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In the title monomeric compound, [Zn(C5H2N2O4)(H2O)4], the ZnII atom has a distorted octa­hedral environment and the molecules are linked by O—H...O and N—H...O hydrogen bonds, forming a three-dimensional supra­molecular structure.

Supporting information

cif

Crystallographic Information File (CIF) https://doi.org/10.1107/S1600536806036087/ga2003sup1.cif
Contains datablocks global, I

hkl

Structure factor file (CIF format) https://doi.org/10.1107/S1600536806036087/ga2003Isup2.hkl
Contains datablock I

CCDC reference: 604080

Key indicators

  • Single-crystal X-ray study
  • T = 293 K
  • Mean [sigma](C-C) = 0.003 Å
  • R factor = 0.026
  • wR factor = 0.072
  • Data-to-parameter ratio = 13.9

checkCIF/PLATON results

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Alert level C PLAT250_ALERT_2_C Large U3/U1 Ratio for Average U(i,j) Tensor .... 2.06
Alert level G PLAT199_ALERT_1_G Check the Reported _cell_measurement_temperature 293 K PLAT200_ALERT_1_G Check the Reported _diffrn_ambient_temperature . 293 K
0 ALERT level A = In general: serious problem 0 ALERT level B = Potentially serious problem 1 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 0 ALERT type 3 Indicator that the structure quality may be low 0 ALERT type 4 Improvement, methodology, query or suggestion 0 ALERT type 5 Informative message, check

