Bis{4-[(4H-1,2,4-triazol-4-yl)iminomethyl]pyridinium} diaquapentanitratocerate(III)

Sun, Q.; Zheng, F.; Sun, X.; Wang, W.

doi:10.1107/S1600536808043109

metal-organic compounds

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ISSN: 2056-9890

Volume 65| Part 1| January 2009| Page m124

doi:10.1107/S1600536808043109

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Bis{4-[(4H-1,2,4-triazol-4-yl)iminomethyl]pyridinium} diaquapentanitratocerate(III)

Qiaozhen Sun,^a ^* Feng Zheng,^a Xiaodan Sun ^a and Wei Wang ^a

^aDepartment of Materials Chemistry, School of Materials Science and Engineering, Central South University, Changsha, 410083, People's Republic of China
^*Correspondence e-mail: rosesunqz@yahoo.com.cn

(Received 20 September 2008; accepted 18 December 2008; online 24 December 2008)

The asymmetric unit of the title compound, (C₈H₈N₅)₂[Ce(NO₃)₅(H₂O)₂], contains one independent protonated 4-pyridylmethyleneamino-1,2,4-triazole cation and half of a centrosymmetric [Ce(NO₃)₅(H₂O)₂]²⁻ anion. The Ce atom coordinated by five NO₃⁻ anions and two water molecules, exhibiting a distorted 10-coordination. In the crystal structure, intermolecular O—H⋯N and N—H⋯O hydrogen bonds result in the formation of a supramolecular structure.

Related literature

For related compounds based on 4-amido-1,2,4-triazoles Schiff base ligands, see: Drabent et al. (2003 , 2004 ); Wang et al. (2006 ). For the preparation of the ligand, see: Colautti et al. (1971 ).

Experimental

Crystal data

(C₈H₈N₅)₂[Ce(NO₃)₅(H₂O)₂]
M_r = 834.59
Monoclinic, C 2/c
a = 10.322 (4) Å
b = 16.126 (6) Å
c = 17.595 (7) Å
β = 100.107 (4)°
V = 2883.2 (19) Å³
Z = 4
Mo Kα radiation
μ = 1.69 mm⁻¹
T = 293 (2) K
0.20 × 0.18 × 0.15 mm

Data collection

Bruker SMART CCD area-detector diffractometer
Absorption correction: multi-scan (SADABS; Bruker, 2000 ) T_min = 0.682, T_max = 0.781
5464 measured reflections
2374 independent reflections
2164 reflections with I > 2σ(I)
R_int = 0.039

Refinement

R[F² > 2σ(F²)] = 0.024
wR(F²) = 0.051
S = 1.02
2374 reflections
231 parameters
3 restraints
H atoms treated by a mixture of independent and constrained refinement
Δρ_max = 0.47 e Å⁻³
Δρ_min = −0.39 e Å⁻³

Table 1
Hydrogen-bond geometry (Å, °)

D—H⋯A	D—H	H⋯A	D⋯A	D—H⋯A
OW1—HW1A⋯N7	0.85 (2)	1.96 (2)	2.805 (3)	176 (3)
OW1—HW1B⋯N8ⁱ	0.85 (2)	2.03 (3)	2.876 (3)	178 (3)
N4—H4B⋯O4ⁱⁱ	0.86	1.95	2.804 (3)	172
N4—H4B⋯N2ⁱⁱ	0.86	2.69	3.518 (4)	162
Symmetry codes: (i) $[-x+{\script{3\over 2}}, -y+{\script{1\over 2}}, -z+1]$ ; (ii) $[x+{\script{3\over 2}}, y+{\script{1\over 2}}, z]$ .

Data collection: SMART (Bruker, 2000); cell refinement: SAINT (Bruker, 2000); data reduction: SAINT; program(s) used to solve structure: SHELXTL (Sheldrick, 2008 ); program(s) used to refine structure: SHELXTL; molecular graphics: SHELXTL; software used to prepare material for publication: SHELXTL.

