Supporting information
Crystallographic Information File (CIF) https://doi.org/10.1107/S1600536804008979/fl6099sup1.cif | |
Structure factor file (CIF format) https://doi.org/10.1107/S1600536804008979/fl6099Isup2.hkl |
CCDC reference: 239076
Key indicators
- Single-crystal X-ray study
- T = 110 K
- Mean (C-C) = 0.006 Å
- Disorder in solvent or counterion
- R factor = 0.058
- wR factor = 0.139
- Data-to-parameter ratio = 16.2
checkCIF/PLATON results
No syntax errors found
Alert level A PLAT432_ALERT_2_A Short Inter X...Y Contact I1B .. C34 .. 3.14 Ang.
Author Response: This non-bonded interatomic contact is between the minor component (5%) of a disordered iodide ion and C34, a carbon atom with a prolate thermal ellipsoid. This C atom can also be split into two positions but was refined anisotropically (see text). The intermolecular contacts between the major component and aromatic ring make chemical sense. It is likely that by splitting C34 the intermolecular contacts between two minor component would be reasonable. Refining I1 without splitting atoms results in all the non-bonded contacts making chemical sense. Splitting I1 was preferred as it lowered the residual electron density and improved the R-values. The short contact is a result of residual disorder that has not been modelled. The short distance is also due partly to favourable interactions between the iodide ions and the cationic aromatic rings. |
PROBLEM: Short Inter X...Y Contact C24 ..C3SB= 2.92 Ang. RESPONSE: These non-bonded interatomic contacts are between the minor component (25%) of a disordered acetonitrile solvent molecule and carbon atom with a prolate thermal ellipsoid. The intermolecular contacts between the major components make chemical sense. PROBLEM: Short Inter X...Y Contact C33..C4SB = 3.04 Ang. RESPONSE: These non-bonded interatomic contacts are between the minor component of a disordered acetonitrile solvent molecule and carbon atom with a prolate thermal ellipsoid. The intermolecular contacts between the major components make chemical sense. PLAT702_ALERT_1_A Angle Calc 55.70(2), Rep 55.79(2), Dev.. 4.50 Sigma CO3 -CO4 -CO2 1.555 1.555 1.555
Alert level B PLAT220_ALERT_2_B Large Non-Solvent C Ueq(max)/Ueq(min) ... 3.88 Ratio
Author Response: Please see _publ_section_exptl_refinement. This is likely to be due to partial disorder. The anisotropic displacement parameters for some of the carbon atoms have a component perpendicular to the rings that is much larger than those nearly parallel to the rings. Following the advice given in the SHELX frequently-asked-questions; these atoms were not split. However, this approach results in larger ellipsoids for these atoms (and the physical validity of these ellipsoids representing harmonic motion may be doubtful). |
PLAT432_ALERT_2_B Short Inter X...Y Contact C24 .. C3SB .. 2.92 Ang.
Author Response: This non-bonded interatomic contact is between the minor component (5%) of a disordered iodide ion and C34, a carbon atom with a prolate thermal ellipsoid. This C atom can also be split into two positions but was refined anisotropically (see text). The intermolecular contacts between the major component and aromatic ring make chemical sense. It is likely that by splitting C34 the intermolecular contacts between two minor component would be reasonable. Refining I1 without splitting atoms results in all the non-bonded contacts making chemical sense. Splitting I1 was preferred as it lowered the residual electron density and improved the R-values. The short contact is a result of residual disorder that has not been modelled. The short distance is also due partly to favourable interactions between the iodide ions and the cationic aromatic rings. |
PROBLEM: Short Inter X...Y Contact C24 ..C3SB= 2.92 Ang. RESPONSE: These non-bonded interatomic contacts are between the minor component (25%) of a disordered acetonitrile solvent molecule and carbon atom with a prolate thermal ellipsoid. The intermolecular contacts between the major components make chemical sense. PROBLEM: Short Inter X...Y Contact C33..C4SB = 3.04 Ang. RESPONSE: These non-bonded interatomic contacts are between the minor component of a disordered acetonitrile solvent molecule and carbon atom with a prolate thermal ellipsoid. The intermolecular contacts between the major components make chemical sense. PLAT432_ALERT_2_B Short Inter X...Y Contact C33 .. C4SB .. 3.04 Ang.
Author Response: This non-bonded interatomic contact is between the minor component (5%) of a disordered iodide ion and C34, a carbon atom with a prolate thermal ellipsoid. This C atom can also be split into two positions but was refined anisotropically (see text). The intermolecular contacts between the major component and aromatic ring make chemical sense. It is likely that by splitting C34 the intermolecular contacts between two minor component would be reasonable. Refining I1 without splitting atoms results in all the non-bonded contacts making chemical sense. Splitting I1 was preferred as it lowered the residual electron density and improved the R-values. The short contact is a result of residual disorder that has not been modelled. The short distance is also due partly to favourable interactions between the iodide ions and the cationic aromatic rings. |
PROBLEM: Short Inter X...Y Contact C24 ..C3SB= 2.92 Ang. RESPONSE: These non-bonded interatomic contacts are between the minor component (25%) of a disordered acetonitrile solvent molecule and carbon atom with a prolate thermal ellipsoid. The intermolecular contacts between the major components make chemical sense. PROBLEM: Short Inter X...Y Contact C33..C4SB = 3.04 Ang. RESPONSE: These non-bonded interatomic contacts are between the minor component of a disordered acetonitrile solvent molecule and carbon atom with a prolate thermal ellipsoid. The intermolecular contacts between the major components make chemical sense. PLAT432_ALERT_2_B Short Inter X...Y Contact C34 .. C3SB .. 3.03 Ang.
Author Response: This non-bonded interatomic contact is between the minor component (5%) of a disordered iodide ion and C34, a carbon atom with a prolate thermal ellipsoid. This C atom can also be split into two positions but was refined anisotropically (see text). The intermolecular contacts between the major component and aromatic ring make chemical sense. It is likely that by splitting C34 the intermolecular contacts between two minor component would be reasonable. Refining I1 without splitting atoms results in all the non-bonded contacts making chemical sense. Splitting I1 was preferred as it lowered the residual electron density and improved the R-values. The short contact is a result of residual disorder that has not been modelled. The short distance is also due partly to favourable interactions between the iodide ions and the cationic aromatic rings. |
PROBLEM: Short Inter X...Y Contact C24 ..C3SB= 2.92 Ang. RESPONSE: These non-bonded interatomic contacts are between the minor component (25%) of a disordered acetonitrile solvent molecule and carbon atom with a prolate thermal ellipsoid. The intermolecular contacts between the major components make chemical sense. PROBLEM: Short Inter X...Y Contact C33..C4SB = 3.04 Ang. RESPONSE: These non-bonded interatomic contacts are between the minor component of a disordered acetonitrile solvent molecule and carbon atom with a prolate thermal ellipsoid. The intermolecular contacts between the major components make chemical sense.
Alert level C PLAT029_ALERT_3_C _diffrn_measured_fraction_theta_full Low ....... 0.97
Author Response: The completeness drops from 99% to 97% between 25 and 27 degrees. |
PLAT042_ALERT_1_C Calc. and Rep. MoietyFormula Strings Differ .... ? PLAT165_ALERT_3_C Nr. of Status R Flagged Non-Hydrogen Atoms ..... 12 PLAT202_ALERT_3_C Isotropic non-H Atoms in Anion/Solvent ......... 6
Author Response: see _publ_section_exptl_refinement. |
PLAT213_ALERT_2_C Atom C23 has ADP max/min Ratio ............. 3.40 prolat PLAT213_ALERT_2_C Atom F43F has ADP max/min Ratio ............. 3.40 prolat PLAT222_ALERT_3_C Large Non-Solvent H Ueq(max)/Ueq(min) ... 3.39 Ratio PLAT241_ALERT_2_C Check High U(eq) as Compared to Neighbors .... C23 PLAT241_ALERT_2_C Check High U(eq) as Compared to Neighbors .... C33 PLAT241_ALERT_2_C Check High U(eq) as Compared to Neighbors .... C34 PLAT242_ALERT_2_C Check Low U(eq) as Compared to Neighbors .... C42 PLAT242_ALERT_2_C Check Low U(eq) as Compared to Neighbors .... C44B PLAT301_ALERT_3_C Main Residue Disorder ......................... 5.00 Perc. PLAT302_ALERT_4_C Anion/Solvent Disorder ......................... 44.00 Perc. PLAT432_ALERT_2_C Short Inter X...Y Contact C4SA .. C34 .. 3.16 Ang.
