Download citation
Download citation
link to html
The structure of the title compound, {[Co(C2O4)(C5H5N)2]·0.25H2O}n, has been determined at ca 110 K with relatively high precision, revealing the polymeric aggregation mode of this species.

Supporting information

cif

Crystallographic Information File (CIF) https://doi.org/10.1107/S1600536804007512/hg6032sup1.cif
Contains datablocks I, global

hkl

Structure factor file (CIF format) https://doi.org/10.1107/S1600536804007512/hg6032Isup2.hkl
Contains datablock I

CCDC reference: 239038

Key indicators

  • Single-crystal X-ray study
  • T = 110 K
  • H-atom completeness 96%
  • R factor = 0.039
  • wR factor = 0.115
  • Data-to-parameter ratio = 15.8

checkCIF/PLATON results

No syntax errors found



Alert level B PLAT369_ALERT_2_B Long C(sp2)-C(sp2) Bond C7 - C7_a ... 1.57 Ang.
Alert level C PLAT029_ALERT_3_C _diffrn_measured_fraction_theta_full Low ....... 0.97 PLAT041_ALERT_1_C Calc. and Rep. SumFormula Strings Differ .... ? PLAT042_ALERT_1_C Calc. and Rep. MoietyFormula Strings Differ .... ? PLAT068_ALERT_1_C Reported F000 Differs from Calcd (or Missing)... ? PLAT302_ALERT_4_C Anion/Solvent Disorder ......................... 25.00 Perc. PLAT311_ALERT_2_C Isolated Disordered Oxygen Atom (No H's ?) ..... <O20 PLAT369_ALERT_2_C Long C(sp2)-C(sp2) Bond C6 - C6_b ... 1.56 Ang.
Alert level G FORMU01_ALERT_2_G There is a discrepancy between the atom counts in the _chemical_formula_sum and the formula from the _atom_site* data. Atom count from _chemical_formula_sum:C12 H10.5 Co1 N2 O4.25 Atom count from the _atom_site data: C12 H10 Co1 N2 O4.25 CELLZ01_ALERT_1_G Difference between formula and atom_site contents detected. CELLZ01_ALERT_1_G WARNING: H atoms missing from atom site list. Is this intentional? From the CIF: _cell_formula_units_Z 4 From the CIF: _chemical_formula_sum C12 H10.5 Co N2 O4.25 TEST: Compare cell contents of formula and atom_site data atom Z*formula cif sites diff C 48.00 48.00 0.00 H 42.00 40.00 2.00 Co 4.00 4.00 0.00 N 8.00 8.00 0.00 O 17.00 17.00 0.00
0 ALERT level A = In general: serious problem 1 ALERT level B = Potentially serious problem 7 ALERT level C = Check and explain 3 ALERT level G = General alerts; check 5 ALERT type 1 CIF construction/syntax error, inconsistent or missing data 4 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 1 ALERT type 4 Improvement, methodology, query or suggestion

Computing details top

Data collection: COLLECT (Nonius, 1999); cell refinement: DENZO (Otwinowski & Minor, 1997); data reduction: DENZO; program(s) used to solve structure: SIR97 (Altomare et al., 1994); program(s) used to refine structure: SHELXL97 (Sheldrick, 1997); molecular graphics: ORTEPIII (Burnett & Johnson, 1996) and Mercury (Bruno et al., 2002); software used to prepare material for publication: SHELXL97.

