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In the centrosymmetric trinuclear cation of the title compound, [Ni3(C2H5N5)6(H2O)6](SO4)3·18H2O, the six 3,5-diamino-1,2,4-triazole ligands each bridge two metal atoms; the Ni atom in the centre (site symmetry 3 2) of the cluster is coordinated by six N atoms in an octa­hedral geometry. The other metal atom (site symmetry 3) is connected to three N atoms and three O atoms. The sulfate anion on the \overline{3} site is heavily disordered whereas that on the 3 site is ordered. The hexa­cation, dianions and uncoordinated water mol­ecules inter­act through numerous O—H...O and N—H...O hydrogen bonds, forming a three-dimensional network.

Supporting information

cif

Crystallographic Information File (CIF) https://doi.org/10.1107/S160053680702051X/hb2392sup1.cif
Contains datablocks global, I

hkl

Structure factor file (CIF format) https://doi.org/10.1107/S160053680702051X/hb2392Isup2.hkl
Contains datablock I

CCDC reference: 648073

Key indicators

  • Single-crystal X-ray study
  • T = 295 K
  • Mean [sigma](S-O) = 0.005 Å
  • Disorder in solvent or counterion
  • R factor = 0.047
  • wR factor = 0.180
  • Data-to-parameter ratio = 11.5

