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The title complex, [Co(C20H25N2O)2]ClO4, is very similar to the mononuclear complex [Co(C16H23N2O)2]ClO4, which we reported recently [You, Qu, Liu, Tan & Zhu (2003). Acta Cryst. E59, m1038-m1040]. 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/S1600536804008414/lh6194sup1.cif
Contains datablocks global, I

hkl

Structure factor file (CIF format) https://doi.org/10.1107/S1600536804008414/lh6194Isup2.hkl
Contains datablock I

CCDC reference: 239060

Key indicators

  • Single-crystal X-ray study
  • T = 293 K
  • Mean [sigma](C-C) = 0.008 Å
  • Disorder in solvent or counterion
  • R factor = 0.075
  • wR factor = 0.213
  • Data-to-parameter ratio = 15.4

checkCIF/PLATON results

No syntax errors found



Alert level C PLAT029_ALERT_3_C _diffrn_measured_fraction_theta_full Low ....... 0.98 PLAT094_ALERT_2_C Ratio of Maximum / Minimum Residual Density .... 2.61 PLAT152_ALERT_1_C Supplied and Calc Volume s.u. Inconsistent ..... ? PLAT244_ALERT_4_C Low Solvent U(eq) as Compared to Neighbors .... Cl1 PLAT302_ALERT_4_C Anion/Solvent Disorder ......................... 38.00 Perc. PLAT341_ALERT_3_C Low Bond Precision on C-C bonds (x 1000) Ang ... 8 PLAT420_ALERT_2_C D-H Without Acceptor N2 - H2A ... ? PLAT790_ALERT_4_C Centre of Gravity not Within Unit Cell: Resd. # 2 Cl O4
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 1 ALERT type 1 CIF construction/syntax error, inconsistent or missing data 2 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-(cyclohexylamino)propyliminomethyl]naphthalato}cobalt(III) chlorate top
Crystal data top
[Co(C20H25N2O)2]ClO4Z = 1
Mr = 777.22F(000) = 410
Triclinic, P1Dx = 1.326 Mg m3
Hall symbol: -P 1Mo Kα radiation, λ = 0.71073 Å
a = 9.061 (2) ÅCell parameters from 2138 reflections
b = 10.378 (2) Åθ = 2.8–25.6°
c = 11.464 (2) ŵ = 0.56 mm1
α = 78.01 (3)°T = 293 K
β = 67.79 (3)°Block, brown
γ = 81.41 (3)°0.27 × 0.22 × 0.10 mm
V = 973.3 (3) Å3
Data collection top
Bruker SMART CCD
diffractometer
3849 independent reflections
Radiation source: fine-focus sealed tube2551 reflections with I > 2σ(I)
Graphite monochromatorRint = 0.031
φ and ω scansθmax = 26.5°, θmin = 2.0°
Absorption correction: multi-scan
(SADABS; Sheldrick, 1996)
