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In the title compound, [Co(C20H25N2O)2]ClO4, there are two independent centrosymmetric molecules of the cation, in which the central CoIII atoms are six-coordinated by four N atoms and two O atoms from two Schiff bases, giving approximately octahedral coordination environments.
Supporting information
CCDC reference: 245154
Key indicators
- Single-crystal X-ray study
- T = 293 K
- Mean (C-C) = 0.009 Å
- R factor = 0.105
- wR factor = 0.231
- Data-to-parameter ratio = 14.9
checkCIF/PLATON results
No syntax errors found
Alert level A
PLAT241_ALERT_2_A Check High U(eq) as Compared to Neighbors .... O3
| Author Response: The atom O3 belongs to a disordered perchlorate anion.
Large displacement parameters are quite usual for these types of
molecules, especially when disordered.
|
PLAT241_ALERT_2_A Check High U(eq) as Compared to Neighbors .... O4A
| Author Response: The atom O3 belongs to a disordered perchlorate anion.
Large displacement parameters are quite usual for these types of
molecules, especially when disordered.
|
PLAT241_ALERT_2_A Check High U(eq) as Compared to Neighbors .... O5
| Author Response: The atom O3 belongs to a disordered perchlorate anion.
Large displacement parameters are quite usual for these types of
molecules, especially when disordered.
|
PLAT241_ALERT_2_A Check High U(eq) as Compared to Neighbors .... O6
| Author Response: The atom O3 belongs to a disordered perchlorate anion.
Large displacement parameters are quite usual for these types of
molecules, especially when disordered.
|
PLAT242_ALERT_2_A Check Low U(eq) as Compared to Neighbors .... Cl1
| Author Response: (see above) The atom Cl1 belongs to the disordered perchlorate
anion.
|
Other Alerts are generated by the CheckCIF routine because of this
feature.
PLAT242_ALERT_2_A Check Low U(eq) as Compared to Neighbors .... Cl1A
| Author Response: (see above) The atom Cl1 belongs to the disordered perchlorate
anion.
|
Other Alerts are generated by the CheckCIF routine because of this
feature.
Alert level B
PLAT241_ALERT_2_B Check High U(eq) as Compared to Neighbors .... O5A
| Author Response: The atom O3 belongs to a disordered perchlorate anion.
Large displacement parameters are quite usual for these types of
molecules, especially when disordered.
|
Alert level C
RFACG01_ALERT_3_C The value of the R factor is > 0.10
R factor given 0.105
PLAT029_ALERT_3_C _diffrn_measured_fraction_theta_full Low ....... 0.98
PLAT042_ALERT_1_C Calc. and Rep. MoietyFormula Strings Differ .... ?
PLAT094_ALERT_2_C Ratio of Maximum / Minimum Residual Density .... 3.63
PLAT215_ALERT_3_C Disordered O4A has ADP max/min Ratio ....... 3.50
PLAT220_ALERT_2_C Large Non-Solvent C Ueq(max)/Ueq(min) ... 2.74 Ratio
PLAT241_ALERT_2_C Check High U(eq) as Compared to Neighbors .... C18
| Author Response: The atom O3 belongs to a disordered perchlorate anion.
Large displacement parameters are quite usual for these types of
molecules, especially when disordered.
|
PLAT241_ALERT_2_C Check High U(eq) as Compared to Neighbors .... C33
| Author Response: The atom O3 belongs to a disordered perchlorate anion.
Large displacement parameters are quite usual for these types of
molecules, especially when disordered.
|
PLAT242_ALERT_2_C Check Low U(eq) as Compared to Neighbors .... C35
| Author Response: (see above) The atom Cl1 belongs to the disordered perchlorate
anion.
|
Other Alerts are generated by the CheckCIF routine because of this
feature.
PLAT242_ALERT_2_C Check Low U(eq) as Compared to Neighbors .... O3A
| Author Response: (see above) The atom Cl1 belongs to the disordered perchlorate
anion.
|
Other Alerts are generated by the CheckCIF routine because of this
feature.
PLAT242_ALERT_2_C Check Low U(eq) as Compared to Neighbors .... O6A
| Author Response: (see above) The atom Cl1 belongs to the disordered perchlorate
anion.
|
Other Alerts are generated by the CheckCIF routine because of this
feature.
PLAT301_ALERT_3_C Main Residue Disorder ......................... 5.00 Perc.
PLAT313_ALERT_2_C Oxygen with three covalent bonds (rare) ........ O3
PLAT313_ALERT_2_C Oxygen with three covalent bonds (rare) ........ O5A
PLAT341_ALERT_3_C Low Bond Precision on C-C bonds (x 1000) Ang ... 9
PLAT420_ALERT_2_C D-H Without Acceptor N2 - H2 ... ?
PLAT420_ALERT_2_C D-H Without Acceptor N4 - H4 ... ?