Author Response: This non-bonded interatomic contact is between the minor component (5%) of a disordered iodide ion and C34, a carbon atom with a prolate thermal ellipsoid. This C atom can also be split into two positions but was refined anisotropically (see text). The intermolecular contacts between the major component and aromatic ring make chemical sense. It is likely that by splitting C34 the intermolecular contacts between two minor component would be reasonable. Refining I1 without splitting atoms results in all the non-bonded contacts making chemical sense. Splitting I1 was preferred as it lowered the residual electron density and improved the R-values. The short contact is a result of residual disorder that has not been modelled. The short distance is also due partly to favourable interactions between the iodide ions and the cationic aromatic rings. |
PROBLEM: Short Inter X...Y Contact C24 ..C3SB= 2.92 Ang. RESPONSE: These non-bonded interatomic contacts are between the minor component (25%) of a disordered acetonitrile solvent molecule and carbon atom with a prolate thermal ellipsoid. The intermolecular contacts between the major components make chemical sense. PROBLEM: Short Inter X...Y Contact C33..C4SB = 3.04 Ang. RESPONSE: These non-bonded interatomic contacts are between the minor component of a disordered acetonitrile solvent molecule and carbon atom with a prolate thermal ellipsoid. The intermolecular contacts between the major components make chemical sense. PLAT432_ALERT_2_C Short Inter X...Y Contact C34 .. C4SB .. 3.17 Ang.
Author Response: This non-bonded interatomic contact is between the minor component (5%) of a disordered iodide ion and C34, a carbon atom with a prolate thermal ellipsoid. This C atom can also be split into two positions but was refined anisotropically (see text). The intermolecular contacts between the major component and aromatic ring make chemical sense. It is likely that by splitting C34 the intermolecular contacts between two minor component would be reasonable. Refining I1 without splitting atoms results in all the non-bonded contacts making chemical sense. Splitting I1 was preferred as it lowered the residual electron density and improved the R-values. The short contact is a result of residual disorder that has not been modelled. The short distance is also due partly to favourable interactions between the iodide ions and the cationic aromatic rings. |
PROBLEM: Short Inter X...Y Contact C24 ..C3SB= 2.92 Ang. RESPONSE: These non-bonded interatomic contacts are between the minor component (25%) of a disordered acetonitrile solvent molecule and carbon atom with a prolate thermal ellipsoid. The intermolecular contacts between the major components make chemical sense. PROBLEM: Short Inter X...Y Contact C33..C4SB = 3.04 Ang. RESPONSE: These non-bonded interatomic contacts are between the minor component of a disordered acetonitrile solvent molecule and carbon atom with a prolate thermal ellipsoid. The intermolecular contacts between the major components make chemical sense. PLAT720_ALERT_4_C Number of Unusual/Non-Standard Label(s) ........ 26 PLAT735_ALERT_1_C D-H Calc 0.967(19), Rep 0.967(9) ...... 2.11 su-Rat O2 -H2O 1.555 1.555
2 ALERT level A = In general: serious problem 4 ALERT level B = Potentially serious problem 18 ALERT level C = Check and explain 0 ALERT level G = General alerts; check 3 ALERT type 1 CIF construction/syntax error, inconsistent or missing data 14 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: SMART (Bruker, 2001); cell refinement: SAINT (Bruker, 2001); data reduction: SAINT; program(s) used to solve structure: SHELXS97 (Sheldrick, 1997); program(s) used to refine structure: X-SEED (Barbour, 2001) and SHELXL97 (Sheldrick, 1997); molecular graphics: SHELXTL (Bruker, 2000).
[Co4(C2F3O2)2(OH)4(C10H8N2)4]I2·2C2H3N·H2O | F(000) = 5936 |
Mr = 1508.45 | Dx = 1.790 Mg m−3 |
Orthorhombic, Pbca | Mo Kα radiation, λ = 0.71073 Å |
Hall symbol: -P 2ac 2ab | Cell parameters from 5517 reflections |
a = 20.027 (1) Å | θ = 2.5–27.3° |
b = 18.774 (1) Å | µ = 2.35 mm−1 |
c = 29.771 (2) Å | T = 110 K |
V = 11194 (1) Å3 | Prism, brown |
Z = 8 | 0.29 × 0.25 × 0.11 mm |
SMART APEX CCD area-detector diffractometer | 12523 independent reflections |
Radiation source: fine-focus sealed tube | 8819 reflections with I > 2σ(I) |
Graphite monochromator | Rint = 0.068 |
ω and φ scans | θmax = 27.5°, θmin = 2.4° |
Absorption correction: multi-scan (SADABS; Bruker, 2003) | h = −25→23 |
Tmin = 0.549, Tmax = 0.782 | k = −24→24 |
72201 measured reflections | l = −38→23 |
