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Acta Cryst. (2007). E63, m2482
https://doi.org/10.1107/S1600536807042614
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Bis(salicylhydrazide-κ2N,O)sulfatozinc(II) monohydrate

W. Luo, X.-G. Meng, X. Li, G.-Z. Cheng and Z.-P. Ji
The title complex, [Zn(SO4)(C7H8N2O2)2]·H2O, contains neutral mol­ecules of a mononuclear ZnII complex, in which the salicylhydrazide ligand is N,O-chelated to the ZnII ion. The ZnII ion is coordinated, in a tetragonal–pyramidal environment, by two O atoms and two N atoms from two salicylhydrazide ligands forming a basal plane, and one O atom from the sulfate anion occupying the apical position. The water mol­ecule is disordered over two positions; the site occupancy factors are ca 0.6 and 0.4.
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Supporting information

cif

Crystallographic Information File (CIF) https://doi.org/10.1107/S1600536807042614/bv2063sup1.cif
Contains datablocks global, I

hkl

Structure factor file (CIF format) https://doi.org/10.1107/S1600536807042614/bv2063Isup2.hkl
Contains datablock I

CCDC reference: 663566

checkCIF report

Key indicators

  • Single-crystal X-ray study
  • T = 293 K
  • Mean [sigma](C-C) = 0.004 Å
  • Disorder in solvent or counterion
  • R factor = 0.048
  • wR factor = 0.101
  • Data-to-parameter ratio = 14.3

checkCIF/PLATON results

No syntax errors found




Alert level C
ABSTM02_ALERT_3_C  The ratio of Tmax/Tmin expected RT(exp) is > 1.10
            Absorption corrections should be applied.
            Tmin and Tmax expected:      0.770     0.888
            RT(exp) =      1.153
PLAT042_ALERT_1_C Calc. and Rep. MoietyFormula Strings Differ ....          ?
PLAT057_ALERT_3_C Correction for Absorption Required   RT(exp) ...       1.16
PLAT302_ALERT_4_C Anion/Solvent Disorder .........................      50.00 Perc.
PLAT313_ALERT_2_C Oxygen with three covalent bonds (rare) ........         O9
PLAT480_ALERT_4_C Long H...A H-Bond Reported H3B    ..  O9      ..       2.63 Ang.
PLAT480_ALERT_4_C Long H...A H-Bond Reported H9C    ..  O2      ..       2.61 Ang.
PLAT790_ALERT_4_C Centre of Gravity not Within Unit Cell: Resd.  #          2
              H4 O2


Alert level G
PLAT199_ALERT_1_G Check the Reported _cell_measurement_temperature        293 K
PLAT860_ALERT_3_G Note: Number of Least-Squares Restraints .......          6


   0 ALERT level A = In general: serious problem
   0 ALERT level B = Potentially serious problem
   8 ALERT level C = Check and explain
   2 ALERT level G = General alerts; check

   2 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
   3 ALERT type 3 Indicator that the structure quality may be low
   4 ALERT type 4 Improvement, methodology, query or suggestion
   0 ALERT type 5 Informative message, check
Comment top

The molecular self-assembly of supramolecular architectures has received much attention during recent decades (Tao et al., 2000). The structures and properties of such systems depend on the coordination and geometric preferences of both the central metal ions and the bridging building blocks, as well as on the influence of weaker non-covalent interactions, such as hydrogen bonds and π-π stacking interactions. In this paper, we report the synthesis and crystal structure of the title compound, (I), [ZnSO4(C7H8N2O2)2].H2O, (Fig.1) a novel ZnII complex formed by the ligand salicylhydrazide. The ZnII ion is situated in a tetragonal-pyramidal enviroment consisting of two O atoms and two N atoms from two ligands in the basal plane,and an O atom from the sulfate anion in the apical position. Intermolecular O—H···O hydrogen bonds (Table 1) result in a two-dimensional network.

Related literature top

For related literature, see: Tao et al. (2000).

Experimental top

Salicylhydrazide (15.2 mg, 0.1 mmol) was dissolved in a mixed solvent (20 ml) of DMF and methanol (1:1), then ZnSO4.7H2O (28.7 mg, 0.1 mmol) was added, stired for 10 min and filtered. Colourless single crystals suitable for X-ray diffraction analysis were obtained by slow diffusion of the filtrate for one week,.