h = 1110
Tmin = 0.863, Tmax = 0.946k = 1311
4553 measured reflectionsl = 1411
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)] = 0.075Hydrogen site location: inferred from neighbouring sites
wR(F2) = 0.213H-atom parameters constrained
S = 1.04 w = 1/[σ2(Fo2) + (0.1068P)2]
where P = (Fo2 + 2Fc2)/3
3849 reflections(Δ/σ)max < 0.001
250 parametersΔρmax = 0.79 e Å3
0 restraintsΔρmin = 0.30 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)
Co10.00000.00000.00000.0354 (3)
Cl10.1065 (7)0.4967 (5)0.5145 (4)0.1154 (16)0.50
O10.1410 (4)0.1332 (3)0.0814 (3)0.0417 (8)
O20.218 (2)0.5225 (13)0.6350 (11)0.196 (8)0.50
O30.2237 (19)0.4347 (13)0.4360 (11)0.159 (6)0.50
O40.0010 (13)0.6075 (8)0.4867 (8)0.197 (4)
N10.0675 (4)0.1236 (4)0.1558 (3)0.0383 (9)
N20.1705 (4)0.0483 (4)0.0503 (4)0.0433 (10)
H2A0.26040.02700.01340.080*
C10.3264 (5)0.0066 (5)0.2438 (4)0.0407 (11)
C20.2795 (5)0.1151 (5)0.1734 (4)0.0414 (11)
C30.3837 (6)0.2289 (5)0.2039 (5)0.0539 (13)
H3A0.34780.31410.15930.080*
C40.5337 (7)0.2200 (6)0.2943 (5)0.0595 (15)
H4A0.60200.29840.31540.080*
C50.7496 (7)0.0841 (8)0.4457 (5)0.0700 (18)
H5A0.82010.16250.46140.080*
C60.8003 (7)0.0390 (9)0.5061 (6)0.077 (2)
H6A0.90810.04660.56530.080*
C70.7019 (8)0.1483 (8)0.4832 (6)0.0743 (19)
H7A0.74030.23270.52810.080*
C80.5477 (6)0.1409 (6)0.3983 (5)0.0612 (15)
H8A0.47870.21980.38120.080*
C90.4877 (6)0.0186 (5)0.3351 (4)0.0469 (12)
C100.5887 (6)0.0943 (6)0.3584 (5)0.0548 (14)
C110.2076 (5)0.1150 (5)0.2424 (4)0.0417 (11)
H11A0.23470.18760.31190.080*
C120.0467 (6)0.2293 (5)0.1802 (5)0.0491 (13)
H12A0.06640.29030.12240.080*
H12B0.00140.27600.26570.080*
C130.2009 (6)0.1782 (5)0.1653 (6)0.0584 (15)
H13A0.27930.19660.08530.080*
H13B0.23710.22590.23210.080*
C140.1936 (7)0.0355 (5)0.1642 (5)0.0547 (14)
H14A0.10540.01490.23860.080*
H14B0.28950.01440.17080.080*
C150.1791 (5)0.1940 (5)0.0406 (5)0.0429 (11)
H15A0.12320.23880.01460.080*
C160.3513 (6)0.2299 (5)0.0240 (5)0.0576 (14)
H16A0.40050.19520.10250.080*
H16B0.41060.19260.03060.080*
C170.3551 (7)0.3781 (6)0.0497 (6)0.0704 (17)
H17A0.30140.41350.10870.080*
H17B0.46370.40180.08940.080*
C180.2716 (8)0.4373 (6)0.0702 (7)0.0739 (18)
H18A0.26870.53180.04780.080*
H18B0.33150.41010.12580.080*
C190.1050 (8)0.3951 (6)0.1384 (6)0.0701 (17)
