Download citation
Download citation
link to html
The title compound, [Co(C16H23N2O)2]ClO4, has been synthesized and characterized. The crystal structure was determined by X-ray crystallography from single-crystal data. It is a mononuclear compound, and the central CoIII atom, lying on an inversion center, is coordinated by four N atoms and two O atoms from two Schiff bases, giving an approximately octahedral coordination environment.

Supporting information

cif

Crystallographic Information File (CIF) https://doi.org/10.1107/S1600536803023092/cf6284sup1.cif
Contains datablocks global, I

hkl

Structure factor file (CIF format) https://doi.org/10.1107/S1600536803023092/cf6284Isup2.hkl
Contains datablock I

CCDC reference: 226662

Key indicators

  • Single-crystal X-ray study
  • T = 298 K
  • Mean [sigma](C-C) = 0.007 Å
  • Disorder in solvent or counterion
  • R factor = 0.066
  • wR factor = 0.149
  • Data-to-parameter ratio = 13.7

checkCIF/PLATON results

No syntax errors found



Alert level A PLAT029_ALERT_3_A _diffrn_measured_fraction_theta_full Low ....... 0.97
Alert level C PLAT125_ALERT_4_C No _symmetry_space_group_name_Hall Given ....... ? PLAT244_ALERT_4_C Low Solvent U(eq) as Compared to Neighbors .... Cl1 PLAT302_ALERT_4_C Anion/Solvent Disorder ......................... 44.00 Perc. PLAT341_ALERT_3_C Low Bond Precision on C-C bonds (x 1000) Ang ... 7 PLAT420_ALERT_2_C D-H Without Acceptor N2 - H2 ... ?
1 ALERT level A = In general: serious problem 0 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 1 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 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.

Trans-bis{2-[(3-cyclohexylaminopropylimino)methyl]}cobalt(III) chlorate top
Crystal data top
[Co(C16H23N2O)2]ClO4Z = 1
Mr = 677.11F(000) = 358
Triclinic, P1Dx = 1.417 Mg m3
a = 8.547 (5) ÅMo Kα radiation, λ = 0.71073 Å
b = 9.431 (6) ÅCell parameters from 822 reflections
c = 10.222 (6) Åθ = 2.5–22.1°
α = 96.143 (10)°µ = 0.68 mm1
β = 94.232 (9)°T = 298 K
γ = 103.217 (9)°Block, brown
V = 793.4 (8) Å30.22 × 0.15 × 0.13 mm
Data collection top
Bruker SMART CCD area-detector
diffractometer
2732 independent reflections
Radiation source: fine-focus sealed tube1653 reflections with I > 2σ(I)
Graphite monochromatorRint = 0.045
φ and ω scansθmax = 25.0°, θmin = 2.2°
Absorption correction: multi-scan
(SADABS; Sheldrick, 1996)
h = 109
Tmin = 0.866, Tmax = 0.917k = 711
4017 measured reflectionsl = 1112
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)] = 0.066Hydrogen site location: inferred from neighbouring sites
wR(F2) = 0.149H-atom parameters constrained
S = 0.90 w = 1/[σ2(Fo2) + (0.0674P)2]
where P = (Fo2 + 2Fc2)/3
2732 reflections(Δ/σ)max < 0.001
200 parametersΔρmax = 0.47 e Å3
8 restraintsΔρmin = 0.34 e Å3
Special details top

Experimental. C, H and N elemental analyses were performed on a Perkin-Elmer elemental analyser. The IR spectra were recorded in the 4000–600 cm-1 region using a Smart OMNI-Sampler spectrophotometer.

