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The title compound, [Ni2(C3H2O4)2(C4H4N2)(H2O)2]n, has been prepared from the hydro­thermal reaction of nickel(II) chloride, malonic acid and pyrazine. The NiII atoms are linked via coordinated malonates, forming a two-dimensional network with cavities of 6.14 × 5.60 Å. These sheet structures are further connected into a three-dimensional network by bridging pyrazine ligands which have inversion symmetry, the mean distance between the layers being 7.39 Å. The coordination geometry around the NiII atom is a tetra­gonally elongated octa­hedron, with pyrazine N and aqua O atoms at the apical positions.

Supporting information

cif

Crystallographic Information File (CIF) https://doi.org/10.1107/S1600536805026358/ob6558sup1.cif
Contains datablocks global, I

hkl

Structure factor file (CIF format) https://doi.org/10.1107/S1600536805026358/ob6558Isup2.hkl
Contains datablock I

CCDC reference: 1164252

Key indicators

  • Single-crystal X-ray study
  • T = 293 K
  • Mean [sigma](C-C) = 0.005 Å
  • R factor = 0.033
  • wR factor = 0.089
  • Data-to-parameter ratio = 10.9

checkCIF/PLATON results

No syntax errors found



Alert level C PLAT041_ALERT_1_C Calc. and Rep. SumFormula Strings Differ .... ? PLAT042_ALERT_1_C Calc. and Rep. MoietyFormula Strings Differ .... ? PLAT045_ALERT_1_C Calculated and Reported Z Differ by ............ 2.00 Ratio PLAT125_ALERT_4_C No _symmetry_space_group_name_Hall Given ....... ? PLAT164_ALERT_4_C Nr. of Refined C-H H-Atoms in Heavy-At Struct... 4 PLAT199_ALERT_1_C Check the Reported _cell_measurement_temperature 293 K PLAT200_ALERT_1_C Check the Reported _diffrn_ambient_temperature . 293 K PLAT764_ALERT_4_C Overcomplete CIF Bond List Detected (Rep/Expd) . 1.27 Ratio
0 ALERT level A = In general: serious problem 0 ALERT level B = Potentially serious problem 8 ALERT level C = Check and explain 0 ALERT level G = General alerts; check 5 ALERT type 1 CIF construction/syntax error, inconsistent or missing data 0 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 3 ALERT type 4 Improvement, methodology, query or suggestion

Computing details top

Data collection: SMART (Siemens, 1996); cell refinement: SMART; data reduction: SAINT (Siemens, 1996); program(s) used to solve structure: SHELXS97 (Sheldrick, 1997a); program(s) used to refine structure: SHELXL97 (Sheldrick, 1997a); molecular graphics: SHELXTL (Sheldrick, 1997b); software used to prepare material for publication: SHELXTL.

