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The title compound, [Co(C14H18N2O6)], is the first structurally characterized example of a β-ketoiminato CoII complex without axial ligands. It adopts a square-planar cis-[CoN2O2] coordination geometry, and lies on a mirror plane. The planar complexes are stacked along 21 screw axes parallel to b to form columns, the Co...Co distance in the column being 3.5213 (2) Å.

Supporting information

cif

Crystallographic Information File (CIF) https://doi.org/10.1107/S1600536803029520/ob6330sup1.cif
Contains datablocks global, I

hkl

Structure factor file (CIF format) https://doi.org/10.1107/S1600536803029520/ob6330Isup2.hkl
Contains datablock I

CCDC reference: 234789

Key indicators

  • Single-crystal X-ray study
  • T = 298 K
  • Mean [sigma](C-C) = 0.004 Å
  • R factor = 0.041
  • wR factor = 0.135
  • Data-to-parameter ratio = 11.1

checkCIF/PLATON results

No syntax errors found



Alert level B PLAT222_ALERT_3_B Large Non-Solvent H Ueq(max)/Ueq(min) ... 4.14 Ratio PLAT241_ALERT_2_B Check High U(eq) as Compared to Neighbors .... C5
Alert level C PLAT242_ALERT_2_C Check Low U(eq) as Compared to Neighbors .... C13 PLAT250_ALERT_2_C Large U3/U1 ratio for average U(i,j) tensor .... 2.75 PLAT301_ALERT_3_C Main Residue Disorder ......................... 4.00 Perc. PLAT380_ALERT_4_C Incorrectly Oriented X(sp2)-Methyl Moiety ...... C1 PLAT380_ALERT_4_C Incorrectly Oriented X(sp2)-Methyl Moiety ...... C8
0 ALERT level A = In general: serious problem 2 ALERT level B = Potentially serious problem 5 ALERT level C = Check and explain 0 ALERT level G = General alerts; check 0 ALERT type 1 CIF construction/syntax error, inconsistent or missing data 3 ALERT type 2 Indicator that the structure model may be wrong or deficient 2 ALERT type 3 Indicator that the structure quality may be low 2 ALERT type 4 Improvement, methodology, query or suggestion

Computing details top

Data collection: WinAFC Diffractometer Control Software (Rigaku, 1999); cell refinement: WinAFC Diffractometer Control Software; data reduction: TEXSAN (Molecular Structure Corporation, 2001); program(s) used to solve structure: SIR92 (Altomare et al., 1994); program(s) used to refine structure: SHELXL97 (Sheldrick, 1997); molecular graphics: ORTEPII (Johnson, 1976); software used to prepare material for publication: TEXSAN.

(I) top
Crystal data top
C14H18CoN2O6F(000) = 764.0
Mr = 369.23Dx = 1.549 Mg m3
Orthorhombic, PnmaMo Kα radiation, λ = 0.7107 Å
Hall symbol: -P 2ac 2nCell parameters from 25 reflections
a = 14.791 (2) Åθ = 10.0–12.1°
b = 6.939 (1) ŵ = 1.12 mm1
c = 15.424 (3) ÅT = 298 K
V = 1583.0 (4) Å3Needle, red
Z = 40.50 × 0.23 × 0.20 mm
Data collection top
Rigaku AFC-7R
diffractometer
Rint = 0.050
ω–2θ scansθmax = 27.5°
Absorption correction: ψ scan
(North et al., 1968)
h = 719
Tmin = 0.742, Tmax = 0.800k = 93
2447 measured reflectionsl = 200
1963 independent reflections3 standard reflections every 150 reflections
1581 reflections with I > 2σ(I) intensity decay: 0.6%
Refinement top
Refinement on F2H-atom parameters constrained
R[F2 > 2σ(F2)] = 0.041 w = 1/[σ2(Fo2) + (0.1P)2]
where P = (Fo2 + 2Fc2)/3
wR(F2) = 0.135(Δ/σ)max < 0.001
S = 1.05Δρmax = 0.44 e Å3
1581 reflectionsΔρmin = 0.78 e Å3
142 parameters
Special details top

Refinement. Refinement using reflections with F2 > 0.0 σ(F2). The weighted R-factor (wR), goodness of fit (S) and R-factor (gt) are based on F, with F set to zero for negative F. The threshold expression of F2 > 2.0 σ(F2) is used only for calculating R-factor (gt).

Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top
xyzUiso*/UeqOcc. (<1)
Co10.50923 (3)0.25000.98257 (3)0.0360 (2)
O10.5773 (2)0.25000.8809 (2)0.0449 (6)
O20.4834 (2)0.25000.6226 (2)0.070 (1)
O30.3441 (2)0.25000.6744 (2)0.0690 (9)
O40.6176 (2)0.25001.0443 (1)0.0443 (5)
O50.6521 (3)0.25001.3160 (2)0.106 (2)
O60.5053 (2)0.25001.3285 (2)0.078 (1)
N10.4016 (2)0.25000.9228 (2)0.0415 (6)
N20.4412 (2)0.25001.0821 (2)0.0467 (7)
C10.6280 (3)0.25000.7369 (3)0.082 (2)
C20.5518 (2)0.25000.8010 (2)0.0435 (7)
C30.4606 (2)0.25000.7764 (2)0.0385 (7)
C40.3906 (2)0.25000.8393 (2)0.0433 (7)
C50.3214 (3)0.25000.9798 (3)0.078 (2)
C60.4351 (2)0.25000.6841 (2)0.0446 (8)
C70.3115 (3)0.25000.5870 (3)0.082 (2)
C80.7296 (3)0.25001.1516 (3)0.076 (2)
C90.6317 (2)0.25001.1266 (2)0.0445 (7)
C100.5621 (2)0.25001.1877 (2)0.0425 (7)
C110.4700 (3)0.25001.1614 (2)0.0496 (8)
C120.3443 (3)0.1965 (7)1.0658 (3)0.048 (2)0.50
C130.5810 (3)0.25001.2824 (2)0.0551 (9)
C140.5142 (4)0.25001.4220 (3)0.084 (2)
H10.66500.13820.74490.1042*
H20.60560.25000.67910.1042*
H30.32920.25000.81840.0508*
H4A0.29510.37550.98050.0929*0.50
H4B0.27770.16090.95780.0929*0.50
H50.24680.25000.58600.0967*
H60.33160.13710.55730.0967*
H70.73530.25001.21400.0926*
H80.75950.13931.12920.0926*
H90.42460.25001.20600.0580*
H100.45730.25001.44950.1023*
H110.54850.13931.44010.1023*
H120.33570.06171.07380.0252*0.50
H130.30570.26351.10610.0252*0.50
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
Co10.0277 (3)0.0518 (3)0.0285 (3)0.00000.0039 (2)0.0000
O10.029 (1)0.074 (2)0.032 (1)0.00000.0019 (8)0.0000
O20.046 (2)0.132 (3)0.032 (1)0.00000.002 (1)0.0000
O30.037 (1)0.130 (3)0.040 (1)0.00000.006 (1)0.0000
O40.035 (1)0.067 (1)0.031 (1)0.00000.0019 (9)0.0000
O50.072 (2)0.207 (5)0.040 (2)0.00000.011 (2)0.0000
O60.084 (3)0.125 (3)0.027 (1)0.00000.007 (1)0.0000
N10.027 (1)0.062 (2)0.035 (1)0.00000.008 (1)0.0000
N20.034 (1)0.072 (2)0.035 (1)0.00000.007 (1)0.0000
C10.035 (2)0.170 (5)0.040 (2)0.00000.009 (2)0.0000
C20.034 (2)0.064 (2)0.032 (2)0.00000.006 (1)0.0000
C30.033 (1)0.051 (2)0.032 (2)0.00000.002 (1)0.0000
C40.032 (2)0.060 (2)0.037 (2)0.00000.001 (1)0.0000
C50.030 (2)0.162 (5)0.043 (2)0.00000.011 (1)0.0000
C60.038 (2)0.061 (2)0.035 (2)0.00000.001 (1)0.0000
C70.049 (2)0.158 (5)0.038 (2)0.00000.016 (2)0.0000
C80.045 (2)0.137 (5)0.046 (2)0.00000.008 (2)0.0000
C90.042 (2)0.052 (2)0.040 (2)0.00000.006 (1)0.0000
C100.047 (2)0.050 (2)0.030 (2)0.00000.001 (1)0.0000
C110.047 (2)0.068 (2)0.034 (2)0.00000.011 (1)0.0000
C120.033 (2)0.068 (4)0.042 (2)0.002 (2)0.013 (2)0.002 (2)
C130.066 (2)0.065 (2)0.034 (2)0.00000.001 (2)0.0000
C140.113 (4)0.115 (5)0.025 (2)0.00000.003 (2)0.0000
Geometric parameters (Å, º) top
Co1—O11.864 (2)C4—H30.965
Co1—O41.865 (2)C5—C121.418 (6)
Co1—N11.840 (3)C5—H4A0.954
Co1—N21.836 (3)C5—H4Ai0.954
O1—C21.288 (4)C5—H4B0.957
