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The two new title complexes, [Mn(C5H3N6)2(H2O)2] and [Zn(C5H3N6)2(H2O)2], are isomorphous. In both compounds, the metal atom is located on an inversion center and is coordinated by four N atoms from two 5-(pyrazin-2-yl)-1H-tetra­zolate anions in the basal plane and by two O atoms of water ligands in the apical positions to form a distorted octa­hedral geometry. Inter­molecular hydrogen-bond inter­actions between the uncoordinated N atoms of the tetra­zolate anions and the H atoms of the water mol­ecules lead to the formation of a three-dimensional network.

Supporting information

cif

Crystallographic Information File (CIF) https://doi.org/10.1107/S010827010604457X/dn3026sup1.cif
Contains datablocks global, I, II

hkl

Structure factor file (CIF format) https://doi.org/10.1107/S010827010604457X/dn3026Isup2.hkl
Contains datablock I

hkl

Structure factor file (CIF format) https://doi.org/10.1107/S010827010604457X/dn3026IIsup3.hkl
Contains datablock II

CCDC references: 632928; 632929

Comment top

Tetrazoles have attracted considerable interest because of their popular functionality and variety of applications (Butler, 1996). It is well known that tetrazoles have been used in many fields, including pharmaceuticals (Singh et al., 1980), speciality explosives (Ostrovskii et al., 1999), photography and information recording systems (Koldobskii & Ostrovskii, 1994), and as precursors to nitrogen-containing heterocycles (Huisgen et al., 1960). Simple heating of an azide salt with a nitrile in an aqueous solution could produce the corresponding tetrazolate (Dimroth & Fester, 1910). In contrast to the previous synthetic methods, the tetrazoles are easily prepared in high yield by addition of sodium azide to a nitrile in water, with the catalysis of Lewis acids such as zinc salts (Demko & Sharpless, 2001). Although the synthetic method has been improved, the role of Lewis acids in the synthesis reaction and the exact intermediates are rarely known (Lin et al., 2005; Wu et al., 2005; Yu et al., 2004). In order to better understand the influence of Lewis acids on the tetrazole synthesis reaction and to get obtain a deeper insight into the intermediates, we report here the syntheses and structures of two isomorphous complexes [Mn(5-PYZTZ)2(H2O)2], (I), and [Zn(5-PYZTZ)2(H2O)2], (II) [5-PYZTZ is 5-(pyrazin-2-yl)-1H-tetrazolate].

In (I), the MnII ion, located on an inversion center, is coordinated to two 5-(pyrazinyl)tetrazolate anions and two aqua ligands to give a distorted octahedral geometry, in which the basal plane is formed by two pyrazine N atoms and two tetrazolate N atoms (atoms N1, N6, N1i and N6i) of two 5-PYZTZ anions (Fig. 1). The apical positions are occupied by two O atoms (O1 and O1i) from two water molecules [symmetry codes: (i) −x, −y, −z + 2]. Intermolecular hydrogen-bonding interactions between the uncoordinated N atoms of the tetrazolate anions and the H atoms of the water molecules result in the formation of a three-dimensional network (Fig. 2, and Table 2).

In (II), the ZnII atom has the same coordination environment as the Mn atom in (I). The three-dimensional structure is also formed by intermolecular hydrogen bonds involving uncoordinated N atoms of the tetrazolate anions and the H atoms of the water molecules.

In (I) and (II), the Mn—N(5-PYZTZ) and Zn—N(5-PYZTZ) distances (Tables 1 and 3) are comparable to the corresponding distances in related manganese (Lin et al., 2005) and zinc complexes (Wang et al., 2005; Zhang et al., 2005), and the Mn—O and Zn—O distances are similar to the corresponding distances in water-coordinated manganese (Mautner et al., 2004) and zinc complexes (Zhang et al., 2005), respectively.

In (I), the N—Mn—N angles (two neighbouring atoms) are in the range 75.15 (7)–104.85 (7)°. The corresponding N—Zn—N angles are in the range 78.34 (7)–101.66 (7)°, indicating that the geometry in (I) is more distorted than that of (II).