6 ALERT level A = In general: serious problem
1 ALERT level B = Potentially serious problem
17 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
18 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
0 ALERT type 4 Improvement, methodology, query or suggestion
Data collection: SMART (Siemens, 1996); cell refinement: SAINT; 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{1-[3-(cyclohexylamino)propyliminomethyl]-2-naphtholato-
κ3O,
N,
N'}cobalt(III) perchlorate
top
Crystal data top
[Co(C20H25N2O)2]ClO4 | F(000) = 1640 |
Mr = 777.22 | Dx = 1.354 Mg m−3 |
Monoclinic, P21/n | Mo Kα radiation, λ = 0.71073 Å |
Hall symbol: -P 2yn | Cell parameters from 3603 reflections |
a = 12.167 (2) Å | θ = 2.2–18.5° |
b = 17.195 (2) Å | µ = 0.57 mm−1 |
c = 19.128 (2) Å | T = 293 K |
β = 107.640 (2)° | Block, brown |
V = 3813.6 (9) Å3 | 0.28 × 0.22 × 0.17 mm |
Z = 4 | |
Data collection top
Bruker SMART CCD diffractometer | 7707 independent reflections |
Radiation source: fine-focus sealed tube | 5356 reflections with I > 2σ(I) |
Graphite monochromator | Rint = 0.088 |
ω scans | θmax = 26.5°, θmin = 2.1° |
Absorption correction: multi-scan (SADABS; Sheldrick, 1996) | h = −15→15 |
Tmin = 0.856, Tmax = 0.909 | k = −21→21 |
38653 measured reflections | l = −24→23 |
Refinement top
Refinement on F2 | Primary atom site location: structure-invariant direct methods |
Least-squares matrix: full | Secondary atom site location: difference Fourier map |
R[F2 > 2σ(F2)] = 0.105 | Hydrogen site location: inferred from neighbouring sites |
wR(F2) = 0.231 | H-atom parameters constrained |
S = 1.16 | w = 1/[σ2(Fo2) + (0.0877P)2 + 4.2908P] where P = (Fo2 + 2Fc2)/3 |
7707 reflections | (Δ/σ)max < 0.001 |
517 parameters | Δρmax = 1.24 e Å−3 |
21 restraints | Δρmin = −0.34 e Å−3 |
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 | x | y | z | Uiso*/Ueq | Occ. (<1) |
Co1 | 1.0000 | 1.0000 | 0.0000 | 0.0343 (3) | |
O1 | 1.0945 (3) | 0.95785 (19) | 0.08938 (18) | 0.0387 (8) | |
N1 | 0.9344 (3) | 1.0728 (2) | 0.0533 (2) | 0.0394 (10) | |
N2 | 0.8711 (3) | 0.9234 (2) | −0.0057 (2) | 0.0385 (10) | |
H2 | 0.8641 | 0.8999 | −0.0495 | 0.046* | |
C1 | 1.0971 (4) | 1.0690 (3) | 0.1648 (3) | 0.0392 (12) | |
C2 | 1.1397 (4) | 0.9979 (3) | 0.1491 (3) | 0.0396 (11) | |
C3 | 1.2386 (4) | 0.9660 (3) | 0.2017 (3) | 0.0444 (12) | |
H3A | 1.2660 | 0.9177 | 0.1928 | 0.053* | |
C4 | 1.2936 (5) | 1.0043 (3) | 0.2641 (3) | 0.0523 (14) | |
H4A | 1.3582 | 0.9816 | 0.2970 | 0.063* | |
C5 | 1.3163 (5) | 1.1192 (4) | 0.3435 (3) | 0.0581 (16) | |
H5A | 1.3816 | 1.0971 | 0.3762 | 0.070* | |
C6 | 1.2823 (5) | 1.1912 (4) | 0.3582 (3) | 0.0606 (17) | |
H6A | 1.3233 | 1.2173 | 0.4006 | 0.073* | |
C7 | 1.1860 (6) | 1.2255 (4) | 0.3092 (4) | 0.0598 (16) | |
H7A | 1.1632 | 1.2751 | 0.3185 | 0.072* | |
C8 | 1.1237 (5) | 1.1858 (4) | 0.2467 (3) | 0.0531 (14) | |
H8A | 1.0588 | 1.2090 | 0.2146 | 0.064* | |
C9 | 1.2566 (4) | 1.0774 (3) | 0.2811 (3) | 0.0426 (12) | |
