Hexaaqua­hexa­kis(μ2-3,5-diamino-4H-1,2,4-triazole)trinickel(II) tris­(hexa­fluoridosilicate) icosa­hydrate

Wu, L.-P.; Zhao, S.-M.; Zhang, G.-F.; Ng, S.W.

doi:10.1107/S1600536808013329

metal-organic compounds

CRYSTALLOGRAPHIC
COMMUNICATIONS

ISSN: 2056-9890

Volume 64| Part 6| June 2008| Page m802

doi:10.1107/S1600536808013329

Open

access

Hexaaquahexakis(μ₂-3,5-diamino-4H-1,2,4-triazole)trinickel(II) tris(hexafluoridosilicate) icosahydrate

Li-Ping Wu,^a ^* Shu-Ming Zhao,^a Guo-Fang Zhang ^a and Seik Weng Ng ^b

^aKey Laboratory of Applied Surface and Colloid Chemistry, Shaanxi Normal University, Ministry of Education, Xi'an 710062, People's Republic of China, and ^bDepartment of Chemistry, University of Malaya, 50603 Kuala Lumpur, Malaysia
^*Correspondence e-mail: wuliping250921@stu.snnu.edu.cn

(Received 7 April 2008; accepted 6 May 2008; online 10 May 2008)

The trinuclear cation of the title compound, [Ni₃(C₂H₅N₅)₆(H₂O)₆][SiF₆]₃·20H₂O, has the six 3,5-diamino-1,2,4-triazole ligands each bridging two metal atoms; the metal atom in the middle, which lies on a special position (of 32 site symmetry), is connected to six N atoms in an octahedral geometry. The other metal atom, which lies on a special position (of 3 site symmetry), is connected to three N atoms and three O atoms. One hexafluroridosilicate anion lies on a site of 3 symmetry and the other lies on a site of $[\overline{3}]$ symmetry. The hexacation, dianions and uncoordinated water molecules interact through hydrogen bonds to form a three-dimensional network. One uncoordinated water molecule is disordered, with site occupancy 0.3.

Related literature

For the structure of the title hexacation as the hydrated sulfate salt, see: Zhang et al. (2007 ).

Experimental

Crystal data

[Ni₃(C₂H₅N₅)₆(H₂O)₆][SiF₆]₃·20H₂O
M_r = 1665.48
Trigonal, $[R \overline 3c ]$
a = 13.024 (1) Å
c = 64.462 (5) Å
V = 9469.8 (9) Å³
Z = 6
Mo Kα radiation
μ = 1.09 mm⁻¹
T = 293 (2) K
0.49 × 0.46 × 0.44 mm

Data collection

Bruker APEX area-detector diffractometer
Absorption correction: multi-scan (SADABS; Sheldrick, 1996 ) T_min = 0.560, T_max = 0.646
25347 measured reflections
2420 independent reflections
2093 reflections with I > 2σ(I)
R_int = 0.021

Refinement

R[F² > 2σ(F²)] = 0.033
wR(F²) = 0.106
S = 1.06
2420 reflections
185 parameters
23 restraints
H atoms treated by a mixture of independent and constrained refinement
Δρ_max = 0.40 e Å⁻³
Δρ_min = −0.42 e Å⁻³

Table 1
Selected bond lengths (Å)

Ni1—N1	2.062 (2)
Ni1—O1	2.104 (2)
Ni2—N2	2.111 (2)

Data collection: SMART (Bruker, 2004 ); cell refinement: 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: X-SEED (Barbour, 2001 ); software used to prepare material for publication: publCIF (Westrip, 2008 ).

Supporting information

Crystal structure: contains datablocks I, global. DOI: 10.1107/S1600536808013329/si2084sup1.cif

Structure factors: contains datablock I. DOI: 10.1107/S1600536808013329/si2084Isup2.hkl

checkCIF report

Comment top

A recent study reported the nickel sulfate complex of 3,5-diamino-1,2,4-triazole. The cation is a centrosymmetric trinuclear hexacation [Ni₃(C₂H₅N₅)₆(H₂O)₆]⁶⁺, whose charge is balanced by the sulfate anions. The N-heterocyclic ligands each bridge two nickel atoms (Zhang et al., 2007). The corresponding synthesis with nickel hexafluoridosilicate in place of nickel sulfate gave the analogous cluster cation (Scheme I, Fig. 1). The cation and anions interact through the coordinated and free water molecules to give rise to a three-dimensional, hydrogen bonded network.