Refinement top

Except the water H atoms, all the H atoms were located at the ideal positions with C–H = 0.93 Å (aromatic), N–H = 0.86 Å (imine) and 0.90 Å (amine), O–H = 0.82 Å(phenol); and Uiso(H) = 1.2Ueq(C) for aromatic H atoms, Uiso(H) = 1.2Ueq(N) for H atoms bonded to N atoms and Uiso(H) = 1.2Ueq(O) for hydroxyl H atoms. The water H atoms were located from the difference maps and refined with the constraints of O–H = 0.82 (1) Å, H–H = 1.35 (1) Å, and the Uiso values of these two H atoms were set 1.5 times of Ueq value of water O9 atom. The water O atom was disordered over two positions with occupancies of 0.589 (3):0.411 (3).

Structure description top

The molecular self-assembly of supramolecular architectures has received much attention during recent decades (Tao et al., 2000). The structures and properties of such systems depend on the coordination and geometric preferences of both the central metal ions and the bridging building blocks, as well as on the influence of weaker non-covalent interactions, such as hydrogen bonds and π-π stacking interactions. In this paper, we report the synthesis and crystal structure of the title compound, (I), [ZnSO4(C7H8N2O2)2].H2O, (Fig.1) a novel ZnII complex formed by the ligand salicylhydrazide. The ZnII ion is situated in a tetragonal-pyramidal enviroment consisting of two O atoms and two N atoms from two ligands in the basal plane,and an O atom from the sulfate anion in the apical position. Intermolecular O—H···O hydrogen bonds (Table 1) result in a two-dimensional network.

For related literature, see: Tao et al. (2000).

Computing details top

Data collection: SMART (Bruker, 2001); cell refinement: SAINT-Plus (Bruker, 2001); data reduction: SAINT-Plus (Bruker, 2001); program(s) used to solve structure: SHELXS97 (Sheldrick, 1997); program(s) used to refine structure: SHELXL97 (Sheldrick, 1997); molecular graphics: PLATON (Spek, 2003); software used to prepare material for publication: PLATON (Spek, 2003).