In both complexes, the bond distances and angles of tetrazole ring [1.303 (3)–1.338 (3) Å and 104.6 (2)–111.6 (2)°] and pyrazine ring [1.325 (3)–1.386 (3) Å and 116.1 (2)–122.5 (2)°] are in the normal ranges observed in pyrazine- or tetrazole-containing complexes (Mautner et al., 2004; Ferigo et al., 1994).

Experimental top

A 4 ml e thanol solution of pyrazine-2-carbonitrile (0.20 mmol, 21.02 mg) and a 4 ml aqueous solution of manganese acetate (0.20 mmol, 49.02 mg) were mixed and stirred for 5 min; a 2 ml aqueous solution of sodium azide (0.20 mmol, 13.01 mg) was added to the mixture. After being stirred for another 5 min, the solution was filtered and the filtrate was slowly evaporated in air. After one week, colourless block crystals of (I) were isolated in 55% yield. Analysis calculated for C10H10MnN12O2: C 31.18, H 2.62, N 43.63%; found C 30.89, H 2.71, N 43.76%. Complex (II) was prepared by a similar procedure in 47% yield. Analysis calculated for C10H10N12O2Zn: C 30.36, H 2.55, N 42.48%; found C 30.09, H 2.41, N 42.65%.

Refinement top

In both complexes, the position of the water H atom was found from a difference Fourier map and refined freely along with an isotropic displacement parameter; all other H atoms were placed in geometrically idealized positions and constrained to ride on their parent atoms with C—H distances of 0.93 Å and Uiso(H) = 1.2Ueq(C).

Computing details top

For both compounds, data collection: SMART (Bruker, 2000); cell refinement: SAINT (Bruker, 2000); data reduction: SAINT; program(s) used to solve structure: SHELXS97 (Sheldrick, 1997); program(s) used to refine structure: SHELXL97 (Sheldrick, 1997); molecular graphics: SHELXTL (Bruker, 2000); software used to prepare material for publication: SHELXTL.

