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The title compound, [Co(C15H35N5)](ClO4)2, conventionally abbreviated [Co(Me5PACP)](ClO4)2, where Me5PACP is 1,4,7,10,13-penta­methyl-1,4,7,10,13-penta­aza­cyclo­penta­dec­ane, displays a significantly distorted trigonal–bipyramidal coordination geometry. The bond lengths and distances are comparable to those previously reported for cobalt(II) complexes with macrocyclic poly­amine ligands. The N—Co—N angle for the axial sites is 160.4 (2)°. The perchlorate anions are not coordinated.

Supporting information

cif

Crystallographic Information File (CIF) https://doi.org/10.1107/S1600536803025030/cf6283sup1.cif
Contains datablocks I, global

hkl

Structure factor file (CIF format) https://doi.org/10.1107/S1600536803025030/cf6283Isup2.hkl
Contains datablock I

CCDC reference: 227739

Key indicators

  • Single-crystal X-ray study
  • T = 293 K
  • R factor = 0.052
  • wR factor = 0.061
  • Data-to-parameter ratio = 8.2

checkCIF/PLATON results

No syntax errors found



Alert level A PLAT027_ALERT_3_A _diffrn_reflns_theta_full too Low .............. 0.00 Deg. PLAT029_ALERT_3_A _diffrn_measured_fraction_theta_full Low ....... 0.00 PLAT037_ALERT_1_A _diffrn_reflns_theta_full .......... Not Given . ? PLAT038_ALERT_1_A _diffrn_measured_fraction_theta_max Not Given . ? PLAT039_ALERT_1_A _diffrn_measured_fraction_theta_full Not Given . ? PLAT761_ALERT_1_A CIF Contains no X-H Bonds ...................... ? PLAT762_ALERT_1_A CIF Contains no X-Y-H or H-Y-H Angles .......... ?
Alert level C REFNR01_ALERT_3_C Ratio of reflections to parameters is < 10 for a centrosymmetric structure sine(theta)/lambda 0.5944 Proportion of unique data used 0.5515 Ratio reflections to parameters 8.2036 PLAT042_ALERT_1_C Calc. and Rep. MoietyFormula Strings Differ .... ? PLAT088_ALERT_3_C Poor Data / Parameter Ratio .................... 8.20 PLAT150_ALERT_1_C Volume as Calculated Differs from that Given = 2437.00 Ang-3 PLAT241_ALERT_2_C Check High U(eq) as Compared to Neighbors .... C2 PLAT244_ALERT_4_C Low Solvent U(eq) as Compared to Neighbors .... Cl1 PLAT244_ALERT_4_C Low Solvent U(eq) as Compared to Neighbors .... Cl2 PLAT341_ALERT_3_C Low Bond Precision on C-C bonds (x 1000) Ang ... 11
7 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 7 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 5 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: MSC/AFC Diffractometer Control Software (Molecular Structure Corporation, 1989); cell refinement: MSC/AFC Diffractometer Control Software; data reduction: TEXSAN (Molecular Structure Corporation, 1989); program(s) used to solve structure: SHELXS86 (Sheldrick, 1985); program(s) used to refine structure: TEXSAN; molecular graphics: ORTEPII (Johnson, 1976); software used to prepare material for publication: TEXSAN.

