trans-Diaqua­bis{1,3-bis­[5-(2-pyrid­yl)-2H-tetra­zol-2-yl]propane}zinc(II) bis­(perchlorate)

Gallardo, H.; Molin, F.; Bortoluzzi, A.J.; Neves, A.

doi:10.1107/S1600536808006703

metal-organic compounds

CRYSTALLOGRAPHIC
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ISSN: 2056-9890

Volume 64| Part 4| April 2008| Pages m541-m542

doi:10.1107/S1600536808006703

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trans-Diaquabis{1,3-bis[5-(2-pyridyl)-2H-tetrazol-2-yl]propane}zinc(II) bis(perchlorate)

Hugo Gallardo,^a ^* Fernando Molin,^a Adailton J. Bortoluzzi ^a and Ademir Neves ^a

^aDepto. de Química, Universidade Federal de Santa Catarina, 88040-900 Florianópolis, Santa Catarina, Brazil
^*Correspondence e-mail: hugo@qmc.ufsc.br

(Received 1 March 2008; accepted 10 March 2008; online 14 March 2008)

The Zn^II ion in the title compound, [Zn(C₁₅H₁₄N₁₀)(H₂O)₂](ClO₄)₂, lies on a centre of symmetry. The distorted N₄O₂ octahedral coordination environment around the Zn atom is composed of two 1,3-bis[5-(2-pyridyl)-2H-tetrazol-2-yl]propane ligands (L1) and two water molecules, coordinated in trans positions. The ligand acts as a typical bidentate chelating ligand through one of its 2-pyridyl-2H-tetrazole units, forming a five-membered Zn—N—C—C—N metallacycle with a small N—Zn—N bite angle [77.40 (8)°]. The other 2-pyridyl-2H-tetrazole unit remains uncoordinated. The average Zn—N distance (2.156 Å) is somewhat longer than the distance between the Zn^II center and the aqua ligand [2.108 (2) Å]. The coordinated pyridyl-tetrazoyl rings are quasi-coplanar, making a dihedral angle of 1.9 (2)°, while the uncoordinated rings show a larger interplanar angle of 21.3 (2)°. The flexible propane spacer displays a zigzag chain. Intermolecular O—H⋯N and O—H⋯O interactions result in two-dimensional polymeric structures parallel to (100). Two C atoms of the spacer are disordered over two positions, with site occupancy factors of ca 0.85 and 0.15.

Related literature

For related literature, see: Fan et al. (2005 ); Gallardo et al. (2001 , 2004 ); Gong et al. (2004 ); Mizukami et al. (2005 ); Rodríguez-Diéguez et al. (2007 ); Wang et al. (2005 ).

Experimental

Crystal data

[Zn(C₁₅H₁₄N₁₀)(H₂O)₂](ClO₄)₂
M_r = 969.03
Monoclinic, P 2₁ /c
a = 7.378 (3) Å
b = 13.354 (3) Å
c = 20.764 (4) Å
β = 99.25 (2)°
V = 2019.2 (10) Å³
Z = 2
Mo Kα radiation
μ = 0.82 mm⁻¹
T = 293 (2) K
0.50 × 0.46 × 0.20 mm

Data collection

Enraf–Nonius CAD-4 diffractometer
Absorption correction: ψ scan (North et al., 1968 ) T_min = 0.682, T_max = 0.853
3873 measured reflections
3576 independent reflections
2826 reflections with I > 2σ(I)
R_int = 0.016
3 standard reflections every 200 reflections intensity decay: 1%

Refinement

R[F² > 2σ(F²)] = 0.035
wR(F²) = 0.097
S = 1.06
3576 reflections
305 parameters
3 restraints
H-atom parameters constrained
Δρ_max = 0.30 e Å⁻³
Δρ_min = −0.41 e Å⁻³

Table 1
Selected bond lengths (Å)

Zn1—O1W	2.1079 (18)
Zn1—N17	2.149 (2)
Zn1—N11	2.170 (2)

Table 2
Hydrogen-bond geometry (Å, °)

D—H⋯A	D—H	H⋯A	D⋯A	D—H⋯A
O1W—H1WA⋯O11	0.86	2.01	2.869 (3)	172
O1W—H1WB⋯N21ⁱ	0.86	1.97	2.833 (3)	178
Symmetry code: (i) $[-x, y-{\script{1\over 2}}, -z+{\script{1\over 2}}]$ .