Figures top
[Figure 1] Fig. 1. A view of the molecule of (I), showing the atom-labelling scheme. Displacement ellipsoids are drawn at the 50% probability level and H atoms have been omitted for clarity [symmetry codes: (i) −x, −y, −z + 2]. Complex (II) is isomorphous.
[Figure 2] Fig. 2. The three-dimensional network in (I), formed via intermolecular hydrogen- bonding interactions, viewed along the a axis.
(I) Diaquabis[5-(pyrazin-2-yl-κN1)-1H-tetrazolato-κN1]manganese(II) top
Crystal data top
[Mn(C5H3N6)2(H2O)2]F(000) = 390
Mr = 385.24Dx = 1.745 Mg m3
Monoclinic, P21/nMo Kα radiation, λ = 0.71073 Å
Hall symbol: -P 2ynCell parameters from 722 reflections
a = 5.9642 (19) Åθ = 2.6–27.1°
b = 11.715 (4) ŵ = 0.94 mm1
c = 10.853 (4) ÅT = 293 K
β = 104.817 (4)°Block, colourless
V = 733.1 (4) Å30.40 × 0.30 × 0.25 mm
Z = 2
Data collection top
Bruker SMART CCD area-detector
diffractometer
1455 independent reflections
Radiation source: fine-focus sealed tube1235 reflections with I > 2σ(I)
Graphite monochromatorRint = 0.042
ϕ and ω scansθmax = 26.0°, θmin = 2.6°
Absorption correction: multi-scan
(SADABS; Bruker, 2000)
h = 76
Tmin = 0.705, Tmax = 0.799k = 814
3288 measured reflectionsl = 1213
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)] = 0.045Hydrogen site location: inferred from neighbouring sites
wR(F2) = 0.120H atoms treated by a mixture of independent and constrained refinement
S = 1.00 w = 1/[σ2(Fo2) + (0.089P)2]
where P = (Fo2 + 2Fc2)/3
1455 reflections(Δ/σ)max < 0.001
123 parametersΔρmax = 0.62 e Å3
3 restraintsΔρmin = 0.62 e Å3
Crystal data top
[Mn(C5H3N6)2(H2O)2]V = 733.1 (4) Å3
Mr = 385.24Z = 2
Monoclinic, P21/nMo Kα radiation
a = 5.9642 (19) ŵ = 0.94 mm1
b = 11.715 (4) ÅT = 293 K
c = 10.853 (4) Å0.40 × 0.30 × 0.25 mm
β = 104.817 (4)°
Data collection top
Bruker SMART CCD area-detector
diffractometer
1455 independent reflections
Absorption correction: multi-scan
(SADABS; Bruker, 2000)
1235 reflections with I > 2σ(I)
Tmin = 0.705, Tmax = 0.799Rint = 0.042
3288 measured reflections
Refinement top
R[F2 > 2σ(F2)] = 0.0453 restraints
wR(F2) = 0.120H atoms treated by a mixture of independent and constrained refinement
S = 1.00Δρmax = 0.62 e Å3
1455 reflectionsΔρmin = 0.62 e Å3
123 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
xyzUiso*/Ueq
Mn10.00000.00001.00000.0361 (2)
N10.1366 (3)0.18434 (15)0.99557 (15)0.0352 (4)
N20.2347 (4)0.41445 (18)0.9712 (3)0.0596 (6)
N30.4259 (3)0.25931 (17)0.78875 (18)0.0427 (5)
N40.5894 (3)0.17956 (19)0.7549 (2)0.0487 (5)
N50.5126 (3)0.08293 (17)0.8089 (2)0.0462 (5)
N60.2960 (3)0.09646 (15)0.88000 (18)0.0395 (5)