checkCIF/PLATON results

No syntax errors found



Alert level B PLAT731_ALERT_1_B Bond Calc 0.84(6), Rep 0.845(10) ...... 6.00 su-Ra O4W -H4W2 1.555 1.555 PLAT735_ALERT_1_B D-H Calc 0.84(6), Rep 0.850(10) ...... 6.00 su-Ra O4W -H8# 1.555 1.555
Alert level C PLAT042_ALERT_1_C Calc. and Rep. MoietyFormula Strings Differ .... ? PLAT062_ALERT_4_C Rescale T(min) & T(max) by ..................... 0.99 PLAT068_ALERT_1_C Reported F000 Differs from Calcd (or Missing)... ? PLAT152_ALERT_1_C Supplied and Calc Volume s.u. Inconsistent ..... ? PLAT244_ALERT_4_C Low 'Solvent' Ueq as Compared to Neighbors for S2 PLAT302_ALERT_4_C Anion/Solvent Disorder ......................... 12.00 Perc. PLAT417_ALERT_2_C Short Inter D-H..H-D H1W2 .. H3W2 .. 2.14 Ang. PLAT720_ALERT_4_C Number of Unusual/Non-Standard Label(s) ........ 12 PLAT731_ALERT_1_C Bond Calc 0.84(3), Rep 0.838(10) ...... 3.00 su-Ra O1W -H1W1 1.555 1.555 PLAT731_ALERT_1_C Bond Calc 0.85(4), Rep 0.852(10) ...... 4.00 su-Ra O2W -H2W2 1.555 1.555 PLAT731_ALERT_1_C Bond Calc 0.85(4), Rep 0.848(10) ...... 4.00 su-Ra O3W -H3W1 1.555 1.555 PLAT731_ALERT_1_C Bond Calc 0.86(3), Rep 0.852(10) ...... 3.00 su-Ra O3W -H3W2 1.555 1.555 PLAT731_ALERT_1_C Bond Calc 0.84(4), Rep 0.838(10) ...... 4.00 su-Ra O4W -H4W1 1.555 1.555 PLAT731_ALERT_1_C Bond Calc 0.84(4), Rep 0.846(10) ...... 4.00 su-Ra N1 -H1N1 1.555 1.555 PLAT731_ALERT_1_C Bond Calc 0.86(3), Rep 0.859(11) ...... 2.73 su-Ra N1 -H1N2 1.555 1.555 PLAT731_ALERT_1_C Bond Calc 0.86(3), Rep 0.855(10) ...... 3.00 su-Ra N4 -H4N1 1.555 1.555 PLAT731_ALERT_1_C Bond Calc 0.85(3), Rep 0.846(10) ...... 3.00 su-Ra N4 -H4N2 1.555 1.555 PLAT731_ALERT_1_C Bond Calc 0.85(3), Rep 0.847(10) ...... 3.00 su-Ra N5 -H5N 1.555 1.555 PLAT732_ALERT_1_C Angle Calc 109(4), Rep 108.3(17) ...... 2.35 su-Ra H2W1 -O2W -H2W2 1.555 1.555 1.555 PLAT732_ALERT_1_C Angle Calc 110(4), Rep 109.4(18) ...... 2.22 su-Ra H3W1 -O3W -H3W2 1.555 1.555 1.555 PLAT732_ALERT_1_C Angle Calc 113(6), Rep 113(2) ...... 3.00 su-Ra H4W1 -O4W -H4W2 1.555 1.555 1.555 PLAT735_ALERT_1_C D-H Calc 0.84(3), Rep 0.840(10) ...... 3.00 su-Ra O1W -H1# 1.555 1.555 PLAT735_ALERT_1_C D-H Calc 0.86(3), Rep 0.860(10) ...... 3.00 su-Ra N4 -H11# 1.555 1.555 PLAT735_ALERT_1_C D-H Calc 0.85(3), Rep 0.850(10) ...... 3.00 su-Ra N4 -H12# 1.555 1.555 PLAT735_ALERT_1_C D-H Calc 0.85(3), Rep 0.850(10) ...... 3.00 su-Ra N5 -H5N 1.555 1.555 PLAT735_ALERT_1_C D-H Calc 0.85(4), Rep 0.850(10) ...... 4.00 su-Ra O2W -H4# 1.555 1.555 PLAT735_ALERT_1_C D-H Calc 0.85(4), Rep 0.850(10) ...... 4.00 su-Ra O3W -H5# 1.555 1.555 PLAT735_ALERT_1_C D-H Calc 0.86(3), Rep 0.850(10) ...... 3.00 su-Ra O3W -H6# 1.555 1.555 PLAT735_ALERT_1_C D-H Calc 0.84(4), Rep 0.840(10) ...... 4.00 su-Ra O4W -H7# 1.555 1.555 PLAT736_ALERT_1_C H...A Calc 1.88(3), Rep 1.890(10) ...... 3.00 su-Ra H1# -O2W 1.555 1.555 PLAT736_ALERT_1_C H...A Calc 1.97(5), Rep 1.97(2) ...... 2.50 su-Ra H5# -O5 1.555 1.555 PLAT736_ALERT_1_C H...A Calc 1.98(5), Rep 1.98(2) ...... 2.50 su-Ra H7# -O6 1.555 16.644 PLAT790_ALERT_4_C Centre of Gravity not Within Unit Cell: Resd. # 6 H2 O
Alert level G FORMU01_ALERT_1_G There is a discrepancy between the atom counts in the _chemical_formula_sum and _chemical_formula_moiety. This is usually due to the moiety formula being in the wrong format. Atom count from _chemical_formula_sum: C12 H78 N30 Ni3 O36 S3 Atom count from _chemical_formula_moiety: PLAT860_ALERT_3_G Note: Number of Least-Squares Restraints ....... 66
0 ALERT level A = In general: serious problem 2 ALERT level B = Potentially serious problem 33 ALERT level C = Check and explain 2 ALERT level G = General alerts; check 30 ALERT type 1 CIF construction/syntax error, inconsistent or missing data 1 ALERT type 2 Indicator that the structure model may be wrong or deficient 1 ALERT type 3 Indicator that the structure quality may be low 5 ALERT type 4 Improvement, methodology, query or suggestion 0 ALERT type 5 Informative message, check

Comment top

3,5-Diamino-1,2,4-triazole (C2H5N5) binds to cobalt to yield a centrosymmetric mixed-valence compound in which six of the ligands function as a bridge to a chain of three cobalt centers. The central metal atom is connected to six N-donor sites whereas the other two are each connected to three N atoms as well as to three water molecules. The charge of the cation is balanced by chloride ions, and the structure of the salt is stabilized by extensive hydrogen bonds (Antolini et al., 1991).

The title nickel analog displays a similar structure (Fig. 1, Table 1), but the charge of the trinuclear cation is balanced by three sulfate dianions. The cations and anions interact through uncoordinated water molecules to give rise to a three-dimensional, hydrogen bonded network (Table 2).

Related literature top

For the structure of a related cobalt-containing complex, see: Antolini et al. (1991).

Experimental top

Single crystals of (I) were grown by slowly diffusing 3,5-diamino-1,2,4-triazole (0.020 g, 0.2 mmol) dissolved in methanol (5 ml) into nickel(II) sulfate hexahydrate (0.027 g, 0.1 mmol) dissolved in water (5 ml).