C10 | 1.1567 (4) | 1.1117 (3) | 0.2309 (3) | 0.0405 (12) | |
C11 | 0.9853 (4) | 1.0954 (3) | 0.1187 (3) | 0.0443 (13) | |
H11A | 0.9473 | 1.1322 | 0.1386 | 0.053* | |
C12 | 0.8111 (4) | 1.0939 (3) | 0.0219 (3) | 0.0482 (14) | |
H12A | 0.7953 | 1.1093 | −0.0290 | 0.058* | |
H12B | 0.7925 | 1.1372 | 0.0488 | 0.058* | |
C13 | 0.7390 (4) | 1.0243 (4) | 0.0271 (3) | 0.0551 (15) | |
H13A | 0.6587 | 1.0399 | 0.0122 | 0.066* | |
H13B | 0.7593 | 1.0083 | 0.0780 | 0.066* | |
C14 | 0.7514 (4) | 0.9547 (3) | −0.0186 (3) | 0.0476 (14) | |
H14A | 0.7035 | 0.9131 | −0.0097 | 0.057* | |
H14B | 0.7210 | 0.9689 | −0.0700 | 0.057* | |
C15 | 0.9013 (4) | 0.8550 (3) | 0.0457 (3) | 0.0425 (12) | |
H15A | 0.9840 | 0.8452 | 0.0558 | 0.051* | |
C16 | 0.8805 (5) | 0.8679 (4) | 0.1178 (3) | 0.0566 (15) | |
H16A | 0.7992 | 0.8778 | 0.1101 | 0.068* | |
H16B | 0.9236 | 0.9130 | 0.1418 | 0.068* | |
C17 | 0.9178 (6) | 0.7968 (5) | 0.1663 (4) | 0.086 (2) | |
H17A | 1.0003 | 0.7893 | 0.1768 | 0.103* | |
H17B | 0.9019 | 0.8050 | 0.2124 | 0.103* | |
C18 | 0.8546 (7) | 0.7251 (5) | 0.1289 (6) | 0.108 (3) | |
H18A | 0.7728 | 0.7311 | 0.1222 | 0.129* | |
H18B | 0.8816 | 0.6802 | 0.1599 | 0.129* | |
C19 | 0.8730 (6) | 0.7116 (4) | 0.0549 (5) | 0.084 (2) | |
H19A | 0.9536 | 0.7001 | 0.0616 | 0.101* | |
H19B | 0.8274 | 0.6675 | 0.0308 | 0.101* | |
C20 | 0.8380 (5) | 0.7829 (3) | 0.0081 (4) | 0.0643 (17) | |
H20A | 0.7556 | 0.7908 | −0.0027 | 0.077* | |
H20B | 0.8542 | 0.7751 | −0.0380 | 0.077* | |
Co2 | 0.5000 | 0.5000 | 0.0000 | 0.0436 (3) | |
O2 | 0.6070 (3) | 0.5363 (2) | −0.0464 (2) | 0.0528 (10) | |
N3 | 0.4999 (4) | 0.6005 (3) | 0.0439 (2) | 0.0442 (11) | |
N4 | 0.6334 (4) | 0.4694 (3) | 0.0877 (2) | 0.0597 (13) | |
H4 | 0.6020 | 0.4289 | 0.1057 | 0.072* | |
C21 | 0.5526 (4) | 0.6699 (3) | −0.0520 (3) | 0.0399 (12) | |
C22 | 0.6034 (5) | 0.6060 (3) | −0.0742 (3) | 0.0454 (13) | |
C23 | 0.6585 (5) | 0.6168 (4) | −0.1293 (3) | 0.0581 (16) | |
H23A | 0.6981 | 0.5756 | −0.1419 | 0.070* | |
C24 | 0.6546 (5) | 0.6852 (4) | −0.1633 (3) | 0.0560 (15) | |
H24A | 0.6927 | 0.6903 | −0.1985 | 0.067* | |
C25 | 0.5859 (5) | 0.8202 (4) | −0.1865 (3) | 0.0585 (16) | |
H25A | 0.6214 | 0.8250 | −0.2231 | 0.070* | |
C26 | 0.5256 (6) | 0.8821 (4) | −0.1710 (4) | 0.0659 (18) | |
H26A | 0.5184 | 0.9279 | −0.1979 | 0.079* | |
C27 | 0.4752 (6) | 0.8757 (4) | −0.1144 (4) | 0.0621 (16) | |
H27A | 0.4361 | 0.9178 | −0.1028 | 0.075* | |
C28 | 0.4831 (5) | 0.8079 (3) | −0.0764 (3) | 0.0503 (14) | |
H28A | 0.4472 | 0.8043 | −0.0400 | 0.060* | |
C29 | 0.5435 (4) | 0.7436 (3) | −0.0905 (3) | 0.0419 (12) | |
C30 | 0.5947 (4) | 0.7496 (3) | −0.1478 (3) | 0.0463 (13) | |
C31 | 0.5200 (4) | 0.6644 (3) | 0.0145 (3) | 0.0433 (13) | |
H31A | 0.5129 | 0.7106 | 0.0381 | 0.052* | |
C32 | 0.4838 (6) | 0.6058 (4) | 0.1166 (3) | 0.0578 (16) | |
H32A | 0.4049 | 0.5922 | 0.1129 | 0.069* | |
H32B | 0.4968 | 0.6590 | 0.1340 | 0.069* | |
C33 | 0.5654 (8) | 0.5523 (5) | 0.1716 (4) | 0.093 (3) | |