Data collection: CAD-4 EXPRESS (Enraf–Nonius, 1994 ); cell refinement: SET4 in CAD-4 EXPRESS; data reduction: HELENA (Spek, 1996 ); program(s) used to solve structure: SIR97 (Altomare et al., 1999 ); program(s) used to refine structure: SHELXL97 (Sheldrick, 2008 ); molecular graphics: PLATON (Spek, 2003 ) and Mercury (Macrae et al., 2006 ); software used to prepare material for publication: SHELXL97 and publCIF (Westrip, 2008 ).

Supporting information

Crystal structure: contains datablocks global, I. DOI: 10.1107/S1600536808006703/bg2168sup1.cif

Structure factors: contains datablock I. DOI: 10.1107/S1600536808006703/bg2168Isup2.hkl

checkCIF report

Comment top

New compounds for the research of supramolecular chemistry and crystal engineering have been extensively described in the literature in the last few years (Wang et al., 2005; Fan et al., 2005; Rodríguez-Diéguez et al., 2007). Self-assembly processes involving organic ligands and metal ions have attracted much attention from the point of view of the development of novel functional materials with unique electronic, magnetic, catalytic and optical properties. However, while an accurate prediction of the overall crystal structure of such materials is not often an easy task, the introduction of rational organic ligands acting as building blocks has been recognized as a crucial synthetic strategy to overcome such difficulties. The syntheses of aromatic molecules containing nitrogen donor groups and which are interconnected by different type of spacers, such as conformationally rigid or flexible molecular skeletons, have been widely utilized as building blocks (Mizukami et al., 2005; Gallardo et al., 2001; Gong et al., 2004).

The synthesis and X-ray crystal structure of the ligand 1,3-Bis-[(2-pyridyl)-2H-tetrazol-5-yl]propane (L1) has been described previously (Gallardo et al., 2004). We report herein the title cation complex [Zn(L1)₂(H₂O)₂]²⁺. The Zn^II atom lies on a center of symmetry and its distorted octahedral coordination is achieved through the interaction with four nitrogen atoms of two trans L1 ligands, defining the equatorial plane and two water molecules in apical positions (Fig. 1). The basal Zn1—N17 (2.149 (2) Å) and Zn1—N11 (2.170 (2) Å) distances are somewhat larger than the apical ones (Zn1—O1W: (2.108 (2) Å). Some conformational differences in the structure of the two 2-pyridyl-2H-tetrazoyl units in the L1 ligand can be observed: the coordination of the pyridyl and tetrazoyl rings of one of the units to the metal center imposes structural rigidity in this moiety, and the rings become rings quasi coplanar with an interplanar angle of 1.9 (2)°. The N11—C10—C16 angle (113.5 (2)°) is smaller than the expected value due to the restriction of the five-membered chelate ring. On the other hand, in the uncoordinated unit the bond the corresponding rings are free to rotate around C20—C26 and the interplanar angle between angle climbs up to 21.3 (2)°. Besides, the N21—C20—C26 angle (116.6 (2)°) is significantly larger than the one in the coordinated unit. A two-dimensional polymeric structure parallel to (100) is formed by intermolecular O—H···N interactions (Fig. 2). Finally, the perchlorate counterion is also connected to the polymeric structure by a O—H···O interaction.

Related literature top

For related literature, see: Fan et al. (2005); Gallardo et al. (2001, 2004); Gong et al. (2004); Mizukami et al. (2005); Rodríguez-Diéguez et al. (2007); Wang et al. (2005).

Experimental top

Ligand L1 (obtained as described in Gallardo et al., 2004) was added to a suspension of Zn(ClO)₄.6H₂O in Ethanol and stirred at 50°C for 30 min. The white product was filtered off and recrystallized from isopropyl alcohol/water (1:1) affording white crystals. Yield: 61%. Elemental analysis. Calc. C₃₀H₃₂Cl₂N₂₀O₁₀Zn: C 37.18, H 3.33, N 28.91%. Found: C 37.27, H 3.29, N 28.98%.