catena-Poly[[bis(pyridine-κN)cobalt(II)]-µ-oxalato] 0.25-hydrate] top
Crystal data top
[Co(C2O4)(C5H5N)2]·0.25H2OF(000) = 630
Mr = 309.65Dx = 1.595 Mg m3
Monoclinic, P21/nMo Kα radiation, λ = 0.71073 Å
Hall symbol: -P 2ynCell parameters from 2213 reflections
a = 9.4320 (3) Åθ = 2.5–27.5°
b = 9.1810 (4) ŵ = 1.34 mm1
c = 14.9370 (5) ÅT = 110 K
β = 94.369 (2)°Rods, pink
V = 1289.71 (8) Å30.35 × 0.15 × 0.10 mm
Z = 4
Data collection top
Nonius KappaCCD
diffractometer
2884 independent reflections
Radiation source: fine-focus sealed tube2213 reflections with I > 2σ(I)
Graphite monochromatorRint = 0.046
Detector resolution: 56 microns pixels mm-1θmax = 27.5°, θmin = 2.5°
φ and ω scansh = 1212
Absorption correction: multi-scan
(Blessing, 1995)
k = 1111
Tmin = 0.652, Tmax = 0.878l = 1919
9965 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)] = 0.039Hydrogen site location: inferred from neighbouring sites
wR(F2) = 0.115H-atom parameters constrained
S = 1.02 w = 1/[σ2(Fo2) + (0.0729P)2 + 0.0368P]
where P = (Fo2 + 2Fc2)/3
2884 reflections(Δ/σ)max < 0.001
182 parametersΔρmax = 0.65 e Å3
0 restraintsΔρmin = 0.77 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*/UeqOcc. (<1)
Co10.24978 (2)0.15117 (3)0.004522 (16)0.01569 (14)
O20.06943 (15)0.14140 (15)0.06838 (10)0.0169 (3)
O30.43149 (15)0.13499 (16)0.07360 (10)0.0178 (3)
O40.13332 (15)0.01654 (16)0.07461 (9)0.0189 (3)
O50.36296 (15)0.01383 (16)0.07210 (9)0.0179 (3)
C60.5203 (2)0.0429 (2)0.04229 (12)0.0160 (4)
C70.0189 (2)0.0461 (2)0.04156 (12)0.0162 (4)
N80.16213 (19)0.3060 (2)0.10054 (12)0.0185 (4)
C90.0459 (2)0.3829 (2)0.08569 (14)0.0233 (5)
H90.00120.36530.03180.028*
C100.0129 (2)0.4867 (3)0.14447 (14)0.0266 (5)
H100.09540.53920.13090.032*
C110.0509 (2)0.5127 (2)0.22363 (14)0.0247 (5)
H110.01350.58380.26520.030*
C120.1697 (2)0.4331 (3)0.24061 (14)0.0277 (5)
H120.21520.44770.29450.033*
C130.2220 (2)0.3316 (3)0.17801 (14)0.0257 (5)
H130.30410.27750.19030.031*
N140.33091 (18)0.3130 (2)0.08869 (11)0.0179 (4)
C150.3387 (2)0.2806 (3)0.17672 (13)0.0246 (5)
H150.31520.18470.19430.029*
C160.3797 (3)0.3812 (3)0.24277 (15)0.0284 (5)
H160.38300.35460.30440.034*
C170.4156 (3)0.5202 (3)0.21822 (15)0.0288 (5)
H170.44560.59050.26230.035*
C180.4068 (3)0.5554 (3)0.12776 (15)0.0301 (5)
H180.42970.65060.10870.036*
C190.3639 (2)0.4487 (2)0.06548 (14)0.0248 (5)
H190.35780.47340.00350.030*
O200.3061 (8)0.7150 (8)0.0786 (5)0.051 (2)0.25
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
Co10.0152 (2)0.0163 (2)0.01580 (19)0.00040 (10)0.00304 (13)0.00001 (10)
O20.0159 (7)0.0196 (8)0.0158 (7)0.0020 (6)0.0040 (6)0.0020 (5)
O30.0161 (8)0.0198 (8)0.0178 (7)0.0024 (6)0.0033 (6)0.0023 (6)
O40.0177 (7)0.0212 (8)0.0184 (7)0.0022 (6)0.0061 (6)0.0032 (6)
O50.0166 (7)0.0195 (8)0.0182 (7)0.0026 (6)0.0042 (6)0.0027 (6)
C60.0183 (10)0.0150 (10)0.0146 (10)0.0039 (8)0.0007 (8)0.0021 (8)