H33A | 0.5957 | 0.5802 | 0.2174 | 0.112* | |
H33B | 0.5214 | 0.5085 | 0.1808 | 0.112* | |
C34 | 0.6615 (7) | 0.5224 (4) | 0.1501 (4) | 0.073 (2) | |
H34A | 0.7132 | 0.4958 | 0.1919 | 0.088* | |
H34B | 0.7033 | 0.5663 | 0.1388 | 0.088* | |
C35 | 0.7352 (5) | 0.4297 (3) | 0.0725 (3) | 0.0450 (13) | |
H35A | 0.7095 | 0.4136 | 0.0209 | 0.054* | |
C36 | 0.8405 (6) | 0.4807 (3) | 0.0826 (4) | 0.0623 (17) | |
H36A | 0.8197 | 0.5268 | 0.0521 | 0.075* | |
H36B | 0.8700 | 0.4972 | 0.1333 | 0.075* | |
C37 | 0.9324 (6) | 0.4355 (5) | 0.0614 (4) | 0.082 (2) | |
H37A | 0.9038 | 0.4216 | 0.0099 | 0.099* | |
H37B | 0.9999 | 0.4681 | 0.0683 | 0.099* | |
C38 | 0.9660 (6) | 0.3628 (5) | 0.1066 (5) | 0.098 (3) | |
H38A | 1.0008 | 0.3765 | 0.1577 | 0.118* | |
H38B | 1.0224 | 0.3339 | 0.0904 | 0.118* | |
C39 | 0.8603 (6) | 0.3128 (4) | 0.0985 (5) | 0.091 (3) | |
H39A | 0.8309 | 0.2946 | 0.0482 | 0.110* | |
H39B | 0.8819 | 0.2676 | 0.1300 | 0.110* | |
C40 | 0.7675 (5) | 0.3563 (3) | 0.1180 (4) | 0.0656 (18) | |
H40A | 0.7939 | 0.3699 | 0.1696 | 0.079* | |
H40B | 0.7000 | 0.3234 | 0.1097 | 0.079* | |
Cl1 | 0.9433 (9) | 0.3785 (6) | 0.3403 (6) | 0.066 (3) | 0.50 |
O3 | 0.9113 (17) | 0.3096 (8) | 0.3110 (12) | 0.160 (12) | 0.50 |
O4 | 0.8611 (12) | 0.4295 (8) | 0.3117 (8) | 0.128 (6) | 0.50 |
O5 | 1.0386 (16) | 0.4001 (10) | 0.3265 (16) | 0.210 (17) | 0.50 |
O6 | 0.962 (2) | 0.3748 (14) | 0.4117 (8) | 0.259 (17) | 0.50 |
Cl1A | 0.9671 (8) | 0.3704 (6) | 0.3553 (5) | 0.059 (2) | 0.50 |
O3A | 1.0713 (12) | 0.3486 (11) | 0.4010 (8) | 0.129 (6) | 0.50 |
O4A | 0.919 (2) | 0.4248 (11) | 0.392 (2) | 0.225 (17) | 0.50 |
O5A | 0.9854 (18) | 0.3954 (17) | 0.2871 (9) | 0.147 (9) | 0.50 |
O6A | 0.9050 (17) | 0.3040 (10) | 0.3470 (12) | 0.119 (8) | 0.50 |
Atomic displacement parameters (Å2) top | U11 | U22 | U33 | U12 | U13 | U23 |
Co1 | 0.0228 (4) | 0.0319 (5) | 0.0451 (6) | 0.0038 (4) | 0.0057 (4) | 0.0083 (4) |
O1 | 0.0312 (17) | 0.0343 (19) | 0.042 (2) | 0.0047 (14) | −0.0007 (15) | 0.0099 (16) |
N1 | 0.028 (2) | 0.037 (2) | 0.049 (3) | 0.0064 (17) | 0.0057 (19) | 0.004 (2) |
N2 | 0.029 (2) | 0.036 (2) | 0.047 (2) | −0.0017 (17) | 0.0065 (18) | 0.0033 (19) |
C1 | 0.033 (3) | 0.043 (3) | 0.042 (3) | 0.001 (2) | 0.011 (2) | 0.010 (2) |
C2 | 0.033 (2) | 0.037 (3) | 0.048 (3) | −0.004 (2) | 0.011 (2) | 0.017 (3) |
C3 | 0.034 (3) | 0.048 (3) | 0.047 (3) | 0.009 (2) | 0.005 (2) | 0.014 (3) |
C4 | 0.044 (3) | 0.063 (4) | 0.044 (3) | 0.005 (3) | 0.005 (2) | 0.025 (3) |
C5 | 0.051 (3) | 0.077 (5) | 0.042 (3) | −0.012 (3) | 0.008 (3) | 0.008 (3) |
C6 | 0.058 (4) | 0.079 (5) | 0.044 (3) | −0.017 (3) | 0.014 (3) | −0.012 (3) |
C7 | 0.065 (4) | 0.058 (4) | 0.064 (4) | −0.010 (3) | 0.032 (3) | −0.011 (3) |
C8 | 0.040 (3) | 0.066 (4) | 0.054 (4) | −0.004 (3) | 0.015 (3) | 0.000 (3) |
C9 | 0.041 (3) | 0.051 (3) | 0.036 (3) | −0.005 (2) | 0.011 (2) | 0.010 (2) |
C10 | 0.041 (3) | 0.044 (3) | 0.038 (3) | −0.002 (2) | 0.014 (2) | 0.009 (2) |
