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The Co atom in the title complex, [Co(H-Pysc)2(H2O)4](CH3COO)2 {where H-Pysc is 3-[2-(amino­carbonyl)­hydrazono­methyl]­pyridine, C14H16N8O2}, occupies an inversion centre and is octahedrally coordinated by four aqua ligands and two mol­ecules of the neutral Schiff base derived from the condensation of pyridine-3-carb­aldehyde and semicarbazone (H-Pysc); the Schiff base mol­ecules act as monodentate ligands, coordinating the metal through the pyridyl N, with the amide O and imine N atoms remaining uncoordinated. The crystal packing is stabilized by intermolecular hydrogen bonds involving the cations and acetate counter-ions.

Supporting information

cif

Crystallographic Information File (CIF) https://doi.org/10.1107/S1600536804011420/hb6043sup1.cif
Contains datablocks global, I

hkl

Structure factor file (CIF format) https://doi.org/10.1107/S1600536804011420/hb6043Isup2.hkl
Contains datablock I

CCDC reference: 242049

Key indicators

  • Single-crystal X-ray study
  • T = 193 K
  • Mean [sigma](C-C) = 0.002 Å
  • R factor = 0.028
  • wR factor = 0.068
  • Data-to-parameter ratio = 13.8

checkCIF/PLATON results

No syntax errors found



Alert level C PLAT029_ALERT_3_C _diffrn_measured_fraction_theta_full Low ....... 0.97 PLAT042_ALERT_1_C Calc. and Rep. MoietyFormula Strings Differ .... ? PLAT152_ALERT_1_C Supplied and Calc Volume s.u. Inconsistent ..... ? PLAT232_ALERT_2_C Hirshfeld Test Diff (M-X) Co1 - N1 .. 5.09 su
0 ALERT level A = In general: serious problem 0 ALERT level B = Potentially serious problem 4 ALERT level C = Check and explain 0 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 1 ALERT type 3 Indicator that the structure quality may be low 0 ALERT type 4 Improvement, methodology, query or suggestion

Computing details top

Data collection: CrystalClear (Rigaku, 1999); cell refinement: CrystalClear (Rigaku, 1999); data reduction: CrystalStructure (Rigaku/MSC, 2000); program(s) used to solve structure: SHELXS97 (Sheldrick, 1997); program(s) used to refine structure: SHELXL97 (Sheldrick, 1997); molecular graphics: SHELXTL (Siemens, 1994); software used to prepare material for publication: SHELXTL.