H19A0.04170.43110.08660.080*
H19B0.05750.42900.21740.080*
C200.1003 (6)0.2460 (5)0.1658 (5)0.0551 (14)
H20A0.15860.20980.22130.080*
H20B0.00730.22030.20730.080*
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
Co10.0288 (5)0.0368 (6)0.0386 (5)0.0063 (4)0.0112 (4)0.0010 (4)
Cl10.185 (4)0.064 (2)0.075 (3)0.012 (3)0.026 (3)0.003 (2)
O10.0342 (18)0.0397 (19)0.0458 (19)0.0033 (14)0.0101 (15)0.0033 (14)
O20.32 (2)0.128 (11)0.060 (7)0.030 (12)0.007 (10)0.001 (7)
O30.219 (15)0.129 (10)0.092 (8)0.052 (10)0.037 (9)0.057 (7)
O40.262 (10)0.132 (7)0.171 (7)0.004 (7)0.054 (7)0.024 (6)
N10.035 (2)0.035 (2)0.043 (2)0.0072 (17)0.0137 (18)0.0012 (17)
N20.039 (2)0.041 (2)0.051 (2)0.0075 (18)0.0181 (19)0.0034 (18)
C10.037 (3)0.047 (3)0.036 (3)0.005 (2)0.011 (2)0.007 (2)
C20.036 (3)0.051 (3)0.038 (3)0.002 (2)0.016 (2)0.009 (2)
C30.056 (3)0.055 (3)0.047 (3)0.007 (3)0.018 (3)0.008 (2)
C40.051 (3)0.076 (4)0.046 (3)0.020 (3)0.016 (3)0.019 (3)
C50.044 (3)0.120 (6)0.042 (3)0.012 (4)0.012 (3)0.024 (3)
C60.043 (4)0.133 (7)0.045 (3)0.014 (4)0.005 (3)0.012 (4)
C70.052 (4)0.105 (6)0.057 (4)0.024 (4)0.006 (3)0.007 (4)
C80.045 (3)0.077 (4)0.055 (3)0.013 (3)0.011 (3)0.007 (3)
C90.039 (3)0.065 (4)0.037 (3)0.002 (3)0.014 (2)0.009 (2)
C100.043 (3)0.086 (4)0.033 (3)0.004 (3)0.013 (2)0.013 (3)
C110.040 (3)0.046 (3)0.037 (3)0.014 (2)0.011 (2)0.001 (2)
C120.041 (3)0.044 (3)0.054 (3)0.003 (2)0.015 (2)0.006 (2)
C130.052 (3)0.052 (3)0.074 (4)0.004 (3)0.036 (3)0.009 (3)
C140.060 (3)0.053 (3)0.059 (3)0.004 (3)0.035 (3)0.000 (3)
C150.034 (3)0.044 (3)0.049 (3)0.007 (2)0.012 (2)0.008 (2)
C160.039 (3)0.060 (4)0.070 (4)0.014 (3)0.007 (3)0.019 (3)
C170.057 (4)0.057 (4)0.089 (5)0.023 (3)0.013 (3)0.004 (3)
C180.096 (5)0.043 (3)0.100 (5)0.011 (3)0.055 (4)0.008 (3)
C190.089 (5)0.055 (4)0.069 (4)0.010 (3)0.030 (4)0.024 (3)
C200.055 (3)0.059 (4)0.050 (3)0.005 (3)0.016 (3)0.013 (3)
Geometric parameters (Å, º) top
Co1—O11.876 (3)C7—C81.371 (7)
Co1—O1i1.876 (3)C7—H7A0.9600
Co1—N11.915 (4)C8—C91.399 (7)
Co1—N1i1.915 (4)C8—H8A0.9600
Co1—N2i1.999 (4)C9—C101.380 (7)
Co1—N21.999 (4)C11—H11A0.9600
Cl1—O21.369 (13)C12—C131.506 (7)
Cl1—O41.389 (9)C12—H12A0.9600
Cl1—O4ii1.555 (10)C12—H12B0.9599
Cl1—O31.622 (15)C13—C141.470 (7)
Cl1—Cl1ii1.824 (12)C13—H13A0.9600