C11 | 0.037 (3) | 0.038 (3) | 0.057 (4) | 0.007 (2) | 0.014 (3) | 0.006 (3) |
C12 | 0.034 (3) | 0.048 (3) | 0.060 (4) | 0.014 (2) | 0.010 (3) | 0.004 (3) |
C13 | 0.027 (3) | 0.069 (4) | 0.068 (4) | 0.013 (3) | 0.013 (3) | 0.011 (3) |
C14 | 0.029 (3) | 0.050 (3) | 0.060 (3) | 0.000 (2) | 0.009 (2) | 0.016 (3) |
C15 | 0.029 (2) | 0.035 (3) | 0.058 (3) | 0.002 (2) | 0.004 (2) | 0.013 (2) |
C16 | 0.044 (3) | 0.065 (4) | 0.058 (4) | −0.006 (3) | 0.011 (3) | 0.011 (3) |
C17 | 0.069 (5) | 0.105 (6) | 0.073 (5) | 0.000 (4) | 0.006 (4) | 0.046 (4) |
C18 | 0.082 (5) | 0.072 (5) | 0.150 (9) | −0.017 (4) | 0.006 (6) | 0.064 (6) |
C19 | 0.065 (5) | 0.050 (4) | 0.114 (7) | −0.013 (3) | −0.005 (4) | 0.023 (4) |
C20 | 0.050 (3) | 0.052 (4) | 0.078 (5) | −0.007 (3) | 0.000 (3) | 0.007 (3) |
Co2 | 0.0567 (6) | 0.0496 (6) | 0.0271 (5) | 0.0174 (5) | 0.0168 (4) | 0.0025 (4) |
O2 | 0.066 (2) | 0.060 (2) | 0.041 (2) | 0.022 (2) | 0.0288 (19) | 0.0080 (19) |
N3 | 0.055 (3) | 0.052 (3) | 0.029 (2) | 0.015 (2) | 0.018 (2) | −0.001 (2) |
N4 | 0.065 (3) | 0.076 (3) | 0.036 (3) | 0.022 (3) | 0.011 (2) | 0.002 (2) |
C21 | 0.036 (3) | 0.049 (3) | 0.035 (3) | 0.003 (2) | 0.012 (2) | −0.006 (2) |
C22 | 0.047 (3) | 0.058 (4) | 0.033 (3) | 0.010 (3) | 0.014 (2) | 0.006 (3) |
C23 | 0.068 (4) | 0.069 (4) | 0.047 (3) | 0.016 (3) | 0.030 (3) | 0.003 (3) |
C24 | 0.059 (4) | 0.077 (4) | 0.042 (3) | −0.002 (3) | 0.029 (3) | −0.006 (3) |
C25 | 0.066 (4) | 0.063 (4) | 0.049 (4) | −0.025 (3) | 0.021 (3) | −0.002 (3) |
C26 | 0.088 (5) | 0.047 (4) | 0.062 (4) | −0.018 (3) | 0.020 (4) | −0.002 (3) |
C27 | 0.072 (4) | 0.054 (4) | 0.065 (4) | −0.012 (3) | 0.027 (3) | −0.009 (3) |
C28 | 0.051 (3) | 0.049 (3) | 0.055 (3) | −0.010 (3) | 0.022 (3) | −0.002 (3) |
C29 | 0.034 (3) | 0.055 (3) | 0.036 (3) | −0.013 (2) | 0.010 (2) | −0.010 (2) |
C30 | 0.042 (3) | 0.058 (4) | 0.038 (3) | −0.012 (3) | 0.011 (2) | −0.006 (3) |
C31 | 0.042 (3) | 0.054 (3) | 0.032 (3) | 0.006 (2) | 0.008 (2) | −0.007 (2) |
C32 | 0.078 (4) | 0.066 (4) | 0.039 (3) | 0.019 (3) | 0.031 (3) | −0.001 (3) |
C33 | 0.131 (7) | 0.110 (6) | 0.035 (3) | 0.056 (6) | 0.022 (4) | 0.002 (4) |
C34 | 0.094 (5) | 0.070 (4) | 0.045 (4) | 0.015 (4) | 0.006 (3) | −0.015 (3) |
C35 | 0.051 (3) | 0.044 (3) | 0.037 (3) | 0.009 (2) | 0.008 (2) | −0.002 (2) |
C36 | 0.078 (4) | 0.048 (3) | 0.058 (4) | −0.013 (3) | 0.018 (3) | 0.003 (3) |
C37 | 0.057 (4) | 0.116 (7) | 0.075 (5) | −0.017 (4) | 0.021 (4) | −0.020 (5) |
C38 | 0.057 (5) | 0.110 (7) | 0.118 (7) | 0.024 (5) | 0.010 (4) | −0.020 (6) |
C39 | 0.078 (5) | 0.052 (4) | 0.119 (7) | 0.021 (4) | −0.007 (5) | −0.009 (4) |
C40 | 0.056 (4) | 0.042 (3) | 0.085 (5) | −0.010 (3) | 0.000 (3) | 0.009 (3) |
Cl1 | 0.064 (4) | 0.066 (4) | 0.061 (4) | 0.000 (3) | 0.008 (3) | 0.007 (3) |
O3 | 0.20 (2) | 0.110 (17) | 0.122 (19) | −0.025 (14) | −0.025 (15) | −0.004 (13) |
O4 | 0.163 (15) | 0.114 (11) | 0.087 (9) | 0.032 (10) | 0.007 (9) | 0.004 (8) |