(I) top
Crystal data top
[Co(C14H16N8O2)2(H2O)4](C2H3O2)2Z = 1
Mr = 577.43F(000) = 301
Triclinic, P1Dx = 1.567 Mg m3
Hall symbol: -P 1Mo Kα radiation, λ = 0.71070 Å
a = 7.8694 (13) ÅCell parameters from 3096 reflections
b = 8.8660 (13) Åθ = 3.7–27.5°
c = 10.2643 (11) ŵ = 0.77 mm1
α = 65.788 (11)°T = 193 K
β = 69.511 (12)°Block, gold
γ = 81.816 (14)°0.60 × 0.37 × 0.20 mm
V = 611.83 (15) Å3
Data collection top
Rigaku Mercury CCD
diffractometer
2723 independent reflections
Radiation source: fine-focus sealed tube2622 reflections with I > 2σ(I)'
Graphite monochromatorRint = 0.021
Detector resolution: 7.31 pixels mm-1θmax = 27.5°, θmin = 3.7°
ω scansh = 109
Absorption correction: multi-scan
(Jacobson, 1998)
k = 1011
Tmin = 0.655, Tmax = 0.861l = 1313
6754 measured reflections
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)] = 0.028Hydrogen site location: inferred from neighbouring sites
wR(F2) = 0.069H atoms treated by a mixture of independent and constrained refinement
S = 1.08 w = 1/[σ2(Fo2) + (0.0279P)2 + 0.3346P]
where P = (Fo2 + 2Fc2)/3
2723 reflections(Δ/σ)max < 0.001
198 parametersΔρmax = 0.29 e Å3
0 restraintsΔρmin = 0.37 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
Co10.50000.00000.50000.01498 (9)
O11.37816 (14)0.70010 (13)0.02356 (12)0.0233 (2)
O20.24898 (14)0.02440 (14)0.48337 (13)0.0228 (2)
O30.63356 (15)0.01926 (14)0.27682 (12)0.0198 (2)
O40.05322 (14)0.10900 (14)0.28199 (12)0.0233 (2)
O50.01709 (15)0.04918 (15)0.18610 (14)0.0300 (3)
N10.46693 (16)0.26596 (15)0.41390 (13)0.0186 (2)
N20.92953 (17)0.56468 (15)0.17095 (14)0.0211 (3)
N31.07651 (17)0.66820 (16)0.09299 (15)0.0232 (3)
N41.26053 (19)0.44072 (16)0.09350 (15)0.0239 (3)
C10.3054 (2)0.34020 (19)0.44966 (17)0.0222 (3)
H10.19930.27350.50580.027*
C20.2880 (2)0.5093 (2)0.40790 (18)0.0257 (3)
H2A0.17180.55780.43320.031*
C30.4421 (2)0.60737 (19)0.32872 (18)0.0237 (3)
H3A0.43340.72370.30140.028*
C40.6097 (2)0.53323 (18)0.28986 (16)0.0189 (3)
C50.61417 (19)0.36214 (18)0.33367 (16)0.0189 (3)
H50.72800.31110.30500.023*
C60.7759 (2)0.63225 (18)0.20950 (16)0.0205 (3)
H60.76950.74790.18580.025*
C71.2459 (2)0.60333 (18)0.05166 (16)0.0190 (3)
C80.09425 (19)0.02792 (17)0.19816 (16)0.0190 (3)
C90.2913 (2)0.0263 (2)0.10722 (19)0.0276 (3)
H9A0.30890.05120.05770.041*
H9B0.36520.00840.17420.041*
H9C0.32820.13750.03060.041*
H2B0.151 (3)0.054 (3)0.560 (3)0.049 (6)*
H2C0.211 (3)0.025 (3)0.416 (3)0.038 (6)*
H3B1.066 (3)0.765 (3)0.086 (2)0.034 (5)*
H3C0.620 (3)0.100 (3)0.210 (3)0.043 (6)*
H3D0.748 (3)0.004 (3)0.256 (3)0.047 (6)*
H4A1.169 (3)0.380 (3)0.148 (2)0.030 (5)*
H4B1.369 (3)0.396 (2)0.069 (2)0.031 (5)*
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
Co10.01197 (13)0.01590 (14)0.01539 (14)0.00217 (9)0.00281 (10)0.00511 (10)
O10.0187 (5)0.0193 (5)0.0250 (5)0.0033 (4)0.0035 (4)0.0040 (4)
O20.0150 (5)0.0309 (6)0.0189 (5)0.0044 (4)0.0053 (4)0.0050 (5)
O30.0171 (5)0.0216 (5)0.0162 (5)0.0001 (4)0.0031 (4)0.0050 (4)
O40.0204 (5)0.0279 (6)0.0219 (5)0.0041 (4)0.0033 (4)0.0116 (4)
O50.0181 (5)0.0368 (7)0.0429 (7)0.0002 (5)0.0061 (5)0.0261 (6)
N10.0172 (6)0.0191 (6)0.0182 (6)0.0014 (5)0.0040 (5)0.0070 (5)
N20.0212 (6)0.0172 (6)0.0213 (6)0.0046 (5)0.0032 (5)0.0057 (5)
N30.0196 (6)0.0143 (6)0.0306 (7)0.0038 (5)0.0029 (5)0.0069 (5)
N40.0200 (6)0.0172 (6)0.0288 (7)0.0023 (5)0.0026 (5)0.0070 (5)