Supporting information

Crystal structure: contains datablock I. DOI: 10.1107/S1600536808043109/wk2094sup1.cif

Structure factors: contains datablock I. DOI: 10.1107/S1600536808043109/wk2094Isup2.hkl

checkCIF report

Comment top

In recent decades, metal coordination polymers containing 1,2,4-triazoles and their derivatives have been studied widely due to their versatile bridging modes with metal ions. Relatively few structurally characterized compounds based on 4-amido-1,2,4-triazoles Schiff base ligands have been reported (Drabent et al., 2004 and 2003; Wang et al., 2006) and these compounds exhibit dinuclear and tetranuclear structures. In this work, 4-Pyridylmethyleneamino-1,2,4-triazole coordinated with metal cerium is shown to generate a new coordination compound and its crystal structure reported.

As depicted in Fig.1, the Ce ion in this complex is ligated by eight oxygen atoms from five NO₃^- anions and two from H₂O molecules. And three NO₃^- anions are bound to Ce ion in bidentate fashion, while the other two in monodentate one. The nitrogen atoms of Schiff base ligand are not involved in the coordination to the Ce center as we supposed. The [Ce(NO₃)₅(H₂O)]^2- unit and the ligands are linked through the O—H···N and N—H···O hydrogen bonds, forming a three dimensional network.

Related literature top

For related compounds based on 4-amido-1,2,4-triazoles Schiff base ligands, see: Drabent et al. (2003, 2004); Wang et al. (2006). For the preparation of the ligand, see: Colautti et al. (1971).

Experimental top

The ligand was prepared according to the reported literature (Colautti et al., 1971). The ligand (0.1 mmol, 0.017 g) and (NH₄)₂Ce(NO₃)₆ (0.1 mmol, 0.055 g) were mixed in acetonitrile and methanol of 1:1. After stirring at room temperature for four hours, the yellow solution was filtered and evaporated at room temperature. A few days later the red block crystals were obtained.

Computing details top

Data collection: SMART (Bruker, 2000); cell refinement: SAINT (Bruker, 2000); data reduction: SAINT (Bruker, 2000); program(s) used to solve structure: SHELXTL (Sheldrick, 2008); program(s) used to refine structure: SHELXTL (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 the title molecule, with the atom-numbering scheme. Displacement ellipsoids are drawn at the 30% probability level. [symmetry codes: (A) 1 - x, y, 0.5 - z.]
	Fig. 2. A packing diagram of the title compound along a axis. The dash lines indicate hydrogen bonding.

Bis{4-[(4H-1,2,4-triazol-4-yl)iminomethyl]pyridinium} diaquapentanitratocerate(III) top

Crystal data top

(C₈H₈N₅)₂[Ce(NO₃)₅(H₂O)₂]	F(000) = 1660
M_r = 834.59	D_x = 1.923 Mg m⁻³
Monoclinic, C2/c	Mo Kα radiation, λ = 0.71073 Å
a = 10.322 (4) Å	Cell parameters from 4413 reflections
b = 16.126 (6) Å	θ = 2.4–27.9°
c = 17.595 (7) Å	µ = 1.69 mm⁻¹
β = 100.107 (4)°	T = 293 K
V = 2883.2 (19) Å³	Block, red
Z = 4	0.2 × 0.18 × 0.15 mm

Data collection top

Bruker SMART CCD area-detector diffractometer	2374 independent reflections
Radiation source: fine-focus sealed tube	2164 reflections with I > 2σ(I)
Graphite monochromator	R_int = 0.039
ϕ & ω scans	θ_max = 25.0°, θ_min = 2.4°
Absorption correction: multi-scan (SADABS; Bruker, 2000)	h = −8→12
T_min = 0.682, T_max = 0.781	k = −19→17
5464 measured reflections	l = −20→20