O5 | 0.15 (2) | 0.104 (13) | 0.45 (5) | 0.007 (13) | 0.19 (3) | 0.05 (2) |
O6 | 0.34 (4) | 0.34 (4) | 0.051 (10) | 0.05 (3) | −0.019 (16) | 0.001 (16) |
Cl1A | 0.059 (4) | 0.064 (4) | 0.064 (5) | −0.008 (3) | 0.030 (4) | 0.004 (3) |
O3A | 0.089 (9) | 0.191 (16) | 0.086 (9) | 0.024 (10) | −0.006 (7) | −0.056 (10) |
O4A | 0.22 (2) | 0.105 (13) | 0.46 (5) | −0.020 (14) | 0.27 (3) | −0.08 (2) |
O5A | 0.120 (15) | 0.24 (2) | 0.079 (9) | −0.047 (14) | 0.032 (9) | 0.052 (11) |
O6A | 0.115 (12) | 0.081 (11) | 0.15 (2) | −0.025 (8) | 0.022 (12) | 0.043 (12) |
Geometric parameters (Å, º) top
Co1—O1 | 1.892 (3) | Co2—N4 | 2.019 (5) |
Co1—O1i | 1.892 (3) | Co2—N4ii | 2.019 (4) |
Co1—N1i | 1.933 (4) | O2—C22 | 1.307 (6) |
Co1—N1 | 1.933 (4) | N3—C31 | 1.289 (7) |
Co1—N2 | 2.026 (4) | N3—C32 | 1.465 (6) |
Co1—N2i | 2.026 (4) | N4—C34 | 1.458 (8) |
O1—C2 | 1.304 (6) | N4—C35 | 1.517 (7) |
N1—C11 | 1.276 (7) | N4—H4 | 0.9100 |
N1—C12 | 1.483 (6) | C21—C22 | 1.390 (7) |
N2—C14 | 1.501 (6) | C21—C31 | 1.448 (7) |
N2—C15 | 1.505 (6) | C21—C29 | 1.451 (7) |
N2—H2 | 0.9100 | C22—C23 | 1.422 (7) |
C1—C2 | 1.395 (7) | C23—C24 | 1.337 (8) |
C1—C10 | 1.451 (7) | C23—H23A | 0.9300 |
C1—C11 | 1.452 (7) | C24—C30 | 1.407 (8) |
C2—C3 | 1.424 (7) | C24—H24A | 0.9300 |
C3—C4 | 1.351 (8) | C25—C26 | 1.375 (9) |
C3—H3A | 0.9300 | C25—C30 | 1.409 (8) |
C4—C9 | 1.405 (8) | C25—H25A | 0.9300 |
C4—H4A | 0.9300 | C26—C27 | 1.401 (9) |
C5—C6 | 1.362 (9) | C26—H26A | 0.9300 |
C5—C9 | 1.393 (8) | C27—C28 | 1.361 (8) |
C5—H5A | 0.9300 | C27—H27A | 0.9300 |
C6—C7 | 1.390 (9) | C28—C29 | 1.398 (8) |
C6—H6A | 0.9300 | C28—H28A | 0.9300 |
C7—C8 | 1.386 (8) | C29—C30 | 1.419 (7) |
C7—H7A | 0.9300 | C31—H31A | 0.9300 |
C8—C10 | 1.398 (8) | C32—C33 | 1.519 (9) |
C8—H8A | 0.9300 | C32—H32A | 0.9700 |
C9—C10 | 1.428 (7) | C32—H32B | 0.9700 |
C11—H11A | 0.9300 | C33—C34 | 1.445 (10) |
C12—C13 | 1.504 (8) | C33—H33A | 0.9700 |
C12—H12A | 0.9700 | C33—H33B | 0.9700 |
C12—H12B | 0.9700 | C34—H34A | 0.9700 |
C13—C14 | 1.516 (8) | C34—H34B | 0.9700 |
C13—H13A | 0.9700 | C35—C36 | 1.516 (8) |
C13—H13B | 0.9700 | C35—C40 | 1.517 (8) |
C14—H14A | 0.9700 | C35—H35A | 0.9800 |
C14—H14B | 0.9700 | C36—C37 | 1.515 (9) |
C15—C16 | 1.492 (8) | C36—H36A | 0.9700 |
C15—C20 | 1.521 (8) | C36—H36B | 0.9700 |
C15—H15A | 0.9800 | C37—C38 | 1.503 (11) |
C16—C17 | 1.518 (9) | C37—H37A | 0.9700 |
C16—H16A | 0.9700 | C37—H37B | 0.9700 |
C16—H16B | 0.9700 | C38—C39 | 1.516 (11) |
C17—C18 | 1.514 (12) | C38—H38A | 0.9700 |
C17—H17A | 0.9700 | C38—H38B | 0.9700 |
C17—H17B | 0.9700 | C39—C40 | 1.493 (10) |
C18—C19 | 1.516 (13) | C39—H39A | 0.9700 |
C18—H18A | 0.9700 | C39—H39B | 0.9700 |
C18—H18B | 0.9700 | C40—H40A | 0.9700 |
C19—C20 | 1.502 (9) | C40—H40B | 0.9700 |
C19—H19A | 0.9700 | Cl1—O3 | 1.318 (11) |
C19—H19B | 0.9700 | Cl1—O6 | 1.318 (11) |
C20—H20A | 0.9700 | Cl1—O5 | 1.318 (11) |
C20—H20B | 0.9700 | Cl1—O4 | 1.318 (11) |
Co2—O2ii | 1.890 (4) | Cl1A—O6A | 1.351 (17) |