Figures top
[Figure 1] Fig. 1. Molecular structure of (I), showing the atom-numbering scheme.
[Figure 2] Fig. 2. Part of the crystal structure of (I), showing the formation of the two-dimensional network.
Bis(salicylhydrazide-κ2N,O)sulfatozinc(II) monohydrate top
Crystal data top
[Zn(SO4)(C7H8N2O2)2]·H2OZ = 2
Mr = 483.75F(000) = 496
Triclinic, P1Dx = 1.723 Mg m−3
Hall symbol: -P 1Mo Kα radiation, λ = 0.71073 Å
a = 7.2028 (6) ÅCell parameters from 2048 reflections
b = 8.8006 (7) Åθ = 2.5–25.1°
c = 15.6983 (13) ŵ = 1.49 mm−1
α = 101.930 (1)°T = 293 K
β = 95.491 (2)°Plate, colourless
γ = 104.210 (1)°0.20 × 0.15 × 0.08 mm
V = 932.50 (13) Å3
Data collection top
Bruker SMART APEX CCD area-detector
diffractometer		2757 reflections with I > 2σ(I)
Radiation source: fine-focus sealed tubeRint = 0.078
Graphite monochromatorθmax = 27.0°, θmin = 2.5°
0.3° wide ω exposures scansh = −9→9
8372 measured reflectionsk = −11→11
3978 independent reflectionsl = −18→19
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)] = 0.048Hydrogen site location: inferred from neighbouring sites
wR(F2) = 0.101H atoms treated by a mixture of independent and constrained refinement
S = 0.92 w = 1/[σ2(Fo2) + (0.0377P)2]
where P = (Fo2 + 2Fc2)/3
3978 reflections(Δ/σ)max = 0.012
278 parametersΔρmax = 0.58 e Å−3
6 restraintsΔρmin = −0.51 e Å−3
Crystal data top
[Zn(SO4)(C7H8N2O2)2]·H2Oγ = 104.210 (1)°
Mr = 483.75V = 932.50 (13) Å3
Triclinic, P1Z = 2
a = 7.2028 (6) ÅMo Kα radiation
b = 8.8006 (7) ŵ = 1.49 mm−1
c = 15.6983 (13) ÅT = 293 K
α = 101.930 (1)°0.20 × 0.15 × 0.08 mm
β = 95.491 (2)°
Data collection top
Bruker SMART APEX CCD area-detector
diffractometer		2757 reflections with I > 2σ(I)
8372 measured reflectionsRint = 0.078
3978 independent reflections
Refinement top
R[F2 > 2σ(F2)] = 0.0486 restraints
wR(F2) = 0.101H atoms treated by a mixture of independent and constrained refinement
S = 0.92Δρmax = 0.58 e Å−3
3978 reflectionsΔρmin = −0.51 e Å−3
278 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*/UeqOcc. (<1)
Zn10.13536 (4)0.88473 (3)0.314727 (19)0.03306 (9)
C10.3139 (4)1.2506 (3)0.18144 (15)0.0286 (6)
C20.4106 (4)1.4158 (3)0.20697 (16)0.0298 (6)
C30.4111 (4)1.5095 (3)0.14579 (17)0.0436 (8)
H3A0.47341.61940.16270.052*
C40.3203 (4)1.4411 (3)0.06052 (18)0.0466 (8)
H4A0.32251.50500.02010.056*
C50.2259 (4)1.2786 (3)0.03429 (18)0.0452 (8)
H5A0.16411.2327−0.02340.054*
C60.2246 (4)1.1852 (3)0.09485 (16)0.0374 (7)
H6A0.16211.07540.07710.045*
C70.2938 (4)1.1418 (3)0.24223 (15)0.0284 (6)
C8−0.1049 (4)0.3849 (3)0.21322 (16)0.0293 (6)
C9−0.1469 (4)0.2470 (3)0.24732 (16)0.0316 (7)
C10−0.2507 (4)0.1002 (3)0.19232 (18)0.0404 (8)
H10A−0.28210.00950.21540.049*