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)] = 0.024	Hydrogen site location: geom, H2O from difmap
wR(F²) = 0.051	H atoms treated by a mixture of independent and constrained refinement
S = 1.02	w = 1/[σ²(F_o²) + (0.0252P)²] where P = (F_o² + 2F_c²)/3
2374 reflections	(Δ/σ)_max = 0.001
231 parameters	Δρ_max = 0.47 e Å⁻³
3 restraints	Δρ_min = −0.39 e Å⁻³

Crystal data top

(C₈H₈N₅)₂[Ce(NO₃)₅(H₂O)₂]	V = 2883.2 (19) Å³
M_r = 834.59	Z = 4
Monoclinic, C2/c	Mo Kα radiation
a = 10.322 (4) Å	µ = 1.69 mm⁻¹
b = 16.126 (6) Å	T = 293 K
c = 17.595 (7) Å	0.2 × 0.18 × 0.15 mm
β = 100.107 (4)°

Data collection top

Bruker SMART CCD area-detector diffractometer	2374 independent reflections
Absorption correction: multi-scan (SADABS; Bruker, 2000)	2164 reflections with I > 2σ(I)
T_min = 0.682, T_max = 0.781	R_int = 0.039
5464 measured reflections

Refinement top

R[F² > 2σ(F²)] = 0.024	3 restraints
wR(F²) = 0.051	H atoms treated by a mixture of independent and constrained refinement
S = 1.02	Δρ_max = 0.47 e Å⁻³
2374 reflections	Δρ_min = −0.39 e Å⁻³
231 parameters

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
Ce1	0.5000	0.326614 (13)	0.2500	0.03115 (9)
O1	0.5000	0.0598 (2)	0.2500	0.0705 (10)
O2	0.4319 (2)	0.17726 (13)	0.28901 (13)	0.0562 (6)
O3	0.1789 (3)	0.2766 (2)	0.29302 (17)	0.1053 (11)
O4	0.2177 (3)	0.27312 (16)	0.41595 (15)	0.0779 (8)
O5	0.3593 (2)	0.32656 (13)	0.35615 (12)	0.0503 (5)
O6	0.7035 (2)	0.54285 (14)	0.34535 (13)	0.0652 (7)
O7	0.53719 (19)	0.45902 (12)	0.33599 (10)	0.0453 (5)
O8	0.70260 (19)	0.42680 (12)	0.28267 (11)	0.0448 (5)
OW1	0.6436 (2)	0.27739 (13)	0.37050 (11)	0.0416 (5)
HW1A	0.7155 (19)	0.3003 (18)	0.3907 (15)	0.065 (11)*
HW1B	0.617 (3)	0.2462 (16)	0.4032 (13)	0.063 (11)*
N1	0.5000	0.1364 (2)	0.2500	0.0469 (9)
N2	0.2502 (3)	0.29172 (15)	0.35287 (16)	0.0478 (6)
N3	0.6495 (2)	0.47807 (15)	0.32205 (12)	0.0411 (6)
N4	1.5004 (3)	0.66662 (14)	0.40465 (18)	0.0529 (7)
H4B	1.5642	0.7007	0.4036	0.063*
N5	1.1739 (2)	0.46981 (15)	0.46894 (14)	0.0462 (6)
N6	1.0647 (2)	0.41729 (13)	0.46749 (12)	0.0372 (5)
N7	0.8835 (2)	0.34651 (15)	0.44223 (14)	0.0457 (6)
N8	0.9425 (2)	0.33038 (14)	0.51796 (14)	0.0434 (6)
C1	1.3894 (3)	0.57624 (18)	0.47348 (16)	0.0440 (7)
H1A	1.3802	0.5513	0.5199	0.053*
C2	1.4894 (3)	0.6306 (2)	0.47130 (18)	0.0505 (8)
H2A	1.5495	0.6424	0.5159	0.061*
C3	1.4172 (3)	0.65205 (19)	0.3402 (2)	0.0524 (9)
H3A	1.4272	0.6796	0.2951	0.063*
C4	1.3168 (3)	0.59701 (18)	0.33902 (16)	0.0432 (7)
H4A	1.2594	0.5858	0.2932	0.052*
C5	1.3012 (3)	0.55803 (16)	0.40681 (16)	0.0368 (6)
C6	1.1905 (3)	0.49910 (17)	0.40619 (17)	0.0457 (7)
H6A	1.1356	0.4847	0.3604	0.055*
C7	0.9585 (3)	0.39815 (18)	0.41384 (17)	0.0444 (7)
H7A	0.9418	0.4190	0.3638	0.053*
C8	1.0501 (3)	0.37400 (17)	0.53134 (16)	0.0417 (7)
H8A	1.1085	0.3752	0.5780	0.050*

