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
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)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) |