C10.3427 (4)0.2294 (2)1.0515 (2)0.0418 (5)
H10.45790.18241.09990.050*
C20.3900 (4)0.3431 (2)1.0400 (3)0.0521 (6)
H20.53560.37101.08170.063*
C30.0290 (4)0.3704 (2)0.9159 (3)0.0501 (6)
H30.08540.41790.86790.060*
C40.0218 (3)0.25603 (17)0.92695 (19)0.0348 (5)
C50.2472 (3)0.20629 (19)0.86497 (19)0.0353 (5)
O10.1025 (4)0.04281 (18)0.83085 (19)0.0563 (5)
H1A0.219 (4)0.016 (2)0.811 (3)0.065 (11)*
H1B0.048 (4)0.0985 (17)0.784 (2)0.054 (8)*
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
Mn10.0436 (3)0.0235 (3)0.0400 (3)0.00143 (16)0.0082 (2)0.00348 (17)
N10.0377 (9)0.0316 (9)0.0361 (9)0.0004 (7)0.0089 (7)0.0022 (7)
N20.0541 (13)0.0357 (11)0.0817 (16)0.0108 (9)0.0041 (11)0.0006 (11)
N30.0383 (10)0.0401 (11)0.0464 (10)0.0022 (8)0.0044 (8)0.0080 (9)
N40.0385 (10)0.0501 (12)0.0520 (11)0.0031 (9)0.0012 (8)0.0041 (10)
N50.0382 (10)0.0435 (12)0.0527 (12)0.0074 (8)0.0039 (8)0.0011 (9)
N60.0378 (9)0.0313 (10)0.0464 (10)0.0032 (7)0.0055 (8)0.0004 (8)
C10.0368 (11)0.0430 (13)0.0419 (12)0.0025 (9)0.0033 (9)0.0015 (10)
C20.0430 (12)0.0495 (14)0.0590 (15)0.0092 (11)0.0043 (11)0.0062 (12)
C30.0471 (13)0.0310 (12)0.0664 (16)0.0002 (10)0.0038 (11)0.0068 (11)
C40.0379 (11)0.0281 (11)0.0376 (11)0.0010 (8)0.0080 (9)0.0009 (8)
C50.0371 (10)0.0318 (11)0.0367 (11)0.0022 (9)0.0088 (8)0.0024 (9)
O10.0677 (12)0.0510 (11)0.0573 (11)0.0235 (10)0.0290 (9)0.0199 (10)
Geometric parameters (Å, º) top
Mn1—N12.313 (2)N4—N51.303 (3)
Mn1—N1i2.313 (2)N5—N61.334 (2)
Mn1—N62.217 (2)N6—C51.338 (3)
Mn1—N6i2.217 (2)C1—C21.375 (3)
Mn1—O12.138 (2)C1—H10.9300
Mn1—O1i2.138 (2)C2—H20.9300
N1—C11.332 (3)C3—C41.386 (3)
N1—C41.339 (3)C3—H30.9300
N2—C31.325 (3)C4—C51.462 (3)
N2—C21.327 (3)O1—H1A0.84 (3)
N3—C51.325 (3)O1—H1B0.84 (3)
N3—N41.332 (3)
N6—Mn1—N175.15 (7)N5—N6—Mn1141.9 (2)
N6i—Mn1—N1i75.15 (7)C5—N6—Mn1113.3 (1)
N6—Mn1—N1i104.85 (7)N1—C1—C2121.9 (2)
N6i—Mn1—N1104.85 (7)N1—C1—H1119.0
O1—Mn1—N191.23 (7)C2—C1—H1119.0
O1i—Mn1—N1i91.23 (7)N2—C2—C1122.1 (2)
O1—Mn1—N688.56 (8)N2—C2—H2118.9
O1i—Mn1—N6i88.56 (8)C1—C2—H2118.9
O1—Mn1—N1i88.77 (7)N2—C3—C4122.4 (2)
O1i—Mn1—N188.77 (7)N2—C3—H3118.8
O1—Mn1—N6i91.44 (8)C4—C3—H3118.8
O1i—Mn1—N691.44 (8)N1—C4—C3121.0 (2)
C1—N1—C4116.3 (2)N1—C4—C5116.2 (2)
C1—N1—Mn1130.5 (1)C3—C4—C5122.8 (2)
C4—N1—Mn1113.3 (1)N3—C5—N6111.2 (2)
C3—N2—C2116.2 (2)N3—C5—C4126.8 (2)
C5—N3—N4105.0 (2)N6—C5—C4122.0 (2)
N5—N4—N3109.7 (2)Mn1—O1—H1A124 (2)
N4—N5—N6109.5 (2)Mn1—O1—H1B124 (2)
N5—N6—C5104.6 (2)H1A—O1—H1B111 (2)
Symmetry code: (i) x, y, z+2.
Hydrogen-bond geometry (Å, º) top
D—H···AD—HH···AD···AD—H···A
O1—H1B···N4ii0.84 (1)2.66 (2)3.378 (3)145 (2)
