metal-organic compounds
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
Crystallographic Information File (CIF) https://doi.org/10.1107/S1600536803025030/cf6283sup1.cif | |
Structure factor file (CIF format) https://doi.org/10.1107/S1600536803025030/cf6283Isup2.hkl |
CCDC reference: 227739
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)2 | F(000) = 1140.00 |
Mr = 543.31 | Dx = 1.480 Mg m−3 |
Monoclinic, P21/n | Mo Kα radiation, λ = 0.7107 Å |
Hall symbol: -P 2yn | Cell parameters from 20 reflections |
a = 9.451 (2) Å | θ = 13.7–21.1° |
b = 15.294 (4) Å | µ = 0.97 mm−1 |
c = 17.049 (4) Å | T = 293 K |
β = 98.47 (2)° | Prism, red |
V = 2437.0 (10) Å3 | 0.30 × 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 tube | Rint = 0.031 |
Graphite monochromator | θmax = 25.0°, θmin = 6.0° |
ω/2θ scans | h = 0→10 |
Absorption correction: ψ scan (TEXSAN; Molecular Structure Corporation, 1989) | k = 0→18 |
Tmin = 0.79, Tmax = 0.82 | l = −20→20 |
4450 measured reflections | 3 standard reflections every 200 reflections |
4165 independent reflections | intensity decay: 2.9% |
Refinement top
Refinement on F | 0 restraints |
Least-squares matrix: full | H-atom parameters not refined |
R[F2 > 2σ(F2)] = 0.052 | Weighting scheme based on measured s.u.'s w = 1/[σ2(Fo)] |
wR(F2) = 0.061 | (Δ/σ)max = 0.005 |
S = 1.75 | Δρmax = 0.70 e Å−3 |
2297 reflections | Δρmin = −0.37 e Å−3 |
280 parameters |
Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top
x | y | z | Uiso*/Ueq | ||
Co | 0.26413 (9) | 0.22704 (5) | 0.41065 (5) | 0.0373 | |
Cl1 | 0.7445 (2) | 0.1772 (1) | 0.5787 (1) | 0.0571 | |
Cl2 | 0.2845 (2) | 0.0170 (1) | 0.7889 (1) | 0.0639 | |
O1 | 0.8092 (7) | 0.2540 (4) | 0.5575 (5) | 0.1081 | |
O2 | 0.6774 (7) | 0.1331 (4) | 0.5102 (3) | 0.1057 | |
O3 | 0.6424 (6) | 0.1961 (4) | 0.6293 (3) | 0.0965 | |
O4 | 0.8538 (7) | 0.1219 (5) | 0.6178 (4) | 0.1019 | |
O5 | 0.4309 (9) | 0.0152 (6) | 0.8169 (5) | 0.1595 | |
O6 | 0.204 (1) | 0.0163 (6) | 0.8491 (5) | 0.1899 | |
O7 | 0.254 (1) | 0.0902 (5) | 0.7459 (5) | 0.1821 | |
O8 | 0.2613 (8) | −0.0579 (5) | 0.7431 (6) | 0.1682 | |
N1 | 0.3516 (6) | 0.1456 (3) | 0.3213 (3) | 0.0461 | |
N2 | 0.4157 (6) | 0.3142 (4) | 0.3766 (3) | 0.0530 | |
N3 | 0.2420 (7) | 0.3355 (3) | 0.4952 (3) | 0.0527 | |
N4 | 0.2197 (5) | 0.1485 (3) | 0.5088 (3) | 0.0418 | |
N5 | 0.0689 (6) | 0.1782 (4) | 0.3532 (3) | 0.0494 | |
C1 | 0.4590 (9) | 0.1985 (5) | 0.2858 (5) | 0.0627 | |
C2 | 0.5289 (9) | 0.2622 (5) | 0.3452 (5) | 0.0739 | |
C3 | 0.4769 (9) | 0.3588 (5) | 0.4514 (5) | 0.0737 | |
C4 | 0.359 (1) | 0.4000 (5) | 0.4888 (5) | 0.0743 | |
C5 | 0.2702 (8) | 0.2904 (5) | 0.5726 (4) | 0.0567 | |
C6 | 0.1815 (8) | 0.2085 (4) | 0.5708 (4) | 0.0541 | |
C7 | 0.0955 (8) | 0.0940 (5) | 0.4785 (5) | 0.0583 | |
C8 | −0.0064 (8) | 0.1421 (5) | 0.4169 (5) | 0.0637 | |
C9 | 0.0993 (8) | 0.1079 (5) | 0.2969 (5) | 0.0659 | |
