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Homoleptic 2,2′-bi­pyridine (bipy) metalates of iron and cobalt have been synthesized directly from the corresponding homo­leptic anthracene metalates. In the iron structure, bis­[([2.2.2]cryptand)potassium(I)] tris­(2,2′-bi­pyridine)­fer­rate(–I) anthracene(–I), [K(C18H36N2O6)]2[Fe(C10H8N2)3](C14H10), the asymmetric unit contains one potassium complex cation in a general position, the Fe center and one and a half bipy ligands of the ferrate complex on a crystallographic twofold axis that includes the Fe atom, and one half of an anthracene radical anion whose other half is generated by a crystallographic inversion center. The cations and anions are well separated and the geometry about the Fe center is essentially octa­hedral. In the cobalt structure, ([2.2.2]cryptand)potassium(I) bis­(2,2′-bi­pyridine)­cobaltate(–I) anthracene hemisolvate tetra­hydro­furan (THF) disolvate, [K(C18H36N2O6)][Co(C10H8N2)2]·0.5C14H10·2C4H8O, the asymmetric unit contains the cation, anion, and both cocrystallized THF solvent mol­ecules in general positions, and one half of a cocrystallized anthracene mol­ecule whose other half is generated by a crystallographic inversion center. The cation and anion are well separated and the ligand planes in the cobaltate anion are periplanar. Each anthracene mol­ecule is midway between and is oriented perpendicular to a pair of symmetry-related bipy ligands such that aromatic donor–acceptor inter­actions may play a role in the packing arrangement. The lengths of the bonds that connect the bipy rings support the assertion that the ligands are bipy radical anions in the iron structure. However, in the case of cobalt, these lengths are between the known ranges for a bipy radical anion and a bipy dianion, and therefore no conclusion can be made from the crystallography alone. One cocrystallized THF solvent mol­ecule in the cobalt structure was modeled as disordered over three positions with appropriate geometric and thermal restraints, which resulted in a refined component mass ratio of 0.412 (4):0.387 (3):0.201 (3).

Supporting information

cif

Crystallographic Information File (CIF) https://doi.org/10.1107/S2053229614017070/ov3050sup1.cif
Contains datablocks 1, 2, global

hkl

Structure factor file (CIF format) https://doi.org/10.1107/S2053229614017070/ov30501sup2.hkl
Contains datablock 1

hkl

Structure factor file (CIF format) https://doi.org/10.1107/S2053229614017070/ov30502sup3.hkl
Contains datablock 2

CCDC references: 1015727; 1015728

Introduction top

The 2,2'-bi­pyridine (bipy) ligand is used extensively in electrochemistry because of its superb redox activity. Anionic homoleptic bipy transition metalates like [Ti(bipy)3]-, [Mn(bipy)3]-, and [Cr(bipy)3]3- were first reported nearly 50 years ago (Uhlig, 1988, and references therein). The first homoleptic bipy ferrate [Fe(bipy)3]- was synthesized in the mid-1960s from both electrochemical (Tanaka & Sato, 1966) and chemical (Hall & Reynolds, 1966; Mahon & Reynolds, 1967) means, followed a few years later by the cobaltate [Co(bipy)2]-, which was generated by electrochemical methods (Dhar & Kurcz, 1974). Despite the long-known existence of these anions, this is first report of their structures by single-crystal X-ray diffraction. We report here the structure of bis­[([2.2.2]cryptand)potassium(I)] tris­(2,2'-bi­pyridine)­ferrate(–I) anthracene(–I), (I), and ([2.2.2]cryptand)potassium(I) bis­(2,2'-bi­pyridine)­cobaltate(–I) anthracene hemisolvate tetra­hydro­furan (THF) disolvate, (2).

Experimental top

Synthesis and crystallization top

Details for the synthesis and preliminary characterization of [K(18-crown-6)(THF)2][Fe(bipy)3].3THF (THF is tetra­hydro­furan and bipy is 2,2'-bi­pyridine) can be found elsewhere (Brennessel, 2009). Crystal data for this salt: trigonal, R3, a = 14.9665 (2), c = 48.766 (8) Å, V = 9460 (2) Å3, Z = 6; T = 173 (2) K, 3734 reflections (3014 for [I > 2σ(I)]).