(I) top
Crystal data top
[Co(C15H35N5)](ClO4)2F(000) = 1140.00
Mr = 543.31Dx = 1.480 Mg m3
Monoclinic, P21/nMo Kα radiation, λ = 0.7107 Å
Hall symbol: -P 2ynCell parameters from 20 reflections
a = 9.451 (2) Åθ = 13.7–21.1°
b = 15.294 (4) ŵ = 0.97 mm1
c = 17.049 (4) ÅT = 293 K
β = 98.47 (2)°Prism, red
V = 2437.0 (10) Å30.30 × 0.20 × 0.20 mm
Z = 4.0
Data collection top
Rigaku AFC-7R
diffractometer
2297 reflections with I > 3σ(I)
Radiation source: X-ray tubeRint = 0.031
Graphite monochromatorθmax = 25.0°, θmin = 6.0°
ω/2θ scansh = 010
Absorption correction: ψ scan
(TEXSAN; Molecular Structure Corporation, 1989)
k = 018
Tmin = 0.79, Tmax = 0.82l = 2020
4450 measured reflections3 standard reflections every 200 reflections
4165 independent reflections intensity decay: 2.9%
Refinement top
Refinement on F0 restraints
Least-squares matrix: fullH-atom parameters not refined
R[F2 > 2σ(F2)] = 0.052Weighting scheme based on measured s.u.'s w = 1/[σ2(Fo)]
wR(F2) = 0.061(Δ/σ)max = 0.005
S = 1.75Δρmax = 0.70 e Å3
2297 reflectionsΔρmin = 0.37 e Å3
280 parameters
Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top
xyzUiso*/Ueq
Co0.26413 (9)0.22704 (5)0.41065 (5)0.0373
Cl10.7445 (2)0.1772 (1)0.5787 (1)0.0571
Cl20.2845 (2)0.0170 (1)0.7889 (1)0.0639
O10.8092 (7)0.2540 (4)0.5575 (5)0.1081
O20.6774 (7)0.1331 (4)0.5102 (3)0.1057
O30.6424 (6)0.1961 (4)0.6293 (3)0.0965
O40.8538 (7)0.1219 (5)0.6178 (4)0.1019
O50.4309 (9)0.0152 (6)0.8169 (5)0.1595
O60.204 (1)0.0163 (6)0.8491 (5)0.1899
O70.254 (1)0.0902 (5)0.7459 (5)0.1821
O80.2613 (8)0.0579 (5)0.7431 (6)0.1682
N10.3516 (6)0.1456 (3)0.3213 (3)0.0461
N20.4157 (6)0.3142 (4)0.3766 (3)0.0530
N30.2420 (7)0.3355 (3)0.4952 (3)0.0527
N40.2197 (5)0.1485 (3)0.5088 (3)0.0418
N50.0689 (6)0.1782 (4)0.3532 (3)0.0494
C10.4590 (9)0.1985 (5)0.2858 (5)0.0627
C20.5289 (9)0.2622 (5)0.3452 (5)0.0739
C30.4769 (9)0.3588 (5)0.4514 (5)0.0737
C40.359 (1)0.4000 (5)0.4888 (5)0.0743
C50.2702 (8)0.2904 (5)0.5726 (4)0.0567
C60.1815 (8)0.2085 (4)0.5708 (4)0.0541
C70.0955 (8)0.0940 (5)0.4785 (5)0.0583
C80.0064 (8)0.1421 (5)0.4169 (5)0.0637
C90.0993 (8)0.1079 (5)0.2969 (5)0.0659
C100.2283 (9)0.1279 (5)0.2607 (5)0.0648
C110.4180 (8)0.0632 (5)0.3531 (5)0.0626
C120.352 (1)0.3781 (5)0.3168 (5)0.0821
C130.1053 (10)0.3818 (5)0.4893 (5)0.0733
C140.3356 (8)0.0901 (5)0.5454 (4)0.0623
C150.0212 (9)0.2460 (5)0.3082 (5)0.0749
H10.41380.23050.24190.0715*
H20.52940.16050.26930.0715*