Refinement top

The N– and O-bound H atoms were found in difference maps and refined with distance restraints of O–H = N–H = 0.85 (1) Å; for the water molecules, an additional H···H = 1.39±0.01 Å restraint was imposed. The Uiso values of the H atoms were tied to those of the parent atoms by a factor of 1.2.

The O atoms of one of the sulfate ions are diordered. For the ordered and disordered sulfate ions, the S–O distance was restrained to 1.45±0.01 Å and the O···O distance to 2.35±0.01 Å; the vibration of the oxygen atoms was restrained to be nearly isotropic.

Structure description top

3,5-Diamino-1,2,4-triazole (C2H5N5) binds to cobalt to yield a centrosymmetric mixed-valence compound in which six of the ligands function as a bridge to a chain of three cobalt centers. The central metal atom is connected to six N-donor sites whereas the other two are each connected to three N atoms as well as to three water molecules. The charge of the cation is balanced by chloride ions, and the structure of the salt is stabilized by extensive hydrogen bonds (Antolini et al., 1991).

The title nickel analog displays a similar structure (Fig. 1, Table 1), but the charge of the trinuclear cation is balanced by three sulfate dianions. The cations and anions interact through uncoordinated water molecules to give rise to a three-dimensional, hydrogen bonded network (Table 2).

For the structure of a related cobalt-containing complex, see: Antolini et al. (1991).

Computing details top

Data collection: SMART (Bruker, 2004); cell refinement: SAINT (Bruker, 2004); data reduction: SAINT; program(s) used to solve structure: SHELXS97 (Sheldrick, 1997); program(s) used to refine structure: SHELXL97 (Sheldrick, 1997); molecular graphics: X-SEED (Barbour, 2001); software used to prepare material for publication: publCIF (Westrip, 2007).