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)] = 0.058 | Hydrogen site location: inferred from neighbouring sites |
wR(F2) = 0.139 | H atoms treated by a mixture of independent and constrained refinement |
S = 1.04 | w = 1/[σ2(Fo2) + (0.0647P)2 + 25.7334P] where P = (Fo2 + 2Fc2)/3 |
12523 reflections | (Δ/σ)max = 0.028 |
775 parameters | Δρmax = 1.67 e Å−3 |
119 restraints | Δρmin = −1.00 e Å−3 |
Experimental. Approximately a hemisphere of diffraction data in reciprocal space were collected by a combination of three sets of exposures: two 180° ω scans and one 120° φ scan. Exposure times of 30 s per frame and scan widths of 0.3° were used throughout the data collection. Crystal decay was monitored by analyzing duplicate reflections, and found to be negligible, therefore no decay correction was applied. |
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. |
x | y | z | Uiso*/Ueq | Occ. (<1) | |
I2 | 0.296668 (14) | 0.400138 (13) | 0.450074 (11) | 0.03723 (8) | |
Co1 | 0.43734 (3) | 0.31144 (2) | 0.320826 (17) | 0.01960 (12) | |
O1 | 0.44966 (13) | 0.20114 (11) | 0.32619 (8) | 0.0215 (6) | |
H1O | 0.4320 (18) | 0.1739 (16) | 0.3019 (9) | 0.069 (17)* | |
N1 | 0.41889 (16) | 0.42192 (14) | 0.31238 (11) | 0.0234 (8) | |
C1 | 0.4653 (2) | 0.47305 (18) | 0.31425 (14) | 0.0282 (10) | |
H1 | 0.5101 | 0.4597 | 0.3205 | 0.034* | |
I1A | 0.364753 (15) | 0.061955 (13) | 0.261046 (11) | 0.03361 (8) | 0.95 |
I1B | 0.3522 (3) | 0.0722 (3) | 0.2433 (2) | 0.03361 (8) | 0.05 |
Co2 | 0.42488 (3) | 0.18820 (2) | 0.393762 (18) | 0.02272 (12) | |
O2 | 0.42332 (12) | 0.29918 (11) | 0.38973 (8) | 0.0216 (6) | |
H2O | 0.3887 (7) | 0.3236 (12) | 0.4063 (8) | 0.066 (16)* | |
N2 | 0.33570 (16) | 0.31483 (14) | 0.29947 (10) | 0.0224 (8) | |
C2 | 0.4512 (2) | 0.54448 (19) | 0.30746 (14) | 0.0339 (11) | |
H2 | 0.4857 | 0.5793 | 0.3077 | 0.041* | |
Co3 | 0.52116 (3) | 0.30662 (2) | 0.413899 (18) | 0.02237 (12) | |
O3 | 0.52924 (13) | 0.19984 (11) | 0.39703 (9) | 0.0241 (6) | |
H3O | 0.5519 (9) | 0.1707 (10) | 0.4190 (6) | 0.055 (15)* | |
N3 | 0.32011 (18) | 0.17277 (16) | 0.39045 (11) | 0.0285 (8) | |
C3 | 0.3854 (2) | 0.56350 (18) | 0.30025 (16) | 0.0378 (12) | |
H3 | 0.3737 | 0.6122 | 0.2965 | 0.045* | |
Co4 | 0.55359 (3) | 0.20911 (2) | 0.329054 (18) | 0.02201 (12) | |
O4 | 0.53587 (13) | 0.31587 (11) | 0.34428 (9) | 0.0222 (6) | |
H4O | 0.5569 (17) | 0.3531 (14) | 0.3272 (12) | 0.085 (19)* | |
N4 | 0.41555 (18) | 0.07583 (15) | 0.39407 (11) | 0.0286 (9) | |
C4 | 0.3368 (2) | 0.51174 (19) | 0.29849 (15) | 0.0333 (11) | |
H4 | 0.2914 | 0.5244 | 0.2939 | 0.040* | |
O5 | 0.46842 (13) | 0.30578 (12) | 0.25254 (9) | 0.0248 (7) | |
N5 | 0.52437 (17) | 0.41605 (15) | 0.43030 (11) | 0.0270 (8) | |
C5 | 0.2415 (2) | 0.3892 (2) | 0.28443 (15) | 0.0344 (11) | |
H5 | 0.2228 | 0.4357 | 0.2831 | 0.041* | |
O6 | 0.55586 (13) | 0.22913 (12) | 0.25788 (9) | 0.0246 (7) | |
N6 | 0.61695 (17) | 0.31856 (15) | 0.44431 (11) | 0.0282 (9) | |
C6 | 0.2028 (2) | 0.3310 (2) | 0.27458 (15) | 0.0352 (11) | |
H6 | 0.1572 | 0.3365 | 0.2663 | 0.042* | |
O7 | 0.41777 (14) | 0.18869 (12) | 0.46542 (9) | 0.0308 (7) | |
N7 | 0.65964 (17) | 0.21521 (17) | 0.33497 (12) | 0.0302 (9) | |
C7 | 0.2318 (2) | 0.2636 (2) | 0.27697 (14) | 0.0310 (11) | |
H7 | 0.2066 | 0.2222 | 0.2698 | 0.037* | |
O8 | 0.48689 (14) | 0.28129 (13) | 0.48059 (9) | 0.0284 (7) | |
N8 | 0.58596 (17) | 0.10333 (15) | 0.31528 (11) | 0.0288 (9) | |
C8 | 0.2977 (2) | 0.25828 (19) | 0.28991 (14) | 0.0277 (10) | |
H8 | 0.3170 | 0.2122 | 0.2921 | 0.033* | |
C9 | 0.3550 (2) | 0.44045 (18) | 0.30352 (14) | 0.0261 (10) | |
C10 | 0.30814 (19) | 0.38028 (18) | 0.29645 (13) | 0.0247 (9) | |
C11 | 0.2741 (2) | 0.2242 (2) | 0.39259 (14) | 0.0312 (11) | |
H11 | 0.2887 | 0.2722 | 0.3938 | 0.037* | |
C12 | 0.2065 (2) | 0.2108 (2) | 0.39319 (16) | 0.0395 (12) | |
H12 | 0.1753 | 0.2489 | 0.3948 | 0.047* | |
C13 | 0.1850 (3) | 0.1415 (3) | 0.39137 (18) | 0.0516 (15) | |
H13 | 0.1387 | 0.1308 | 0.3913 | 0.062* | |
C14 | 0.2324 (2) | 0.0869 (2) | 0.38961 (17) | 0.0440 (13) | |
H14 | 0.2186 | 0.0385 | 0.3890 | 0.053* | |
C15 | 0.3415 (3) | −0.0222 (2) | 0.38323 (18) | 0.0516 (14) | |
H15 | 0.2973 | −0.0393 | 0.3790 | 0.062* | |
C16 | 0.3937 (3) | −0.0685 (2) | 0.38442 (19) | 0.0606 (17) | |
H16 | 0.3865 | −0.1181 | 0.3802 | 0.073* | |
C17 | 0.4569 (3) | −0.0430 (2) | 0.39176 (18) | 0.0538 (15) | |
H17 | 0.4937 | −0.0747 | 0.3938 | 0.065* | |
C18 | 0.4663 (2) | 0.0298 (2) | 0.39609 (14) | 0.0357 (12) | |
H18 | 0.5102 | 0.0476 | 0.4007 | 0.043* | |
C19 | 0.2993 (2) | 0.1042 (2) | 0.38882 (14) | 0.0348 (11) | |