Computing details top

Data collection: CAD-4 EXPRESS (Enraf–Nonius, 1994); cell refinement: SET4 in CAD-4 EXPRESS (Enraf–Nonius, 1994); data reduction: HELENA (Spek, 1996); program(s) used to solve structure: SIR97 (Altomare et al., 1999); program(s) used to refine structure: SHELXL97 (Sheldrick, 2008); molecular graphics: PLATON (Spek, 2003) and Mercury (Macrae et al., 2006); software used to prepare material for publication: SHELXL97 (Sheldrick, 2008) and publCIF (Westrip, 2008).

Figures top

	Fig. 1. The molecular structure of the cation complex showing the labeling scheme. Displacement ellipsoids are shown at the 40% probability level. Symmetry code: (i) -x, -y, -z
	Fig. 2. A detail of the two-dimensional polymeric strucuture formed by hydrogen bonding.

trans-Diaquabis{1,3-bis[5-(2-pyridyl)-2H-tetrazol-2-yl]propane}zinc(II) bis(perchlorate) top

Crystal data top

[Zn(C₁₅H₁₄N₁₀)(H₂O)₂](ClO₄)₂	F(000) = 992
M_r = 969.03	D_x = 1.594 Mg m⁻³
Monoclinic, P2₁/c	Mo Kα radiation, λ = 0.71069 Å
Hall symbol: -P 2ybc	Cell parameters from 25 reflections
a = 7.378 (3) Å	θ = 9.6–15.4°
b = 13.354 (3) Å	µ = 0.82 mm⁻¹
c = 20.764 (4) Å	T = 293 K
β = 99.25 (2)°	Prismatic, colorless
V = 2019.2 (10) Å³	0.50 × 0.46 × 0.20 mm
Z = 2

Data collection top

Enraf–Nonius CAD-4 diffractometer	2826 reflections with I > 2σ(I)
Radiation source: fine-focus sealed tube	R_int = 0.016
Graphite monochromator	θ_max = 25.1°, θ_min = 2.5°
ω–2θ scans	h = 0→8
Absorption correction: ψ scan (North et al., 1968)	k = 0→15
T_min = 0.682, T_max = 0.853	l = −24→24
3873 measured reflections	3 standard reflections every 200 reflections
3576 independent reflections	intensity decay: 1%

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)] = 0.035	Hydrogen site location: inferred from neighbouring sites
wR(F²) = 0.097	H-atom parameters constrained
S = 1.06	w = 1/[σ²(F_o²) + (0.0463P)² + 1.2496P] where P = (F_o² + 2F_c²)/3
3576 reflections	(Δ/σ)_max < 0.001
305 parameters	Δρ_max = 0.30 e Å⁻³
3 restraints	Δρ_min = −0.41 e Å⁻³

Crystal data top

[Zn(C₁₅H₁₄N₁₀)(H₂O)₂](ClO₄)₂	V = 2019.2 (10) Å³
M_r = 969.03	Z = 2
Monoclinic, P2₁/c	Mo Kα radiation
a = 7.378 (3) Å	µ = 0.82 mm⁻¹
b = 13.354 (3) Å	T = 293 K
c = 20.764 (4) Å	0.50 × 0.46 × 0.20 mm
β = 99.25 (2)°

Data collection top

Enraf–Nonius CAD-4 diffractometer	2826 reflections with I > 2σ(I)
Absorption correction: ψ scan (North et al., 1968)	R_int = 0.016
T_min = 0.682, T_max = 0.853	3 standard reflections every 200 reflections
3873 measured reflections	intensity decay: 1%
3576 independent reflections

Refinement top

R[F² > 2σ(F²)] = 0.035	3 restraints
wR(F²) = 0.097	H-atom parameters constrained
S = 1.06	Δρ_max = 0.30 e Å⁻³
3576 reflections	Δρ_min = −0.41 e Å⁻³
305 parameters