Atomic displacement parameters (Å²) top

	U¹¹	U²²	U³³	U¹²	U¹³	U²³
Ce1	0.02878 (14)	0.03952 (14)	0.02512 (12)	0.000	0.00461 (9)	0.000
O1	0.061 (2)	0.043 (2)	0.097 (3)	0.000	−0.015 (2)	0.000
O2	0.0595 (15)	0.0588 (14)	0.0529 (13)	−0.0164 (12)	0.0170 (12)	−0.0075 (11)
O3	0.113 (3)	0.105 (2)	0.077 (2)	−0.0392 (19)	−0.0401 (19)	−0.0047 (17)
O4	0.086 (2)	0.0829 (18)	0.0775 (17)	−0.0295 (15)	0.0491 (16)	−0.0101 (14)
O5	0.0423 (13)	0.0648 (13)	0.0487 (12)	−0.0198 (11)	0.0215 (10)	−0.0070 (10)
O6	0.0732 (17)	0.0559 (14)	0.0640 (15)	−0.0263 (13)	0.0049 (13)	−0.0135 (11)
O7	0.0409 (12)	0.0547 (12)	0.0417 (11)	−0.0040 (10)	0.0107 (10)	−0.0061 (9)
O8	0.0358 (12)	0.0544 (13)	0.0450 (11)	−0.0019 (10)	0.0090 (10)	−0.0021 (10)
OW1	0.0351 (12)	0.0502 (12)	0.0361 (11)	−0.0123 (10)	−0.0035 (10)	0.0090 (10)
N1	0.036 (2)	0.052 (2)	0.047 (2)	0.000	−0.0087 (18)	0.000
N2	0.0502 (18)	0.0448 (14)	0.0493 (16)	−0.0041 (13)	0.0110 (15)	−0.0076 (12)
N3	0.0437 (15)	0.0478 (15)	0.0288 (12)	−0.0036 (13)	−0.0019 (11)	0.0036 (11)
N4	0.0437 (16)	0.0403 (15)	0.080 (2)	−0.0064 (12)	0.0264 (16)	−0.0004 (14)
N5	0.0458 (16)	0.0478 (14)	0.0457 (14)	−0.0041 (12)	0.0101 (12)	0.0040 (12)
N6	0.0311 (13)	0.0360 (12)	0.0440 (14)	−0.0087 (10)	0.0053 (11)	0.0049 (10)
N7	0.0367 (14)	0.0475 (15)	0.0499 (15)	−0.0104 (12)	−0.0008 (12)	0.0030 (11)
N8	0.0391 (14)	0.0423 (13)	0.0472 (14)	−0.0063 (12)	0.0029 (12)	0.0071 (11)
C1	0.0500 (19)	0.0494 (18)	0.0351 (15)	−0.0024 (15)	0.0143 (15)	0.0040 (13)
C2	0.046 (2)	0.0555 (19)	0.0474 (19)	−0.0051 (17)	0.0011 (16)	−0.0111 (16)
C3	0.055 (2)	0.054 (2)	0.056 (2)	0.0130 (17)	0.0306 (19)	0.0225 (16)
C4	0.0393 (18)	0.0563 (18)	0.0335 (15)	0.0104 (15)	0.0046 (14)	0.0039 (13)
C5	0.0314 (16)	0.0354 (15)	0.0449 (16)	0.0002 (13)	0.0105 (14)	−0.0005 (12)
C6	0.0474 (19)	0.0477 (18)	0.0397 (17)	0.0000 (15)	0.0011 (15)	−0.0002 (13)
C7	0.0393 (18)	0.0503 (18)	0.0412 (16)	−0.0034 (15)	0.0000 (15)	0.0071 (14)
C8	0.0376 (17)	0.0434 (17)	0.0419 (16)	−0.0050 (14)	0.0013 (14)	0.0052 (13)