Figures top
[Figure 1] Fig. 1. View of the trinuclear cation in (I) at the 50% ellipsoid probability level. Hydrogen atoms are shown as spheres of arbitrary radius. Symmetry codes: (i) 1 - y, x-y, z; (ii) 1 - x + y, 1 - x, z; (iii) x-y + 1/3, 2/3 - y, 1/6 - z; (iv) 4/3 - x, 2/3 - x + y,1/6 - z; (v) 1/3 + y,x - 1/3,1/6 - z.
Hexaaquahexakis(µ2-3,5-diamino-1,2,4-triazole)trinickel(II) trisulfate octadecahydrate top
Crystal data top
[Ni3(C2H5N5)6(H2O)6](SO4)3·18H2ODx = 1.681 Mg m3
Mr = 1491.35Mo Kα radiation, λ = 0.71073 Å
Trigonal, R3cCell parameters from 7201 reflections
Hall symbol: -R 3 2"cθ = 3.2–28.2°
a = 12.664 (2) ŵ = 1.17 mm1
c = 63.653 (6) ÅT = 295 K
V = 8841 (2) Å3Block, blue
Z = 60.43 × 0.32 × 0.23 mm
F(000) = 4680
Data collection top
Bruker APEX CCD
diffractometer
2269 independent reflections
Radiation source: fine-focus sealed tube1868 reflections with I > 2σ(I)
Graphite monochromatorRint = 0.026
φ and ω scansθmax = 27.5°, θmin = 3.2°
Absorption correction: multi-scan
(SADABS; Sheldrick, 1996)
h = 1615
Tmin = 0.676, Tmax = 0.775k = 1616
24396 measured reflectionsl = 8281
Refinement top
Refinement on F2Primary atom site location: structure-invariant direct methods
Least-squares matrix: fullSecondary atom site location: difference Fourier map
R[F2 > 2σ(F2)] = 0.047Hydrogen site location: inferred from neighbouring sites
wR(F2) = 0.180All H-atom parameters refined
S = 1.33 w = 1/[σ2(Fo2) + (0.1P)2 + 1P]
where P = (Fo2 + 2Fc2)/3
2269 reflections(Δ/σ)max = 0.001
197 parametersΔρmax = 0.91 e Å3
66 restraintsΔρmin = 0.64 e Å3
Crystal data top
[Ni3(C2H5N5)6(H2O)6](SO4)3·18H2OZ = 6
Mr = 1491.35Mo Kα radiation
Trigonal, R3cµ = 1.17 mm1
a = 12.664 (2) ÅT = 295 K
c = 63.653 (6) Å0.43 × 0.32 × 0.23 mm
V = 8841 (2) Å3
Data collection top
Bruker APEX CCD
diffractometer
2269 independent reflections
Absorption correction: multi-scan
(SADABS; Sheldrick, 1996)
1868 reflections with I > 2σ(I)
Tmin = 0.676, Tmax = 0.775Rint = 0.026
24396 measured reflections
Refinement top
R[F2 > 2σ(F2)] = 0.04766 restraints
wR(F2) = 0.180All H-atom parameters refined
S = 1.33Δρmax = 0.91 e Å3
2269 reflectionsΔρmin = 0.64 e Å3
197 parameters
Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top
xyzUiso*/UeqOcc. (<1)
Ni10.66670.33330.08330.0208 (3)
Ni20.66670.33330.025169 (9)0.0238 (2)
S11.00000.00000.00000.0730 (9)
S20.66670.33330.08615 (2)0.0328 (3)
O11.0719 (19)0.068 (2)0.0183 (3)0.118 (14)0.1666667
O20.8739 (9)0.0434 (17)0.0039 (3)0.071 (7)0.1666667
O31.040 (2)0.0874 (19)0.0174 (3)0.098 (11)0.1666667
O41.0253 (16)0.0949 (13)0.0048 (3)0.065 (6)0.1666667
O50.66670.33330.06391 (8)0.107 (3)
O60.6948 (4)0.4519 (3)0.09445 (7)0.0967 (12)
O1w0.8185 (2)0.3878 (2)0.00548 (3)0.0359 (5)
H1w10.875 (2)0.390 (3)0.0128 (4)0.043*
H1w20.812 (3)0.352 (3)0.0060 (3)0.043*
O2W1.0048 (2)0.4140 (3)0.03031 (5)0.0591 (8)
H2w11.060 (3)0.4875 (15)0.0326 (8)0.071*
H2w21.038 (3)0.370 (3)0.0293 (8)0.071*
O3w0.8269 (3)0.3208 (3)0.03537 (4)0.0596 (7)
H3w10.781 (4)0.314 (3)0.0456 (5)0.072*
H3w20.818 (4)0.251 (2)0.0324 (6)0.072*
O4w1.1016 (4)0.2587 (4)0.03766 (9)0.0919 (12)