Related literature top

For the structure of the title hexacation as the hydrated sulfate salt, see: Zhang et al. (2007).

Experimental top

Single crystal of the compound were grown by diffusing 3,5-diamino-1,2,4-triazole (0.020 g, 0.2 mmol) dissolved in methanol (5 ml) into nickle(II) hexafluorosilicate (0.027 g, 0.1 mmol) dissolved in water (5 ml).

Computing details top

Data collection: SMART (Bruker, 2004); cell refinement: 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: X-SEED (Barbour, 2001); software used to prepare material for publication: publCIF (Westrip, 2008).

Figures top

Fig. 1. Thermal ellipsoid plot of the title compound. Displacement ellipsoids are drawn at the 25% probability level.

Hexaaquahexakis(µ₂-3,5-diamino-4H-1,2,4-triazole)trinickel(II) tris(hexafluoridosilicate) icosahydrate top

Crystal data top

[Ni₃(C₂H₅N₅)₆(H₂O)₆][SiF₆]₃·20H₂O	D_x = 1.752 Mg m⁻³
M_r = 1665.48	Mo Kα radiation, λ = 0.71073 Å
Trigonal, R3c	Cell parameters from 5839 reflections
Hall symbol: -R 3 2"c	θ = 3.1–28.2°
a = 13.024 (1) Å	µ = 1.09 mm⁻¹
c = 64.462 (5) Å	T = 293 K
V = 9469.8 (9) Å³	Block, blue
Z = 6	0.49 × 0.46 × 0.44 mm
F(000) = 5160

Data collection top

Bruker APEX area-detector diffractometer	2420 independent reflections
Radiation source: fine-focus sealed tube	2093 reflections with I > 2σ(I)
Graphite monochromator	R_int = 0.021
ϕ and ω scans	θ_max = 27.5°, θ_min = 3.1°
Absorption correction: multi-scan (SADABS; Sheldrick, 1996)	h = −16→16
T_min = 0.560, T_max = 0.646	k = −16→16
25347 measured reflections	l = −79→83

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)] = 0.033	Hydrogen site location: inferred from neighbouring sites
wR(F²) = 0.106	H atoms treated by a mixture of independent and constrained refinement
S = 1.06	w = 1/[σ²(F_o²) + (0.0612P)² + 17.0807P] where P = (F_o² + 2F_c²)/3
2420 reflections	(Δ/σ)_max = 0.001
185 parameters	Δρ_max = 0.40 e Å⁻³
23 restraints	Δρ_min = −0.43 e Å⁻³

Crystal data top

[Ni₃(C₂H₅N₅)₆(H₂O)₆][SiF₆]₃·20H₂O	Z = 6
M_r = 1665.48	Mo Kα radiation
Trigonal, R3c	µ = 1.09 mm⁻¹
a = 13.024 (1) Å	T = 293 K
c = 64.462 (5) Å	0.49 × 0.46 × 0.44 mm
V = 9469.8 (9) Å³

Data collection top

Bruker APEX area-detector diffractometer	2420 independent reflections
Absorption correction: multi-scan (SADABS; Sheldrick, 1996)	2093 reflections with I > 2σ(I)
T_min = 0.560, T_max = 0.646	R_int = 0.021
25347 measured reflections

Refinement top

R[F² > 2σ(F²)] = 0.033	23 restraints
wR(F²) = 0.106	H atoms treated by a mixture of independent and constrained refinement
S = 1.06	w = 1/[σ²(F_o²) + (0.0612P)² + 17.0807P] where P = (F_o² + 2F_c²)/3
2420 reflections	Δρ_max = 0.40 e Å⁻³
185 parameters	Δρ_min = −0.43 e Å⁻³