Geometric parameters (Å, º) top

Ce1—OW1ⁱ	2.494 (2)	N4—C2	1.331 (4)
Ce1—OW1	2.494 (2)	N4—H4B	0.8600
Ce1—O5	2.5590 (19)	N5—C6	1.240 (3)
Ce1—O5ⁱ	2.5590 (19)	N5—N6	1.406 (3)
Ce1—O7	2.606 (2)	N6—C7	1.350 (3)
Ce1—O7ⁱ	2.606 (2)	N6—C8	1.353 (3)
Ce1—O8	2.625 (2)	N7—C7	1.296 (4)
Ce1—O8ⁱ	2.625 (2)	N7—N8	1.389 (3)
Ce1—O2ⁱ	2.634 (2)	N8—C8	1.301 (4)
Ce1—O2	2.634 (2)	C1—C2	1.360 (4)
O1—N1	1.235 (5)	C1—C5	1.384 (4)
O2—N1	1.253 (3)	C1—H1A	0.9300
O3—N2	1.199 (3)	C2—H2A	0.9300
O4—N2	1.251 (3)	C3—C4	1.362 (4)
O5—N2	1.251 (3)	C3—H3A	0.9300
O6—N3	1.221 (3)	C4—C5	1.383 (4)
O7—N3	1.264 (3)	C4—H4A	0.9300
O8—N3	1.264 (3)	C5—C6	1.485 (4)
OW1—HW1A	0.849 (10)	C6—H6A	0.9300
OW1—HW1B	0.846 (10)	C7—H7A	0.9300
N1—O2ⁱ	1.253 (3)	C8—H8A	0.9300
N4—C3	1.318 (4)