Computing details top

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

Tetraaqua(pyrazole-3,5-dicarboxylato)zinc(II) top
Crystal data top
[Zn(C5H2N2O4)(H2O)4]Z = 2
Mr = 291.52F(000) = 296
Triclinic, P1Dx = 1.947 Mg m3
Hall symbol: -P 1Mo Kα radiation, λ = 0.71073 Å
a = 6.148 (2) ÅCell parameters from 998 reflections
b = 7.726 (3) Åθ = 2.7–26.4°
c = 10.852 (4) ŵ = 2.50 mm1
α = 87.169 (4)°T = 293 K
β = 80.707 (5)°Block, colourless
γ = 77.899 (5)°0.20 × 0.10 × 0.08 mm
V = 497.3 (3) Å3
Data collection top
Bruker SMART 1000 CCD area-detector
diffractometer
1832 reflections with I > 2σ(I)
Radiation source: fine-focus sealed tubeRint = 0.019
Graphite monochromatorθmax = 26.4°, θmin = 2.7°
φ and ω scansh = 73
2887 measured reflectionsk = 99
2010 independent reflectionsl = 1313
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)] = 0.026Hydrogen site location: inferred from neighbouring sites
wR(F2) = 0.072H-atom parameters constrained
S = 0.96 w = 1/[σ2(Fo2) + (0.0412P)2 + 0.3209P]
where P = (Fo2 + 2Fc2)/3
2010 reflections(Δ/σ)max < 0.001
145 parametersΔρmax = 0.27 e Å3
0 restraintsΔρmin = 0.48 e Å3
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
Zn10.27903 (4)0.23826 (3)0.36054 (2)0.01836 (11)
N10.3620 (3)0.2782 (3)0.16210 (17)0.0209 (4)
N20.2629 (3)0.3391 (3)0.06362 (17)0.0215 (4)
H20.12690.39840.06850.026*
O10.6328 (3)0.1378 (2)0.32265 (14)0.0219 (4)
O20.9125 (3)0.0374 (3)0.17012 (17)0.0385 (5)
O30.1461 (3)0.4624 (3)0.16510 (16)0.0336 (5)
O40.4547 (3)0.2919 (2)0.26440 (14)0.0221 (4)
C10.7195 (4)0.1140 (3)0.2067 (2)0.0207 (5)
C50.5692 (4)0.1939 (3)0.1155 (2)0.0187 (4)
C40.6031 (4)0.2016 (3)0.0147 (2)0.0206 (5)
H40.73270.15350.06890.025*
C30.4029 (4)0.2959 (3)0.0451 (2)0.0189 (5)
C20.3274 (4)0.3545 (3)0.1670 (2)0.0183 (4)
O5W0.2042 (3)0.0079 (2)0.33609 (16)0.0252 (4)
H5A0.10400.00720.28880.038*
H5B0.30980.09590.31400.038*
O6W0.0754 (3)0.3467 (2)0.37557 (15)0.0212 (3)
H6A0.07650.41310.31070.032*
H6B0.15010.26700.37060.032*
O7W0.2555 (3)0.1832 (2)0.54798 (15)0.0314 (4)
H7A0.31710.23520.59570.047*
H7B0.26390.07610.57250.047*
O8W0.3034 (4)0.4884 (3)0.40308 (19)0.0413 (5)
H8A0.22790.55510.46170.062*
H8B0.37160.54670.34670.062*
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
Zn10.01881 (16)0.02150 (16)0.01318 (15)0.00056 (10)0.00211 (10)0.00125 (10)
N10.0193 (10)0.0278 (11)0.0120 (9)0.0033 (8)0.0021 (7)0.0000 (8)
N20.0173 (9)0.0283 (11)0.0141 (9)0.0060 (8)0.0027 (7)0.0006 (8)
O10.0206 (8)0.0301 (9)0.0138 (8)0.0001 (7)0.0053 (6)0.0007 (6)
O20.0201 (9)0.0642 (14)0.0230 (9)0.0142 (9)0.0067 (7)0.0078 (9)
O30.0285 (10)0.0452 (11)0.0164 (8)0.0162 (8)0.0032 (7)0.0014 (8)
O40.0231 (8)0.0262 (9)0.0128 (7)0.0032 (7)0.0010 (6)0.0015 (6)
C10.0181 (11)0.0248 (12)0.0189 (11)0.0001 (9)0.0063 (9)0.0027 (9)
C50.0168 (11)0.0231 (11)0.0150 (10)0.0007 (9)0.0026 (8)0.0025 (8)
C40.0170 (11)0.0277 (12)0.0143 (10)0.0016 (9)0.0013 (8)0.0033 (9)
C30.0202 (11)0.0213 (11)0.0135 (10)0.0010 (9)0.0013 (8)0.0021 (8)