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

	x	y	z	U_iso*/U_eq	Occ. (<1)
Ni1	0.6667	0.3333	0.140787 (6)	0.02689 (14)
Ni2	0.6667	0.3333	0.0833	0.02377 (16)
Si1	1.0000	0.0000	0.083802 (16)	0.0331 (2)
Si2	0.3333	−0.3333	0.1667	0.0552 (5)
F1	0.89685 (14)	0.00226 (15)	0.09960 (2)	0.0623 (4)
F2	1.00168 (16)	0.10635 (14)	0.06943 (3)	0.0648 (4)
F3	0.3983 (3)	−0.3868 (3)	0.15169 (5)	0.1399 (12)
O1	0.72286 (15)	0.24063 (14)	0.16010 (2)	0.0398 (3)
H11	0.723 (3)	0.1843 (18)	0.1533 (3)	0.060*
H12	0.699 (3)	0.217 (2)	0.1724 (2)	0.060*
O2	0.7536 (2)	0.0854 (2)	0.13625 (4)	0.0660 (5)
H21	0.713 (2)	0.0108 (10)	0.1358 (6)	0.099*
H22	0.8267 (10)	0.108 (3)	0.1361 (7)	0.099*
O3	0.65459 (19)	0.15616 (17)	0.19955 (3)	0.0599 (5)
H31	0.5874 (17)	0.094 (2)	0.1978 (5)	0.090*
H32	0.650 (3)	0.197 (2)	0.2092 (4)	0.090*
O4	0.6041 (2)	−0.1661 (3)	0.12859 (4)	0.0796 (6)
H41	0.576 (3)	−0.184 (4)	0.1164 (3)	0.119*
H42	0.551 (3)	−0.182 (4)	0.1374 (4)	0.119*
O5	0.664 (3)	−0.1549 (17)	0.0893 (3)	0.185 (7)	0.3333
H51	0.7382	−0.1072	0.0905	0.278*	0.3333
H52	0.6338	−0.1239	0.0816	0.278*	0.3333
N1	0.61588 (14)	0.43372 (14)	0.12352 (2)	0.0290 (3)
N2	0.59282 (14)	0.41343 (14)	0.10195 (2)	0.0293 (3)
N3	0.52872 (17)	0.53100 (17)	0.11289 (3)	0.0381 (4)
H3	0.500 (2)	0.576 (2)	0.1117 (4)	0.057*
N4	0.5100 (2)	0.4865 (2)	0.07683 (3)	0.0508 (5)
H4A	0.514 (3)	0.449 (3)	0.0663 (4)	0.076*
H4B	0.468 (2)	0.517 (3)	0.0744 (6)	0.076*
N5	0.5810 (2)	0.5478 (2)	0.14862 (3)	0.0556 (6)
H5A	0.625 (3)	0.540 (3)	0.1574 (4)	0.083*
H5B	0.535 (3)	0.575 (3)	0.1509 (5)	0.083*
C1	0.57611 (18)	0.50413 (18)	0.12943 (3)	0.0343 (4)
C2	0.54160 (17)	0.47436 (17)	0.09630 (3)	0.0336 (4)