C11−0.3077 (4)0.0858 (3)0.10502 (19)0.0434 (8)
H11A−0.3756−0.01420.06890.052*
C12−0.2645 (4)0.2206 (3)0.06998 (18)0.0452 (8)
H12A−0.30250.21170.01040.054*
C13−0.1651 (4)0.3667 (3)0.12426 (17)0.0386 (7)
H13A−0.13700.45690.10070.046*
C140.0002 (4)0.5478 (2)0.26454 (15)0.0281 (6)
N10.3799 (3)1.1983 (2)0.32565 (12)0.0316 (6)
H1A0.45401.29520.34370.038*
N20.3466 (3)1.0954 (2)0.38360 (12)0.0299 (5)
H2A0.30471.14330.43160.036*
H2B0.45671.07190.40110.036*
N30.0868 (3)0.5710 (2)0.34653 (13)0.0361 (6)
H3B0.08200.49140.37090.043*
N40.1867 (3)0.7301 (2)0.39233 (14)0.0371 (6)
H4B0.31460.73970.40300.044*
H4C0.14460.75490.44420.044*
O10.1941 (3)0.99810 (18)0.21592 (10)0.0369 (5)
O20.5027 (3)1.48017 (18)0.29031 (11)0.0441 (6)
H2C0.52561.57870.30090.066*
O30.0069 (3)0.66568 (18)0.23094 (11)0.0434 (5)
O4−0.0854 (3)0.26218 (19)0.33444 (11)0.0471 (6)
H4D−0.08490.17330.34280.071*
O5−0.0905 (3)0.95954 (19)0.35224 (11)0.0407 (5)
O6−0.4187 (3)0.7940 (2)0.33021 (12)0.0438 (5)
O7−0.1873 (3)0.78945 (19)0.45077 (11)0.0414 (5)
O8−0.3047 (2)1.02338 (19)0.45151 (11)0.0403 (5)
S1−0.25252 (9)0.88909 (6)0.39720 (4)0.02728 (16)
O9'−0.2612 (6)0.4713 (4)0.4754 (2)0.0685 (12)0.589 (3)
H9A−0.235 (3)0.5609 (9)0.4650 (14)0.103*0.589 (3)
H9B−0.2009 (19)0.4211 (16)0.4438 (14)0.103*0.589 (3)
O9−0.3556 (8)0.4900 (6)0.5003 (3)0.0685 (12)0.411 (3)
H9C−0.359 (3)0.5274 (19)0.4567 (8)0.103*0.411 (3)
H9D−0.4656 (14)0.478 (4)0.5129 (13)0.103*0.411 (3)
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
Zn10.03925 (18)0.01937 (13)0.04079 (17)0.00402 (12)0.00967 (14)0.01088 (12)
C10.0320 (14)0.0254 (11)0.0308 (13)0.0077 (10)0.0100 (11)0.0096 (10)
C20.0326 (14)0.0254 (11)0.0325 (13)0.0060 (10)0.0080 (11)0.0101 (10)
C30.0506 (18)0.0314 (12)0.0536 (16)0.0083 (12)0.0144 (14)0.0211 (12)
C40.0535 (18)0.0486 (14)0.0452 (15)0.0132 (13)0.0067 (14)0.0290 (12)
C50.0493 (17)0.0499 (15)0.0371 (15)0.0132 (14)0.0041 (14)0.0131 (13)
C60.0407 (16)0.0332 (12)0.0384 (14)0.0078 (12)0.0085 (13)0.0102 (11)
C70.0285 (13)0.0235 (11)0.0334 (13)0.0058 (10)0.0089 (11)0.0072 (10)
C80.0269 (13)0.0216 (11)0.0383 (14)0.0058 (10)0.0042 (11)0.0058 (10)
C90.0333 (14)0.0225 (11)0.0375 (14)0.0072 (11)0.0006 (12)0.0064 (10)
C100.0390 (16)0.0250 (12)0.0528 (16)0.0033 (12)0.0002 (14)0.0091 (12)
C110.0413 (16)0.0254 (13)0.0523 (17)0.0062 (12)−0.0048 (14)−0.0063 (13)
C120.0490 (18)0.0399 (14)0.0398 (16)0.0083 (14)−0.0060 (14)0.0045 (13)
C130.0451 (17)0.0301 (12)0.0384 (15)0.0070 (12)0.0000 (13)0.0103 (11)
C140.0314 (13)0.0191 (10)0.0344 (13)0.0061 (10)0.0075 (11)0.0076 (10)
N10.0387 (12)0.0190 (9)0.0330 (11)−0.0013 (9)0.0033 (10)0.0094 (8)
N20.0347 (11)0.0276 (9)0.0311 (10)0.0079 (9)0.0082 (9)0.0144 (8)
N30.0470 (13)0.0181 (9)0.0401 (12)0.0059 (9)−0.0039 (11)0.0083 (9)