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

	x	y	z	U_iso*/U_eq	Occ. (<1)
Zn1	0.0000	0.5000	0.5000	0.03313 (13)
O1W	0.1357 (3)	0.37083 (13)	0.54150 (8)	0.0414 (4)
H1WA	0.2079	0.3821	0.5779	0.050*
H1WB	0.0630	0.3224	0.5479	0.050*
C1	0.2499 (4)	0.4082 (2)	0.26479 (13)	0.0525 (8)
H1C	0.3610	0.4474	0.2763	0.063*	0.848 (8)
H1B	0.2857	0.3387	0.2618	0.063*	0.848 (8)
H1A'	0.3789	0.4082	0.2838	0.063*	0.152 (8)
H1B'	0.2230	0.3455	0.2416	0.063*	0.152 (8)
C2	0.1502 (6)	0.4409 (3)	0.19841 (17)	0.0478 (12)	0.848 (8)
H2A	0.0335	0.4063	0.1884	0.057*	0.848 (8)
H2B	0.2233	0.4235	0.1652	0.057*	0.848 (8)
C2'	0.212 (2)	0.5004 (19)	0.2178 (9)	0.062 (9)	0.152 (8)
H2A'	0.3042	0.4990	0.1893	0.075*	0.152 (8)
H2B'	0.2302	0.5620	0.2428	0.075*	0.152 (8)
C3	0.1192 (7)	0.5522 (3)	0.19766 (16)	0.0473 (11)	0.848 (8)
H3A	0.0221	0.5680	0.2224	0.057*	0.848 (8)
H3B	0.2299	0.5865	0.2177	0.057*	0.848 (8)
C3'	0.031 (2)	0.5010 (16)	0.1744 (9)	0.048 (6)	0.152 (8)
H3A'	−0.0017	0.4382	0.1521	0.058*	0.152 (8)
H3B'	−0.0640	0.5198	0.1994	0.058*	0.152 (8)
C10	−0.2250 (3)	0.36570 (18)	0.40158 (11)	0.0336 (5)
N11	−0.2337 (3)	0.40794 (15)	0.46025 (9)	0.0330 (5)
C12	−0.3779 (4)	0.3837 (2)	0.48910 (13)	0.0407 (6)
H12	−0.3880	0.4129	0.5290	0.049*
C13	−0.5122 (4)	0.3170 (2)	0.46167 (15)	0.0488 (7)
H13	−0.6099	0.3013	0.4831	0.059*
C14	−0.4989 (4)	0.2741 (2)	0.40210 (15)	0.0505 (7)
H14	−0.5869	0.2285	0.3831	0.061*
C15	−0.3538 (4)	0.2996 (2)	0.37130 (13)	0.0433 (6)
H15	−0.3432	0.2727	0.3308	0.052*
C16	−0.0630 (3)	0.39652 (18)	0.37349 (11)	0.0333 (5)
N17	0.0622 (3)	0.45884 (16)	0.40591 (10)	0.0351 (5)
N18	0.1900 (3)	0.47270 (17)	0.36914 (10)	0.0404 (5)
N19	0.1370 (3)	0.41780 (17)	0.31670 (10)	0.0395 (5)
N20	−0.0198 (3)	0.36842 (17)	0.31667 (10)	0.0414 (5)
C20	0.1645 (4)	0.6352 (2)	−0.02723 (13)	0.0393 (6)
N21	0.1096 (3)	0.71610 (16)	−0.06368 (11)	0.0429 (5)
C22	0.1892 (4)	0.7317 (2)	−0.11638 (14)	0.0534 (8)
H22	0.1536	0.7876	−0.1420	0.064*
C23	0.3205 (5)	0.6698 (3)	−0.13475 (16)	0.0654 (9)
H23	0.3741	0.6845	−0.1712	0.078*
C24	0.3713 (5)	0.5852 (3)	−0.09787 (17)	0.0697 (10)
H24	0.4573	0.5409	−0.1098	0.084*
C25	0.2923 (4)	0.5676 (2)	−0.04327 (15)	0.0552 (8)
H25	0.3242	0.5113	−0.0176	0.066*
C26	0.0884 (4)	0.62351 (19)	0.03362 (13)	0.0394 (6)
N27	−0.0628 (3)	0.66990 (18)	0.04770 (12)	0.0485 (6)
N28	−0.0761 (4)	0.64443 (19)	0.10824 (12)	0.0540 (6)
N29	0.0649 (4)	0.58592 (19)	0.12805 (12)	0.0539 (6)
N30	0.1722 (3)	0.56958 (19)	0.08358 (11)	0.0513 (6)
Cl1	0.34362 (10)	0.38846 (6)	0.71439 (3)	0.0497 (2)
O11	0.3975 (4)	0.4197 (2)	0.65481 (12)	0.0874 (8)
O12	0.4636 (4)	0.3152 (2)	0.74296 (16)	0.1075 (11)
O13	0.1623 (4)	0.3525 (3)	0.70176 (15)	0.1099 (11)
O14	0.3557 (5)	0.4722 (3)	0.75703 (19)	0.1274 (13)

