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
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.
[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 |
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 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 |
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* |
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) |
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) |
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