H4w11.099 (6)0.229 (6)0.0495 (4)0.110*
H4w21.111 (7)0.220 (5)0.0278 (6)0.110*
N10.3477 (3)0.1713 (3)0.08987 (5)0.0489 (9)
H1n10.394 (3)0.157 (4)0.0974 (6)0.059*
H1n20.2696 (11)0.134 (3)0.0909 (8)0.059*
N20.5086 (2)0.2574 (2)0.06450 (3)0.0265 (5)
N30.5114 (2)0.2826 (2)0.04272 (3)0.0255 (5)
N40.3585 (3)0.2501 (3)0.01736 (4)0.0492 (8)
H4n10.404 (3)0.290 (3)0.0070 (4)0.059*
H4n20.292 (2)0.194 (3)0.0123 (6)0.059*
N50.3218 (2)0.1958 (3)0.05358 (4)0.0348 (6)
H5n0.2477 (13)0.177 (3)0.0544 (6)0.042*
C10.3940 (3)0.2063 (3)0.07033 (5)0.0307 (6)
C20.3987 (2)0.2440 (3)0.03683 (4)0.0308 (6)
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
Ni10.0225 (3)0.0225 (3)0.0173 (5)0.01127 (16)0.0000.000
Ni20.0269 (3)0.0269 (3)0.0177 (4)0.01346 (15)0.0000.000
S10.0772 (13)0.0772 (13)0.0646 (19)0.0386 (7)0.0000.000
S20.0295 (4)0.0295 (4)0.0392 (7)0.0148 (2)0.0000.000
O10.118 (17)0.127 (16)0.108 (17)0.061 (11)0.007 (9)0.000 (10)
O20.059 (10)0.080 (10)0.080 (10)0.039 (8)0.015 (7)0.016 (8)
O30.108 (13)0.096 (14)0.083 (13)0.045 (9)0.012 (8)0.011 (9)
O40.069 (9)0.051 (8)0.098 (10)0.047 (7)0.024 (8)0.001 (7)
O50.131 (4)0.131 (4)0.058 (4)0.065 (2)0.0000.000
O60.092 (3)0.062 (2)0.134 (3)0.037 (2)0.002 (3)0.023 (2)
O1w0.0364 (12)0.0448 (12)0.0269 (10)0.0205 (10)0.0055 (9)0.0021 (9)
O2W0.0448 (15)0.0558 (16)0.0683 (18)0.0187 (12)0.0077 (13)0.0059 (14)
O3w0.0704 (19)0.0721 (18)0.0478 (14)0.0442 (16)0.0095 (13)0.0148 (13)
O4w0.065 (2)0.074 (2)0.139 (3)0.0363 (19)0.018 (3)0.031 (3)
N10.0305 (15)0.077 (2)0.0313 (15)0.0208 (14)0.0076 (12)0.0115 (13)
N20.0267 (12)0.0321 (12)0.0191 (11)0.0135 (9)0.0011 (9)0.0009 (8)
N30.0267 (11)0.0309 (11)0.0199 (10)0.0153 (9)0.0014 (8)0.0008 (9)
N40.0322 (14)0.073 (2)0.0317 (14)0.0182 (14)0.0094 (11)0.0048 (13)
N50.0228 (11)0.0443 (14)0.0337 (13)0.0141 (11)0.0003 (10)0.0005 (11)
C10.0249 (14)0.0370 (15)0.0267 (14)0.0128 (11)0.0016 (11)0.0001 (10)
C20.0293 (14)0.0344 (15)0.0287 (13)0.0159 (12)0.0040 (10)0.0023 (11)
Geometric parameters (Å, º) top
Ni1—N22.108 (2)S2—O51.415 (5)
Ni1—N2i2.108 (2)S2—O6ii1.458 (3)
Ni1—N2ii2.108 (2)S2—O6i1.458 (3)
Ni1—N2iii2.108 (2)S2—O61.458 (3)
Ni1—N2iv2.108 (2)O1w—H1w10.838 (10)
Ni1—N2v2.108 (2)O1w—H1w20.841 (10)
Ni2—N32.065 (2)O2W—H2w10.853 (10)
Ni2—N3i2.065 (2)O2W—H2w20.852 (10)
Ni2—N3ii2.065 (2)O3w—H3w10.848 (10)
Ni2—O1w2.101 (2)O3w—H3w20.852 (10)
Ni2—O1wi2.101 (2)O4w—H4w10.838 (10)
Ni2—O1wii2.101 (2)O4w—H4w20.845 (10)
S1—O4vi1.422 (8)N1—C11.352 (4)
S1—O4vii1.422 (8)N1—H1n10.846 (10)
S1—O4viii1.422 (8)N1—H1n20.859 (11)
S1—O41.422 (8)N2—C11.313 (4)
S1—O4ix1.422 (8)N2—N31.419 (3)
S1—O4x1.422 (8)N3—C21.311 (3)
S1—O2vii1.427 (9)N4—C21.357 (4)
S1—O2x1.427 (9)N4—H4n10.855 (10)
S1—O21.427 (9)N4—H4n20.846 (10)
S1—O2viii1.427 (9)N5—C21.365 (4)
S1—O2vi1.427 (9)N5—C11.367 (4)
S1—O2ix1.427 (9)N5—H5n0.847 (10)
N2iii—Ni1—N2iv90.85 (8)O2vii—S1—O2viii117.0 (4)
N2iii—Ni1—N2v90.85 (8)O4vi—S1—O2vi113.1 (8)
N2iv—Ni1—N2v90.85 (8)O2vii—S1—O2vi117.0 (4)
N2iii—Ni1—N2i177.85 (11)O2viii—S1—O2vi117.0 (4)
N2iv—Ni1—N2i90.70 (12)O4ix—S1—O2ix113.1 (8)
N2v—Ni1—N2i87.63 (12)O2x—S1—O2ix117.0 (4)