O2—C61.187 (4)C5—H4Bi0.957
O3—C61.354 (4)C7—H50.956
O3—C71.431 (5)C7—H60.955
O4—C91.286 (4)C7—H6i0.955
O5—C131.172 (6)C8—C91.499 (6)
O6—C131.326 (5)C8—H70.966
O6—C141.448 (5)C8—H80.951
N1—C41.299 (4)C8—H8i0.951
N1—C51.477 (5)C9—C101.395 (5)
N2—C111.295 (4)C10—C111.421 (5)
N2—C121.502 (5)C10—C131.486 (5)
C1—C21.500 (5)C11—H90.961
C1—H10.957C12—H120.952
C1—H1i0.957C12—H130.964
C1—H20.951C14—H100.943
C2—C31.401 (5)C14—H110.962
C3—C41.418 (4)C14—H11i0.962
C3—C61.472 (4)
O1—Co1—O488.04 (10)O2—C6—C3128.2 (3)
O1—Co1—N192.6 (1)O3—C6—C3111.2 (3)
O1—Co1—N2179.5 (1)O3—C7—H5110.6
O4—Co1—N1179.4 (1)O3—C7—H6110.3
O4—Co1—N292.5 (1)O3—C7—H6i110.3
N1—Co1—N286.8 (1)H5—C7—H6107.7
Co1—O1—C2130.3 (2)H5—C7—H6i107.7
C6—O3—C7116.0 (3)H6—C7—H6i110.2
Co1—O4—C9130.0 (2)C9—C8—H7109.8
C13—O6—C14117.2 (4)C9—C8—H8110.9
Co1—N1—C4127.2 (2)C9—C8—H8i110.9
Co1—N1—C5113.4 (2)H7—C8—H8108.8
C4—N1—C5119.4 (3)H7—C8—H8i108.8
Co1—N2—C11127.6 (3)H8—C8—H8i107.7
Co1—N2—C12112.5 (2)O4—C9—C8114.1 (3)
C11—N2—C12118.2 (3)O4—C9—C10123.2 (3)
C2—C1—H1110.1C8—C9—C10122.7 (3)
C2—C1—H1i110.1C9—C10—C11120.9 (3)
C2—C1—H2110.8C9—C10—C13121.6 (3)
H1—C1—H1i108.2C11—C10—C13117.4 (3)
H1—C1—H2108.8N2—C11—C10125.8 (3)
H1i—C1—H2108.8N2—C11—H9116.4
O1—C2—C1114.3 (3)C10—C11—H9117.8
O1—C2—C3122.7 (3)N2—C12—C5108.7 (3)
C1—C2—C3123.0 (3)N2—C12—H12110.4
C2—C3—C4121.1 (3)N2—C12—H13109.7
C2—C3—C6120.6 (3)C5—C12—H12110.3
C4—C3—C6118.3 (3)C5—C12—H13109.6
N1—C4—C3126.0 (3)H12—C12—H13108.1
N1—C4—H3116.7O5—C13—O6121.3 (4)
C3—C4—H3117.4O5—C13—C10127.1 (4)
N1—C5—C12111.4 (3)O6—C13—C10111.6 (3)
N1—C5—H4A109.5O6—C14—H10111.6
N1—C5—H4B109.3O6—C14—H11109.7
C12—C5—H4A109.1O6—C14—H11i109.7
C12—C5—H4B108.9H10—C14—H11109.9
H4A—C5—H4B108.5H10—C14—H11i109.9
O2—C6—O3120.6 (3)H11—C14—H11i105.9
Co1—O1—C2—C1180.0O5—C13—C10—C11180.0
Co1—O1—C2—C30.0000 (1)O6—C13—C10—C9180.0000 (1)
Co1—O4—C9—C8180.0O6—C13—C10—C110.0000 (1)
Co1—O4—C9—C100.0000 (2)N1—Co1—O1—C20.0000 (4)
Co1—N1—C4—C30.0000 (1)N1—Co1—N2—C11180.0
Co1—N1—C5—C1216.3 (2)N1—Co1—N2—C1215.5 (2)
Co1—N2—C11—C100.0000 (1)N1—C4—C3—C20.0000 (1)
Co1—N2—C12—C527.9 (3)N1—C4—C3—C6180.0
O1—Co1—O4—C9180.0N1—C5—C12—N227.3 (3)
O1—Co1—N1—C40.0000 (1)N2—Co1—O4—C90.0
O1—Co1—N1—C5180.0000 (1)N2—Co1—N1—C4180.0
O1—C2—C3—C40.0N2—Co1—N1—C50.0000 (1)
O1—C2—C3—C6180.0N2—C11—C10—C90.0000 (1)
O2—C6—O3—C70.0000 (2)N2—C11—C10—C13180.0
O2—C6—C3—C20.0000 (2)C1—C2—C3—C4180.0
O2—C6—C3—C4180.0C1—C2—C3—C60.0
O3—C6—C3—C2180.0C3—C4—N1—C5180.0
O3—C6—C3—C40.0000 (2)C3—C6—O3—C7180.0
O4—Co1—O1—C2180.0C4—N1—C5—C12163.7 (2)
O4—Co1—N2—C110.0000 (1)C5—C12—N2—C11166.1 (2)
O4—Co1—N2—C12164.5 (2)C8—C9—C10—C11180.0
O4—C9—C10—C110.0000 (2)C8—C9—C10—C130.0000 (3)
O4—C9—C10—C13180.0C10—C11—N2—C12163.7 (2)
O5—C13—O6—C140.0000 (1)C10—C13—O6—C14180.0
O5—C13—C10—C90.0
Symmetry code: (i) x, y+1/2, z.
 

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