O1—C21.308 (5)C13—H13B0.9600
O4—Cl1ii1.555 (10)C14—H14A0.9600
N1—C111.286 (5)C14—H14B0.9600
N1—C121.450 (6)C15—C201.514 (7)
N2—C141.479 (6)C15—C161.519 (6)
N2—C151.505 (6)C15—H15A0.9601
N2—H2A0.9000C16—C171.508 (8)
C1—C21.379 (7)C16—H16A0.9600
C1—C111.434 (7)C16—H16B0.9600
C1—C91.446 (6)C17—C181.505 (9)
C2—C31.414 (7)C17—H17A0.9601
C3—C41.365 (7)C17—H17B0.9600
C3—H3A0.9600C18—C191.498 (8)
C4—C101.418 (8)C18—H18A0.9600
C4—H4A0.9601C18—H18B0.9600
C5—C61.375 (9)C19—C201.517 (7)
C5—C101.428 (7)C19—H19A0.9600
C5—H5A0.9600C19—H19B0.9600
C6—C71.339 (9)C20—H20A0.9600
C6—H6A0.9599C20—H20B0.9600
O1—Co1—O1i180.0C8—C9—C1122.5 (5)
O1—Co1—N190.34 (15)C9—C10—C4120.1 (5)
O1i—Co1—N189.66 (15)C9—C10—C5119.9 (6)
O1—Co1—N1i89.66 (15)C4—C10—C5120.0 (6)
O1i—Co1—N1i90.34 (15)N1—C11—C1125.7 (4)
N1—Co1—N1i180.0N1—C11—H11A117.0
O1—Co1—N2i90.13 (15)C1—C11—H11A117.4
O1i—Co1—N2i89.87 (15)N1—C12—C13112.0 (4)
N1—Co1—N2i90.66 (15)N1—C12—H12A108.5
N1i—Co1—N2i89.34 (15)C13—C12—H12A110.3
O1—Co1—N289.87 (15)N1—C12—H12B109.4
O1i—Co1—N290.13 (15)C13—C12—H12B108.6
N1—Co1—N289.34 (15)H12A—C12—H12B107.9
N1i—Co1—N290.66 (15)C14—C13—C12115.2 (5)
N2i—Co1—N2180.0C14—C13—H13A107.4
O2—Cl1—O4110.2 (8)C12—C13—H13A107.7
O2—Cl1—O4ii108.4 (9)C14—C13—H13B109.5
O4—Cl1—O4ii103.7 (6)C12—C13—H13B109.1
O2—Cl1—O399.6 (10)H13A—C13—H13B107.7
O4—Cl1—O3122.8 (8)C13—C14—N2114.2 (4)
O4ii—Cl1—O3111.7 (7)C13—C14—H14A107.5
O2—Cl1—Cl1ii122.1 (10)N2—C14—H14A108.4
O4—Cl1—Cl1ii55.9 (5)C13—C14—H14B109.6
O4ii—Cl1—Cl1ii47.8 (4)N2—C14—H14B109.1
O3—Cl1—Cl1ii136.7 (6)H14A—C14—H14B107.8
C2—O1—Co1125.3 (3)N2—C15—C20114.8 (4)
Cl1—O4—Cl1ii76.3 (6)N2—C15—C16110.4 (4)
C11—N1—C12118.1 (4)C20—C15—C16110.8 (4)
C11—N1—Co1123.2 (3)N2—C15—H15A106.8
C12—N1—Co1118.6 (3)C20—C15—H15A106.8
C14—N2—C15115.2 (4)C16—C15—H15A106.8
C14—N2—Co1116.0 (3)C17—C16—C15109.4 (5)
C15—N2—Co1115.4 (3)C17—C16—H16A110.2
C14—N2—H2A102.5C15—C16—H16A110.0
C15—N2—H2A102.2C17—C16—H16B108.9
Co1—N2—H2A102.3C15—C16—H16B109.9
C2—C1—C11119.2 (4)H16A—C16—H16B108.4
C2—C1—C9120.0 (5)C18—C17—C16111.9 (5)
C11—C1—C9119.9 (4)C18—C17—H17A108.7
O1—C2—C1124.1 (4)C16—C17—H17A107.9
O1—C2—C3117.0 (4)C18—C17—H17B110.4
C1—C2—C3118.9 (4)C16—C17—H17B110.1
C4—C3—C2121.5 (5)H17A—C17—H17B107.8
C4—C3—H3A119.6C19—C18—C17111.5 (5)