N40.0423 (13)0.0186 (9)0.0418 (12)0.0058 (9)−0.0080 (11)−0.0020 (9)
O10.0485 (11)0.0223 (8)0.0329 (9)−0.0027 (8)0.0042 (9)0.0069 (7)
O20.0637 (13)0.0206 (8)0.0398 (10)−0.0020 (9)0.0017 (10)0.0083 (8)
O30.0654 (13)0.0218 (8)0.0363 (10)0.0002 (9)−0.0027 (9)0.0108 (7)
O40.0676 (13)0.0212 (8)0.0474 (11)0.0032 (9)−0.0051 (10)0.0141 (8)
O50.0403 (10)0.0380 (8)0.0565 (10)0.0153 (8)0.0240 (9)0.0259 (8)
O60.0394 (11)0.0298 (9)0.0507 (11)0.0004 (8)−0.0059 (9)0.0009 (9)
O70.0475 (11)0.0395 (8)0.0477 (10)0.0167 (8)0.0143 (9)0.0244 (8)
O80.0418 (10)0.0385 (9)0.0399 (10)0.0200 (8)0.0024 (9)−0.0013 (8)
S10.0293 (3)0.0204 (3)0.0324 (3)0.0048 (2)0.0054 (3)0.0090 (2)
O9'0.089 (3)0.0608 (14)0.0756 (19)0.0311 (19)0.029 (2)0.0403 (14)
O90.089 (3)0.0608 (14)0.0756 (19)0.0311 (19)0.029 (2)0.0403 (14)
Geometric parameters (Å, º) top
Zn1—O51.9937 (19)C11—H11A0.9300
Zn1—O12.0343 (16)C12—C131.367 (3)
Zn1—O32.0361 (15)C12—H12A0.9300
Zn1—N42.079 (2)C13—H13A0.9300
Zn1—N22.0962 (17)C14—O31.250 (3)
C1—C61.386 (3)C14—N31.328 (3)
C1—C21.403 (3)N1—N21.407 (2)
C1—C71.478 (3)N1—H1A0.8600
C2—O21.348 (3)N2—H2A0.9000
C2—C31.389 (3)N2—H2B0.9000
C3—C41.374 (3)N3—N41.409 (2)
C3—H3A0.9300N3—H3B0.8600
C4—C51.380 (3)N4—H4B0.9000
C4—H4A0.9300N4—H4C0.9000
C5—C61.379 (4)O2—H2C0.8200
C5—H5A0.9300O4—H4D0.8200
C6—H6A0.9300O5—S11.4928 (18)
C7—O11.252 (2)O6—S11.4634 (17)
C7—N11.331 (3)O7—S11.4588 (17)
C8—C131.386 (3)O8—S11.4585 (17)
C8—C91.404 (3)O9'—H9A0.819 (9)
C8—C141.466 (3)O9'—H9B0.821 (9)
C9—O41.365 (3)O9'—H9C1.011 (18)
C9—C101.384 (3)O9—H9A1.191 (19)
C10—C111.363 (4)O9—H9C0.819 (9)
C10—H10A0.9300O9—H9D0.822 (9)
C11—C121.388 (4)
O5—Zn1—O1101.24 (7)C13—C12—H12A120.5
O5—Zn1—O3102.77 (8)C11—C12—H12A120.5
O1—Zn1—O393.86 (6)C12—C13—C8122.3 (2)
O5—Zn1—N4107.05 (8)C12—C13—H13A118.9
O1—Zn1—N4151.69 (9)C8—C13—H13A118.9
O3—Zn1—N478.90 (7)O3—C14—N3119.87 (19)
O5—Zn1—N295.68 (7)O3—C14—C8119.7 (2)
O1—Zn1—N279.12 (7)N3—C14—C8120.5 (2)
O3—Zn1—N2161.25 (8)C7—N1—N2118.25 (17)
N4—Zn1—N299.01 (7)C7—N1—H1A120.9
C6—C1—C2118.6 (2)N2—N1—H1A120.9
C6—C1—C7117.3 (2)N1—N2—Zn1107.10 (12)
C2—C1—C7124.0 (2)N1—N2—H2A110.3
O2—C2—C3121.3 (2)Zn1—N2—H2A110.3
O2—C2—C1119.2 (2)N1—N2—H2B110.3
C3—C2—C1119.5 (2)Zn1—N2—H2B110.3
C4—C3—C2120.5 (2)H2A—N2—H2B108.6
C4—C3—H3A119.7C14—N3—N4117.91 (18)
C2—C3—H3A119.7C14—N3—H3B121.0
C3—C4—C5120.7 (2)N4—N3—H3B121.0
C3—C4—H4A119.7N3—N4—Zn1108.09 (14)
C5—C4—H4A119.7N3—N4—H4B110.1
C6—C5—C4119.0 (2)Zn1—N4—H4B110.1
C6—C5—H5A120.5N3—N4—H4C110.1
C4—C5—H5A120.5Zn1—N4—H4C110.1
C5—C6—C1121.7 (2)H4B—N4—H4C108.4
C5—C6—H6A119.1C7—O1—Zn1113.80 (15)
C1—C6—H6A119.1C2—O2—H2C109.5
O1—C7—N1120.1 (2)C14—O3—Zn1114.63 (14)
O1—C7—C1120.3 (2)C9—O4—H4D109.5