Co2—O2 | 1.890 (4) | Cl1A—O3A | 1.357 (17) |
Co2—N3ii | 1.922 (4) | Cl1A—O4A | 1.403 (19) |
Co2—N3 | 1.922 (4) | Cl1A—O5A | 1.453 (16) |
| | | |
O1—Co1—O1i | 180 | O2ii—Co2—N4 | 91.06 (19) |
O1—Co1—N1i | 89.65 (16) | O2—Co2—N4 | 88.94 (19) |
O1i—Co1—N1i | 90.35 (16) | N3ii—Co2—N4 | 91.2 (2) |
O1—Co1—N1 | 90.35 (16) | N3—Co2—N4 | 88.8 (2) |
O1i—Co1—N1 | 89.65 (16) | O2ii—Co2—N4ii | 88.94 (19) |
N1i—Co1—N1 | 180 | O2—Co2—N4ii | 91.06 (19) |
O1—Co1—N2 | 92.75 (15) | N3ii—Co2—N4ii | 88.8 (2) |
O1i—Co1—N2 | 87.25 (15) | N3—Co2—N4ii | 91.2 (2) |
N1i—Co1—N2 | 89.25 (17) | N4—Co2—N4ii | 180 |
N1—Co1—N2 | 90.75 (17) | C22—O2—Co2 | 123.4 (3) |
O1—Co1—N2i | 87.25 (15) | C31—N3—C32 | 117.2 (5) |
O1i—Co1—N2i | 92.75 (15) | C31—N3—Co2 | 123.4 (3) |
N1i—Co1—N2i | 90.75 (17) | C32—N3—Co2 | 119.2 (4) |
N1—Co1—N2i | 89.25 (17) | C34—N4—C35 | 115.9 (5) |
N2—Co1—N2i | 180 | C34—N4—Co2 | 116.5 (4) |
C2—O1—Co1 | 124.6 (3) | C35—N4—Co2 | 117.1 (3) |
C11—N1—C12 | 116.9 (4) | C34—N4—H4 | 100.9 |
C11—N1—Co1 | 124.0 (3) | C35—N4—H4 | 100.9 |
C12—N1—Co1 | 118.2 (3) | Co2—N4—H4 | 100.9 |
C14—N2—C15 | 114.8 (4) | C22—C21—C31 | 118.8 (5) |
C14—N2—Co1 | 118.2 (3) | C22—C21—C29 | 120.6 (5) |
C15—N2—Co1 | 116.2 (3) | C31—C21—C29 | 120.3 (5) |
C14—N2—H2 | 101.1 | O2—C22—C21 | 124.4 (5) |
C15—N2—H2 | 101.1 | O2—C22—C23 | 117.2 (5) |
Co1—N2—H2 | 101.1 | C21—C22—C23 | 118.4 (5) |
C2—C1—C10 | 120.7 (4) | C24—C23—C22 | 121.4 (6) |
C2—C1—C11 | 119.0 (5) | C24—C23—H23A | 119.3 |
C10—C1—C11 | 120.0 (5) | C22—C23—H23A | 119.3 |
O1—C2—C1 | 124.5 (4) | C23—C24—C30 | 122.3 (5) |
O1—C2—C3 | 117.2 (5) | C23—C24—H24A | 118.9 |
C1—C2—C3 | 118.4 (5) | C30—C24—H24A | 118.9 |
C4—C3—C2 | 121.5 (5) | C26—C25—C30 | 120.9 (6) |
C4—C3—H3A | 119.2 | C26—C25—H25A | 119.5 |
C2—C3—H3A | 119.2 | C30—C25—H25A | 119.5 |
C3—C4—C9 | 122.2 (5) | C25—C26—C27 | 119.5 (6) |
C3—C4—H4A | 118.9 | C25—C26—H26A | 120.3 |
C9—C4—H4A | 118.9 | C27—C26—H26A | 120.3 |
C6—C5—C9 | 122.2 (6) | C28—C27—C26 | 120.2 (6) |
C6—C5—H5A | 118.9 | C28—C27—H27A | 119.9 |
C9—C5—H5A | 118.9 | C26—C27—H27A | 119.9 |
C5—C6—C7 | 119.5 (6) | C27—C28—C29 | 122.1 (6) |
C5—C6—H6A | 120.2 | C27—C28—H28A | 119.0 |
C7—C6—H6A | 120.2 | C29—C28—H28A | 119.0 |
C8—C7—C6 | 120.1 (6) | C28—C29—C30 | 118.0 (5) |
C8—C7—H7A | 119.9 | C28—C29—C21 | 123.8 (5) |
C6—C7—H7A | 119.9 | C30—C29—C21 | 118.1 (5) |
C7—C8—C10 | 121.2 (6) | C24—C30—C25 | 121.9 (5) |
C7—C8—H8A | 119.4 | C24—C30—C29 | 118.9 (5) |
C10—C8—H8A | 119.4 | C25—C30—C29 | 119.2 (5) |
C5—C9—C4 | 122.6 (5) | N3—C31—C21 | 125.3 (5) |
C5—C9—C10 | 118.7 (5) | N3—C31—H31A | 117.3 |
C4—C9—C10 | 118.7 (5) | C21—C31—H31A | 117.3 |
C8—C10—C9 | 118.2 (5) | N3—C32—C33 | 111.8 (5) |
C8—C10—C1 | 123.3 (5) | N3—C32—H32A | 109.2 |
C9—C10—C1 | 118.4 (5) | C33—C32—H32A | 109.2 |
N1—C11—C1 | 125.9 (5) | N3—C32—H32B | 109.2 |
N1—C11—H11A | 117.1 | C33—C32—H32B | 109.2 |
C1—C11—H11A | 117.1 | H32A—C32—H32B | 107.9 |
N1—C12—C13 | 108.5 (4) | C34—C33—C32 | 115.7 (6) |