Synthesis of (1) top

A room-temperature solution of excess bipy in THF was added to a deep-orange room-temperature THF solution of [K([2.2.2]cryptand)][Fe(η4-C14H10)2].0.5THF (Brennessel et al., 2007) that was known to contain an impurity of [K([2.2.2]cryptand)](C14H10). A yield was not determined because of the unknown amount of impurity in the starting material, and this product was only characterized by single-crystal X-ray diffraction. Purple–black plates were grown from a pentane-layered THF solution at 273 K.

Synthesis of (2) top

A solution of bipy (0.180 g, 1.15 mmol) in tetra­hydro­furan (30 ml, 195 K) was added to a deep pink–red solution of [K([2.2.2]cryptand)][Co(η4-C14H10)2].0.5THF (0.500 g, 0.577 mmol; Brennessel et al., 2002) in THF (60 ml, 195 K). The resulting solution was warmed slowly to room temperature, at which point it was deep purple. After the solvent was removed under vacuum, pentane (100 ml) was added with vigorous stirring. The product was filtered, washed with pentane (2 × 20 ml), and dried under vacuum, yielding a purple–black solid (yield 0.362 g, 62%). This product was only characterized by single-crystal X-ray diffraction. Purple–black rods were grown from a pentane-layered THF solution at 273 K.

Refinement top

Crystal data, data collection and structure refinement details are summarized in Table 1. The cocrystallized tetra­hydro­furan (THF) solvent molecule (O8/C43–C46) in (2) is located in a pocket that includes its inversion symmetry equivalent. After being modeled as disordered over two general positions, a third orientation could be found from the difference map. Thus, the molecule was modeled as disordered over three positions, with a refined ratio of 0.412 (4):0.387 (3):0.201 (3). Analogous bond lengths and angles among the three positions of the disordered THF molecule and both directions around the ring of the ordered THF molecule (O7/C39–C42) were restrained to be similar. Anistropic displacement parameters for pairs of near isopositional atoms were heavily restrained to be similar. Additionally, anisotropic displacement parameters for all atoms in the two major components of the disorder were restrained to be similar, and separately, the same for all the atoms in the ring of the third component. H atoms were placed geometrically and treated as riding atoms, with methyl­ene C—H = 0.99 Å and sp2 C—H = 0.95 Å, and with Uiso(H) = 1.2Ueq(C).

Results and discussion top

Both (1) and (2) were synthesized directly from homoleptic bis­(anthracene)metalate precursors, [M(η4-C14H10)2]- [M = Fe (Brennessel et al., 2007) and Co (Brennessel et al., 2002; Brennessel & Ellis, 2012)], the former of which is a 17-electron species. In the case of iron, two structures of the homoleptic bipy ferrate were determined. For the first, a solution of [K(18-crown-6)(THF)2][Fe(η4-C14H10)2] was reacted with excess bipy in THF at room temperature, and the crude product was layered with pentane. The resulting purple–black blocks were formulated as [K(18-crown-6)(THF)2][Fe(bipy)3].3THF based on a single-crystal X-ray experiment (Brennessel, 2009). However, due to the severe disorder in the crown ether and cocrystallized THF and the overall poor quality of the structure, a different crystallization was performed. The starting material for the second attempt was a sample of [K([2.2.2]cryptand)][Fe(η4-C14H10)2].0.5THF (Brennessel et al., 2007) that contained a known impurity of anthracene radical anion in the form of [K([2.2.2]cryptand)](C14H10) (the two salts are very difficult to separate). Single crystals were again grown from the crude reaction mixture by diffusion of pentane into a THF solution of the mixture, which resulted in good quality purple–black plates that were formulated as [K([2.2.2]cryptand)]2[Fe(bipy)3][C14H10], (1) (Fig. 1), based on this single-crystal X-ray experiment.