Atomic displacement parameters (Å²) top

	U¹¹	U²²	U³³	U¹²	U¹³	U²³
Zn1	0.0396 (2)	0.0337 (2)	0.0263 (2)	−0.00564 (18)	0.00595 (16)	−0.00305 (17)
O1W	0.0500 (11)	0.0362 (10)	0.0370 (10)	−0.0037 (8)	0.0033 (8)	0.0006 (8)
C1	0.0586 (18)	0.066 (2)	0.0379 (15)	0.0157 (16)	0.0229 (14)	0.0050 (14)
C2	0.067 (3)	0.048 (2)	0.0299 (19)	−0.006 (2)	0.0123 (19)	−0.0028 (16)
C2'	0.028 (10)	0.13 (3)	0.028 (10)	0.024 (15)	0.012 (8)	0.024 (15)
C3	0.061 (3)	0.050 (2)	0.0314 (19)	0.004 (2)	0.0107 (19)	−0.0017 (16)
C3'	0.038 (11)	0.067 (15)	0.042 (11)	0.008 (11)	0.009 (9)	0.025 (11)
C10	0.0382 (14)	0.0300 (13)	0.0308 (12)	0.0017 (11)	0.0003 (10)	0.0012 (10)
N11	0.0355 (11)	0.0312 (11)	0.0319 (11)	−0.0005 (9)	0.0043 (9)	0.0027 (9)
C12	0.0395 (14)	0.0410 (15)	0.0422 (14)	0.0031 (12)	0.0087 (12)	0.0041 (12)
C13	0.0338 (14)	0.0504 (17)	0.0623 (19)	−0.0011 (13)	0.0082 (13)	0.0105 (15)
C14	0.0404 (15)	0.0460 (17)	0.0608 (19)	−0.0081 (13)	−0.0045 (14)	−0.0024 (14)
C15	0.0445 (15)	0.0411 (15)	0.0420 (15)	−0.0022 (12)	0.0000 (12)	−0.0062 (12)
C16	0.0401 (14)	0.0293 (12)	0.0294 (12)	0.0008 (11)	0.0026 (11)	0.0015 (10)
N17	0.0405 (12)	0.0364 (11)	0.0295 (11)	−0.0032 (10)	0.0088 (9)	0.0005 (9)
N18	0.0467 (13)	0.0425 (13)	0.0332 (12)	0.0003 (10)	0.0102 (10)	0.0000 (9)
N19	0.0478 (13)	0.0429 (12)	0.0291 (11)	0.0050 (11)	0.0099 (10)	0.0025 (9)
N20	0.0505 (14)	0.0447 (13)	0.0287 (11)	0.0032 (11)	0.0060 (10)	−0.0049 (10)
C20	0.0429 (15)	0.0370 (14)	0.0373 (14)	−0.0021 (12)	0.0045 (12)	0.0000 (11)
N21	0.0537 (14)	0.0359 (12)	0.0386 (12)	−0.0020 (11)	0.0054 (11)	0.0000 (10)
C22	0.067 (2)	0.0500 (18)	0.0426 (16)	−0.0033 (15)	0.0075 (15)	0.0075 (14)
C23	0.069 (2)	0.086 (3)	0.0469 (17)	−0.0004 (19)	0.0247 (16)	0.0100 (18)
C24	0.068 (2)	0.081 (2)	0.066 (2)	0.0221 (19)	0.0282 (18)	0.0054 (19)
C25	0.0602 (19)	0.0541 (19)	0.0534 (18)	0.0129 (16)	0.0153 (15)	0.0094 (15)
C26	0.0448 (15)	0.0314 (14)	0.0418 (15)	0.0009 (12)	0.0066 (12)	−0.0003 (11)
N27	0.0533 (15)	0.0432 (13)	0.0511 (14)	0.0121 (11)	0.0145 (12)	0.0072 (11)
N28	0.0587 (16)	0.0535 (15)	0.0535 (15)	0.0171 (13)	0.0207 (13)	0.0091 (12)
N29	0.0618 (16)	0.0559 (15)	0.0484 (14)	0.0193 (13)	0.0228 (12)	0.0112 (12)
N30	0.0565 (15)	0.0568 (15)	0.0440 (13)	0.0168 (12)	0.0189 (12)	0.0100 (12)
Cl1	0.0474 (4)	0.0528 (4)	0.0465 (4)	0.0002 (3)	0.0006 (3)	0.0051 (3)
O11	0.0928 (19)	0.109 (2)	0.0586 (15)	−0.0223 (17)	0.0069 (14)	0.0235 (15)
O12	0.104 (2)	0.095 (2)	0.113 (2)	0.0239 (18)	−0.0123 (19)	0.0464 (19)
O13	0.0612 (17)	0.168 (3)	0.098 (2)	−0.0375 (19)	0.0047 (15)	−0.009 (2)
O14	0.141 (3)	0.111 (2)	0.137 (3)	−0.016 (2)	0.042 (3)	−0.068 (2)