Poly[diaquabis(µ3-malonato)(µ-pyrazine)dinickel(II)] top
Crystal data top
[Ni2(C3H2O4)2(C4H4N2)(H2O)2]F(000) = 444
Mr = 437.6Dx = 1.951 Mg m3
Monoclinic, P21/nMo Kα radiation, λ = 0.71073 Å
a = 6.9783 (5) ÅCell parameters from 1338 reflections
b = 14.5612 (9) Åθ = 1.7–25.2°
c = 7.3348 (5) ŵ = 2.59 mm1
β = 92.181 (2)°T = 293 K
V = 744.77 (9) Å3Column, green
Z = 20.42 × 0.37 × 0.33 mm
Data collection top
Siemens SMART CCD area-detector
diffractometer
1338 independent reflections
Radiation source: fine-focus sealed tube1118 reflections with I > 2σ(I)
Graphite monochromatorRint = 0.023
φ and ω scansθmax = 25.2°, θmin = 2.8°
Absorption correction: multi-scan
(SADABS; Sheldrick, 1996)
h = 83
Tmin = 0.375, Tmax = 0.426k = 1317
2429 measured reflectionsl = 88
Refinement top
Refinement on F2Secondary atom site location: difference Fourier map
Least-squares matrix: fullHydrogen site location: inferred from neighbouring sites
R[F2 > 2σ(F2)] = 0.033H atoms treated by a mixture of independent and constrained refinement
wR(F2) = 0.089 w = 1/[σ2(Fo2) + (0.0643P)2]
where P = (Fo2 + 2Fc2)/3
S = 1.00(Δ/σ)max < 0.001
1338 reflectionsΔρmax = 0.60 e Å3
123 parametersΔρmin = 0.40 e Å3
9 restraintsExtinction correction: SHELXL97 (Sheldrick, 1997a), Fc*=kFc[1+0.001xFc2λ3/sin(2θ)]-1/4
Primary atom site location: structure-invariant direct methodsExtinction coefficient: 0.018 (3)
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
Ni10.66238 (5)0.69131 (3)0.08101 (5)0.0187 (2)
C10.4150 (5)0.6682 (2)0.2436 (4)0.0262 (7)
C20.3873 (6)0.6085 (3)0.4106 (5)0.0337 (8)
C30.9173 (5)0.8403 (2)0.0878 (4)0.0260 (7)
C41.0475 (5)0.5745 (3)0.0907 (6)0.0415 (10)
C50.8212 (5)0.4954 (3)0.0546 (5)0.0382 (9)
N10.8671 (4)0.57184 (19)0.0373 (4)0.0293 (6)
O10.5251 (3)0.62248 (17)0.2949 (3)0.0330 (6)
O20.8363 (3)0.75257 (17)0.2697 (3)0.0328 (6)
O30.4672 (4)0.81041 (18)0.0870 (3)0.0371 (6)
O40.8300 (3)0.7640 (2)0.1097 (3)0.0362 (6)
O50.5142 (3)0.63277 (17)0.1252 (3)0.0334 (6)
H11.074 (6)0.622 (2)0.156 (5)0.059 (13)*
H20.703 (3)0.495 (3)0.096 (4)0.039 (10)*
H30.465 (4)0.5595 (19)0.408 (5)0.042 (11)*
H40.271 (3)0.584 (3)0.407 (7)0.070 (16)*
H50.388 (5)0.797 (3)0.004 (5)0.055 (14)*
H60.409 (8)0.802 (5)0.190 (4)0.059 (13)*
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
Ni10.0229 (3)0.0177 (3)0.0157 (3)0.00064 (15)0.00199 (16)0.00056 (15)
C10.0295 (16)0.0246 (19)0.0246 (16)0.0007 (14)0.0019 (13)0.0041 (14)
C20.053 (2)0.024 (2)0.0239 (17)0.0054 (18)0.0030 (15)0.0010 (15)
C30.0305 (16)0.0230 (19)0.0247 (16)0.0020 (15)0.0032 (13)0.0051 (14)
C40.038 (2)0.034 (2)0.054 (2)0.0056 (17)0.0166 (17)0.0159 (19)
C50.0317 (18)0.029 (2)0.055 (2)0.0014 (16)0.0129 (17)0.0089 (18)
N10.0305 (14)0.0263 (16)0.0312 (15)0.0016 (12)0.0016 (11)0.0009 (13)
O10.0423 (13)0.0255 (13)0.0306 (12)0.0016 (11)0.0055 (10)0.0028 (11)
O20.0448 (14)0.0288 (15)0.0256 (12)0.0079 (11)0.0105 (10)0.0027 (10)
O30.0398 (14)0.0416 (17)0.0303 (14)0.0022 (11)0.0046 (11)0.0016 (11)
O40.0469 (15)0.0352 (16)0.0261 (12)0.0122 (12)0.0048 (10)0.0040 (11)
O50.0395 (12)0.0294 (14)0.0324 (13)0.0033 (11)0.0149 (10)0.0003 (11)
Geometric parameters (Å, º) top
Ni1—O52.050 (2)C3—O1ii1.245 (4)
Ni1—O12.066 (2)C3—O41.280 (5)
Ni1—O22.076 (2)C3—C2iii1.506 (5)
Ni1—O42.079 (2)C4—N11.334 (4)
Ni1—O32.205 (3)C4—C5iv1.388 (5)
Ni1—N12.266 (3)C4—H10.87 (2)
Ni1—H62.50 (5)C5—N11.346 (5)
C1—O51.243 (4)C5—C4iv1.388 (5)
C1—O2i1.280 (4)C5—H20.890 (19)
C1—C21.520 (5)O1—C3v1.245 (4)
C2—C3i1.506 (5)O2—C1iii1.280 (4)
C2—H30.896 (18)O3—H60.85 (2)
C2—H40.886 (19)O3—H50.86 (2)
O5—Ni1—O197.24 (10)C3i—C2—H3110 (2)
O5—Ni1—O2173.93 (9)C1—C2—H3110 (2)
O1—Ni1—O288.19 (10)C3i—C2—H4109 (3)
O5—Ni1—O490.12 (10)C1—C2—H4110 (3)
O1—Ni1—O4172.21 (9)H3—C2—H4104 (2)
O2—Ni1—O484.35 (9)O1ii—C3—O4124.6 (3)
O5—Ni1—O390.76 (9)O1ii—C3—C2iii116.2 (3)
O1—Ni1—O395.62 (10)O4—C3—C2iii119.1 (3)
O2—Ni1—O391.43 (10)N1—C4—C5iv123.1 (3)
O4—Ni1—O386.81 (11)N1—C4—H1114 (3)
O5—Ni1—N184.79 (9)C5iv—C4—H1123 (3)
O1—Ni1—N190.39 (9)N1—C5—C4iv122.3 (3)
O2—Ni1—N192.46 (10)N1—C5—H2115 (3)
O4—Ni1—N187.72 (10)C4iv—C5—H2123 (3)
O3—Ni1—N1172.94 (10)C4—N1—C5114.6 (3)
O5—Ni1—H697.6 (16)C4—N1—Ni1122.2 (2)
O1—Ni1—H676.6 (11)C5—N1—Ni1123.1 (2)
O2—Ni1—H686.3 (17)C3v—O1—Ni1124.3 (2)
O4—Ni1—H6105.0 (13)C1iii—O2—Ni1126.6 (2)
O3—Ni1—H619.6 (9)Ni1—O3—H6100 (4)
N1—Ni1—H6167.0 (11)Ni1—O3—H5103 (3)
O5—C1—O2i124.7 (3)H6—O3—H5107 (4)
O5—C1—C2114.7 (3)C3—O4—Ni1128.0 (2)
O2i—C1—C2120.6 (3)C1—O5—Ni1130.8 (2)
C3i—C2—C1113.3 (3)
Symmetry codes: (i) x1/2, y+3/2, z+1/2; (ii) x+1/2, y+3/2, z+1/2; (iii) x+1/2, y+3/2, z1/2; (iv) x+2, y+1, z; (v) x1/2, y+3/2, z1/2.
Hydrogen-bond geometry (Å, º) top
D—H···AD—HH···AD···AD—H···A
O3—H5···O2i0.86 (2)1.91 (4)2.693 (3)151 (4)
O3—H6···O4v0.85 (2)1.82 (5)2.623 (3)155 (7)
Symmetry codes: (i) x1/2, y+3/2, z+1/2; (v) x1/2, y+3/2, z1/2.
 

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