OW1ⁱ—Ce1—OW1	142.88 (10)	N3—O7—Ce1	97.65 (15)
OW1ⁱ—Ce1—O5	106.96 (7)	N3—O8—Ce1	96.72 (15)
OW1—Ce1—O5	73.02 (8)	Ce1—OW1—HW1A	124.3 (19)
OW1ⁱ—Ce1—O5ⁱ	73.02 (8)	Ce1—OW1—HW1B	123.5 (19)
OW1—Ce1—O5ⁱ	106.96 (7)	HW1A—OW1—HW1B	109.8 (16)
O5—Ce1—O5ⁱ	179.96 (9)	O1—N1—O2	121.74 (18)
OW1ⁱ—Ce1—O7	139.41 (7)	O1—N1—O2ⁱ	121.74 (18)
OW1—Ce1—O7	76.24 (7)	O2—N1—O2ⁱ	116.5 (4)
O5—Ce1—O7	67.74 (6)	O3—N2—O5	122.7 (3)
O5ⁱ—Ce1—O7	112.29 (7)	O3—N2—O4	120.8 (3)
OW1ⁱ—Ce1—O7ⁱ	76.24 (7)	O5—N2—O4	116.5 (3)
OW1—Ce1—O7ⁱ	139.41 (7)	O6—N3—O7	121.6 (2)
O5—Ce1—O7ⁱ	112.29 (7)	O6—N3—O8	121.8 (2)
O5ⁱ—Ce1—O7ⁱ	67.74 (6)	O7—N3—O8	116.6 (2)
O7—Ce1—O7ⁱ	69.97 (9)	C3—N4—C2	122.5 (3)
OW1ⁱ—Ce1—O8	135.54 (6)	C3—N4—H4B	118.8
OW1—Ce1—O8	71.22 (7)	C2—N4—H4B	118.8
O5—Ce1—O8	111.88 (6)	C6—N5—N6	116.7 (3)
O5ⁱ—Ce1—O8	68.15 (7)	C7—N6—C8	105.5 (2)
O7—Ce1—O8	48.56 (6)	C7—N6—N5	134.4 (2)
O7ⁱ—Ce1—O8	69.72 (6)	C8—N6—N5	120.1 (2)
OW1ⁱ—Ce1—O8ⁱ	71.22 (6)	C7—N7—N8	107.4 (2)
OW1—Ce1—O8ⁱ	135.54 (6)	C8—N8—N7	106.8 (2)
O5—Ce1—O8ⁱ	68.15 (7)	C2—C1—C5	120.2 (3)
O5ⁱ—Ce1—O8ⁱ	111.88 (6)	C2—C1—H1A	119.9
O7—Ce1—O8ⁱ	69.72 (6)	C5—C1—H1A	119.9
O7ⁱ—Ce1—O8ⁱ	48.56 (6)	N4—C2—C1	119.3 (3)
O8—Ce1—O8ⁱ	104.04 (9)	N4—C2—H2A	120.4
OW1ⁱ—Ce1—O2ⁱ	68.49 (7)	C1—C2—H2A	120.4
OW1—Ce1—O2ⁱ	77.56 (7)	N4—C3—C4	120.5 (3)
O5—Ce1—O2ⁱ	113.68 (7)	N4—C3—H3A	119.7
O5ⁱ—Ce1—O2ⁱ	66.29 (7)	C4—C3—H3A	119.7
O7—Ce1—O2ⁱ	151.86 (7)	C3—C4—C5	119.2 (3)
O7ⁱ—Ce1—O2ⁱ	128.09 (7)	C3—C4—H4A	120.4
O8—Ce1—O2ⁱ	112.40 (7)	C5—C4—H4A	120.4
O8ⁱ—Ce1—O2ⁱ	138.12 (7)	C4—C5—C1	118.4 (3)
OW1ⁱ—Ce1—O2	77.56 (7)	C4—C5—C6	119.4 (3)
OW1—Ce1—O2	68.49 (7)	C1—C5—C6	122.2 (2)
O5—Ce1—O2	66.29 (7)	N5—C6—C5	117.6 (3)
O5ⁱ—Ce1—O2	113.68 (7)	N5—C6—H6A	121.2
O7—Ce1—O2	128.09 (7)	C5—C6—H6A	121.2
O7ⁱ—Ce1—O2	151.86 (7)	N7—C7—N6	110.1 (2)
O8—Ce1—O2	138.12 (7)	N7—C7—H7A	124.9
O8ⁱ—Ce1—O2	112.40 (7)	N6—C7—H7A	124.9
O2ⁱ—Ce1—O2	47.72 (10)	N8—C8—N6	110.1 (3)
N1—O2—Ce1	97.88 (19)	N8—C8—H8A	124.9
N2—O5—Ce1	126.02 (17)	N6—C8—H8A	124.9