C10 | 0.2283 (9) | 0.1279 (5) | 0.2607 (5) | 0.0648 | |
C11 | 0.4180 (8) | 0.0632 (5) | 0.3531 (5) | 0.0626 | |
C12 | 0.352 (1) | 0.3781 (5) | 0.3168 (5) | 0.0821 | |
C13 | 0.1053 (10) | 0.3818 (5) | 0.4893 (5) | 0.0733 | |
C14 | 0.3356 (8) | 0.0901 (5) | 0.5454 (4) | 0.0623 | |
C15 | −0.0212 (9) | 0.2460 (5) | 0.3082 (5) | 0.0749 | |
H1 | 0.4138 | 0.2305 | 0.2419 | 0.0715* | |
H2 | 0.5294 | 0.1605 | 0.2693 | 0.0715* | |
H3 | 0.5857 | 0.2294 | 0.3898 | 0.0873* | |
H4 | 0.5960 | 0.2980 | 0.3238 | 0.0715* | |
H5 | 0.5254 | 0.3170 | 0.4876 | 0.0715* | |
H6 | 0.5441 | 0.4023 | 0.4410 | 0.0715* | |
H7 | 0.3175 | 0.4475 | 0.4547 | 0.0734* | |
H8 | 0.3931 | 0.4231 | 0.5389 | 0.0715* | |
H9 | 0.3693 | 0.2753 | 0.5837 | 0.0715* | |
H10 | 0.2478 | 0.3283 | 0.6135 | 0.0715* | |
H11 | 0.1963 | 0.1803 | 0.6205 | 0.0715* | |
H12 | 0.0821 | 0.2236 | 0.5579 | 0.0715* | |
H13 | 0.0454 | 0.0787 | 0.5218 | 0.0715* | |
H14 | 0.1255 | 0.0427 | 0.4555 | 0.0715* | |
H15 | −0.0498 | 0.1896 | 0.4423 | 0.0715* | |
H16 | −0.0811 | 0.1036 | 0.3947 | 0.0715* | |
H17 | 0.1136 | 0.0543 | 0.3252 | 0.0715* | |
H18 | 0.0192 | 0.1022 | 0.2563 | 0.0715* | |
H19 | 0.2498 | 0.0801 | 0.2290 | 0.0715* | |
H20 | 0.2105 | 0.1786 | 0.2278 | 0.0715* | |
H21 | 0.4587 | 0.0328 | 0.3135 | 0.0715* | |
H22 | 0.3510 | 0.0275 | 0.3738 | 0.0715* | |
H23 | 0.4948 | 0.0767 | 0.3960 | 0.0946* | |
H24 | 0.2605 | 0.3982 | 0.3309 | 0.0715* | |
H25 | 0.4110 | 0.4277 | 0.3153 | 0.0715* | |
H26 | 0.3326 | 0.3522 | 0.2660 | 0.0715* | |
H27 | 0.1101 | 0.4247 | 0.5296 | 0.0715* | |
H28 | 0.0853 | 0.4090 | 0.4387 | 0.0715* | |
H29 | 0.0311 | 0.3412 | 0.4951 | 0.0715* | |
H30 | 0.4143 | 0.1242 | 0.5707 | 0.0715* | |
H31 | 0.3679 | 0.0546 | 0.5057 | 0.0715* | |
H32 | 0.3021 | 0.0537 | 0.5839 | 0.0715* | |
H33 | −0.0387 | 0.2932 | 0.3407 | 0.0715* | |
H34 | 0.0353 | 0.2712 | 0.2677 | 0.0883* | |
H35 | −0.1046 | 0.2235 | 0.2800 | 0.0715* |
Atomic displacement parameters (Å2) top
U11 | U22 | U33 | U12 | U13 | U23 | |
Co | 0.0477 (5) | 0.0263 (4) | 0.0373 (5) | −0.0046 (5) | 0.0044 (4) | 0.0012 (4) |
Cl1 | 0.059 (1) | 0.061 (1) | 0.051 (1) | −0.006 (1) | 0.0087 (9) | −0.0080 (10) |
Cl2 | 0.084 (2) | 0.052 (1) | 0.060 (1) | 0.008 (1) | 0.025 (1) | 0.003 (1) |
O1 | 0.105 (5) | 0.063 (4) | 0.162 (7) | −0.014 (4) | 0.037 (5) | 0.005 (4) |
O2 | 0.128 (5) | 0.128 (6) | 0.056 (4) | −0.036 (5) | 0.001 (4) | −0.036 (4) |
O3 | 0.065 (4) | 0.136 (6) | 0.094 (5) | −0.006 (4) | 0.029 (3) | −0.048 (4) |
O4 | 0.095 (5) | 0.124 (6) | 0.087 (5) | 0.037 (4) | 0.014 (4) | 0.017 (4) |
O5 | 0.112 (7) | 0.205 (9) | 0.152 (8) | −0.012 (6) | −0.011 (6) | −0.078 (7) |
O6 | 0.26 (1) | 0.204 (9) | 0.141 (7) | 0.151 (8) | 0.144 (8) | 0.099 (7) |
O7 | 0.32 (1) | 0.118 (7) | 0.116 (6) | 0.064 (8) | 0.073 (7) | 0.070 (6) |
O8 | 0.105 (6) | 0.125 (6) | 0.28 (1) | −0.024 (5) | 0.042 (6) | −0.122 (7) |