C10.0162 (7)0.0249 (8)0.0227 (7)0.0021 (5)0.0034 (5)0.0084 (6)
C20.0196 (7)0.0261 (8)0.0287 (8)0.0052 (6)0.0065 (6)0.0107 (6)
C30.0249 (7)0.0179 (7)0.0265 (8)0.0033 (6)0.0089 (6)0.0075 (6)
C40.0205 (7)0.0189 (7)0.0171 (6)0.0007 (5)0.0063 (5)0.0063 (5)
C50.0168 (6)0.0186 (7)0.0199 (7)0.0007 (5)0.0040 (5)0.0073 (5)
C60.0235 (7)0.0151 (7)0.0212 (7)0.0020 (5)0.0067 (6)0.0053 (5)
C70.0214 (7)0.0189 (7)0.0155 (6)0.0017 (5)0.0052 (5)0.0057 (5)
C80.0172 (6)0.0181 (7)0.0181 (7)0.0001 (5)0.0053 (5)0.0038 (5)
C90.0196 (7)0.0308 (8)0.0299 (8)0.0013 (6)0.0027 (6)0.0134 (7)
Geometric parameters (Å, º) top
Co1—O22.0895 (11)N3—H3B0.83 (2)
Co1—O2i2.0895 (11)N4—C71.3251 (19)
Co1—O32.1039 (11)N4—H4A0.84 (2)
Co1—O3i2.1039 (11)N4—H4B0.89 (2)
Co1—N1i2.1647 (13)C1—C21.381 (2)
Co1—N12.1647 (13)C1—H10.9500
O1—C71.2504 (17)C2—C31.385 (2)
O2—H2B0.86 (3)C2—H2A0.9500
O2—H2C0.79 (2)C3—C41.389 (2)
O3—H3C0.79 (3)C3—H3A0.9500
O3—H3D0.86 (3)C4—C51.393 (2)
O4—C81.2682 (18)C4—C61.463 (2)
O5—C81.2514 (18)C5—H50.9500
N1—C51.3361 (18)C6—H60.9500
N1—C11.3482 (19)C8—C91.506 (2)
N2—C61.277 (2)C9—H9A0.9800
N2—N31.3684 (17)C9—H9B0.9800
N3—C71.3689 (19)C9—H9C0.9800
O2—Co1—O2i180.0N1—C1—C2122.58 (14)
O2—Co1—O391.17 (5)N1—C1—H1118.7
O2i—Co1—O388.83 (5)C2—C1—H1118.7
O2—Co1—O3i88.83 (5)C1—C2—C3119.19 (14)
O2i—Co1—O3i91.17 (5)C1—C2—H2A120.4
O3—Co1—O3i180.0C3—C2—H2A120.4
O2—Co1—N1i90.50 (5)C2—C3—C4119.04 (14)
O2i—Co1—N1i89.50 (5)C2—C3—H3A120.5
O3—Co1—N1i91.34 (5)C4—C3—H3A120.5
O3i—Co1—N1i88.66 (5)C3—C4—C5117.92 (13)
O2—Co1—N189.50 (5)C3—C4—C6120.60 (13)
O2i—Co1—N190.50 (5)C5—C4—C6121.45 (13)
O3—Co1—N188.66 (5)N1—C5—C4123.48 (13)
O3i—Co1—N191.34 (5)N1—C5—H5118.3
N1i—Co1—N1180.0C4—C5—H5118.3
Co1—O2—H2B123.6 (16)N2—C6—C4120.62 (13)
Co1—O2—H2C128.8 (16)N2—C6—H6119.7
H2B—O2—H2C102 (2)C4—C6—H6119.7
Co1—O3—H3C119.2 (17)O1—C7—N4123.54 (14)
Co1—O3—H3D115.1 (15)O1—C7—N3118.51 (13)
H3C—O3—H3D108 (2)N4—C7—N3117.95 (13)
C5—N1—C1117.75 (13)O5—C8—O4124.59 (13)
C5—N1—Co1119.07 (10)O5—C8—C9118.56 (13)
C1—N1—Co1122.86 (10)O4—C8—C9116.85 (13)
C6—N2—N3116.26 (13)C8—C9—H9A109.5
N2—N3—C7119.31 (13)C8—C9—H9B109.5
N2—N3—H3B119.9 (14)H9A—C9—H9B109.5
C7—N3—H3B119.7 (14)C8—C9—H9C109.5
C7—N4—H4A120.5 (14)H9A—C9—H9C109.5
C7—N4—H4B119.6 (13)H9B—C9—H9C109.5
H4A—N4—H4B119.8 (19)
O2—Co1—N1—C5149.69 (11)C1—C2—C3—C41.7 (2)
O2i—Co1—N1—C530.31 (11)C2—C3—C4—C50.3 (2)
O3—Co1—N1—C558.51 (11)C2—C3—C4—C6178.48 (14)
O3i—Co1—N1—C5121.49 (11)C1—N1—C5—C42.2 (2)
O2—Co1—N1—C136.96 (12)Co1—N1—C5—C4171.50 (11)
O2i—Co1—N1—C1143.04 (12)C3—C4—C5—N11.7 (2)
O3—Co1—N1—C1128.15 (12)C6—C4—C5—N1176.43 (13)
O3i—Co1—N1—C151.85 (12)N3—N2—C6—C4178.43 (13)
C6—N2—N3—C7178.28 (14)C3—C4—C6—N2178.51 (14)
C5—N1—C1—C20.6 (2)C5—C4—C6—N23.4 (2)
Co1—N1—C1—C2172.80 (12)N2—N3—C7—O1177.82 (13)
N1—C1—C2—C31.3 (2)N2—N3—C7—N42.0 (2)
Symmetry code: (i) x+1, y, z+1.
Hydrogen-bond geometry (Å, º) top
D—H···AD—HH···AD···AD—H···A
O2—H2C···O40.79 (2)2.02 (2)2.7839 (16)164 (2)
O2—H2B···O4ii0.86 (3)1.79 (3)2.6524 (16)179 (2)
O3—H3D···O5iii0.86 (3)1.79 (3)2.6438 (16)171 (2)
O3—H3C···O1iv0.79 (3)2.00 (3)2.7846 (16)172 (2)
N3—H3B···O5v0.83 (2)2.19 (2)2.9462 (18)151.6 (19)
N4—H4B···O1vi0.89 (2)2.02 (2)2.9075 (18)175.5 (18)
N4—H4A···O4iii0.84 (2)2.35 (2)3.0893 (18)147.3 (18)
Symmetry codes: (ii) x, y, z+1; (iii) x+1, y, z; (iv) x+2, y+1, z; (v) x+1, y+1, z; (vi) x+3, y+1, z.
 

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