O1—H1B···N3ii0.84 (1)1.91 (1)2.733 (3)168 (3)
O1—H1A···N4iii0.84 (3)2.70 (2)3.408 (3)144 (3)
O1—H1A···N5iii0.84 (3)1.98 (1)2.788 (3)162 (3)
Symmetry codes: (ii) x1/2, y1/2, z+3/2; (iii) x+1, y, z.
(II) diaquabis[5-(pyrazin-2-yl-κN1)-1H-tetrazolato-κN1]zinc(II) top
Crystal data top
[Zn(C5H3N6)2(H2O)2]F(000) = 400
Mr = 395.67Dx = 1.830 Mg m3
Monoclinic, P21/nMo Kα radiation, λ = 0.71073 Å
Hall symbol: -P 2ynCell parameters from 904 reflections
a = 6.0906 (18) Åθ = 2.7–26.6°
b = 11.456 (3) ŵ = 1.75 mm1
c = 10.686 (3) ÅT = 293 K
β = 105.634 (4)°Block, colourless
V = 718.0 (3) Å30.40 × 0.30 × 0.25 mm
Z = 2
Data collection top
Bruker SMART CCD area-detector
diffractometer
1406 independent reflections
Radiation source: fine-focus sealed tube1161 reflections with I > 2σ(I)
Graphite monochromatorRint = 0.034
ϕ and ω scansθmax = 26.0°, θmin = 2.7°
Absorption correction: multi-scan
(SADABS; Bruker, 2000)
h = 77
Tmin = 0.541, Tmax = 0.669k = 1412
3206 measured reflectionsl = 1213
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)] = 0.027Hydrogen site location: inferred from neighbouring sites
wR(F2) = 0.071H atoms treated by a mixture of independent and constrained refinement
S = 0.99 w = 1/[σ2(Fo2) + (0.04P)2]
where P = (Fo2 + 2Fc2)/3
1406 reflections(Δ/σ)max < 0.001
123 parametersΔρmax = 0.43 e Å3
3 restraintsΔρmin = 0.37 e Å3
Crystal data top
[Zn(C5H3N6)2(H2O)2]V = 718.0 (3) Å3
Mr = 395.67Z = 2
Monoclinic, P21/nMo Kα radiation
a = 6.0906 (18) ŵ = 1.75 mm1
b = 11.456 (3) ÅT = 293 K
c = 10.686 (3) Å0.40 × 0.30 × 0.25 mm
β = 105.634 (4)°
Data collection top
Bruker SMART CCD area-detector
diffractometer
1406 independent reflections
Absorption correction: multi-scan
(SADABS; Bruker, 2000)
1161 reflections with I > 2σ(I)
Tmin = 0.541, Tmax = 0.669Rint = 0.034
3206 measured reflections
Refinement top
R[F2 > 2σ(F2)] = 0.0273 restraints
wR(F2) = 0.071H atoms treated by a mixture of independent and constrained refinement
S = 0.99Δρmax = 0.43 e Å3
1406 reflectionsΔρmin = 0.37 e Å3
123 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
xyzUiso*/Ueq
Zn10.00000.00001.00000.03186 (14)
N10.1349 (3)0.17741 (15)0.99843 (15)0.0305 (4)
N20.2365 (3)0.41201 (18)0.9749 (2)0.0530 (6)
N30.4229 (3)0.25458 (17)0.79147 (17)0.0381 (4)
N40.5842 (3)0.17241 (18)0.7606 (2)0.0446 (5)
N50.5051 (3)0.07431 (17)0.81860 (18)0.0405 (5)
N60.2893 (3)0.09058 (15)0.88836 (17)0.0339 (4)
C10.3408 (4)0.2215 (2)1.0550 (2)0.0372 (5)
H10.45380.17271.10380.045*
C20.3896 (4)0.3377 (2)1.0427 (2)0.0457 (6)
H20.53510.36491.08350.055*
C30.0318 (4)0.3683 (2)0.9193 (2)0.0443 (6)