OW1ⁱ—Ce1—O2—N1	72.13 (12)	O7ⁱ—Ce1—O8—N3	76.92 (14)
OW1—Ce1—O2—N1	−92.60 (13)	O8ⁱ—Ce1—O8—N3	41.97 (12)
O5—Ce1—O2—N1	−172.83 (15)	O2ⁱ—Ce1—O8—N3	−159.10 (14)
O5ⁱ—Ce1—O2—N1	7.16 (15)	O2—Ce1—O8—N3	−108.18 (15)
O7—Ce1—O2—N1	−143.28 (10)	Ce1—O2—N1—O1	180.0
O7ⁱ—Ce1—O2—N1	93.88 (17)	Ce1—O2—N1—O2ⁱ	0.0
O8—Ce1—O2—N1	−75.96 (15)	Ce1—O5—N2—O3	−24.5 (4)
O8ⁱ—Ce1—O2—N1	135.54 (11)	Ce1—O5—N2—O4	155.8 (2)
O2ⁱ—Ce1—O2—N1	0.0	Ce1—O7—N3—O6	173.1 (2)
OW1ⁱ—Ce1—O5—N2	14.3 (2)	Ce1—O7—N3—O8	−6.7 (2)
OW1—Ce1—O5—N2	−126.8 (2)	Ce1—O8—N3—O6	−173.2 (2)
O5ⁱ—Ce1—O5—N2	−56 (100)	Ce1—O8—N3—O7	6.6 (2)
O7—Ce1—O5—N2	151.4 (2)	C6—N5—N6—C7	−10.8 (4)
O7ⁱ—Ce1—O5—N2	96.0 (2)	C6—N5—N6—C8	170.9 (3)
O8—Ce1—O5—N2	172.2 (2)	C7—N7—N8—C8	0.5 (3)
O8ⁱ—Ce1—O5—N2	75.3 (2)	C3—N4—C2—C1	0.3 (5)
O2ⁱ—Ce1—O5—N2	−59.2 (2)	C5—C1—C2—N4	0.8 (5)
O2—Ce1—O5—N2	−53.4 (2)	C2—N4—C3—C4	−1.6 (5)
OW1ⁱ—Ce1—O7—N3	−111.82 (16)	N4—C3—C4—C5	1.6 (4)
OW1—Ce1—O7—N3	80.77 (15)	C3—C4—C5—C1	−0.4 (4)
O5—Ce1—O7—N3	157.79 (16)	C3—C4—C5—C6	178.9 (3)
O5ⁱ—Ce1—O7—N3	−22.19 (16)	C2—C1—C5—C4	−0.8 (4)
O7ⁱ—Ce1—O7—N3	−76.37 (14)	C2—C1—C5—C6	179.9 (3)
O8—Ce1—O7—N3	3.83 (13)	N6—N5—C6—C5	177.0 (2)
O8ⁱ—Ce1—O7—N3	−128.32 (16)	C4—C5—C6—N5	−175.0 (3)
O2ⁱ—Ce1—O7—N3	58.9 (2)	C1—C5—C6—N5	4.4 (4)
O2—Ce1—O7—N3	128.58 (14)	N8—N7—C7—N6	−0.2 (3)
OW1ⁱ—Ce1—O8—N3	119.31 (14)	C8—N6—C7—N7	−0.1 (3)
OW1—Ce1—O8—N3	−91.83 (15)	N5—N6—C7—N7	−178.6 (3)
O5—Ce1—O8—N3	−29.79 (16)	N7—N8—C8—N6	−0.6 (3)
O5ⁱ—Ce1—O8—N3	150.24 (15)	C7—N6—C8—N8	0.5 (3)
O7—Ce1—O8—N3	−3.82 (13)	N5—N6—C8—N8	179.2 (2)

Symmetry code: (i) −x+1, y, −z+1/2.

Hydrogen-bond geometry (Å, º) top

D—H···A	D—H	H···A	D···A	D—H···A
OW1—HW1A···N7	0.85 (2)	1.96 (2)	2.805 (3)	176 (3)
OW1—HW1B···N8ⁱⁱ	0.85 (2)	2.03 (3)	2.876 (3)	178 (3)
N4—H4B···O4ⁱⁱⁱ	0.86	1.95	2.804 (3)	172
N4—H4B···N2ⁱⁱⁱ	0.86	2.69	3.518 (4)	162

Symmetry codes: (ii) −x+3/2, −y+1/2, −z+1; (iii) x+3/2, y+1/2, z.