Because the charge assigned to the iron complex in (1) depends on the assignment of the charge on the cocrystallized anthracene species, a close inspection of the latter's bond lengths was required. The addition of an electron to neutral anthracene causes the lengthening of certain bonds and the shortening of others (Rosokha & Kochi, 2006). Fig. 2 shows the bond lengths of the cocrystallized anthracene in (1) along with those from low-temperature structures of known neutral [Cambridge Structural Database (CSD; Version 5.35, update No. 2, Febuary 2014; Allen, 2002) refcode ANTCEN11 (Brock & Dunitz, 1990)] and monoanionic forms (CSD refcode YETPAP; Rosokha & Kochi, 2006). The bond lengths in (1) match more closely with those of anthracene radical anion, and thus the iron complex is formulated as monoanionic.

The geometry of (1) is essentially o­cta­hedral, with only the bite angles of the bipy ligands causing the deviation from the perfect o­cta­hedron. Because the anion lies on a crystallographic twofold axis, there are two unique bite angles of 82.8 (1) and 81.8 (2)°. An electron count of the ferrate when considered as a mono-negative iron center with three neutral bipy ligands gives a 21-electron complex, which is not consistent with a low valent center with three acceptor ligands (Mitchell & Parish, 1969; Elschenbroich, 2005). Further examination suggests that the bipy ligands should not be considered neutral (see below).

A good indicator of the degree of reduction of coordinated bipy is the length of the bond that links the rings (Radonovich et al., 1982; England et al., 2012). In neutral bipy, this bond length is 1.490 (3) Å (CSD refcode BIPYRL03; Chisholm et al., 1981), in the bipy radical anion it is 1.431 (3) (CSD refcode QUPGAK; Gore-Randall et al., 2009) and 1.429 Å [CSD refcode QUPGEO (Gore-Randall et al., 2009); average of four independent bond lengths], and in the bipy dianion it has been reported as 1.376 (4) (CSD refcode JAXQUU; Bock et al., 1999) and 1.399 (6) Å (CSD refcode QUPGIS; Gore-Randall et al., 2009). The two independent values of this bond length in (1) are 1.431 (4) and 1.411 (6) Å, both which are between the neutral and dianionic extremes and essentially coincide with the average for salts of the monoanion. The two resonance structures that are likely the most important contributions to the overall bonding are shown in Fig. 3. ESR (electron spin resonance) spectroscopy has corroborated this by showing that one electron exists on each ligand without hopping (Motten et al., 1981), further supporting the assignment of a metal center with 18 valence electrons. Recent work by Wieghardt has concluded that (1) is best regarded as an FeII, d6 metal center with three bipy radical anionic ligands for which each unpaired electron is found in a ligand π* orbital (England et al., 2012; Scarborough & Wieghardt, 2011).

The cobalt anion was generated from a low-temperature reaction of [K([2.2.2]cryptand)][Co(η4-C14H10)2].0.5THF (Brennessel et al., 2002) and excess bipy at 195 K. The structure was formulated as [K([2.2.2]cryptand)][Co(bipy)2].0.5C14H10.2THF, (2), based on this single-crystal experiment (Fig. 4). Unlike in the case of (1), the cocrystallized anthracene molecule is neutral, as determined by bond-length comparisons with the neutral and anionic anthracene structures (Fig. 2), and thus the cobalt complex is formulated as monoanionic. The twist angle between the two N—Co—N planes is 38.63 (8)°, which indicates that the geometry is between tetra­hedral (90°) and square planar (0°). Qu­anti­fication using Houser's τ4 index gives a value of 0.36 (Yang et al., 2007), which is consistent with the visually observed distorted square-planar geometry.