H30.08070.41780.87120.053*
C40.0205 (3)0.25227 (18)0.9300 (2)0.0299 (5)
C50.2450 (3)0.20180 (18)0.8694 (2)0.0306 (5)
O10.0823 (3)0.03652 (17)0.82549 (18)0.0465 (4)
H1A0.208 (3)0.0164 (19)0.817 (3)0.056 (9)*
H1B0.039 (4)0.0986 (14)0.785 (2)0.058 (9)*
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
Zn10.0328 (2)0.0222 (2)0.0381 (2)0.00033 (14)0.00524 (15)0.00323 (14)
N10.0317 (10)0.0275 (10)0.0316 (9)0.0004 (7)0.0074 (7)0.0006 (7)
N20.0477 (13)0.0330 (12)0.0705 (14)0.0098 (10)0.0029 (11)0.0000 (10)
N30.0318 (10)0.0360 (11)0.0430 (10)0.0012 (8)0.0042 (8)0.0077 (9)
N40.0338 (10)0.0455 (12)0.0491 (11)0.0017 (9)0.0019 (9)0.0055 (10)
N50.0319 (10)0.0388 (12)0.0475 (11)0.0058 (9)0.0050 (8)0.0006 (9)
N60.0291 (9)0.0280 (10)0.0417 (10)0.0019 (8)0.0046 (8)0.0018 (8)
C10.0313 (12)0.0401 (14)0.0366 (12)0.0012 (10)0.0028 (10)0.0019 (10)
C20.0361 (13)0.0428 (15)0.0534 (14)0.0080 (11)0.0034 (11)0.0046 (12)
C30.0397 (13)0.0276 (13)0.0603 (16)0.0013 (10)0.0044 (12)0.0052 (11)
C40.0301 (11)0.0258 (11)0.0332 (11)0.0005 (9)0.0073 (9)0.0011 (9)
C50.0317 (11)0.0264 (11)0.0322 (11)0.0022 (9)0.0062 (9)0.0019 (9)
O10.0492 (12)0.0437 (11)0.0521 (11)0.0157 (9)0.0233 (9)0.0153 (9)
Geometric parameters (Å, º) top
Zn1—N12.194 (2)N4—N51.311 (3)
Zn1—N1i2.194 (2)N5—N61.338 (2)
Zn1—N62.115 (2)N6—C51.329 (3)
Zn1—N6i2.115 (2)C1—C21.377 (3)
Zn1—O12.099 (2)C1—H10.9300
Zn1—O1i2.099 (2)C2—H20.9300
N1—C11.336 (3)C3—C41.379 (3)
N1—C41.339 (3)C3—H30.9300
N2—C21.325 (3)C4—C51.465 (3)
N2—C31.326 (3)O1—H1A0.83 (1)
N3—C51.322 (3)O1—H1B0.84 (1)
N3—N41.336 (3)
N6—Zn1—N178.34 (7)C5—N6—Zn1112.6 (1)
N6i—Zn1—N1i78.34 (7)N5—N6—Zn1142.2 (1)
N6—Zn1—N1i101.66 (7)N1—C1—C2121.5 (2)
N6i—Zn1—N1101.66 (7)N1—C1—H1119.3
O1—Zn1—N189.90 (7)C2—C1—H1119.3
O1i—Zn1—N1i89.90 (7)N2—C2—C1122.4 (2)
O1—Zn1—N687.63 (8)N2—C2—H2118.8
O1i—Zn1—N6i87.63 (8)C1—C2—H2118.8
O1—Zn1—N1i90.10 (7)N2—C3—C4122.5 (2)
O1i—Zn1—N190.10 (7)N2—C3—H3118.8
O1—Zn1—N6i92.37 (8)C4—C3—H3118.8
O1i—Zn1—N692.37 (8)N1—C4—C3121.2 (2)
C1—N1—C4116.4 (2)N1—C4—C5115.3 (2)
C1—N1—Zn1130.9 (2)C3—C4—C5123.6 (2)
C4—N1—Zn1112.7 (1)N3—C5—N6111.6 (2)
C2—N2—C3116.1 (2)N3—C5—C4127.4 (2)
C5—N3—N4104.9 (2)N6—C5—C4121.0 (2)
N5—N4—N3109.6 (2)Zn1—O1—H1A119 (2)
N4—N5—N6108.9 (2)Zn1—O1—H1B121 (2)
C5—N6—N5105.0 (2)H1A—O1—H1B111 (2)
Symmetry code: (i) x, y, z+2.
Hydrogen-bond geometry (Å, º) top
D—H···AD—HH···AD···AD—H···A
O1—H1B···N4ii0.84 (1)2.70 (2)3.460 (3)153 (2)
O1—H1B···N3ii0.84 (1)1.92 (1)2.753 (3)173 (2)
O1—H1A···N4iii0.83 (1)2.66 (2)3.331 (3)140 (2)
O1—H1A···N5iii0.83 (1)2.03 (1)2.834 (3)164 (2)
Symmetry codes: (ii) x1/2, y1/2, z+3/2; (iii) x+1, y, z.