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)
Co11.00001.00000.00000.0385 (3)
Cl11.00000.50000.50000.0832 (7)
N11.0069 (4)0.8041 (4)0.0741 (3)0.0410 (9)
N20.9874 (4)0.9328 (4)0.1815 (3)0.0403 (9)
H21.03461.01780.23490.048*
O10.7746 (3)0.9567 (3)0.0367 (3)0.0400 (7)
O21.1381 (11)0.5758 (10)0.4375 (9)0.110 (3)*0.50
O30.8632 (15)0.5495 (19)0.4658 (16)0.215 (7)*0.50
O41.0488 (13)0.4996 (11)0.6319 (9)0.122 (3)*0.50
O50.9773 (14)0.3416 (11)0.4360 (10)0.138 (4)*0.50
C10.8975 (5)0.7203 (5)0.1588 (4)0.0429 (11)
H10.91960.63390.19690.051*
C20.7440 (5)0.7475 (5)0.2003 (4)0.0395 (11)
C30.6405 (6)0.6461 (5)0.2984 (4)0.0543 (13)
H30.67900.57260.34410.065*
C40.4850 (6)0.6539 (6)0.3272 (5)0.0537 (13)
H40.41750.58630.39220.064*
C50.4287 (6)0.7625 (5)0.2595 (5)0.0521 (13)
H50.32230.76770.27900.063*
C60.5262 (5)0.8633 (5)0.1638 (4)0.0457 (12)
H60.48520.93580.11920.055*
C70.6869 (5)0.8585 (5)0.1322 (4)0.0384 (11)
C81.1320 (6)0.7389 (5)0.0170 (5)0.0492 (12)
H8A1.23690.80710.01100.059*
H8B1.13560.64980.07240.059*
C91.0909 (6)0.7040 (5)0.1203 (5)0.0553 (13)
H9A0.98420.63850.11200.066*
H9B1.16700.65180.15490.066*
C101.0934 (6)0.8353 (5)0.2193 (5)0.0529 (13)
H10A1.06270.80030.30170.063*
H10B1.20370.89400.23610.063*
C110.8212 (5)0.8976 (5)0.2272 (4)0.0453 (12)
H110.76200.96320.18850.054*
C120.7255 (6)0.7406 (5)0.1780 (4)0.0503 (13)
H12A0.72750.72010.08320.060*
H12B0.77340.67120.22040.060*
C130.5524 (6)0.7248 (6)0.2110 (5)0.0615 (15)
H13A0.50420.79250.16620.074*
H13B0.49010.62590.17980.074*
C140.5469 (6)0.7565 (7)0.3587 (5)0.0689 (16)
H14A0.58420.68200.40220.083*
H14B0.43610.75120.37690.083*
C150.6509 (7)0.9069 (6)0.4151 (5)0.0694 (16)
H15A0.60310.98210.38290.083*
H15B0.65370.91830.51080.083*
C160.8209 (6)0.9276 (6)0.3768 (4)0.0556 (14)
H16A0.87400.86140.41910.067*
H16B0.88121.02740.40760.067*
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
Co10.0395 (5)0.0310 (5)0.0443 (5)0.0068 (4)0.0056 (4)0.0042 (4)
Cl10.0609 (13)0.124 (2)0.0680 (14)0.0309 (13)0.0058 (11)0.0085 (14)
N10.047 (2)0.032 (2)0.044 (2)0.0118 (18)0.0086 (18)0.0021 (18)
N20.037 (2)0.032 (2)0.051 (2)0.0068 (16)0.0035 (17)0.0085 (18)
O10.0393 (17)0.0310 (16)0.0473 (17)0.0065 (13)0.0009 (13)0.0014 (14)
C10.051 (3)0.030 (2)0.049 (3)0.012 (2)0.010 (2)0.002 (2)
C20.039 (3)0.034 (2)0.042 (3)0.002 (2)0.008 (2)0.005 (2)
C30.069 (4)0.041 (3)0.047 (3)0.006 (3)0.001 (3)0.000 (2)