C20 | 0.3536 (2) | 0.05043 (19) | 0.38835 (14) | 0.0333 (11) | |
C21 | 0.4749 (2) | 0.4625 (2) | 0.42177 (15) | 0.0366 (12) | |
H21 | 0.4364 | 0.4464 | 0.4061 | 0.044* | |
C22 | 0.4782 (3) | 0.5328 (2) | 0.4349 (2) | 0.0574 (16) | |
H22 | 0.4422 | 0.5643 | 0.4289 | 0.069* | |
C23 | 0.5338 (3) | 0.5563 (2) | 0.4567 (2) | 0.080 (2) | |
H23 | 0.5375 | 0.6050 | 0.4650 | 0.097* | |
C24 | 0.5846 (3) | 0.5093 (2) | 0.4666 (2) | 0.0665 (17) | |
H24 | 0.6228 | 0.5245 | 0.4829 | 0.080* | |
C25 | 0.6870 (2) | 0.3960 (2) | 0.48694 (16) | 0.0433 (13) | |
H25 | 0.6952 | 0.4422 | 0.4988 | 0.052* | |
C26 | 0.7318 (2) | 0.3420 (2) | 0.49523 (15) | 0.0401 (12) | |
H26 | 0.7714 | 0.3504 | 0.5121 | 0.048* | |
C27 | 0.7175 (2) | 0.2747 (2) | 0.47824 (15) | 0.0387 (12) | |
H27 | 0.7464 | 0.2356 | 0.4839 | 0.046* | |
C28 | 0.6604 (2) | 0.2664 (2) | 0.45307 (15) | 0.0358 (12) | |
H28 | 0.6513 | 0.2205 | 0.4411 | 0.043* | |
C29 | 0.5786 (2) | 0.43829 (19) | 0.45204 (15) | 0.0353 (11) | |
C30 | 0.6302 (2) | 0.38387 (19) | 0.46154 (15) | 0.0332 (11) | |
C31 | 0.6951 (2) | 0.2738 (2) | 0.34421 (15) | 0.0363 (12) | |
H59 | 0.6711 | 0.3163 | 0.3501 | 0.044* | |
C32 | 0.7633 (2) | 0.2773 (3) | 0.34585 (18) | 0.0538 (15) | |
H54 | 0.7859 | 0.3197 | 0.3543 | 0.065* | |
C33 | 0.7974 (3) | 0.2167 (4) | 0.3347 (3) | 0.094 (3) | |
H10 | 0.8448 | 0.2171 | 0.3335 | 0.112* | |
C34 | 0.7627 (3) | 0.1554 (4) | 0.3254 (3) | 0.093 (3) | |
H73 | 0.7862 | 0.1131 | 0.3178 | 0.111* | |
C35 | 0.6786 (3) | 0.0227 (3) | 0.31318 (17) | 0.0517 (14) | |
H64 | 0.7254 | 0.0151 | 0.3151 | 0.062* | |
C36 | 0.6363 (3) | −0.0326 (2) | 0.30523 (17) | 0.0510 (14) | |
H42 | 0.6534 | −0.0796 | 0.3025 | 0.061* | |
C37 | 0.5691 (3) | −0.0207 (2) | 0.30110 (15) | 0.0422 (13) | |
H44 | 0.5394 | −0.0589 | 0.2948 | 0.051* | |
C38 | 0.5452 (2) | 0.0482 (2) | 0.30623 (14) | 0.0339 (11) | |
H48 | 0.4986 | 0.0567 | 0.3033 | 0.041* | |
C39 | 0.6518 (2) | 0.0909 (2) | 0.31838 (15) | 0.0375 (12) | |
C40 | 0.6936 (2) | 0.1552 (3) | 0.32697 (16) | 0.0418 (13) | |
C41 | 0.51367 (19) | 0.26641 (18) | 0.23791 (13) | 0.0240 (9) | |
C43 | 0.4479 (2) | 0.23181 (19) | 0.48984 (14) | 0.0286 (10) | |
C44A | 0.4364 (2) | 0.22163 (19) | 0.54045 (15) | 0.0399 (12) | 0.44 |
F43A | 0.4243 (4) | 0.1552 (3) | 0.5538 (2) | 0.051 (2) | 0.44 |
F43C | 0.4879 (4) | 0.2448 (4) | 0.5650 (2) | 0.065 (3) | 0.44 |
F43B | 0.3854 (4) | 0.2642 (4) | 0.5534 (3) | 0.063 (2) | 0.44 |
C44B | 0.4364 (2) | 0.22163 (19) | 0.54045 (15) | 0.0399 (12) | 0.27 |
F43F | 0.4647 (7) | 0.2715 (6) | 0.5658 (4) | 0.067 (4) | 0.27 |
F43E | 0.3707 (4) | 0.2191 (8) | 0.5479 (4) | 0.065 (4) | 0.27 |
F43D | 0.4636 (6) | 0.1585 (5) | 0.5519 (4) | 0.066 (4) | 0.27 |
C44C | 0.4364 (2) | 0.22163 (19) | 0.54045 (15) | 0.0399 (12) | 0.29 |
F43I | 0.4113 (8) | 0.2755 (6) | 0.5629 (4) | 0.066 (4) | 0.29 |
F43H | 0.3961 (6) | 0.1687 (5) | 0.5513 (3) | 0.039 (3) | 0.29 |
F43G | 0.4949 (7) | 0.2105 (6) | 0.5626 (4) | 0.063 (4) | 0.29 |
O1S | 0.6313 (2) | 0.4298 (2) | 0.32043 (17) | 0.0936 (16) | |
H1SA | 0.6520 (17) | 0.4431 (19) | 0.3489 (5) | 0.112* | |
H1SB | 0.636 (3) | 0.4702 (11) | 0.2995 (7) | 0.112* | |
N1SB | 0.5931 (4) | 0.0982 (4) | 0.4584 (3) | 0.0594 (11)* | 0.43 |
C1SB | 0.6110 (4) | 0.0501 (4) | 0.4777 (3) | 0.0594 (11)* | 0.43 |
C2SB | 0.6352 (7) | −0.0116 (6) | 0.5019 (4) | 0.0594 (11)* | 0.43 |
H2S4 | 0.6769 | −0.0283 | 0.4883 | 0.089* | 0.43 |
H2S5 | 0.6017 | −0.0497 | 0.5005 | 0.089* | 0.43 |
H2S6 | 0.6433 | 0.0012 | 0.5334 | 0.089* | 0.43 |
N1SA | 0.6150 (3) | 0.0923 (3) | 0.4401 (2) | 0.0594 (11)* | 0.57 |
C1SA | 0.6291 (3) | 0.0444 (3) | 0.4610 (2) | 0.0594 (11)* | 0.57 |
C2SA | 0.6485 (6) | −0.0171 (4) | 0.4874 (3) | 0.0594 (11)* | 0.57 |
H2S1 | 0.6718 | −0.0513 | 0.4681 | 0.089* | 0.57 |
H2S2 | 0.6085 | −0.0396 | 0.5001 | 0.089* | 0.57 |
H2S3 | 0.6781 | −0.0020 | 0.5118 | 0.089* | 0.57 |
N2SB | 0.6861 (13) | 0.5132 (15) | 0.3849 (8) | 0.127 (2)* | 0.25 |
C3SB | 0.6784 (12) | 0.5672 (14) | 0.4008 (8) | 0.127 (2)* | 0.25 |
C4SB | 0.668 (2) | 0.6369 (16) | 0.4204 (12) | 0.127 (2)* | 0.25 |
H4S4 | 0.6229 | 0.6539 | 0.4126 | 0.191* | 0.25 |
H4S5 | 0.7011 | 0.6702 | 0.4087 | 0.191* | 0.25 |
H4S6 | 0.6719 | 0.6337 | 0.4532 | 0.191* | 0.25 |
N2SA | 0.7149 (4) | 0.4791 (5) | 0.3888 (3) | 0.127 (2)* | 0.75 |
C3SA | 0.7191 (4) | 0.5330 (5) | 0.4054 (3) | 0.127 (2)* | 0.75 |
C4SA | 0.7236 (8) | 0.6028 (5) | 0.4259 (4) | 0.127 (2)* | 0.75 |
H4S1 | 0.6802 | 0.6268 | 0.4238 | 0.191* | 0.75 |
H4S2 | 0.7575 | 0.6312 | 0.4103 | 0.191* | 0.75 |
H4S3 | 0.7361 | 0.5977 | 0.4576 | 0.191* | 0.75 |