H30.58570.22940.38980.0873*
H40.59600.29800.32380.0715*
H50.52540.31700.48760.0715*
H60.54410.40230.44100.0715*
H70.31750.44750.45470.0734*
H80.39310.42310.53890.0715*
H90.36930.27530.58370.0715*
H100.24780.32830.61350.0715*
H110.19630.18030.62050.0715*
H120.08210.22360.55790.0715*
H130.04540.07870.52180.0715*
H140.12550.04270.45550.0715*
H150.04980.18960.44230.0715*
H160.08110.10360.39470.0715*
H170.11360.05430.32520.0715*
H180.01920.10220.25630.0715*
H190.24980.08010.22900.0715*
H200.21050.17860.22780.0715*
H210.45870.03280.31350.0715*
H220.35100.02750.37380.0715*
H230.49480.07670.39600.0946*
H240.26050.39820.33090.0715*
H250.41100.42770.31530.0715*
H260.33260.35220.26600.0715*
H270.11010.42470.52960.0715*
H280.08530.40900.43870.0715*
H290.03110.34120.49510.0715*
H300.41430.12420.57070.0715*
H310.36790.05460.50570.0715*
H320.30210.05370.58390.0715*
H330.03870.29320.34070.0715*
H340.03530.27120.26770.0883*
H350.10460.22350.28000.0715*
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
Co0.0477 (5)0.0263 (4)0.0373 (5)0.0046 (5)0.0044 (4)0.0012 (4)
Cl10.059 (1)0.061 (1)0.051 (1)0.006 (1)0.0087 (9)0.0080 (10)
Cl20.084 (2)0.052 (1)0.060 (1)0.008 (1)0.025 (1)0.003 (1)
O10.105 (5)0.063 (4)0.162 (7)0.014 (4)0.037 (5)0.005 (4)
O20.128 (5)0.128 (6)0.056 (4)0.036 (5)0.001 (4)0.036 (4)
O30.065 (4)0.136 (6)0.094 (5)0.006 (4)0.029 (3)0.048 (4)
O40.095 (5)0.124 (6)0.087 (5)0.037 (4)0.014 (4)0.017 (4)
O50.112 (7)0.205 (9)0.152 (8)0.012 (6)0.011 (6)0.078 (7)
O60.26 (1)0.204 (9)0.141 (7)0.151 (8)0.144 (8)0.099 (7)
O70.32 (1)0.118 (7)0.116 (6)0.064 (8)0.073 (7)0.070 (6)
O80.105 (6)0.125 (6)0.28 (1)0.024 (5)0.042 (6)0.122 (7)
N10.050 (4)0.038 (3)0.051 (4)0.001 (3)0.010 (3)0.002 (3)
N20.073 (4)0.034 (3)0.054 (4)0.011 (3)0.015 (3)0.004 (3)
N30.077 (5)0.036 (3)0.047 (4)0.006 (3)0.014 (3)0.005 (3)
N40.041 (3)0.034 (3)0.052 (3)0.005 (3)0.013 (3)0.005 (3)
N50.049 (4)0.048 (4)0.050 (4)0.002 (3)0.003 (3)0.006 (3)
C10.079 (6)0.054 (5)0.061 (5)0.000 (4)0.033 (4)0.003 (4)
C20.082 (6)0.061 (5)0.088 (6)0.021 (5)0.042 (5)0.004 (5)
C30.090 (6)0.064 (5)0.067 (6)0.040 (5)0.010 (5)0.003 (4)
C40.115 (7)0.052 (5)0.059 (5)0.030 (5)0.023 (5)0.016 (4)
C50.078 (6)0.050 (5)0.043 (4)0.007 (4)0.008 (4)0.005 (3)
C60.072 (5)0.046 (5)0.048 (4)0.003 (4)0.020 (4)0.005 (3)
C70.064 (5)0.049 (5)0.064 (5)0.019 (4)0.016 (4)0.002 (4)
C80.047 (5)0.061 (5)0.083 (6)0.014 (4)0.011 (4)0.012 (5)