N1—C7—C1119.53 (19)S1—O5—Zn1132.28 (10)
C13—C8—C9118.0 (2)O8—S1—O7111.27 (10)
C13—C8—C14117.1 (2)O8—S1—O6109.20 (11)
C9—C8—C14124.9 (2)O7—S1—O6111.30 (10)
O4—C9—C10121.8 (2)O8—S1—O5107.26 (10)
O4—C9—C8118.82 (19)O7—S1—O5108.94 (11)
C10—C9—C8119.4 (2)O6—S1—O5108.75 (11)
C11—C10—C9121.3 (2)H9A—O9'—H9B104.5 (15)
C11—C10—H10A119.4H9A—O9'—H9C54.7 (17)
C9—C10—H10A119.4H9B—O9'—H9C127.7 (18)
C10—C11—C12120.0 (2)H9A—O9—H9C46.1 (16)
C10—C11—H11A120.0H9A—O9—H9D146 (2)
C12—C11—H11A120.0H9C—O9—H9D104.3 (15)
C13—C12—C11119.0 (2)
C6—C1—C2—O2−178.1 (2)C7—N1—N2—Zn1−6.3 (3)
C7—C1—C2—O24.5 (4)O5—Zn1—N2—N1−91.44 (15)
C6—C1—C2—C31.3 (4)O1—Zn1—N2—N18.95 (14)
C7—C1—C2—C3−176.1 (2)O3—Zn1—N2—N178.3 (3)
O2—C2—C3—C4178.4 (3)N4—Zn1—N2—N1160.26 (15)
C1—C2—C3—C4−1.0 (4)O3—C14—N3—N4−1.0 (4)
C2—C3—C4—C50.5 (5)C8—C14—N3—N4179.5 (2)
C3—C4—C5—C6−0.3 (5)C14—N3—N4—Zn16.2 (3)
C4—C5—C6—C10.6 (4)O5—Zn1—N4—N393.69 (16)
C2—C1—C6—C5−1.1 (4)O1—Zn1—N4—N3−83.7 (2)
C7—C1—C6—C5176.4 (3)O3—Zn1—N4—N3−6.42 (15)
C6—C1—C7—O1−2.4 (4)N2—Zn1—N4—N3−167.49 (16)
C2—C1—C7—O1175.1 (2)N1—C7—O1—Zn111.9 (3)
C6—C1—C7—N1178.8 (2)C1—C7—O1—Zn1−166.91 (18)
C2—C1—C7—N1−3.8 (4)O5—Zn1—O1—C782.16 (18)
C13—C8—C9—O4178.8 (2)O3—Zn1—O1—C7−173.99 (18)
C14—C8—C9—O4−0.6 (4)N4—Zn1—O1—C7−100.4 (2)
C13—C8—C9—C10−1.9 (4)N2—Zn1—O1—C7−11.53 (18)
C14—C8—C9—C10178.7 (3)N3—C14—O3—Zn1−5.2 (3)
O4—C9—C10—C11−178.6 (3)C8—C14—O3—Zn1174.31 (18)
C8—C9—C10—C112.1 (4)O5—Zn1—O3—C14−98.63 (19)
C9—C10—C11—C12−1.0 (4)O1—Zn1—O3—C14158.93 (19)
C10—C11—C12—C13−0.2 (4)N4—Zn1—O3—C146.55 (19)
C11—C12—C13—C80.4 (4)N2—Zn1—O3—C1491.9 (3)
C9—C8—C13—C120.7 (4)O1—Zn1—O5—S1155.47 (13)
C14—C8—C13—C12−179.9 (3)O3—Zn1—O5—S158.85 (15)
C13—C8—C14—O310.4 (4)N4—Zn1—O5—S1−23.28 (16)
C9—C8—C14—O3−170.2 (2)N2—Zn1—O5—S1−124.53 (14)
C13—C8—C14—N3−170.1 (2)Zn1—O5—S1—O8147.72 (13)
C9—C8—C14—N39.3 (4)Zn1—O5—S1—O727.17 (17)
O1—C7—N1—N2−3.5 (4)Zn1—O5—S1—O6−94.30 (15)
C1—C7—N1—N2175.4 (2)
Hydrogen-bond geometry (Å, º) top
D—H···AD—HH···AD···AD—H···A
N1—H1A···O20.861.952.613 (2)133
N2—H2A···O7i0.902.143.026 (3)169
N2—H2B···O8ii0.902.002.898 (3)175
N3—H3B···O40.862.012.655 (2)131
N3—H3B···O9′iii0.862.543.085 (4)122
N3—H3B···O9iii0.862.633.158 (6)120
N4—H4B···O6ii0.902.333.053 (3)137
N4—H4C···O8i0.902.242.817 (2)121
N4—H4C···O70.902.493.056 (3)121
O2—H2C···O6iv0.821.792.606 (2)177
O4—H4D···O5v0.821.912.727 (2)175
O9′—H9A···O70.82 (1)2.02 (1)2.833 (4)173 (2)
O9′—H9B···O40.82 (1)2.33 (1)3.144 (4)169 (2)
O9—H9C···O70.82 (1)2.36 (1)2.912 (5)125 (1)
O9—H9C···O2vi0.82 (1)2.61 (1)3.333 (6)147 (1)
O9—H9D···O9vii0.82 (1)1.39 (2)2.130 (11)147 (3)
Symmetry codes: (i) −x, −y+2, −z+1; (ii) x+1, y, z; (iii) −x, −y+1, −z+1; (iv) x+1, y+1, z; (v) x, y−1, z; (vi) x−1, y−1, z; (vii) −x−1, −y+1, −z+1.