F42A | 0.57495 (15) | 0.2445 (2) | 0.17015 (10) | 0.0703 (11) | |
F42C | 0.47636 (15) | 0.20765 (14) | 0.17241 (9) | 0.0547 (8) | |
F42B | 0.4939 (2) | 0.31733 (13) | 0.16567 (9) | 0.0753 (11) | |
C42 | 0.5152 (2) | 0.26139 (18) | 0.18648 (14) | 0.0293 (10) |
U11 | U22 | U33 | U12 | U13 | U23 | |
I2 | 0.02898 (15) | 0.02483 (11) | 0.05786 (19) | −0.00110 (10) | −0.00585 (14) | −0.01132 (12) |
Co1 | 0.0210 (3) | 0.01126 (18) | 0.0265 (3) | 0.00018 (18) | −0.0039 (2) | −0.00075 (18) |
O1 | 0.0241 (14) | 0.0154 (10) | 0.0251 (14) | 0.0001 (10) | −0.0042 (12) | −0.0029 (10) |
N1 | 0.0281 (18) | 0.0181 (13) | 0.0240 (17) | 0.0010 (12) | −0.0043 (14) | 0.0004 (12) |
C1 | 0.028 (2) | 0.0164 (15) | 0.040 (2) | −0.0010 (15) | −0.0107 (19) | −0.0004 (16) |
I1A | 0.02909 (15) | 0.02071 (11) | 0.05103 (19) | −0.00373 (11) | −0.00273 (14) | −0.00458 (12) |
I1B | 0.02909 (15) | 0.02071 (11) | 0.05103 (19) | −0.00373 (11) | −0.00273 (14) | −0.00458 (12) |
Co2 | 0.0291 (3) | 0.01246 (19) | 0.0267 (3) | −0.00248 (19) | −0.0028 (2) | −0.00094 (19) |
O2 | 0.0218 (14) | 0.0152 (10) | 0.0279 (14) | −0.0009 (10) | −0.0028 (12) | −0.0029 (10) |
N2 | 0.0265 (17) | 0.0171 (12) | 0.0235 (17) | 0.0000 (12) | −0.0045 (14) | 0.0004 (12) |
C2 | 0.047 (3) | 0.0175 (16) | 0.037 (2) | −0.0038 (17) | −0.004 (2) | −0.0004 (16) |
Co3 | 0.0262 (3) | 0.01290 (19) | 0.0280 (3) | −0.00040 (18) | −0.0068 (2) | −0.00279 (19) |
O3 | 0.0298 (15) | 0.0149 (10) | 0.0276 (14) | 0.0012 (10) | −0.0077 (12) | 0.0001 (10) |
N3 | 0.036 (2) | 0.0233 (14) | 0.0265 (18) | −0.0089 (14) | 0.0012 (16) | −0.0016 (13) |
C3 | 0.045 (3) | 0.0118 (15) | 0.057 (3) | 0.0050 (16) | −0.002 (2) | −0.0025 (17) |
Co4 | 0.0225 (3) | 0.01451 (19) | 0.0290 (3) | 0.00154 (19) | −0.0046 (2) | −0.00179 (19) |
O4 | 0.0242 (14) | 0.0139 (10) | 0.0286 (14) | −0.0017 (10) | −0.0075 (12) | −0.0008 (10) |
N4 | 0.040 (2) | 0.0180 (13) | 0.0273 (18) | −0.0013 (14) | 0.0017 (16) | −0.0008 (13) |
C4 | 0.032 (2) | 0.0197 (16) | 0.048 (3) | 0.0086 (16) | 0.003 (2) | −0.0014 (17) |
O5 | 0.0278 (15) | 0.0202 (11) | 0.0264 (14) | 0.0038 (10) | −0.0018 (12) | 0.0008 (10) |
N5 | 0.035 (2) | 0.0169 (13) | 0.0286 (18) | 0.0006 (13) | −0.0085 (16) | −0.0035 (12) |
C5 | 0.031 (2) | 0.0257 (18) | 0.047 (3) | 0.0028 (17) | −0.001 (2) | 0.0030 (18) |
O6 | 0.0224 (14) | 0.0209 (11) | 0.0306 (15) | 0.0036 (10) | −0.0004 (12) | 0.0001 (10) |
N6 | 0.0334 (19) | 0.0192 (13) | 0.0320 (19) | −0.0012 (13) | −0.0081 (16) | −0.0014 (13) |
C6 | 0.020 (2) | 0.039 (2) | 0.046 (3) | 0.0007 (17) | −0.005 (2) | 0.0041 (19) |
O7 | 0.0395 (17) | 0.0204 (11) | 0.0325 (16) | −0.0040 (11) | −0.0014 (14) | −0.0013 (11) |
N7 | 0.0240 (18) | 0.0355 (16) | 0.031 (2) | 0.0042 (14) | −0.0027 (16) | 0.0001 (15) |
C7 | 0.030 (2) | 0.0252 (17) | 0.037 (2) | −0.0070 (16) | −0.006 (2) | 0.0006 (17) |
O8 | 0.0356 (16) | 0.0223 (11) | 0.0273 (15) | −0.0009 (11) | −0.0059 (13) | −0.0033 (11) |
N8 | 0.034 (2) | 0.0219 (14) | 0.0302 (19) | 0.0088 (14) | −0.0024 (16) | −0.0055 (13) |
C8 | 0.029 (2) | 0.0204 (16) | 0.033 (2) | −0.0005 (15) | −0.0017 (19) | −0.0011 (16) |
C9 | 0.028 (2) | 0.0198 (15) | 0.030 (2) | 0.0001 (15) | 0.0002 (18) | −0.0015 (15) |
C10 | 0.024 (2) | 0.0200 (15) | 0.030 (2) | 0.0012 (15) | 0.0026 (18) | 0.0023 (15) |
C11 | 0.036 (2) | 0.0253 (17) | 0.032 (2) | −0.0045 (17) | −0.006 (2) | 0.0050 (16) |
C12 | 0.035 (3) | 0.033 (2) | 0.051 (3) | −0.0053 (18) | −0.006 (2) | 0.0074 (19) |
C13 | 0.037 (3) | 0.049 (3) | 0.070 (4) | −0.016 (2) | −0.004 (3) | 0.003 (2) |
C14 | 0.048 (3) | 0.0245 (18) | 0.059 (3) | −0.0145 (19) | −0.004 (3) | 0.0006 (19) |
C15 | 0.064 (3) | 0.0240 (18) | 0.067 (3) | −0.021 (2) | 0.021 (3) | −0.008 (2) |
C16 | 0.084 (4) | 0.0157 (17) | 0.082 (4) | −0.009 (2) | 0.037 (3) | −0.013 (2) |
C17 | 0.071 (4) | 0.0166 (17) | 0.074 (4) | 0.005 (2) | 0.022 (3) | 0.002 (2) |
C18 | 0.052 (3) | 0.0211 (17) | 0.034 (2) | −0.0004 (18) | 0.002 (2) | 0.0017 (17) |
C19 | 0.049 (3) | 0.0248 (17) | 0.031 (2) | −0.0152 (18) | 0.001 (2) | −0.0029 (16) |
C20 | 0.052 (3) | 0.0226 (17) | 0.025 (2) | −0.0087 (18) | 0.010 (2) | −0.0013 (16) |
C21 | 0.040 (3) | 0.0256 (18) | 0.045 (3) | 0.0041 (17) | −0.014 (2) | −0.0092 (18) |
C22 | 0.053 (3) | 0.0250 (19) | 0.094 (4) | 0.015 (2) | −0.032 (3) | −0.018 (2) |
C23 | 0.094 (4) | 0.026 (2) | 0.121 (5) | 0.022 (2) | −0.064 (4) | −0.033 (3) |
C24 | 0.068 (3) | 0.0241 (19) | 0.107 (4) | 0.004 (2) | −0.054 (3) | −0.020 (2) |
C25 | 0.049 (3) | 0.0283 (19) | 0.053 (3) | −0.0069 (19) | −0.028 (2) | −0.0058 (19) |
C26 | 0.042 (3) | 0.039 (2) | 0.039 (3) | −0.007 (2) | −0.022 (2) | −0.0012 (19) |