N1 | 0.050 (4) | 0.038 (3) | 0.051 (4) | 0.001 (3) | 0.010 (3) | −0.002 (3) |
N2 | 0.073 (4) | 0.034 (3) | 0.054 (4) | −0.011 (3) | 0.015 (3) | 0.004 (3) |
N3 | 0.077 (5) | 0.036 (3) | 0.047 (4) | −0.006 (3) | 0.014 (3) | −0.005 (3) |
N4 | 0.041 (3) | 0.034 (3) | 0.052 (3) | −0.005 (3) | 0.013 (3) | 0.005 (3) |
N5 | 0.049 (4) | 0.048 (4) | 0.050 (4) | 0.002 (3) | 0.003 (3) | −0.006 (3) |
C1 | 0.079 (6) | 0.054 (5) | 0.061 (5) | 0.000 (4) | 0.033 (4) | 0.003 (4) |
C2 | 0.082 (6) | 0.061 (5) | 0.088 (6) | −0.021 (5) | 0.042 (5) | 0.004 (5) |
C3 | 0.090 (6) | 0.064 (5) | 0.067 (6) | −0.040 (5) | 0.010 (5) | −0.003 (4) |
C4 | 0.115 (7) | 0.052 (5) | 0.059 (5) | −0.030 (5) | 0.023 (5) | −0.016 (4) |
C5 | 0.078 (6) | 0.050 (5) | 0.043 (4) | −0.007 (4) | 0.008 (4) | −0.005 (3) |
C6 | 0.072 (5) | 0.046 (5) | 0.048 (4) | 0.003 (4) | 0.020 (4) | 0.005 (3) |
C7 | 0.064 (5) | 0.049 (5) | 0.064 (5) | −0.019 (4) | 0.016 (4) | −0.002 (4) |
C8 | 0.047 (5) | 0.061 (5) | 0.083 (6) | −0.014 (4) | 0.011 (4) | −0.012 (5) |
C9 | 0.066 (5) | 0.062 (5) | 0.065 (5) | −0.004 (4) | −0.005 (4) | −0.024 (4) |
C10 | 0.076 (6) | 0.062 (5) | 0.056 (5) | −0.002 (4) | 0.012 (4) | −0.015 (4) |
C11 | 0.078 (6) | 0.044 (4) | 0.071 (5) | 0.018 (4) | 0.025 (4) | 0.004 (4) |
C12 | 0.118 (8) | 0.051 (5) | 0.079 (6) | −0.009 (5) | 0.017 (5) | 0.010 (5) |
C13 | 0.099 (7) | 0.048 (5) | 0.074 (6) | 0.012 (5) | 0.016 (5) | −0.004 (4) |
C14 | 0.070 (5) | 0.061 (5) | 0.057 (5) | 0.019 (4) | 0.015 (4) | 0.017 (4) |
C15 | 0.077 (6) | 0.068 (6) | 0.069 (5) | 0.020 (4) | −0.024 (5) | −0.010 (4) |
Geometric parameters (Å, º) top
Co—N1 | 2.220 (5) | N2—C3 | 1.486 (9) |
Co—N2 | 2.101 (5) | N2—C12 | 1.476 (10) |
Co—N3 | 2.228 (5) | N3—C4 | 1.495 (9) |
Co—N4 | 2.151 (5) | N3—C5 | 1.477 (8) |
Co—N5 | 2.095 (5) | N3—C13 | 1.464 (9) |
Cl(1)—O(1) | 1.396 (6) | N4—C6 | 1.483 (8) |
Cl(1)—O(2) | 1.414 (5) | N4—C7 | 1.470 (8) |
Cl(1)—O(3) | 1.416 (5) | N4—C14 | 1.479 (8) |
Cl(1)—O(4) | 1.423 (6) | N5—C8 | 1.489 (9) |
Cl(2)—O(5) | 1.397 (8) | N5—C9 | 1.497 (9) |
Cl(2)—O(6) | 1.363 (7) | N5—C15 | 1.482 (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—C1 | 1.493 (9) | C(5)—C(6) | 1.505 (9) |
N1—C10 | 1.464 (9) | C(7)—C(8) | 1.51 (1) |
N1—C11 | 1.474 (8) | C(9)—C(10) | 1.48 (1) |
N2—C2 | 1.494 (9) | ||
N1—Co—N2 | 80.1 (2) | C(2)—N(2)—C(3) | 110.0 (6) |
N1—Co—N3 | 160.4 (2) | C(2)—N(2)—C(12) | 110.3 (6) |
N1—Co—N4 | 110.9 (2) | C(3)—N(2)—C(12) | 111.0 (6) |
N1—Co—N5 | 82.6 (2) | Co—N(3)—C(4) | 107.7 (4) |
N2—Co—N3 | 80.7 (2) | Co—N(3)—C(5) | 102.1 (4) |
N2—Co—N4 | 142.1 (2) | Co—N(3)—C(13) | 118.8 (5) |
N2—Co—N5 | 133.4 (2) | C(4)—N(3)—C(5) | 109.6 (6) |
N3—Co—N4 | 82.2 (2) | C(4)—N(3)—C(13) | 109.1 (6) |
N3—Co—N5 | 114.1 (2) | C(5)—N(3)—C(13) | 109.2 (6) |
N4—Co—N5 | 84.6 (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) |