C40.054 (3)0.052 (3)0.047 (3)0.000 (3)0.004 (2)0.003 (3)
C50.043 (3)0.056 (3)0.057 (3)0.010 (3)0.002 (2)0.010 (3)
C60.039 (3)0.042 (3)0.054 (3)0.010 (2)0.001 (2)0.000 (2)
C70.042 (3)0.034 (3)0.038 (2)0.005 (2)0.007 (2)0.008 (2)
C80.049 (3)0.035 (3)0.064 (3)0.010 (2)0.008 (2)0.002 (2)
C90.053 (3)0.041 (3)0.074 (3)0.011 (2)0.004 (3)0.021 (3)
C100.053 (3)0.044 (3)0.061 (3)0.005 (2)0.006 (2)0.020 (3)
C110.046 (3)0.047 (3)0.046 (3)0.013 (2)0.012 (2)0.009 (2)
C120.051 (3)0.049 (3)0.048 (3)0.004 (2)0.011 (2)0.009 (2)
C130.052 (3)0.058 (3)0.069 (3)0.000 (3)0.007 (3)0.015 (3)
C140.058 (3)0.080 (4)0.072 (4)0.011 (3)0.025 (3)0.022 (3)
C150.081 (4)0.078 (4)0.055 (3)0.024 (3)0.022 (3)0.015 (3)
C160.067 (3)0.051 (3)0.046 (3)0.009 (3)0.009 (2)0.003 (2)
Geometric parameters (Å, º) top
Co1—O1i1.876 (3)C6—H60.930
Co1—O11.876 (3)C8—C91.522 (6)
Co1—N11.936 (4)C8—H8A0.970
Co1—N1i1.936 (4)C8—H8B0.970
Co1—N22.026 (3)C9—C101.508 (7)
Co1—N2i2.026 (4)C9—H9A0.970
Cl1—O41.383 (9)C9—H9B0.970
Cl1—O31.390 (12)C10—H10A0.970
Cl1—O21.462 (8)C10—H10B0.970
Cl1—O51.529 (10)C11—C161.525 (6)
N1—C11.283 (5)C11—C121.530 (6)
N1—C81.465 (6)C11—H110.980
N2—C101.490 (6)C12—C131.519 (6)
N2—C111.503 (5)C12—H12A0.970
N2—H20.910C12—H12B0.970
O1—C71.324 (5)C13—C141.514 (7)
C1—C21.436 (6)C13—H13A0.970
C1—H10.930C13—H13B0.970
C2—C71.395 (6)C14—C151.519 (7)
C2—C31.407 (6)C14—H14A0.970
C3—C41.360 (7)C14—H14B0.970
C3—H30.930C15—C161.508 (7)
C4—C51.372 (7)C15—H15A0.970
C4—H40.930C15—H15B0.970
C5—C61.369 (6)C16—H16A0.970
C5—H50.930C16—H16B0.970
C6—C71.400 (6)
O1i—Co1—O1180.0N1—C8—H8A110.1
O1i—Co1—N188.48 (14)C9—C8—H8A110.1
O1—Co1—N191.52 (14)N1—C8—H8B110.1
O1i—Co1—N1i91.52 (14)C9—C8—H8B110.1
O1—Co1—N1i88.48 (14)H8A—C8—H8B108.4
N1—Co1—N1i180.0C10—C9—C8115.2 (4)
O1i—Co1—N286.94 (13)C10—C9—H9A108.5
O1—Co1—N293.06 (13)C8—C9—H9A108.5
N1—Co1—N289.66 (15)C10—C9—H9B108.5
N1i—Co1—N290.34 (15)C8—C9—H9B108.5
O1i—Co1—N2i93.06 (13)H9A—C9—H9B107.5
O1—Co1—N2i86.94 (13)N2—C10—C9116.5 (4)
N1—Co1—N2i90.34 (15)N2—C10—H10A108.2
N1i—Co1—N2i89.66 (15)C9—C10—H10A108.2
N2—Co1—N2i180.0N2—C10—H10B108.2
O4—Cl1—O3119.5 (7)C9—C10—H10B108.2
O4—Cl1—O2108.5 (5)H10A—C10—H10B107.3
O3—Cl1—O2110.9 (7)N2—C11—C16113.5 (4)
O4—Cl1—O5105.4 (5)N2—C11—C12113.2 (4)
O3—Cl1—O5109.4 (8)C16—C11—C12109.6 (4)
O2—Cl1—O5101.6 (5)N2—C11—H11106.7
C1—N1—C8117.1 (4)C16—C11—H11106.7
