531 (18)	173.2
O6—H6B···O3ⁱⁱⁱ	0.85	1.97	2.785 (2)	161.9

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

Acknowledgements

The authors are grateful to Sichuan University of Science and Engineering for financial support.

References

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