N2iii—Ni1—N287.64 (12)O2—S1—O2ix117.0 (4)
N2iv—Ni1—N2177.85 (11)O5—S2—O6ii111.26 (18)
N2v—Ni1—N290.70 (12)O5—S2—O6i111.26 (19)
N2i—Ni1—N290.85 (8)O6ii—S2—O6i107.6 (2)
N2iii—Ni1—N2ii90.70 (12)O5—S2—O6111.26 (18)
N2iv—Ni1—N2ii87.64 (12)O6ii—S2—O6107.6 (2)
N2v—Ni1—N2ii177.85 (11)O6i—S2—O6107.6 (2)
N2i—Ni1—N2ii90.85 (8)Ni2—O1w—H1w1108 (2)
N2—Ni1—N2ii90.85 (8)Ni2—O1w—H1w2121 (2)
N3i—Ni2—N3ii93.50 (8)H1w1—O1w—H1w2110.9 (17)
N3i—Ni2—N393.50 (8)H2w1—O2W—H2w2108.3 (17)
N3ii—Ni2—N393.50 (8)H3w1—O3w—H3w2109.4 (18)
N3i—Ni2—O1w90.39 (9)H4w1—O4w—H4w2113 (2)
N3ii—Ni2—O1w87.94 (9)C1—N1—H1n1111 (3)
N3—Ni2—O1w175.77 (8)C1—N1—H1n2116 (3)
N3i—Ni2—O1wii87.94 (9)H1n1—N1—H1n2125 (4)
N3ii—Ni2—O1wii175.77 (8)C1—N2—N3106.5 (2)
N3—Ni2—O1wii90.39 (9)C1—N2—Ni1128.87 (19)
O1w—Ni2—O1wii88.07 (9)N3—N2—Ni1122.82 (17)
N3i—Ni2—O1wi175.77 (8)C2—N3—N2107.2 (2)
N3ii—Ni2—O1wi90.39 (9)C2—N3—Ni2130.62 (18)
N3—Ni2—O1wi87.94 (9)N2—N3—Ni2120.73 (16)
O1w—Ni2—O1wi88.07 (9)C2—N4—H4n1125 (3)
O1wii—Ni2—O1wi88.07 (9)C2—N4—H4n2123 (3)
O4vi—S1—O4vii115.6 (5)H4n1—N4—H4n2107 (4)
O4vi—S1—O4viii115.6 (5)C2—N5—C1105.8 (2)
O4—S1—O4ix115.6 (5)C2—N5—H5n128 (2)
O4—S1—O4x115.6 (5)C1—N5—H5n125 (2)
O4ix—S1—O4x115.6 (5)N2—C1—N1127.9 (3)
O4vii—S1—O2vii113.1 (8)N2—C1—N5110.4 (3)
O4x—S1—O2x113.1 (8)N1—C1—N5121.7 (3)
O4—S1—O2113.1 (8)N3—C2—N4127.6 (3)
O2x—S1—O2117.0 (4)N3—C2—N5110.1 (2)
O4viii—S1—O2viii113.1 (8)N4—C2—N5122.3 (3)
N2iii—Ni1—N2—C141.1 (2)N3i—Ni2—N3—N232.54 (16)
N2v—Ni1—N2—C149.7 (2)N3ii—Ni2—N3—N261.19 (14)
N2i—Ni1—N2—C1137.3 (3)O1wii—Ni2—N3—N2120.50 (19)
N2ii—Ni1—N2—C1131.8 (3)O1wi—Ni2—N3—N2151.45 (19)
N2iii—Ni1—N2—N3121.4 (2)N3—N2—C1—N1176.9 (3)
N2v—Ni1—N2—N3147.8 (2)Ni1—N2—C1—N112.1 (4)
N2i—Ni1—N2—N360.12 (14)N3—N2—C1—N50.5 (3)
N2ii—Ni1—N2—N330.75 (16)Ni1—N2—C1—N5165.2 (2)
C1—N2—N3—C20.7 (3)C2—N5—C1—N20.1 (3)
Ni1—N2—N3—C2166.61 (18)C2—N5—C1—N1177.4 (3)
C1—N2—N3—Ni2168.31 (18)N2—N3—C2—N4179.5 (3)
Ni1—N2—N3—Ni225.8 (3)Ni2—N3—C2—N414.5 (5)
N3i—Ni2—N3—C2131.8 (3)N2—N3—C2—N50.7 (3)
N3ii—Ni2—N3—C2134.5 (3)Ni2—N3—C2—N5166.6 (2)
O1wii—Ni2—N3—C243.8 (3)C1—N5—C2—N30.4 (3)
O1wi—Ni2—N3—C244.2 (3)C1—N5—C2—N4179.3 (3)
Symmetry codes: (i) y+1, xy, z; (ii) x+y+1, x+1, z; (iii) xy+1/3, y+2/3, z+1/6; (iv) x+4/3, x+y+2/3, z+1/6; (v) y+1/3, x1/3, z+1/6; (vi) y+1, x+y+1, z; (vii) xy, x1, z; (viii) x+2, y, z; (ix) y+1, xy1, z; (x) x+y+2, x+1, z.
Hydrogen-bond geometry (Å, º) top
D—H···AD—HH···AD···AD—H···A
O1w—H1w1···O2w0.84 (1)1.89 (1)2.719 (4)173 (3)
O1w—H1w2···O3w0.84 (1)1.94 (2)2.754 (3)162 (4)
N4—H4n1···O1wi0.86 (1)2.33 (3)2.962 (4)131 (4)
N4—H4n2···O2ii0.85 (1)2.41 (3)3.15 (2)147 (4)
N5—H5n···O6xi0.85 (1)2.08 (2)2.843 (5)150 (3)
O2W—H2w1···O3wxii0.85 (1)2.12 (1)2.962 (4)168 (4)
O2W—H2w2···O4w0.85 (1)2.01 (2)2.828 (5)160 (5)
O3w—H3w1···O50.85 (1)1.97 (2)2.787 (5)162 (4)
O3w—H3w2···O4wvii0.85 (1)2.10 (2)2.885 (5)154 (5)
O4w—H4w1···O6xiii0.84 (1)1.98 (2)2.786 (6)163 (6)
O4w—H4w2···O10.85 (1)1.83 (4)2.57 (2)145 (6)
Symmetry codes: (i) y+1, xy, z; (ii) x+y+1, x+1, z; (vii) xy, x1, z; (xi) x+y+1/3, y1/3, z+1/6; (xii) x+2, y+1, z; (xiii) x+y+4/3, y1/3, z+1/6.

