Tetrakis(2,2′-bi­pyridine)­tetra-μ3-hydro­xo-di-μ-tri­fluoro­acetato-tetracobalt(II) diiodide diaceto­nitrile monohydrate: a compound containing a tetranuclear `cubane'-type cobalt(II) core

Zhao, H.; Bacsa, J.; Dunbar, K.R.

doi:10.1107/S1600536804008979

Tetrakis(2,2′-bipyridine)tetra-μ₃-hydroxo-di-μ-trifluoroacetato-tetracobalt(II) diiodide diacetonitrile monohydrate: a compound containing a tetranuclear `cubane'-type cobalt(II) core

A new compound, [Co₄(C₂F₃O₂)₂(OH)₄(C₁₀H₈N₂)₄]I₂·2C₂H₃N·H₂O, containing a tetranuclear cobalt(II)–hydroxo core with a cube-like structural geometry is reported. The four Co^II coordination polyhedra are irregular octahedra and the Co^II atoms are linked by three hydroxo and trifluoroacetate ions resulting in a Co₄O₄ core with approximate tetrahedral symmetry. The coordination polyhedra share edges with short Co

Co distances. A bond valence analysis shows that a cube-like arrangement of atoms in a tetranuclear cluster is ideal for the clusters [M₄(OR)₄]⁴⁺ (R is a strongly binding group) and [M₄O₄]⁸⁺ when the metal ions are in oxidation states of +2 and +4, respectively.

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Supporting information

	Crystallographic Information File (CIF) https://doi.org/10.1107/S1600536804008979/fl6099sup1.cif Contains datablocks global, I
	Structure factor file (CIF format) https://doi.org/10.1107/S1600536804008979/fl6099Isup2.hkl Contains datablock I

CCDC reference: 239076

checkCIF report

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.

 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.

 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.

 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.

 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.

 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

Computing details top

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).

Tetrakis(2,2'-bipyridine)tetra-µ₃-hydroxo-di-µ-trifluoroacetato- tetracobalt(II) diiodide diacetonitrile monohydrate top

Crystal data top

[Co₄(C₂F₃O₂)₂(OH)₄(C₁₀H₈N₂)₄]I₂·2C₂H₃N·H₂O	F(000) = 5936
M_r = 1508.45	D_x = 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

Data collection top

SMART APEX CCD area-detector diffractometer	12523 independent reflections
Radiation source: fine-focus sealed tube	8819 reflections with I > 2σ(I)
Graphite monochromator	R_int = 0.068
ω and φ scans	θ_max = 27.5°, θ_min = 2.4°
Absorption correction: multi-scan (SADABS; Bruker, 2003)	h = −25→23
T_min = 0.549, T_max = 0.782	k = −24→24
72201 measured reflections	l = −38→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)] = 0.058	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(F_o²) + (0.0647P)² + 25.7334P] where P = (F_o² + 2F_c²)/3
12523 reflections	(Δ/σ)_max = 0.028
775 parameters	Δρ_max = 1.67 e Å⁻³
119 restraints	Δρ_min = −1.00 e Å⁻³

Special details top

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.

Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å²) top

	x	y	z	U_iso*/U_eq	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)

Atomic displacement parameters (Å²) top

	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)

Geometric parameters (Å, º) top

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)

Hydrogen-bond geometry (Å, º) top

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.

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Tetrakis(2,2′-bi­pyridine)­tetra-μ3-hydro­xo-di-μ-tri­fluoro­acetato-tetracobalt(II) diiodide diaceto­nitrile monohydrate: a compound containing a tetranuclear `cubane'-type cobalt(II) core

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Key indicators

checkCIF/PLATON results

Tetrakis(2,2′-bipyridine)tetra-μ₃-hydroxo-di-μ-trifluoroacetato-tetracobalt(II) diiodide diacetonitrile monohydrate: a compound containing a tetranuclear `cubane'-type cobalt(II) core