Experimental details

Crystal data
Chemical formula	(C₈H₈N₅)₂[Ce(NO₃)₅(H₂O)₂]
M_r	834.59
Crystal system, space group	Monoclinic, C2/c
Temperature (K)	293
a, b, c (Å)	10.322 (4), 16.126 (6), 17.595 (7)
β (°)	100.107 (4)
V (Å³)	2883.2 (19)
Z	4
Radiation type	Mo Kα
µ (mm⁻¹)	1.69
Crystal size (mm)	0.2 × 0.18 × 0.15

Data collection
Diffractometer	Bruker SMART CCD area-detector diffractometer
Absorption correction	Multi-scan (SADABS; Bruker, 2000)
T_min, T_max	0.682, 0.781
No. of measured, independent and observed [I > 2σ(I)] reflections	5464, 2374, 2164
R_int	0.039
(sin θ/λ)_max (Å⁻¹)	0.595

Refinement
R[F² > 2σ(F²)], wR(F²), S	0.024, 0.051, 1.02
No. of reflections	2374
No. of parameters	231
No. of restraints	3
H-atom treatment	H atoms treated by a mixture of independent and constrained refinement
Δρ_max, Δρ_min (e Å⁻³)	0.47, −0.39

Computer programs: SMART (Bruker, 2000), SAINT (Bruker, 2000), SHELXTL (Sheldrick, 2008).

Hydrogen-bond geometry (Å, º) top

D—H···A	D—H	H···A	D···A	D—H···A
OW1—HW1A···N7	0.85 (2)	1.96 (2)	2.805 (3)	176 (3)
OW1—HW1B···N8ⁱ	0.85 (2)	2.03 (3)	2.876 (3)	178 (3)
N4—H4B···O4ⁱⁱ	0.86	1.95	2.804 (3)	172
N4—H4B···N2ⁱⁱ	0.86	2.69	3.518 (4)	162

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

Acknowledgements

The authors acknowledge financial support from the Innovation Program for College Students of Central South University (grant No. 081053308).

References

Bruker (2000). SMART, SAINT and SADABS. Bruker AXS Inc., Madison, Wisconsin, USA. Google Scholar
Colautti, A., Ferlauto, R. J., Maurich, V., De Nardo, M., Nisi, C., Rubessa, F. & Runti, C. (1971). Chim. Ther. 6, 367–379. CAS Google Scholar
Drabent, K., Bialońska, A. & Ciunik, Z. (2004). Inorg. Chem. Commun. 7, 224–227. Web of Science CSD CrossRef CAS Google Scholar
Drabent, K., Ciunik, Z. & Chmielewski, P. J. (2003). Eur. J. Inorg. Chem. pp. 1548–1554. CSD CrossRef Google Scholar
Sheldrick, G. M. (2008). Acta Cryst. A64, 112–122. Web of Science CrossRef CAS IUCr Journals Google Scholar
Wang, Y., Yi, L., Yang, X., Ding, B., Cheng, P., Liao, D.-Z. & Yan, S.-P. (2006). Inorg. Chem. 45, 5822–5829. Web of Science CSD CrossRef PubMed CAS Google Scholar

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Volume 65| Part 1| January 2009| Page m124

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metal-organic compounds\(\def\hfill{\hskip 5em}\def\hfil{\hskip 3em}\def\eqno#1{\hfil {#1}}\)

Bis{4-[(4H-1,2,4-triazol-4-yl)imino­methyl]pyridinium} di­aqua­pentanitratocerate(III)

Related literature

Experimental

Crystal data

Data collection

Refinement

Supporting information

Acknowledgements

References

metal-organic compounds

Bis{4-[(4H-1,2,4-triazol-4-yl)iminomethyl]pyridinium} diaquapentanitratocerate(III)