C27 | 0.038 (3) | 0.036 (2) | 0.042 (3) | 0.0073 (19) | −0.010 (2) | 0.0054 (19) |
C28 | 0.041 (3) | 0.0246 (17) | 0.042 (3) | 0.0020 (17) | −0.009 (2) | −0.0038 (18) |
C29 | 0.041 (3) | 0.0184 (16) | 0.046 (3) | 0.0011 (16) | −0.019 (2) | −0.0080 (17) |
C30 | 0.037 (2) | 0.0228 (16) | 0.040 (2) | −0.0038 (17) | −0.014 (2) | −0.0035 (17) |
C31 | 0.029 (2) | 0.042 (2) | 0.038 (3) | −0.0067 (18) | −0.003 (2) | 0.0054 (19) |
C32 | 0.028 (3) | 0.073 (3) | 0.060 (3) | −0.017 (2) | 0.006 (3) | −0.008 (3) |
C33 | 0.024 (3) | 0.107 (5) | 0.150 (7) | −0.005 (3) | 0.010 (4) | −0.050 (5) |
C34 | 0.026 (3) | 0.091 (4) | 0.161 (7) | 0.012 (3) | 0.008 (4) | −0.054 (4) |
C35 | 0.048 (3) | 0.053 (2) | 0.054 (3) | 0.031 (2) | −0.011 (3) | −0.017 (2) |
C36 | 0.074 (4) | 0.036 (2) | 0.044 (3) | 0.026 (2) | −0.002 (3) | −0.008 (2) |
C37 | 0.072 (3) | 0.0220 (17) | 0.033 (2) | 0.006 (2) | 0.003 (2) | −0.0021 (17) |
C38 | 0.045 (3) | 0.0262 (18) | 0.031 (2) | 0.0022 (18) | −0.002 (2) | 0.0000 (17) |
C39 | 0.037 (3) | 0.041 (2) | 0.035 (2) | 0.0142 (19) | −0.002 (2) | −0.0134 (19) |
C40 | 0.030 (3) | 0.056 (3) | 0.039 (3) | 0.012 (2) | −0.002 (2) | −0.015 (2) |
C41 | 0.025 (2) | 0.0186 (15) | 0.029 (2) | −0.0075 (14) | −0.0003 (17) | 0.0010 (15) |
C43 | 0.035 (2) | 0.0218 (16) | 0.029 (2) | 0.0059 (16) | −0.0044 (19) | −0.0009 (16) |
C44A | 0.054 (3) | 0.034 (2) | 0.032 (2) | −0.006 (2) | 0.002 (2) | −0.0072 (18) |
F43A | 0.069 (5) | 0.030 (3) | 0.054 (4) | 0.006 (3) | −0.005 (4) | 0.007 (3) |
F43C | 0.092 (6) | 0.079 (5) | 0.025 (4) | −0.028 (5) | −0.009 (4) | 0.002 (4) |
F43B | 0.058 (5) | 0.081 (5) | 0.051 (5) | 0.019 (4) | 0.013 (4) | −0.011 (4) |
C44B | 0.054 (3) | 0.034 (2) | 0.032 (2) | −0.006 (2) | 0.002 (2) | −0.0072 (18) |
F43F | 0.099 (9) | 0.070 (7) | 0.033 (6) | −0.051 (7) | −0.009 (7) | −0.019 (5) |
F43E | 0.044 (6) | 0.112 (9) | 0.039 (6) | −0.016 (7) | 0.021 (5) | −0.003 (7) |
F43D | 0.095 (9) | 0.068 (7) | 0.034 (6) | 0.032 (7) | −0.008 (6) | 0.022 (5) |
C44C | 0.054 (3) | 0.034 (2) | 0.032 (2) | −0.006 (2) | 0.002 (2) | −0.0072 (18) |
F43I | 0.110 (11) | 0.052 (6) | 0.035 (6) | −0.007 (7) | 0.000 (7) | −0.016 (5) |
F43H | 0.055 (7) | 0.036 (5) | 0.027 (5) | −0.007 (5) | 0.003 (5) | 0.004 (4) |
F43G | 0.088 (8) | 0.066 (7) | 0.037 (6) | −0.024 (6) | −0.021 (6) | 0.024 (5) |
O1S | 0.055 (3) | 0.088 (3) | 0.137 (4) | 0.020 (2) | 0.030 (3) | 0.062 (3) |
F42A | 0.0443 (18) | 0.130 (3) | 0.0363 (17) | 0.0133 (19) | 0.0084 (14) | −0.0041 (18) |
F42C | 0.071 (2) | 0.0491 (14) | 0.0437 (16) | −0.0208 (14) | −0.0039 (15) | −0.0076 (13) |
F42B | 0.158 (3) | 0.0340 (13) | 0.0341 (16) | 0.0388 (17) | 0.0113 (19) | 0.0088 (11) |
C42 | 0.032 (2) | 0.0202 (16) | 0.036 (2) | 0.0011 (16) | 0.0028 (19) | 0.0025 (16) |
Co1—O2 | 2.083 (3) | C14—C19 | 1.380 (6) |
Co1—O1 | 2.091 (2) | C14—H14 | 0.9500 |
Co1—O4 | 2.095 (3) | C15—C16 | 1.360 (7) |
Co1—N1 | 2.122 (3) | C15—C20 | 1.394 (5) |
Co1—O5 | 2.129 (3) | C15—H15 | 0.9500 |
Co1—N2 | 2.134 (3) | C16—C17 | 1.370 (8) |
Co1—Co4 | 3.0283 (7) | C16—H16 | 0.9500 |
O1—Co2 | 2.086 (3) | C17—C18 | 1.386 (5) |
O1—Co4 | 2.088 (3) | C17—H17 | 0.9500 |
O1—H1O | 0.952 (18) | C18—H18 | 0.9500 |
N1—C1 | 1.338 (5) | C19—C20 | 1.484 (6) |
N1—C9 | 1.353 (5) | C21—C22 | 1.377 (6) |
C1—C2 | 1.385 (5) | C21—H21 | 0.9500 |
C1—H1 | 0.9500 | C22—C23 | 1.362 (7) |
Co2—O2 | 2.087 (2) | C22—H22 | 0.9500 |
Co2—O3 | 2.104 (3) | C23—C24 | 1.379 (7) |
Co2—N4 | 2.118 (3) | C23—H23 | 0.9500 |
Co2—N3 | 2.120 (4) | C24—C29 | 1.407 (5) |
Co2—O7 | 2.138 (3) | C24—H24 | 0.9500 |
Co2—Co3 | 3.0034 (7) | C25—C26 | 1.377 (6) |
Co2—Co4 | 3.2419 (8) | C25—C30 | 1.385 (6) |
O2—Co3 | 2.092 (3) | C25—H25 | 0.9500 |
O2—H2O | 0.967 (19) | C26—C27 | 1.390 (6) |
N2—C8 | 1.337 (5) | C26—H26 | 0.9500 |
N2—C10 | 1.350 (4) | C27—C28 | 1.376 (6) |
C2—C3 | 1.383 (6) | C27—H27 | 0.9500 |
C2—H2 | 0.9500 | C28—H28 | 0.9500 |
Co3—O3 | 2.073 (2) | C29—C30 | 1.481 (6) |
Co3—O4 | 2.101 (3) | C31—C32 | 1.368 (6) |
Co3—N5 | 2.113 (3) | C31—H59 | 0.9500 |
Co3—N6 | 2.133 (3) | C32—C33 | 1.366 (8) |
Co3—O8 | 2.154 (3) | C32—H54 | 0.9500 |
Co3—Co4 | 3.1864 (7) | C33—C34 | 1.373 (9) |
O3—Co4 | 2.089 (3) | C33—H10 | 0.9500 |
O3—H3O | 0.966 (9) | C34—C40 | 1.386 (7) |
N3—C11 | 1.336 (5) | C34—H73 | 0.9500 |
N3—C19 | 1.354 (5) | C35—C36 | 1.361 (7) |
C3—C4 | 1.376 (6) | C35—C39 | 1.396 (6) |
C3—H3 | 0.9500 | C35—H64 | 0.9500 |
Co4—O4 | 2.085 (2) | C36—C37 | 1.370 (7) |
Co4—N8 | 2.129 (3) | C36—H42 | 0.9500 |
Co4—N7 | 2.134 (3) | C37—C38 | 1.388 (5) |
Co4—O6 | 2.152 (3) | C37—H44 | 0.9500 |
O4—H4O | 0.962 (18) | C38—H48 | 0.9500 |