Atomic displacement parameters (Å²) top

	U¹¹	U²²	U³³	U¹²	U¹³	U²³
Ni1	0.02997 (17)	0.02997 (17)	0.0207 (2)	0.01499 (9)	0.000	0.000
Ni2	0.0253 (2)	0.0253 (2)	0.0207 (3)	0.01265 (10)	0.000	0.000
Si1	0.0300 (3)	0.0300 (3)	0.0394 (5)	0.01500 (15)	0.000	0.000
Si2	0.0333 (5)	0.0333 (5)	0.0992 (15)	0.0166 (2)	0.000	0.000
F1	0.0555 (9)	0.0683 (10)	0.0701 (10)	0.0363 (8)	0.0170 (7)	0.0016 (8)
F2	0.0710 (10)	0.0574 (9)	0.0741 (10)	0.0382 (8)	−0.0004 (8)	0.0199 (8)
F3	0.146 (3)	0.176 (3)	0.163 (3)	0.129 (3)	0.0160 (19)	−0.025 (2)
O1	0.0497 (8)	0.0454 (8)	0.0292 (7)	0.0274 (7)	−0.0020 (6)	0.0041 (6)
O2	0.0624 (12)	0.0722 (13)	0.0750 (13)	0.0424 (11)	−0.0019 (10)	−0.0133 (11)
O3	0.0764 (13)	0.0541 (11)	0.0436 (9)	0.0283 (10)	0.0132 (9)	−0.0001 (8)
O4	0.0709 (15)	0.0812 (15)	0.0871 (16)	0.0383 (13)	−0.0030 (12)	−0.0025 (14)
O5	0.119 (7)	0.216 (10)	0.178 (13)	0.051 (7)	−0.015 (9)	−0.010 (8)
N1	0.0349 (8)	0.0329 (8)	0.0226 (7)	0.0194 (6)	0.0006 (6)	−0.0010 (6)
N2	0.0352 (8)	0.0355 (8)	0.0219 (7)	0.0213 (7)	−0.0009 (6)	−0.0005 (6)
N3	0.0476 (10)	0.0440 (10)	0.0366 (9)	0.0334 (8)	−0.0010 (7)	−0.0015 (7)
N4	0.0743 (15)	0.0720 (14)	0.0343 (10)	0.0578 (13)	−0.0109 (9)	−0.0043 (9)
N5	0.0821 (16)	0.0803 (15)	0.0348 (10)	0.0635 (14)	−0.0071 (10)	−0.0157 (10)
C1	0.0390 (10)	0.0367 (10)	0.0319 (9)	0.0224 (9)	0.0008 (8)	−0.0023 (8)
C2	0.0377 (10)	0.0374 (10)	0.0312 (9)	0.0229 (9)	−0.0009 (7)	0.0006 (7)

Geometric parameters (Å, º) top

Ni1—N1	2.062 (2)	Si2—F3	1.649 (3)
Ni1—N1ⁱ	2.062 (2)	O1—H11	0.86 (3)
Ni1—N1ⁱⁱ	2.062 (2)	O1—H12	0.85 (3)
Ni1—O1	2.104 (2)	O2—H21	0.84 (3)
Ni1—O1ⁱ	2.104 (2)	O2—H22	0.84 (3)
Ni1—O1ⁱⁱ	2.104 (2)	O3—H31	0.85 (3)
Ni2—N2ⁱⁱⁱ	2.111 (2)	O3—H32	0.84 (3)
Ni2—N2^iv	2.111 (2)	O4—H41	0.85 (3)
Ni2—N2^v	2.111 (2)	O4—H42	0.84 (3)
Ni2—N2ⁱⁱ	2.111 (2)	O5—H51	0.85
Ni2—N2ⁱ	2.111 (2)	O5—H52	0.85
Ni2—N2	2.111 (2)	N1—C1	1.315 (2)
Si1—F2	1.6574 (15)	N1—N2	1.419 (2)
Si1—F2^vi	1.6574 (15)	N2—C2	1.318 (3)
Si1—F2^vii	1.6574 (15)	N3—C2	1.356 (3)
Si1—F1^vii	1.6976 (15)	N3—C1	1.362 (3)
Si1—F1^vi	1.6976 (15)	N3—H3	0.85 (1)
Si1—F1	1.6976 (15)	N4—C2	1.354 (3)
Si2—F3^viii	1.649 (3)	N4—H4A	0.85 (3)
Si2—F3^ix	1.649 (3)	N4—H4B	0.84 (3)
Si2—F3^x	1.649 (3)	N5—C1	1.350 (3)
Si2—F3^xi	1.649 (3)	N5—H5A	0.84 (3)
Si2—F3^xii	1.649 (3)	N5—H5B	0.85 (3)