C70.0179 (10)0.0168 (10)0.0137 (10)0.0032 (8)0.0005 (8)0.0016 (8)
N80.0177 (9)0.0184 (9)0.0195 (9)0.0006 (7)0.0007 (7)0.0017 (7)
C90.0249 (12)0.0265 (12)0.0194 (10)0.0021 (10)0.0063 (9)0.0006 (9)
C100.0251 (12)0.0296 (13)0.0253 (11)0.0078 (10)0.0030 (9)0.0004 (9)
C110.0305 (12)0.0227 (12)0.0206 (10)0.0031 (10)0.0001 (9)0.0052 (9)
C120.0281 (12)0.0349 (14)0.0210 (11)0.0043 (10)0.0067 (9)0.0076 (10)
C130.0254 (12)0.0313 (14)0.0209 (11)0.0031 (10)0.0052 (9)0.0026 (9)
N140.0169 (9)0.0175 (9)0.0193 (9)0.0000 (7)0.0021 (7)0.0044 (7)
C150.0287 (12)0.0239 (12)0.0208 (10)0.0013 (10)0.0002 (9)0.0019 (9)
C160.0365 (13)0.0293 (13)0.0190 (11)0.0003 (11)0.0003 (9)0.0017 (9)
C170.0315 (13)0.0310 (13)0.0243 (11)0.0043 (10)0.0054 (9)0.0086 (10)
C180.0346 (13)0.0259 (13)0.0305 (12)0.0105 (11)0.0063 (10)0.0020 (10)
C190.0276 (12)0.0274 (13)0.0202 (10)0.0046 (10)0.0059 (9)0.0003 (9)
O200.063 (5)0.038 (5)0.050 (5)0.017 (4)0.006 (4)0.006 (4)
Geometric parameters (Å, º) top
Co1—O32.0721 (15)C10—C111.388 (3)
Co1—O22.0903 (14)C10—H100.9500
Co1—O42.1209 (15)C11—C121.377 (3)
Co1—O52.1350 (14)C11—H110.9500
Co1—N142.1375 (18)C12—C131.384 (3)
Co1—N82.1400 (18)C12—H120.9500
O2—C71.252 (2)C13—H130.9500
O3—C61.255 (3)N14—C191.337 (3)
O4—C7i1.251 (2)N14—C151.345 (3)
O5—C6ii1.247 (2)C15—C161.385 (3)
C6—O5ii1.248 (2)C15—H150.9500
C6—C6ii1.561 (4)C16—C171.377 (3)
C7—O4i1.251 (2)C16—H160.9500
C7—C7i1.566 (4)C17—C181.385 (3)
N8—C91.337 (3)C17—H170.9500
N8—C131.346 (3)C18—C191.389 (3)
C9—C101.383 (3)C18—H180.9500
C9—H90.9500C19—H190.9500
O3—Co1—O2173.27 (6)C9—C10—C11118.7 (2)
O3—Co1—O496.84 (6)C9—C10—H10120.6
O2—Co1—O479.32 (5)C11—C10—H10120.6
O3—Co1—O579.47 (5)C12—C11—C10118.5 (2)
O2—Co1—O594.81 (5)C12—C11—H11120.7
O4—Co1—O588.19 (6)C10—C11—H11120.7
O3—Co1—N1496.06 (6)C11—C12—C13119.1 (2)
O2—Co1—N1487.46 (6)C11—C12—H12120.5
O4—Co1—N14166.50 (6)C13—C12—H12120.5
O5—Co1—N1490.25 (7)N8—C13—C12123.2 (2)
O3—Co1—N890.33 (6)N8—C13—H13118.4
O2—Co1—N895.13 (6)C12—C13—H13118.4
O4—Co1—N889.56 (7)C19—N14—C15117.59 (19)
O5—Co1—N8169.22 (6)C19—N14—Co1123.92 (14)
N14—Co1—N894.35 (8)C15—N14—Co1118.27 (15)
C7—O2—Co1114.27 (12)N14—C15—C16122.7 (2)
C6—O3—Co1114.62 (12)N14—C15—H15118.6
C7i—O4—Co1113.14 (12)C16—C15—H15118.6
C6ii—O5—Co1112.29 (12)C17—C16—C15119.3 (2)
O5ii—C6—O3126.38 (17)C17—C16—H16120.4
O5ii—C6—C6ii117.3 (2)C15—C16—H16120.4
O3—C6—C6ii116.3 (2)C16—C17—C18118.5 (2)
O4i—C7—O2126.75 (18)C16—C17—H17120.7
O4i—C7—C7i116.8 (2)C18—C17—H17120.7
O2—C7—C7i116.5 (2)C17—C18—C19118.8 (2)
C9—N8—C13116.94 (19)C17—C18—H18120.6
C9—N8—Co1121.30 (14)C19—C18—H18120.6
C13—N8—Co1121.76 (15)N14—C19—C18123.0 (2)
N8—C9—C10123.57 (19)N14—C19—H19118.5
N8—C9—H9118.2C18—C19—H19118.5
C10—C9—H9118.2
Symmetry codes: (i) x, y, z; (ii) x+1, y, z.
 

Follow Acta Cryst. E
Sign up for e-alerts
Follow Acta Cryst. on Twitter
Follow us on facebook
Sign up for RSS feeds