Geometric parameters (Å, º) top

Zn1—O1Wⁱ	2.1079 (18)	C12—H12	0.9300
Zn1—O1W	2.1079 (18)	C13—C14	1.381 (4)
Zn1—N17ⁱ	2.149 (2)	C13—H13	0.9300
Zn1—N17	2.149 (2)	C14—C15	1.375 (4)
Zn1—N11ⁱ	2.170 (2)	C14—H14	0.9300
Zn1—N11	2.170 (2)	C15—H15	0.9300
O1W—H1WA	0.8646	C16—N20	1.325 (3)
O1W—H1WB	0.8638	C16—N17	1.341 (3)
C1—N19	1.470 (3)	N17—N18	1.319 (3)
C1—C2	1.519 (4)	N18—N19	1.319 (3)
C1—C2'	1.569 (17)	N19—N20	1.331 (3)
C1—H1C	0.9700	C20—N21	1.343 (3)
C1—H1B	0.9700	C20—C25	1.385 (4)
C1—H1A'	0.9700	C20—C26	1.471 (4)
C1—H1B'	0.9700	N21—C22	1.339 (4)
C2—C3	1.503 (5)	C22—C23	1.373 (5)
C2—H2A	0.9700	C22—H22	0.9300
C2—H2B	0.9699	C23—C24	1.383 (5)
C2'—C3'	1.485 (17)	C23—H23	0.9300
C2'—H2A'	0.9700	C24—C25	1.375 (4)
C2'—H2B'	0.9700	C24—H24	0.9300
C3—N29	1.505 (4)	C25—H25	0.9300
C3—H3A	0.9701	C26—N30	1.331 (3)
C3—H3B	0.9700	C26—N27	1.348 (3)
C3'—N29	1.534 (14)	N27—N28	1.321 (3)
C3'—H3A'	0.9699	N28—N29	1.313 (3)
C3'—H3B'	0.9700	N29—N30	1.327 (3)
C10—N11	1.353 (3)	Cl1—O12	1.387 (3)
C10—C15	1.373 (4)	Cl1—O13	1.406 (3)
C10—C16	1.470 (3)	Cl1—O14	1.420 (3)
N11—C12	1.342 (3)	Cl1—O11	1.421 (3)
C12—C13	1.385 (4)