N1—C12—H12A | 110.0 | C34—C33—H33A | 108.4 |
C13—C12—H12A | 110.0 | C32—C33—H33A | 108.4 |
N1—C12—H12B | 110.0 | C34—C33—H33B | 108.4 |
C13—C12—H12B | 110.0 | C32—C33—H33B | 108.4 |
H12A—C12—H12B | 108.4 | H33A—C33—H33B | 107.4 |
C12—C13—C14 | 115.3 (5) | C33—C34—N4 | 116.5 (6) |
C12—C13—H13A | 108.4 | C33—C34—H34A | 108.2 |
C14—C13—H13A | 108.4 | N4—C34—H34A | 108.2 |
C12—C13—H13B | 108.4 | C33—C34—H34B | 108.2 |
C14—C13—H13B | 108.4 | N4—C34—H34B | 108.2 |
H13A—C13—H13B | 107.5 | H34A—C34—H34B | 107.3 |
N2—C14—C13 | 116.7 (4) | C36—C35—C40 | 110.3 (5) |
N2—C14—H14A | 108.1 | C36—C35—N4 | 115.0 (5) |
C13—C14—H14A | 108.1 | C40—C35—N4 | 110.4 (5) |
N2—C14—H14B | 108.1 | C36—C35—H35A | 106.9 |
C13—C14—H14B | 108.1 | C40—C35—H35A | 106.9 |
H14A—C14—H14B | 107.3 | N4—C35—H35A | 106.9 |
C16—C15—N2 | 114.3 (4) | C37—C36—C35 | 109.4 (5) |
C16—C15—C20 | 110.8 (5) | C37—C36—H36A | 109.8 |
N2—C15—C20 | 109.8 (4) | C35—C36—H36A | 109.8 |
C16—C15—H15A | 107.2 | C37—C36—H36B | 109.8 |
N2—C15—H15A | 107.2 | C35—C36—H36B | 109.8 |
C20—C15—H15A | 107.2 | H36A—C36—H36B | 108.2 |
C15—C16—C17 | 110.0 (6) | C38—C37—C36 | 111.6 (6) |
C15—C16—H16A | 109.7 | C38—C37—H37A | 109.3 |
C17—C16—H16A | 109.7 | C36—C37—H37A | 109.3 |
C15—C16—H16B | 109.7 | C38—C37—H37B | 109.3 |
C17—C16—H16B | 109.7 | C36—C37—H37B | 109.3 |
H16A—C16—H16B | 108.2 | H37A—C37—H37B | 108.0 |
C18—C17—C16 | 110.6 (6) | C37—C38—C39 | 109.8 (6) |
C18—C17—H17A | 109.5 | C37—C38—H38A | 109.7 |
C16—C17—H17A | 109.5 | C39—C38—H38A | 109.7 |
C18—C17—H17B | 109.5 | C37—C38—H38B | 109.7 |
C16—C17—H17B | 109.5 | C39—C38—H38B | 109.7 |
H17A—C17—H17B | 108.1 | H38A—C38—H38B | 108.2 |
C17—C18—C19 | 111.6 (6) | C40—C39—C38 | 111.9 (6) |
C17—C18—H18A | 109.3 | C40—C39—H39A | 109.2 |
C19—C18—H18A | 109.3 | C38—C39—H39A | 109.2 |
C17—C18—H18B | 109.3 | C40—C39—H39B | 109.2 |
C19—C18—H18B | 109.3 | C38—C39—H39B | 109.2 |
H18A—C18—H18B | 108.0 | H39A—C39—H39B | 107.9 |
C20—C19—C18 | 109.6 (7) | C39—C40—C35 | 111.0 (6) |
C20—C19—H19A | 109.7 | C39—C40—H40A | 109.4 |
C18—C19—H19A | 109.7 | C35—C40—H40A | 109.4 |
C20—C19—H19B | 109.7 | C39—C40—H40B | 109.4 |
C18—C19—H19B | 109.7 | C35—C40—H40B | 109.4 |
H19A—C19—H19B | 108.2 | H40A—C40—H40B | 108.0 |
C19—C20—C15 | 111.8 (5) | O3—Cl1—O6 | 109.47 (14) |
C19—C20—H20A | 109.3 | O3—Cl1—O5 | 109.51 (14) |
C15—C20—H20A | 109.3 | O6—Cl1—O5 | 109.48 (14) |
C19—C20—H20B | 109.3 | O3—Cl1—O4 | 109.47 (14) |
C15—C20—H20B | 109.3 | O6—Cl1—O4 | 109.46 (13) |
H20A—C20—H20B | 107.9 | O5—Cl1—O4 | 109.45 (14) |
O2ii—Co2—O2 | 180 | O6A—Cl1A—O3A | 102.9 (13) |
O2ii—Co2—N3ii | 90.02 (18) | O6A—Cl1A—O4A | 108.5 (12) |
O2—Co2—N3ii | 89.98 (18) | O3A—Cl1A—O4A | 108.2 (17) |
O2ii—Co2—N3 | 89.98 (18) | O6A—Cl1A—O5A | 112.2 (15) |
O2—Co2—N3 | 90.02 (18) | O3A—Cl1A—O5A | 107.1 (11) |
N3ii—Co2—N3 | 180 | O4A—Cl1A—O5A | 116.9 (18) |
Symmetry codes: (i) −x+2, −y+2, −z; (ii) −x+1, −y+1, −z. |
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