N1ⁱⁱ—Ni1—N1ⁱ	93.61 (6)	F1^vi—Si1—F1	87.74 (9)
N1ⁱⁱ—Ni1—N1	93.61 (6)	F3^viii—Si2—F3^ix	89.21 (17)
N1ⁱ—Ni1—N1	93.61 (6)	F3^viii—Si2—F3^x	89.21 (17)
N1ⁱⁱ—Ni1—O1	87.31 (6)	F3^ix—Si2—F3^x	89.21 (17)
N1ⁱ—Ni1—O1	90.45 (6)	F3^viii—Si2—F3^xi	90.79 (17)
N1—Ni1—O1	175.77 (6)	F3^ix—Si2—F3^xi	90.79 (17)
N1ⁱⁱ—Ni1—O1ⁱ	90.45 (6)	F3^x—Si2—F3^xi	179.995 (1)
N1ⁱ—Ni1—O1ⁱ	175.77 (6)	F3^viii—Si2—F3^xii	90.79 (17)
N1—Ni1—O1ⁱ	87.31 (6)	F3^ix—Si2—F3^xii	179.995 (1)
O1—Ni1—O1ⁱ	88.56 (6)	F3^x—Si2—F3^xii	90.79 (17)
N1ⁱⁱ—Ni1—O1ⁱⁱ	175.78 (6)	F3^xi—Si2—F3^xii	89.21 (17)
N1ⁱ—Ni1—O1ⁱⁱ	87.31 (6)	F3^viii—Si2—F3	179.997 (1)
N1—Ni1—O1ⁱⁱ	90.45 (6)	F3^ix—Si2—F3	90.79 (17)
O1—Ni1—O1ⁱⁱ	88.56 (6)	F3^x—Si2—F3	90.79 (17)
O1ⁱ—Ni1—O1ⁱⁱ	88.56 (6)	F3^xi—Si2—F3	89.21 (17)
N2ⁱⁱⁱ—Ni2—N2^iv	90.87 (6)	F3^xii—Si2—F3	89.21 (17)
N2ⁱⁱⁱ—Ni2—N2^v	90.87 (6)	Ni1—O1—H11	110 (2)
N2^iv—Ni2—N2^v	90.87 (6)	Ni1—O1—H12	126 (2)
N2ⁱⁱⁱ—Ni2—N2ⁱⁱ	87.57 (8)	H11—O1—H12	109 (2)
N2^iv—Ni2—N2ⁱⁱ	177.79 (8)	H21—O2—H22	111 (2)
N2^v—Ni2—N2ⁱⁱ	90.72 (8)	H31—O3—H32	110 (2)
N2ⁱⁱⁱ—Ni2—N2ⁱ	90.72 (8)	H41—O4—H42	111 (2)
N2^iv—Ni2—N2ⁱ	87.57 (8)	H51—O5—H52	109.4
N2^v—Ni2—N2ⁱ	177.79 (8)	C1—N1—N2	107.04 (15)
N2ⁱⁱ—Ni2—N2ⁱ	90.88 (6)	C1—N1—Ni1	130.48 (12)
N2ⁱⁱⁱ—Ni2—N2	177.79 (8)	N2—N1—Ni1	121.05 (11)
N2^iv—Ni2—N2	90.72 (8)	C2—N2—N1	106.38 (15)
N2^v—Ni2—N2	87.57 (8)	C2—N2—Ni2	129.31 (13)
N2ⁱⁱ—Ni2—N2	90.88 (6)	N1—N2—Ni2	122.87 (12)
N2ⁱ—Ni2—N2	90.88 (6)	C2—N3—C1	106.38 (16)
F2—Si1—F2^vi	91.80 (9)	C2—N3—H3	122 (2)
F2—Si1—F2^vii	91.80 (9)	C1—N3—H3	132 (2)
F2^vi—Si1—F2^vii	91.80 (9)	C2—N4—H4A	125 (2)
F2—Si1—F1^vii	90.36 (8)	C2—N4—H4B	122 (3)
F2^vi—Si1—F1^vii	177.12 (10)	H4A—N4—H4B	111 (3)
F2^vii—Si1—F1^vii	90.03 (8)	C1—N5—H5A	117 (2)
F2—Si1—F1^vi	177.12 (10)	C1—N5—H5B	116 (2)
F2^vi—Si1—F1^vi	90.03 (8)	H5A—N5—H5B	126 (3)
F2^vii—Si1—F1^vi	90.36 (8)	N1—C1—N5	127.37 (19)
F1^vii—Si1—F1^vi	87.74 (9)	N1—C1—N3	109.86 (16)
F2—Si1—F1	90.03 (8)	N5—C1—N3	122.76 (18)
F2^vi—Si1—F1	90.36 (8)	N2—C2—N4	126.92 (19)
F2^vii—Si1—F1	177.12 (10)	N2—C2—N3	110.33 (17)
F1^vii—Si1—F1	87.74 (9)	N4—C2—N3	122.67 (19)