N4—C18 | 1.335 (5) | C39—C40 | 1.490 (6) |
N4—C20 | 1.340 (6) | C41—C42 | 1.534 (6) |
C4—C9 | 1.395 (5) | C43—C44A | 1.537 (6) |
C4—H4 | 0.9500 | C44A—F43A | 1.331 (6) |
O5—C41 | 1.248 (4) | C44A—F43C | 1.336 (8) |
N5—C29 | 1.331 (5) | C44A—F43B | 1.353 (7) |
N5—C21 | 1.344 (5) | O1S—H1SA | 0.977 (16) |
C5—C6 | 1.372 (6) | O1S—H1SB | 0.988 (16) |
C5—C10 | 1.392 (6) | N1SB—C1SB | 1.1291 |
C5—H5 | 0.9500 | C1SB—C2SB | 1.4491 |
O6—C41 | 1.248 (4) | C2SB—H2S4 | 0.9800 |
N6—C28 | 1.336 (5) | C2SB—H2S5 | 0.9800 |
N6—C30 | 1.355 (5) | C2SB—H2S6 | 0.9800 |
C6—C7 | 1.394 (6) | N1SA—C1SA | 1.1291 |
C6—H6 | 0.9500 | C1SA—C2SA | 1.4491 |
O7—C43 | 1.245 (5) | C2SA—H2S1 | 0.9800 |
N7—C31 | 1.338 (5) | C2SA—H2S2 | 0.9800 |
N7—C40 | 1.337 (6) | C2SA—H2S3 | 0.9800 |
C7—C8 | 1.379 (6) | N2SB—C3SB | 1.1290 |
C7—H7 | 0.9500 | C3SB—C4SB | 1.4491 |
O8—C43 | 1.244 (5) | C4SB—H4S4 | 0.9800 |
N8—C39 | 1.342 (6) | C4SB—H4S5 | 0.9800 |
N8—C38 | 1.346 (5) | C4SB—H4S6 | 0.9800 |
C8—H8 | 0.9500 | N2SA—C3SA | 1.1290 |
C9—C10 | 1.483 (5) | C3SA—C4SA | 1.4491 |
C11—C12 | 1.378 (6) | C4SA—H4S1 | 0.9800 |
C11—H11 | 0.9500 | C4SA—H4S2 | 0.9800 |
C12—C13 | 1.372 (6) | C4SA—H4S3 | 0.9800 |
C12—H12 | 0.9500 | F42A—C42 | 1.330 (5) |
C13—C14 | 1.397 (7) | F42C—C42 | 1.341 (5) |
C13—H13 | 0.9500 | F42B—C42 | 1.292 (5) |
O2—Co1—O1 | 80.29 (9) | C41—O6—Co4 | 123.6 (2) |
O2—Co1—O4 | 78.6 (1) | C28—N6—C30 | 117.5 (4) |
O1—Co1—O4 | 84.42 (9) | C28—N6—Co3 | 126.3 (3) |
O2—Co1—N1 | 101.6 (1) | C30—N6—Co3 | 115.6 (3) |
O1—Co1—N1 | 175.91 (11) | C5—C6—C7 | 118.5 (4) |
O4—Co1—N1 | 99.5 (1) | C5—C6—H6 | 120.8 |
O2—Co1—O5 | 166.98 (10) | C7—C6—H6 | 120.8 |
O1—Co1—O5 | 89.37 (9) | C43—O7—Co2 | 123.6 (3) |
O4—Co1—O5 | 92.57 (10) | C31—N7—C40 | 117.3 (4) |
N1—Co1—O5 | 89.2 (1) | C31—N7—Co4 | 126.2 (3) |
O2—Co1—N2 | 99.68 (11) | C40—N7—Co4 | 116.4 (3) |
O1—Co1—N2 | 99.49 (10) | C8—C7—C6 | 118.7 (4) |
O4—Co1—N2 | 175.47 (10) | C8—C7—H7 | 120.7 |
N1—Co1—N2 | 76.7 (1) | C6—C7—H7 | 120.7 |
O5—Co1—N2 | 89.7 (1) | C43—O8—Co3 | 124.7 (3) |
O2—Co1—Co4 | 87.36 (7) | C39—N8—C38 | 118.5 (3) |
N1—Co1—Co4 | 139.78 (9) | C39—N8—Co4 | 116.6 (3) |
O5—Co1—Co4 | 79.68 (7) | C38—N8—Co4 | 124.8 (3) |
N2—Co1—Co4 | 140.94 (7) | N2—C8—C7 | 123.1 (3) |
Co2—O1—Co4 | 101.9 (1) | N2—C8—H8 | 118.4 |
Co2—O1—Co1 | 99.3 (1) | C7—C8—H8 | 118.4 |
Co4—O1—Co1 | 92.85 (9) | N1—C9—C4 | 120.9 (3) |
Co2—O1—H1O | 125 (2) | N1—C9—C10 | 115.5 (3) |
Co4—O1—H1O | 116 (2) | C4—C9—C10 | 123.5 (4) |
Co1—O1—H1O | 115 (2) | N2—C10—C5 | 121.3 (3) |
C1—N1—C9 | 118.8 (3) | N2—C10—C9 | 115.2 (3) |
C1—N1—Co1 | 125.1 (3) | C5—C10—C9 | 123.4 (3) |
C9—N1—Co1 | 116.1 (2) | N3—C11—C12 | 123.2 (4) |
N1—C1—C2 | 123.2 (4) | N3—C11—H11 | 118.4 |
N1—C1—H1 | 118.4 | C12—C11—H11 | 118.4 |
C2—C1—H1 | 118.4 | C13—C12—C11 | 118.7 (4) |
O1—Co2—O2 | 80.32 (9) | C13—C12—H12 | 120.7 |
O1—Co2—O3 | 78.2 (1) | C11—C12—H12 | 120.7 |
O2—Co2—O3 | 85.05 (9) | C12—C13—C14 | 119.0 (5) |
O1—Co2—N4 | 98.1 (1) | C12—C13—H13 | 120.5 |
O2—Co2—N4 | 173.35 (12) | C14—C13—H13 | 120.5 |
O3—Co2—N4 | 101.0 (1) | C19—C14—C13 | 119.2 (4) |
O1—Co2—N3 | 101.9 (1) | C19—C14—H14 | 120.4 |
O2—Co2—N3 | 96.84 (11) | C13—C14—H14 | 120.4 |
O3—Co2—N3 | 178.11 (10) | C16—C15—C20 | 119.2 (5) |
N4—Co2—N3 | 77.10 (13) | C16—C15—H15 | 120.4 |
O1—Co2—O7 | 167.81 (10) | C20—C15—H15 | 120.4 |
O2—Co2—O7 | 92.98 (10) | C15—C16—C17 | 119.4 (4) |
O3—Co2—O7 | 91.12 (11) | C15—C16—H16 | 120.3 |
N4—Co2—O7 | 89.67 (11) | C17—C16—H16 | 120.3 |
N3—Co2—O7 | 88.91 (12) | C16—C17—C18 | 119.0 (5) |
O1—Co2—Co3 | 87.33 (7) | C16—C17—H17 | 120.5 |
N4—Co2—Co3 | 142.48 (10) | C18—C17—H17 | 120.5 |
N3—Co2—Co3 | 138.22 (8) | N4—C18—C17 | 122.0 (5) |
O7—Co2—Co3 | 80.82 (7) | N4—C18—H18 | 119.0 |
O2—Co2—Co4 | 81.77 (7) | C17—C18—H18 | 119.0 |
N4—Co2—Co4 | 101.14 (10) | N3—C19—C14 | 121.5 (4) |
N3—Co2—Co4 | 140.87 (9) | N3—C19—C20 | 114.9 (4) |
O7—Co2—Co4 | 130.19 (8) | C14—C19—C20 | 123.6 (4) |
Co3—Co2—Co4 | 61.21 (2) | N4—C20—C15 | 121.6 (4) |
Co1—O2—Co2 | 99.5 (1) | N4—C20—C19 | 115.8 (3) |
Co1—O2—Co3 | 101.8 (1) | C15—C20—C19 | 122.6 (4) |
Co2—O2—Co3 | 91.88 (9) | N5—C21—C22 | 122.2 (4) |
Co1—O2—H2O | 123.1 (17) | N5—C21—H21 | 118.9 |
Co2—O2—H2O | 117.1 (15) | C22—C21—H21 | 118.9 |
Co3—O2—H2O | 117.7 (12) | C23—C22—C21 | 119.0 (4) |
C8—N2—C10 | 118.4 (3) | C23—C22—H22 | 120.5 |
C8—N2—Co1 | 125.7 (2) | C21—C22—H22 | 120.5 |
C10—N2—Co1 | 115.9 (2) | C22—C23—C24 | 119.8 (4) |
C3—C2—C1 | 117.8 (4) | C22—C23—H23 | 120.1 |
C3—C2—H2 | 121.1 | C24—C23—H23 | 120.1 |
C1—C2—H2 | 121.1 | C23—C24—C29 | 118.5 (5) |
O3—Co3—O2 | 85.7 (1) | C23—C24—H24 | 120.8 |