O1Wⁱ—Zn1—O1W	180.00 (9)	C10—N11—Zn1	115.41 (16)
O1Wⁱ—Zn1—N17ⁱ	90.32 (8)	N11—C12—C13	122.5 (3)
O1W—Zn1—N17ⁱ	89.68 (8)	N11—C12—H12	118.7
O1Wⁱ—Zn1—N17	89.68 (8)	C13—C12—H12	118.7
O1W—Zn1—N17	90.32 (8)	C14—C13—C12	119.1 (3)
N17ⁱ—Zn1—N17	180.00 (4)	C14—C13—H13	120.5
O1Wⁱ—Zn1—N11ⁱ	89.32 (8)	C12—C13—H13	120.5
O1W—Zn1—N11ⁱ	90.68 (8)	C15—C14—C13	119.1 (3)
N17ⁱ—Zn1—N11ⁱ	77.40 (8)	C15—C14—H14	120.5
N17—Zn1—N11ⁱ	102.60 (8)	C13—C14—H14	120.5
O1Wⁱ—Zn1—N11	90.68 (8)	C10—C15—C14	118.7 (3)
O1W—Zn1—N11	89.32 (8)	C10—C15—H15	120.7
N17ⁱ—Zn1—N11	102.60 (8)	C14—C15—H15	120.7
N17—Zn1—N11	77.40 (8)	N20—C16—N17	112.2 (2)
N11ⁱ—Zn1—N11	180.00 (9)	N20—C16—C10	127.0 (2)
Zn1—O1W—H1WA	113.6	N17—C16—C10	120.9 (2)
Zn1—O1W—H1WB	114.1	N18—N17—C16	107.2 (2)
H1WA—O1W—H1WB	107.9	N18—N17—Zn1	140.15 (17)
N19—C1—C2	113.0 (3)	C16—N17—Zn1	112.61 (16)
N19—C1—C2'	108.8 (8)	N17—N18—N19	104.8 (2)
N19—C1—H1C	109.1	N18—N19—N20	114.7 (2)
C2—C1—H1C	109.6	N18—N19—C1	121.8 (2)
N19—C1—H1B	108.9	N20—N19—C1	123.4 (2)
C2—C1—H1B	108.3	C16—N20—N19	101.1 (2)
H1C—C1—H1B	107.8	N21—C20—C25	123.0 (3)
N19—C1—H1A'	109.6	N21—C20—C26	116.6 (2)
C2'—C1—H1A'	108.6	C25—C20—C26	120.4 (2)
C2'—C1—H1B'	111.6	C22—N21—C20	116.9 (2)
H1A'—C1—H1B'	108.1	N21—C22—C23	123.8 (3)
C3—C2—C1	110.2 (3)	N21—C22—H22	118.1
C3—C2—H2A	109.9	C23—C22—H22	118.1
C1—C2—H2A	110.0	C22—C23—C24	118.6 (3)
C3—C2—H2B	109.3	C22—C23—H23	120.7
C1—C2—H2B	109.4	C24—C23—H23	120.7
H2A—C2—H2B	108.0	C25—C24—C23	118.9 (3)
C3'—C2'—C1	115.7 (15)	C25—C24—H24	120.6
C3'—C2'—H2A'	106.3	C23—C24—H24	120.6
C1—C2'—H2A'	106.9	C24—C25—C20	118.8 (3)
C3'—C2'—H2B'	110.7	C24—C25—H25	120.6
C1—C2'—H2B'	109.7	C20—C25—H25	120.6
H2A'—C2'—H2B'	107.1	N30—C26—N27	112.1 (2)
C2—C3—N29	108.8 (3)	N30—C26—C20	122.2 (2)
C2—C3—H3A	109.5	N27—C26—C20	125.5 (2)
N29—C3—H3A	109.8	N28—N27—C26	106.2 (2)
C2—C3—H3B	110.3	N29—N28—N27	106.0 (2)
N29—C3—H3B	110.2	N28—N29—N30	114.3 (2)
H3A—C3—H3B	108.2	N28—N29—C3	123.6 (3)
C2'—C3'—N29	99.4 (12)	N30—N29—C3	121.5 (3)
C2'—C3'—H3A'	114.6	N28—N29—C3'	115.9 (7)
N29—C3'—H3A'	113.1	N30—N29—C3'	119.4 (9)
C2'—C3'—H3B'	109.5	N29—N30—C26	101.5 (2)
N29—C3'—H3B'	110.4	O12—Cl1—O13	111.2 (2)
H3A'—C3'—H3B'	109.4	O12—Cl1—O14	108.5 (2)
N11—C10—C15	123.4 (2)	O13—Cl1—O14	110.3 (2)
N11—C10—C16	113.5 (2)	O12—Cl1—O11	109.3 (2)
C15—C10—C16	123.0 (2)	O13—Cl1—O11	109.19 (18)
C12—N11—C10	117.2 (2)	O14—Cl1—O11	108.3 (2)
C12—N11—Zn1	127.24 (17)

Symmetry code: (i) −x, −y+1, −z+1.