C1—N1—Co1124.1 (3)C12—C11—H11106.7
C8—N1—Co1118.2 (3)C13—C12—C11108.7 (4)
C10—N2—C11115.5 (3)C13—C12—H12A110.0
C10—N2—Co1117.5 (3)C11—C12—H12A110.0
C11—N2—Co1115.5 (3)C13—C12—H12B110.0
C10—N2—H2101.4C11—C12—H12B110.0
C11—N2—H2101.4H12A—C12—H12B108.3
Co1—N2—H2101.4C14—C13—C12110.7 (4)
C7—O1—Co1126.3 (3)C14—C13—H13A109.5
N1—C1—C2126.1 (4)C12—C13—H13A109.5
N1—C1—H1117.0C14—C13—H13B109.5
C2—C1—H1117.0C12—C13—H13B109.5
C7—C2—C3119.6 (4)H13A—C13—H13B108.1
C7—C2—C1121.2 (4)C13—C14—C15112.0 (4)
C3—C2—C1118.5 (4)C13—C14—H14A109.2
C4—C3—C2121.0 (5)C15—C14—H14A109.2
C4—C3—H3119.5C13—C14—H14B109.2
C2—C3—H3119.5C15—C14—H14B109.2
C3—C4—C5119.3 (4)H14A—C14—H14B107.9
C3—C4—H4120.3C16—C15—C14111.6 (5)
C5—C4—H4120.3C16—C15—H15A109.3
C6—C5—C4121.2 (5)C14—C15—H15A109.3
C6—C5—H5119.4C16—C15—H15B109.3
C4—C5—H5119.4C14—C15—H15B109.3
C5—C6—C7120.8 (5)H15A—C15—H15B108.0
C5—C6—H6119.6C15—C16—C11111.0 (4)
C7—C6—H6119.6C15—C16—H16A109.4
O1—C7—C2123.7 (4)C11—C16—H16A109.4
O1—C7—C6118.2 (4)C15—C16—H16B109.4
C2—C7—C6118.1 (4)C11—C16—H16B109.4
N1—C8—C9108.2 (4)H16A—C16—H16B108.0
O1i—Co1—N1—C1156.9 (3)C4—C5—C6—C70.0 (7)
O1—Co1—N1—C123.1 (3)Co1—O1—C7—C216.1 (5)
N2—Co1—N1—C1116.2 (4)Co1—O1—C7—C6166.0 (3)
N2i—Co1—N1—C163.8 (4)C3—C2—C7—O1178.6 (4)
O1i—Co1—N1—C832.2 (3)C1—C2—C7—O18.4 (6)
O1—Co1—N1—C8147.8 (3)C3—C2—C7—C60.7 (6)
N2—Co1—N1—C854.8 (3)C1—C2—C7—C6169.5 (4)
N2i—Co1—N1—C8125.2 (3)C5—C6—C7—O1178.5 (4)
O1i—Co1—N2—C1046.4 (3)C5—C6—C7—C20.5 (6)
O1—Co1—N2—C10133.6 (3)C1—N1—C8—C9101.2 (4)
N1—Co1—N2—C1042.1 (3)Co1—N1—C8—C970.4 (4)
N1i—Co1—N2—C10137.9 (3)N1—C8—C9—C1064.0 (5)
O1i—Co1—N2—C11171.8 (3)C11—N2—C10—C992.5 (5)
O1—Co1—N2—C118.2 (3)Co1—N2—C10—C949.3 (5)
N1—Co1—N2—C1199.7 (3)C8—C9—C10—N256.3 (6)
N1i—Co1—N2—C1180.3 (3)C10—N2—C11—C1668.3 (5)
N1—Co1—O1—C727.2 (3)Co1—N2—C11—C16149.1 (3)
N1i—Co1—O1—C7152.8 (3)C10—N2—C11—C1257.5 (5)
N2—Co1—O1—C7116.9 (3)Co1—N2—C11—C1285.1 (4)
N2i—Co1—O1—C763.1 (3)N2—C11—C12—C13171.1 (4)
C8—N1—C1—C2162.6 (4)C16—C11—C12—C1361.0 (5)
Co1—N1—C1—C28.5 (6)C11—C12—C13—C1459.6 (6)
N1—C1—C2—C712.2 (7)C12—C13—C14—C1555.7 (7)
N1—C1—C2—C3177.6 (4)C13—C14—C15—C1652.6 (7)
C7—C2—C3—C40.5 (7)C14—C15—C16—C1154.1 (6)
C1—C2—C3—C4170.0 (4)N2—C11—C16—C15173.5 (4)
C2—C3—C4—C50.0 (7)C12—C11—C16—C1558.8 (6)
C3—C4—C5—C60.2 (7)
Symmetry code: (i) x+2, y+2, z.
 

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