O3—Co3—O4 | 80.21 (9) | C29—C24—H24 | 120.8 |
O2—Co3—O4 | 78.3 (1) | C26—C25—C30 | 120.8 (4) |
O3—Co3—N5 | 173.75 (12) | C26—C25—H25 | 119.6 |
O2—Co3—N5 | 99.95 (11) | C30—C25—H25 | 119.6 |
O4—Co3—N5 | 98.24 (11) | C25—C26—C27 | 118.0 (4) |
O3—Co3—N6 | 97.72 (11) | C25—C26—H26 | 121.0 |
O2—Co3—N6 | 174.46 (12) | C27—C26—H26 | 121.0 |
O4—Co3—N6 | 106.50 (12) | C28—C27—C26 | 118.2 (4) |
N5—Co3—N6 | 76.84 (12) | C28—C27—H27 | 120.9 |
O3—Co3—O8 | 91.99 (10) | C26—C27—H27 | 120.9 |
O2—Co3—O8 | 90.22 (10) | N6—C28—C27 | 124.4 (4) |
O4—Co3—O8 | 166.52 (10) | N6—C28—H28 | 117.8 |
N5—Co3—O8 | 90.65 (11) | C27—C28—H28 | 117.8 |
N6—Co3—O8 | 85.33 (12) | N5—C29—C24 | 121.1 (4) |
O4—Co3—Co2 | 87.38 (7) | N5—C29—C30 | 116.5 (3) |
N5—Co3—Co2 | 141.76 (10) | C24—C29—C30 | 122.4 (4) |
N6—Co3—Co2 | 137.73 (8) | N6—C30—C25 | 121.1 (4) |
O8—Co3—Co2 | 79.40 (7) | N6—C30—C29 | 114.5 (4) |
O2—Co3—Co4 | 83.10 (7) | C25—C30—C29 | 124.3 (4) |
N5—Co3—Co4 | 137.37 (9) | N7—C31—C32 | 125.3 (4) |
N6—Co3—Co4 | 102.33 (9) | N7—C31—H59 | 117.4 |
O8—Co3—Co4 | 131.98 (7) | C32—C31—H59 | 117.4 |
Co2—Co3—Co4 | 63.09 (2) | C33—C32—C31 | 116.7 (5) |
Co3—O3—Co4 | 99.9 (1) | C33—C32—H54 | 121.6 |
Co3—O3—Co2 | 92.0 (1) | C31—C32—H54 | 121.6 |
Co4—O3—Co2 | 101.29 (11) | C32—C33—C34 | 119.6 (5) |
Co3—O3—H3O | 114.9 (14) | C32—C33—H10 | 120.2 |
Co4—O3—H3O | 126.3 (14) | C34—C33—H10 | 120.2 |
Co2—O3—H3O | 116.1 (13) | C33—C34—C40 | 120.0 (6) |
C11—N3—C19 | 118.4 (4) | C33—C34—H73 | 120.0 |
C11—N3—Co2 | 125.6 (3) | C40—C34—H73 | 120.0 |
C19—N3—Co2 | 115.9 (3) | C36—C35—C39 | 118.7 (5) |
C4—C3—C2 | 119.8 (3) | C36—C35—H64 | 120.7 |
C4—C3—H3 | 120.1 | C39—C35—H64 | 120.7 |
C2—C3—H3 | 120.1 | C35—C36—C37 | 120.2 (4) |
O4—Co4—O1 | 84.73 (9) | C35—C36—H42 | 119.9 |
O4—Co4—O3 | 80.20 (9) | C37—C36—H42 | 119.9 |
O1—Co4—O3 | 78.5 (1) | C36—C37—C38 | 118.7 (4) |
O4—Co4—N8 | 172.0 (1) | C36—C37—H44 | 120.6 |
O1—Co4—N8 | 103.2 (1) | C38—C37—H44 | 120.6 |
O3—Co4—N8 | 100.4 (1) | N8—C38—C37 | 122.0 (4) |
O4—Co4—N7 | 95.73 (11) | N8—C38—H48 | 119.0 |
O1—Co4—N7 | 177.39 (12) | C37—C38—H48 | 119.0 |
O3—Co4—N7 | 99.02 (12) | N8—C39—C35 | 121.9 (4) |
N8—Co4—N7 | 76.29 (13) | N8—C39—C40 | 115.0 (4) |
O4—Co4—O6 | 92.8 (1) | C35—C39—C40 | 123.1 (4) |
O1—Co4—O6 | 89.6 (1) | N7—C40—C34 | 120.7 (5) |
O3—Co4—O6 | 166.7 (1) | N7—C40—C39 | 115.3 (4) |
N8—Co4—O6 | 88.10 (11) | C34—C40—C39 | 123.9 (5) |
N7—Co4—O6 | 92.92 (12) | O6—C41—O5 | 131.1 (4) |
O3—Co4—Co1 | 87.23 (7) | O6—C41—C42 | 115.3 (3) |
N8—Co4—Co1 | 144.13 (10) | O5—C41—C42 | 113.5 (3) |
N7—Co4—Co1 | 137.53 (9) | O8—C43—O7 | 131.4 (4) |
O6—Co4—Co1 | 79.97 (7) | O8—C43—C44A | 113.9 (3) |
O1—Co4—Co3 | 82.55 (7) | O7—C43—C44A | 114.8 (3) |
N8—Co4—Co3 | 138.65 (9) | F43A—C44A—F43C | 106.4 (5) |
N7—Co4—Co3 | 96.12 (9) | F43A—C44A—F43B | 109.3 (6) |
O6—Co4—Co3 | 133.18 (7) | F43C—C44A—F43B | 103.6 (5) |
Co1—Co4—Co3 | 62.80 (2) | F43A—C44A—C43 | 115.9 (4) |
O4—Co4—Co2 | 81.49 (7) | F43C—C44A—C43 | 112.2 (4) |
N8—Co4—Co2 | 104.10 (9) | F43B—C44A—C43 | 108.7 (5) |
N7—Co4—Co2 | 138.48 (10) | H1SA—O1S—H1SB | 108 (2) |
O6—Co4—Co2 | 128.53 (7) | N1SB—C1SB—C2SB | 178.9 |
Co1—Co4—Co2 | 60.90 (2) | N1SA—C1SA—C2SA | 178.8 |
Co3—Co4—Co2 | 55.79 (2) | N2SB—C3SB—C4SB | 178.85 (14) |
Co4—O4—Co1 | 92.85 (9) | C3SB—C4SB—H4S4 | 109.5 |
Co4—O4—Co3 | 99.1 (1) | C3SB—C4SB—H4S5 | 109.5 |
Co1—O4—Co3 | 101.2 (1) | H4S4—C4SB—H4S5 | 109.5 |
Co4—O4—H4O | 121 (2) | C3SB—C4SB—H4S6 | 109.5 |
Co1—O4—H4O | 105 (2) | H4S4—C4SB—H4S6 | 109.5 |
Co3—O4—H4O | 130 (2) | H4S5—C4SB—H4S6 | 109.5 |
C18—N4—C20 | 118.7 (3) | N2SA—C3SA—C4SA | 178.8 |
C18—N4—Co2 | 125.3 (3) | C3SA—C4SA—H4S1 | 109.5 |
C20—N4—Co2 | 115.8 (3) | C3SA—C4SA—H4S2 | 109.5 |
C3—C4—C9 | 119.3 (4) | H4S1—C4SA—H4S2 | 109.5 |
C3—C4—H4 | 120.3 | C3SA—C4SA—H4S3 | 109.5 |
C9—C4—H4 | 120.3 | H4S1—C4SA—H4S3 | 109.5 |
C41—O5—Co1 | 125.1 (2) | H4S2—C4SA—H4S3 | 109.5 |
C29—N5—C21 | 119.3 (3) | F42B—C42—F42A | 108.4 (4) |
C29—N5—Co3 | 116.2 (2) | F42B—C42—F42C | 105.7 (4) |
C21—N5—Co3 | 124.4 (3) | F42A—C42—F42C | 103.2 (3) |
C6—C5—C10 | 120.0 (4) | F42B—C42—C41 | 115.0 (3) |
C6—C5—H5 | 120.0 | F42A—C42—C41 | 113.4 (3) |
C10—C5—H5 | 120.0 | F42C—C42—C41 | 110.3 (3) |
D—H···A | D—H | H···A | D···A | D—H···A |
O1—H1O···I1A | 0.95 (2) | 2.78 (2) | 3.672 (2) | 157 (3) |
O2—H2O···I2 | 0.97 (1) | 2.67 (1) | 3.641 (2) | 176 (2) |
O3—H3O···N1SA | 0.97 (1) | 2.04 (1) | 2.944 (7) | 155 (2) |
O4—H4O···O1S | 0.96 (2) | 2.08 (2) | 2.954 (5) | 150 (3) |
O1S—H1SB···I1Ai | 0.99 (2) | 2.49 (3) | 3.471 (4) | 171 (3) |
O1S—H1SA···N2SA | 0.98 (2) | 1.86 (2) | 2.79 (1) | 159 (3) |
Symmetry code: (i) −x+1, y+1/2, −z+1/2. |