Experimental details

Crystal data
Chemical formula[Ni3(C2H5N5)6(H2O)6](SO4)3·18H2O
Mr1491.35
Crystal system, space groupTrigonal, R3c
Temperature (K)295
a, c (Å)12.664 (2), 63.653 (6)
V3)8841 (2)
Z6
Radiation typeMo Kα
µ (mm1)1.17
Crystal size (mm)0.43 × 0.32 × 0.23
Data collection
DiffractometerBruker APEX CCD
Absorption correctionMulti-scan
(SADABS; Sheldrick, 1996)
Tmin, Tmax0.676, 0.775
No. of measured, independent and
observed [I > 2σ(I)] reflections
24396, 2269, 1868
Rint0.026
(sin θ/λ)max1)0.650
Refinement
R[F2 > 2σ(F2)], wR(F2), S 0.047, 0.180, 1.33
No. of reflections2269
No. of parameters197
No. of restraints66
H-atom treatmentAll H-atom parameters refined
Δρmax, Δρmin (e Å3)0.91, 0.64

Computer programs: SMART (Bruker, 2004), SAINT (Bruker, 2004), SAINT, SHELXS97 (Sheldrick, 1997), SHELXL97 (Sheldrick, 1997), X-SEED (Barbour, 2001), publCIF (Westrip, 2007).

Selected bond lengths (Å) top
Ni1—N22.108 (2)Ni2—O1w2.101 (2)
Ni2—N32.065 (2)
Hydrogen-bond geometry (Å, º) top
D—H···AD—HH···AD···AD—H···A
O1w—H1w1···O2w0.84 (1)1.89 (1)2.719 (4)173 (3)
O1w—H1w2···O3w0.84 (1)1.94 (2)2.754 (3)162 (4)
N4—H4n1···O1wi0.86 (1)2.33 (3)2.962 (4)131 (4)
N4—H4n2···O2ii0.85 (1)2.41 (3)3.15 (2)147 (4)
N5—H5n···O6iii0.85 (1)2.08 (2)2.843 (5)150 (3)
O2W—H2w1···O3wiv0.85 (1)2.12 (1)2.962 (4)168 (4)
O2W—H2w2···O4w0.85 (1)2.01 (2)2.828 (5)160 (5)
O3w—H3w1···O50.85 (1)1.97 (2)2.787 (5)162 (4)
O3w—H3w2···O4wv0.85 (1)2.10 (2)2.885 (5)154 (5)
O4w—H4w1···O6vi0.84 (1)1.98 (2)2.786 (6)163 (6)
O4w—H4w2···O10.85 (1)1.83 (4)2.57 (2)145 (6)
Symmetry codes: (i) y+1, xy, z; (ii) x+y+1, x+1, z; (iii) x+y+1/3, y1/3, z+1/6; (iv) x+2, y+1, z; (v) xy, x1, z; (vi) x+y+4/3, y1/3, z+1/6.
 

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