C20.0179 (11)0.0202 (11)0.0145 (10)0.0013 (9)0.0027 (8)0.0008 (8)
O5W0.0220 (8)0.0229 (9)0.0299 (9)0.0015 (7)0.0087 (7)0.0045 (7)
O6W0.0206 (8)0.0240 (9)0.0176 (8)0.0003 (7)0.0043 (6)0.0008 (6)
O7W0.0519 (12)0.0298 (10)0.0162 (8)0.0127 (9)0.0123 (8)0.0032 (7)
O8W0.0578 (13)0.0313 (10)0.0323 (11)0.0217 (9)0.0212 (9)0.0138 (8)
Geometric parameters (Å, º) top
Zn1—O7W2.0456 (18)C1—C51.487 (3)
Zn1—O8W2.050 (2)C5—C41.394 (3)
Zn1—O5W2.0871 (18)C4—C31.374 (3)
Zn1—O12.1300 (17)C4—H40.9300
Zn1—O6W2.1474 (17)C3—C21.490 (3)
Zn1—N12.1537 (19)O5W—H5A0.8499
N1—N21.332 (3)O5W—H5B0.8495
N1—C51.334 (3)O6W—H6A0.8504
N2—C31.354 (3)O6W—H6B0.8500
N2—H20.8600O7W—H7A0.8494
O1—C11.290 (3)O7W—H7B0.8504
O2—C11.222 (3)O8W—H8A0.8501
O3—C21.242 (3)O8W—H8B0.8499
O4—C21.261 (3)
O7W—Zn1—O8W86.63 (8)N1—C5—C4111.0 (2)
O7W—Zn1—O5W88.60 (7)N1—C5—C1116.95 (19)
O8W—Zn1—O5W170.75 (7)C4—C5—C1132.1 (2)
O7W—Zn1—O194.43 (7)C3—C4—C5104.73 (19)
O8W—Zn1—O195.41 (8)C3—C4—H4127.6
O5W—Zn1—O192.86 (7)C5—C4—H4127.6
O7W—Zn1—O6W92.34 (7)N2—C3—C4107.0 (2)
O8W—Zn1—O6W84.95 (8)N2—C3—C2120.5 (2)
O5W—Zn1—O6W87.33 (7)C4—C3—C2132.5 (2)
O1—Zn1—O6W173.23 (6)O3—C2—O4125.0 (2)
O7W—Zn1—N1170.57 (8)O3—C2—C3117.8 (2)
O8W—Zn1—N194.12 (8)O4—C2—C3117.16 (19)
O5W—Zn1—N191.88 (7)Zn1—O5W—H5A107.8
O1—Zn1—N176.14 (7)Zn1—O5W—H5B119.9
O6W—Zn1—N197.09 (7)H5A—O5W—H5B111.7
N2—N1—C5105.68 (18)Zn1—O6W—H6A100.0
N2—N1—Zn1140.20 (15)Zn1—O6W—H6B111.7
C5—N1—Zn1113.11 (15)H6A—O6W—H6B110.3
N1—N2—C3111.63 (18)Zn1—O7W—H7A122.1
N1—N2—H2124.2Zn1—O7W—H7B118.4
C3—N2—H2124.2H7A—O7W—H7B108.8
C1—O1—Zn1116.42 (14)Zn1—O8W—H8A129.2
O2—C1—O1124.6 (2)Zn1—O8W—H8B117.4
O2—C1—C5120.2 (2)H8A—O8W—H8B111.3
O1—C1—C5115.21 (19)
O8W—Zn1—N1—N287.4 (3)Zn1—N1—C5—C4171.08 (16)
O5W—Zn1—N1—N285.6 (3)N2—N1—C5—C1179.2 (2)
O1—Zn1—N1—N2178.1 (3)Zn1—N1—C5—C19.9 (3)
O6W—Zn1—N1—N22.0 (3)O2—C1—C5—N1178.9 (2)
O8W—Zn1—N1—C5106.41 (18)O1—C1—C5—N11.0 (3)
O5W—Zn1—N1—C580.64 (17)O2—C1—C5—C40.1 (4)
O1—Zn1—N1—C511.85 (16)O1—C1—C5—C4177.7 (2)
O6W—Zn1—N1—C5168.18 (17)N1—C5—C4—C30.1 (3)
C5—N1—N2—C30.2 (3)C1—C5—C4—C3178.9 (2)
Zn1—N1—N2—C3167.05 (19)N1—N2—C3—C40.1 (3)
O7W—Zn1—O1—C1167.00 (17)N1—N2—C3—C2178.7 (2)
O8W—Zn1—O1—C1105.97 (17)C5—C4—C3—N20.0 (3)
O5W—Zn1—O1—C178.18 (17)C5—C4—C3—C2178.6 (2)
N1—Zn1—O1—C113.05 (17)N2—C3—C2—O39.4 (3)
Zn1—O1—C1—O2170.4 (2)C4—C3—C2—O3169.0 (3)
Zn1—O1—C1—C511.9 (3)N2—C3—C2—O4171.5 (2)
N2—N1—C5—C40.2 (3)C4—C3—C2—O410.1 (4)
Hydrogen-bond geometry (Å, º) top
D—H···AD—HH···AD···AD—H···A
N2—H2···O3i0.861.962.747 (3)151
O5W—H5A···O2ii0.851.862.702 (3)173
O5W—H5B···O4iii0.851.892.744 (2)180
O6W—H6A···O3i0.851.872.702 (2)165
O6W—H6B···O1ii0.851.972.792 (3)162
O7W—H7A···O4iv0.851.962.785 (3)163
O7W—H7B···O1v0.852.012.801 (3)155
O8W—H8A···O6Wvi0.851.972.797 (3)165
O8W—H8B···O4vii0.851.912.728 (3)162
C4—H4···O2viii0.932.493.392 (3)165
Symmetry codes: (i) x, y+1, z; (ii) x1, y, z; (iii) x+1, y, z; (iv) x, y, z+1; (v) x+1, y, z+1; (vi) x, y+1, z+1; (vii) x+1, y+1, z; (viii) x+2, y, z.
 

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