Experimental details

(I)(II)
Crystal data
Chemical formula[Mn(C5H3N6)2(H2O)2][Zn(C5H3N6)2(H2O)2]
Mr385.24395.67
Crystal system, space groupMonoclinic, P21/nMonoclinic, P21/n
Temperature (K)293293
a, b, c (Å)5.9642 (19), 11.715 (4), 10.853 (4)6.0906 (18), 11.456 (3), 10.686 (3)
β (°) 104.817 (4) 105.634 (4)
V3)733.1 (4)718.0 (3)
Z22
Radiation typeMo KαMo Kα
µ (mm1)0.941.75
Crystal size (mm)0.40 × 0.30 × 0.250.40 × 0.30 × 0.25
Data collection
DiffractometerBruker SMART CCD area-detector
diffractometer
Bruker SMART CCD area-detector
diffractometer
Absorption correctionMulti-scan
(SADABS; Bruker, 2000)
Multi-scan
(SADABS; Bruker, 2000)
Tmin, Tmax0.705, 0.7990.541, 0.669
No. of measured, independent and
observed [I > 2σ(I)] reflections
3288, 1455, 1235 3206, 1406, 1161
Rint0.0420.034
(sin θ/λ)max1)0.6170.617
Refinement
R[F2 > 2σ(F2)], wR(F2), S 0.045, 0.120, 1.00 0.027, 0.071, 0.99
No. of reflections14551406
No. of parameters123123
No. of restraints33
H-atom treatmentH atoms treated by a mixture of independent and constrained refinementH atoms treated by a mixture of independent and constrained refinement
Δρmax, Δρmin (e Å3)0.62, 0.620.43, 0.37

Computer programs: SMART (Bruker, 2000), SAINT (Bruker, 2000), SAINT, SHELXS97 (Sheldrick, 1997), SHELXL97 (Sheldrick, 1997), SHELXTL (Bruker, 2000), SHELXTL.

Selected geometric parameters (Å, º) for (I) top
Mn1—N12.313 (2)Mn1—O12.138 (2)
Mn1—N62.217 (2)
N6—Mn1—N175.15 (7)O1—Mn1—N688.56 (8)
N6—Mn1—N1i104.85 (7)O1—Mn1—N1i88.77 (7)
O1—Mn1—N191.23 (7)O1—Mn1—N6i91.44 (8)
Symmetry code: (i) x, y, z+2.
Hydrogen-bond geometry (Å, º) for (I) top
D—H···AD—HH···AD···AD—H···A
O1—H1B···N4ii0.84 (1)2.66 (2)3.378 (3)145 (2)
O1—H1B···N3ii0.84 (1)1.91 (1)2.733 (3)168 (3)
O1—H1A···N4iii0.84 (3)2.70 (2)3.408 (3)144 (3)
O1—H1A···N5iii0.84 (3)1.98 (1)2.788 (3)162 (3)
Symmetry codes: (ii) x1/2, y1/2, z+3/2; (iii) x+1, y, z.
Selected geometric parameters (Å, º) for (II) top
Zn1—N12.194 (2)Zn1—O12.099 (2)
Zn1—N62.115 (2)
N6—Zn1—N178.34 (7)O1—Zn1—N687.63 (8)
N6—Zn1—N1i101.66 (7)O1—Zn1—N1i90.10 (7)
O1—Zn1—N189.90 (7)O1—Zn1—N6i92.37 (8)
Symmetry code: (i) x, y, z+2.
Hydrogen-bond geometry (Å, º) for (II) top
D—H···AD—HH···AD···AD—H···A
O1—H1B···N4ii0.84 (1)2.70 (2)3.460 (3)153 (2)
O1—H1B···N3ii0.84 (1)1.92 (1)2.753 (3)173 (2)
O1—H1A···N4iii0.83 (1)2.66 (2)3.331 (3)140 (2)
O1—H1A···N5iii0.83 (1)2.03 (1)2.834 (3)164 (2)
Symmetry codes: (ii) x1/2, y1/2, z+3/2; (iii) x+1, y, z.
 

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