Hydrogen-bond geometry (Å, º) top

D—H···A	D—H	H···A	D···A	D—H···A
O1W—H1WA···O11	0.86	2.01	2.869 (3)	172
O1W—H1WB···N21ⁱⁱ	0.86	1.97	2.833 (3)	178

Symmetry code: (ii) −x, y−1/2, −z+1/2.

Experimental details

Crystal data
Chemical formula	[Zn(C₁₅H₁₄N₁₀)(H₂O)₂](ClO₄)₂
M_r	969.03
Crystal system, space group	Monoclinic, P2₁/c
Temperature (K)	293
a, b, c (Å)	7.378 (3), 13.354 (3), 20.764 (4)
β (°)	99.25 (2)
V (Å³)	2019.2 (10)
Z	2
Radiation type	Mo Kα
µ (mm⁻¹)	0.82
Crystal size (mm)	0.50 × 0.46 × 0.20

Data collection
Diffractometer	Enraf–Nonius CAD-4 diffractometer
Absorption correction	ψ scan (North et al., 1968)
T_min, T_max	0.682, 0.853
No. of measured, independent and observed [I > 2σ(I)] reflections	3873, 3576, 2826
R_int	0.016
(sin θ/λ)_max (Å⁻¹)	0.596

Refinement
R[F² > 2σ(F²)], wR(F²), S	0.035, 0.097, 1.06
No. of reflections	3576
No. of parameters	305
No. of restraints	3
H-atom treatment	H-atom parameters constrained
Δρ_max, Δρ_min (e Å⁻³)	0.30, −0.41

Computer programs: , SET4 in CAD-4 EXPRESS (Enraf–Nonius, 1994), HELENA (Spek, 1996), SIR97 (Altomare et al., 1999), PLATON (Spek, 2003) and Mercury (Macrae et al., 2006), SHELXL97 (Sheldrick, 2008) and publCIF (Westrip, 2008).

Selected bond lengths (Å) top

Zn1—O1W	2.1079 (18)	Zn1—N11	2.170 (2)
Zn1—N17	2.149 (2)

Hydrogen-bond geometry (Å, º) top

D—H···A	D—H	H···A	D···A	D—H···A
O1W—H1WA···O11	0.86	2.01	2.869 (3)	172
O1W—H1WB···N21ⁱ	0.86	1.97	2.833 (3)	178

Symmetry code: (i) −x, y−1/2, −z+1/2.

Acknowledgements

The authors thank the Conselho Nacional de Desenvolvimento Científico e Tecnológico (CNPq), Fundação de Apoio à Pesquisa Científica e Tecnológica do Estado de Santa Catarina (FAPESC), Financiadora de Estudos e Projetos (FINEP) and Coordenação de Aperfeiçoamento de Pessoal de Nível Superior (CAPES).

References

Altomare, A., Burla, M. C., Camalli, M., Cascarano, G. L., Giacovazzo, C., Guagliardi, A., Moliterni, A. G. G., Polidori, G. & Spagna, R. (1999). J. Appl. Cryst. 32, 115–119. Web of Science CrossRef CAS IUCr Journals Google Scholar
Enraf–Nonius (1994). CAD-4 EXPRESS. Enraf–Nonius, Delft, The Netherlands. Google Scholar
Fan, R., Zhu, D., Ding, H., Mu, Y., Su, Q. & Xia, H. (2005). Synth. Met. 149, 135–141. Web of Science CSD CrossRef CAS Google Scholar
Gallardo, H., Magnago, R. & Bortoluzzi, A. J. (2001). Liq. Cryst. 28, 1343–1352. CSD CrossRef CAS Google Scholar
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Spek, A. L. (1996). HELENA. University of Utrecht, The Netherlands. Google Scholar
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Volume 64| Part 4| April 2008| Pages m541-m542

doi:10.1107/S1600536808006703

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

trans-Di­aqua­bis­{1,3-bis­­[5-(2-pyrid­yl)-2H-tetra­zol-2-yl]propane}zinc(II) bis­­(perchlorate)

Related literature

Experimental

Crystal data

Data collection

Refinement

Supporting information

Acknowledgements

References

metal-organic compounds

trans-Diaquabis{1,3-bis[5-(2-pyridyl)-2H-tetrazol-2-yl]propane}zinc(II) bis(perchlorate)