Experimental details

Crystal data
Chemical formula[Zn(SO4)(C7H8N2O2)2]·H2O
Mr483.75
Crystal system, space groupTriclinic, P1
Temperature (K)293
a, b, c (Å)7.2028 (6), 8.8006 (7), 15.6983 (13)
α, β, γ (°)101.930 (1), 95.491 (2), 104.210 (1)
V (Å3)932.50 (13)
Z2
Radiation typeMo Kα
µ (mm−1)1.49
Crystal size (mm)0.20 × 0.15 × 0.08
Data collection
DiffractometerBruker SMART APEX CCD area-detector
Absorption correction–
No. of measured, independent and
observed [I > 2σ(I)] reflections		8372, 3978, 2757
Rint0.078
(sin θ/λ)max (Å−1)0.639
Refinement
R[F2 > 2σ(F2)], wR(F2), S 0.048, 0.101, 0.92
No. of reflections3978
No. of parameters278
No. of restraints6
H-atom treatmentH atoms treated by a mixture of independent and constrained refinement
Δρmax, Δρmin (e Å−3)0.58, −0.51

Computer programs: SMART (Bruker, 2001), SAINT-Plus (Bruker, 2001), SHELXS97 (Sheldrick, 1997), SHELXL97 (Sheldrick, 1997), PLATON (Spek, 2003).

Hydrogen-bond geometry (Å, º) top
D—H···AD—HH···AD···AD—H···A
N1—H1A···O20.861.952.613 (2)132.6
N2—H2A···O7i0.902.143.026 (3)168.9
N2—H2B···O8ii0.902.002.898 (3)174.6
N3—H3B···O40.862.012.655 (2)130.8
N3—H3B···O9'iii0.862.543.085 (4)122.0
N3—H3B···O9iii0.862.633.158 (6)120.4
N4—H4B···O6ii0.902.333.053 (3)137.4
N4—H4C···O8i0.902.242.817 (2)121.3
N4—H4C···O70.902.493.056 (3)121.2
O2—H2C···O6iv0.821.792.606 (2)176.7
O4—H4D···O5v0.821.912.727 (2)175.4
O9'—H9A···O70.819 (9)2.018 (8)2.833 (4)173 (2)
O9'—H9B···O40.821 (9)2.334 (11)3.144 (4)168.8 (18)
O9—H9C···O70.819 (9)2.360 (14)2.912 (5)125.3 (13)
O9—H9C···O2vi0.819 (9)2.614 (11)3.333 (6)147.3 (14)
O9—H9D···O9vii0.822 (9)1.39 (2)2.130 (11)147 (3)
Symmetry codes: (i) −x, −y+2, −z+1; (ii) x+1, y, z; (iii) −x, −y+1, −z+1; (iv) x+1, y+1, z; (v) x, y−1, z; (vi) x−1, y−1, z; (vii) −x−1, −y+1, −z+1.
 

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