N1ⁱⁱ—Ni1—N1—C1	−135.1 (2)	N2^iv—Ni2—N2—N1	146.76 (16)
N1ⁱ—Ni1—N1—C1	131.1 (2)	N2^v—Ni2—N2—N1	−122.40 (15)
O1ⁱ—Ni1—N1—C1	−44.81 (19)	N2ⁱⁱ—Ni2—N2—N1	−31.71 (12)
O1ⁱⁱ—Ni1—N1—C1	43.72 (19)	N2ⁱ—Ni2—N2—N1	59.18 (10)
N1ⁱⁱ—Ni1—N1—N2	60.39 (10)	N2—N1—C1—N5	−179.0 (2)
N1ⁱ—Ni1—N1—N2	−33.46 (12)	Ni1—N1—C1—N5	14.9 (3)
O1ⁱ—Ni1—N1—N2	150.67 (13)	N2—N1—C1—N3	−0.1 (2)
O1ⁱⁱ—Ni1—N1—N2	−120.79 (13)	Ni1—N1—C1—N3	−166.30 (14)
C1—N1—N2—C2	0.6 (2)	C2—N3—C1—N1	−0.4 (2)
Ni1—N1—N2—C2	168.37 (13)	C2—N3—C1—N5	178.5 (2)
C1—N1—N2—Ni2	168.09 (13)	N1—N2—C2—N4	176.0 (2)
Ni1—N1—N2—Ni2	−24.17 (18)	Ni2—N2—C2—N4	9.6 (3)
N2^iv—Ni2—N2—C2	−48.86 (15)	N1—N2—C2—N3	−0.9 (2)
N2^v—Ni2—N2—C2	41.98 (14)	Ni2—N2—C2—N3	−167.25 (14)
N2ⁱⁱ—Ni2—N2—C2	132.67 (18)	C1—N3—C2—N2	0.8 (2)
N2ⁱ—Ni2—N2—C2	−136.44 (18)	C1—N3—C2—N4	−176.2 (2)

Symmetry codes: (i) −y+1, x−y, z; (ii) −x+y+1, −x+1, z; (iii) y+1/3, x−1/3, −z+1/6; (iv) x−y+1/3, −y+2/3, −z+1/6; (v) −x+4/3, −x+y+2/3, −z+1/6; (vi) −y+1, x−y−1, z; (vii) −x+y+2, −x+1, z; (viii) −x+2/3, −y−2/3, −z+1/3; (ix) x−y−1/3, x−2/3, −z+1/3; (x) y+2/3, −x+y+1/3, −z+1/3; (xi) −y, x−y−1, z; (xii) −x+y+1, −x, z.