C2—C3—H3A118.9C19—C18—H18A109.9
C3—C4—C10119.8 (5)C17—C18—H18A108.7
C3—C4—H4A120.5C19—C18—H18B109.4
C10—C4—H4A119.7C17—C18—H18B109.2
C6—C5—C10118.8 (6)H18A—C18—H18B108.2
C6—C5—H5A121.3C18—C19—C20112.4 (5)
C10—C5—H5A119.9C18—C19—H19A109.3
C7—C6—C5121.1 (6)C20—C19—H19A108.1
C7—C6—H6A119.6C18—C19—H19B109.6
C5—C6—H6A119.3C20—C19—H19B109.2
C6—C7—C8121.0 (7)H19A—C19—H19B108.1
C6—C7—H7A119.1C15—C20—C19108.4 (4)
C8—C7—H7A119.9C15—C20—H20A109.7
C7—C8—C9120.8 (6)C19—C20—H20A108.5
C7—C8—H8A120.5C15—C20—H20B110.2
C9—C8—H8A118.7C19—C20—H20B111.6
C10—C9—C8118.3 (5)H20A—C20—H20B108.3
C10—C9—C1119.1 (5)
N1—Co1—O1—C232.8 (3)C7—C8—C9—C1179.3 (5)
N1i—Co1—O1—C2147.2 (3)C2—C1—C9—C105.5 (7)
N2i—Co1—O1—C257.9 (3)C11—C1—C9—C10163.4 (4)
N2—Co1—O1—C2122.1 (3)C2—C1—C9—C8172.4 (5)
O2—Cl1—O4—Cl1ii115.8 (10)C11—C1—C9—C818.8 (7)
O4ii—Cl1—O4—Cl1ii0.0C8—C9—C10—C4178.6 (5)
O3—Cl1—O4—Cl1ii127.6 (7)C1—C9—C10—C40.7 (7)
O1—Co1—N1—C1128.4 (4)C8—C9—C10—C50.4 (7)
O1i—Co1—N1—C11151.6 (4)C1—C9—C10—C5178.3 (4)
N2i—Co1—N1—C1161.8 (4)C3—C4—C10—C93.9 (8)
N2—Co1—N1—C11118.2 (4)C3—C4—C10—C5175.1 (5)
O1—Co1—N1—C12149.1 (3)C6—C5—C10—C90.7 (8)
O1i—Co1—N1—C1230.9 (3)C6—C5—C10—C4179.7 (5)
N2i—Co1—N1—C12120.8 (3)C12—N1—C11—C1169.8 (4)
N2—Co1—N1—C1259.2 (3)Co1—N1—C11—C17.6 (6)
O1—Co1—N2—C1499.1 (4)C2—C1—C11—N121.2 (7)
O1i—Co1—N2—C1480.9 (4)C9—C1—C11—N1169.9 (4)
N1—Co1—N2—C148.8 (4)C11—N1—C12—C13125.6 (5)
N1i—Co1—N2—C14171.2 (4)Co1—N1—C12—C1351.9 (5)
O1—Co1—N2—C1540.0 (3)N1—C12—C13—C1415.8 (7)
O1i—Co1—N2—C15140.0 (3)C12—C13—C14—N268.1 (6)
N1—Co1—N2—C15130.4 (3)C15—N2—C14—C13174.1 (4)
N1i—Co1—N2—C1549.6 (3)Co1—N2—C14—C1346.6 (6)
Co1—O1—C2—C115.4 (6)C14—N2—C15—C2039.8 (6)
Co1—O1—C2—C3166.7 (3)Co1—N2—C15—C2099.7 (4)
C11—C1—C2—O117.2 (7)C14—N2—C15—C1686.2 (5)
C9—C1—C2—O1173.9 (4)Co1—N2—C15—C16134.3 (4)
C11—C1—C2—C3160.6 (4)N2—C15—C16—C17172.0 (4)
C9—C1—C2—C38.3 (7)C20—C15—C16—C1759.7 (6)
O1—C2—C3—C4176.9 (4)C15—C16—C17—C1856.0 (7)
C1—C2—C3—C45.1 (7)C16—C17—C18—C1953.6 (7)
C2—C3—C4—C101.0 (8)C17—C18—C19—C2054.2 (7)
C10—C5—C6—C70.7 (9)N2—C15—C20—C19174.6 (4)
C5—C6—C7—C80.3 (10)C16—C15—C20—C1959.5 (6)
C6—C7—C8—C91.4 (9)C18—C19—C20—C1556.8 (6)
C7—C8—C9—C101.4 (8)
Symmetry codes: (i) x, y, z; (ii) x, y1, z+1.
 

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