C90.066 (5)0.062 (5)0.065 (5)0.004 (4)0.005 (4)0.024 (4)
C100.076 (6)0.062 (5)0.056 (5)0.002 (4)0.012 (4)0.015 (4)
C110.078 (6)0.044 (4)0.071 (5)0.018 (4)0.025 (4)0.004 (4)
C120.118 (8)0.051 (5)0.079 (6)0.009 (5)0.017 (5)0.010 (5)
C130.099 (7)0.048 (5)0.074 (6)0.012 (5)0.016 (5)0.004 (4)
C140.070 (5)0.061 (5)0.057 (5)0.019 (4)0.015 (4)0.017 (4)
C150.077 (6)0.068 (6)0.069 (5)0.020 (4)0.024 (5)0.010 (4)
Geometric parameters (Å, º) top
Co—N12.220 (5)N2—C31.486 (9)
Co—N22.101 (5)N2—C121.476 (10)
Co—N32.228 (5)N3—C41.495 (9)
Co—N42.151 (5)N3—C51.477 (8)
Co—N52.095 (5)N3—C131.464 (9)
Cl(1)—O(1)1.396 (6)N4—C61.483 (8)
Cl(1)—O(2)1.414 (5)N4—C71.470 (8)
Cl(1)—O(3)1.416 (5)N4—C141.479 (8)
Cl(1)—O(4)1.423 (6)N5—C81.489 (9)
Cl(2)—O(5)1.397 (8)N5—C91.497 (9)
Cl(2)—O(6)1.363 (7)N5—C151.482 (9)
Cl(2)—O(7)1.346 (7)C(1)—C(2)1.49 (1)
Cl(2)—O(8)1.384 (7)C(3)—C(4)1.51 (1)
N1—C11.493 (9)C(5)—C(6)1.505 (9)
N1—C101.464 (9)C(7)—C(8)1.51 (1)
N1—C111.474 (8)C(9)—C(10)1.48 (1)
N2—C21.494 (9)
N1—Co—N280.1 (2)C(2)—N(2)—C(3)110.0 (6)
N1—Co—N3160.4 (2)C(2)—N(2)—C(12)110.3 (6)
N1—Co—N4110.9 (2)C(3)—N(2)—C(12)111.0 (6)
N1—Co—N582.6 (2)Co—N(3)—C(4)107.7 (4)
N2—Co—N380.7 (2)Co—N(3)—C(5)102.1 (4)
N2—Co—N4142.1 (2)Co—N(3)—C(13)118.8 (5)
N2—Co—N5133.4 (2)C(4)—N(3)—C(5)109.6 (6)
N3—Co—N482.2 (2)C(4)—N(3)—C(13)109.1 (6)
N3—Co—N5114.1 (2)C(5)—N(3)—C(13)109.2 (6)
N4—Co—N584.6 (2)Co—N(4)—C(6)107.8 (4)
O(1)—Cl(1)—O(2)110.3 (4)Co—N(4)—C(7)106.3 (4)
O(1)—Cl(1)—O(3)110.5 (4)Co—N(4)—C(14)116.6 (4)
O(1)—Cl(1)—O(4)107.8 (4)C(6)—N(4)—C(7)109.6 (5)
O(2)—Cl(1)—O(3)109.7 (4)C(6)—N(4)—C(14)108.5 (5)
O(2)—Cl(1)—O(4)108.0 (4)C(7)—N(4)—C(14)108.0 (6)
O(3)—Cl(1)—O(4)110.4 (4)Co—N(5)—C(8)105.9 (4)
O(5)—Cl(2)—O(6)112.0 (6)Co—N(5)—C(9)108.5 (4)
O(5)—Cl(2)—O(7)108.8 (7)Co—N(5)—C(15)113.0 (4)
O(5)—Cl(2)—O(8)104.1 (5)C(8)—N(5)—C(9)111.1 (6)
O(6)—Cl(2)—O(7)108.7 (5)C(8)—N(5)—C(15)109.7 (6)
O(6)—Cl(2)—O(8)111.1 (6)C(9)—N(5)—C(15)108.6 (6)
O(7)—Cl(2)—O(8)112.2 (6)N(1)—C(1)—C(2)109.9 (6)
Co—N(1)—C(1)108.5 (4)N(2)—C(2)—C(1)108.8 (6)
Co—N(1)—C(10)104.4 (4)N(2)—C(3)—C(4)109.6 (7)
Co—N(1)—C(11)114.1 (4)N(3)—C(4)—C(3)110.8 (6)
C(1)—N(1)—C(10)109.4 (6)N(3)—C(5)—C(6)110.1 (6)
C(1)—N(1)—C(11)109.5 (6)N(4)—C(6)—C(5)109.7 (5)
C(10)—N(1)—C(11)110.7 (6)N(4)—C(7)—C(8)111.3 (6)
Co—N(2)—C(2)108.3 (4)N(5)—C(8)—C(7)111.3 (6)
Co—N(2)—C(3)104.4 (4)N(5)—C(9)—C(10)111.6 (6)
Co—N(2)—C(12)112.6 (5)N(1)—C(10)—C(9)111.4 (6)
 

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