Hydrogen-bond geometry (Å, º) top

D—H···A	D—H	H···A	D···A	D—H···A
O1—H11···O2	0.86 (3)	1.88 (3)	2.724 (3)	168 (3)
O1—H12···O3	0.85 (3)	1.89 (3)	2.737 (2)	174 (3)
O2—H21···O4	0.84 (3)	2.07 (3)	2.896 (4)	168 (4)
O2—H22···O3^xiii	0.84 (3)	2.12 (3)	2.961 (3)	175 (4)
O3—H31···O4^ix	0.85 (3)	2.05 (3)	2.861 (3)	159 (3)
O3—H32···F1^ix	0.84 (3)	2.13 (3)	2.904 (2)	153 (3)
O4—H41···F2^xiv	0.85 (3)	2.23 (3)	2.950 (3)	143 (4)
O4—H42···F3^xi	0.84 (3)	2.16 (3)	2.973 (4)	162 (4)
O4—H41···O5	0.85 (3)	2.03 (3)	2.64 (2)	128 (4)
O5—H51···F1	0.85	1.92	2.76 (3)	167
N3—H3···F2ⁱⁱⁱ	0.85 (3)	1.97 (3)	2.764 (2)	157 (3)
N4—H4b···F1ⁱⁱⁱ	0.84 (3)	2.14 (3)	2.974 (3)	170 (3)
N5—H5a···O1ⁱ	0.84 (3)	2.23 (3)	2.942 (3)	142 (3)
N5—H5b···F3^xv	0.85 (3)	2.08 (3)	2.909 (3)	167 (3)

Symmetry codes: (i) −y+1, x−y, z; (iii) y+1/3, x−1/3, −z+1/6; (ix) x−y−1/3, x−2/3, −z+1/3; (xi) −y, x−y−1, z; (xiii) −x+5/3, −y+1/3, −z+1/3; (xiv) y+1/3, x−4/3, −z+1/6; (xv) x, y+1, z.

Experimental details

Crystal data
Chemical formula	[Ni₃(C₂H₅N₅)₆(H₂O)₆][SiF₆]₃·20H₂O
M_r	1665.48
Crystal system, space group	Trigonal, R3c
Temperature (K)	293
a, c (Å)	13.024 (1), 64.462 (5)
V (Å³)	9469.8 (9)
Z	6
Radiation type	Mo Kα
µ (mm⁻¹)	1.09
Crystal size (mm)	0.49 × 0.46 × 0.44

Data collection
Diffractometer	Bruker APEX area-detector diffractometer
Absorption correction	Multi-scan (SADABS; Sheldrick, 1996)
T_min, T_max	0.560, 0.646
No. of measured, independent and observed [I > 2σ(I)] reflections	25347, 2420, 2093
R_int	0.021
(sin θ/λ)_max (Å⁻¹)	0.649

Refinement
R[F² > 2σ(F²)], wR(F²), S	0.033, 0.106, 1.06
No. of reflections	2420
No. of parameters	185
No. of restraints	23
H-atom treatment	H atoms treated by a mixture of independent and constrained refinement
	w = 1/[σ²(F_o²) + (0.0612P)² + 17.0807P] where P = (F_o² + 2F_c²)/3
Δρ_max, Δρ_min (e Å⁻³)	0.40, −0.43

Computer programs: SMART (Bruker, 2004), SAINT (Bruker, 2004), SHELXS97 (Sheldrick, 2008), SHELXL97 (Sheldrick, 2008), X-SEED (Barbour, 2001), publCIF (Westrip, 2008).

Selected bond lengths (Å) top

Ni1—N1	2.062 (2)	Ni2—N2	2.111 (2)
Ni1—O1	2.104 (2)

Acknowledgements

We thank Shaanxi Normal University and the University of Malaya for supporting this study.

References

Barbour, L. J. (2001). J. Supramol. Chem. 1, 189–191. CrossRef CAS Google Scholar
Bruker (2004). SAINT and SMART. Bruker AXS Inc., Madison, Wisconsin, USA. Google Scholar
Sheldrick, G. M. (1996). 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
Westrip, S. P. (2008). publCIF. In preparation. Google Scholar
Zhang, G.-F., Zhao, S.-M., She, J.-B. & Ng, S. W. (2007). Acta Cryst. E63, m1517–m1518. Web of Science CSD CrossRef IUCr Journals Google Scholar

This is an open-access article distributed under the terms of the Creative Commons Attribution (CC-BY) Licence, which permits unrestricted use, distribution, and reproduction in any medium, provided the original authors and source are cited.