Assignment of the exact reduced nature of the bipy ligands in (2) is not clear, however. The C—C bonds that join the pyridine rings in the two independent bipy ligands both refined to 1.405 (3) Å. Given that this bond length for the bipy dianion ranges from ~1.40 to 1.36 Å (Wang et al., 2013) and that for the bipy radical anion is centered around 1.43 Å (Gore-Randall et al., 2009), no obvious conclusion can be drawn. A search of the CSD for transition and inner transition metal complexes containing a minimum of two unsubstituted bipy ligands and whose characteristic bipy C—C bond lengths were in the range of 1.40–1.41 Å yielded exactly five hits. Two of these structures could be eliminated for having too great a range of these bond lengths among bipy ligands in similar environments, and in the other three structures these bond lengths were not discussed in the corresponding articles. Rothwell reported a structure of W(OC6HPh4-2,3,5,6)2(bipy)2 whose characteristic C—C bond lengths are 1.409 (4) and 1.412 (4) Å, and concluded based on structural and 1H and 1H COSY NMR data that the amount of reduction in the bipy ligands is unclear (CSD refcode TAJXAE; Lentz et al., 2003). It seems reasonable to conclude that an unambiguous oxidation state assignment for the Co atom in (2) is not possible without further studies.

Each anthracene molecule in (2) is found in between and is oriented essentially orthogonal to [84.46 (4)°] one bipy ligand on each of the two neighboring cobaltates (Fig. 5), which suggests that aromatic donor–acceptor inter­actions (Martinez & Iverson, 2012) may have been partly responsible for the packing arrangement. The two closest H(anthracene)···plane(bipy) distances are approximately 2.53 and 2.78 Å.

Related literature top

For related literature, see: Allen (2002); Bock et al. (1999); Brennessel (2009); Brennessel & Ellis (2012); Brennessel et al. (2002, 2007); Brock & Dunitz (1990); Chisholm et al. (1981); Dhar & Kurcz (1974); Elschenbroich (2005); England et al. (2012); Gore-Randall, Irwin, Denning & Goicoechea (2009); Hall & Reynolds (1966); Lentz et al. (2003); Mahon & Reynolds (1967); Martinez & Iverson (2012); Mitchell & Parish (1969); Motten et al. (1981); Radonovich et al. (1982); Rosokha & Kochi (2006); Scarborough & Wieghardt (2011); Tanaka & Sato (1966); Uhlig (1988); Wang et al. (2013); Yang et al. (2007).

Computing details top

For both compounds, data collection: SMART (Bruker, 2003); cell refinement: SAINT (Bruker, 2003); data reduction: SAINT (Bruker, 2003); program(s) used to solve structure: SIR97 (Altomare et al., 1999); program(s) used to refine structure: SHELXL2014 (Sheldrick, 2014); molecular graphics: SHELXTL (Sheldrick, 2008); software used to prepare material for publication: SHELXTL (Sheldrick, 2008).

Figures top
[Figure 1] Fig. 1. The structure of (1), showing the atom numbering. H atoms have been omitted for clarity. Displacement ellipsoids are drawn at the 50% probability level. The Fe atom is located on a twofold axis that generates the symmetry equivalent portion by the operation (-x+2, y, -z+1/2). The anthracene radical anion is on an inversion center, and its symmetry equivalent portion is generated by the operation (-x+3/2, -y+1/2, -z+1).
[Figure 2] Fig. 2. (Top) The two forms of anthracene in this study depicted with displacement ellipsoids at the 50% probability level and with H atoms omitted for clarity. (Bottom) Two previously reported structures of radical anionic and neutral anthracene with averaged bond lengths.
[Figure 3] Fig. 3. Resonance structures of the bipy radical anion.
[Figure 4] Fig. 4. The structure of (2), showing the atom numbering. H atoms have been omitted for clarity. Displacement ellipsoids are drawn at the 50% probability level. The anthracene molecule is on an inversion center, and its symmetry-equivalent portion is generated by the operation (-x+1, -y+1, -z+1). Only one position of the three is shown for the disordered THF solvent molecule.
[Figure 5] Fig. 5. Each anthracene molecule is nearly orthogonal to its neighboring bipy ligands. Displacement ellipsoids are drawn at the 50% probability level.
(1) Bis[([2.2.2]cryptand)potassium(I)] tris(2,2'-bipyridine)ferrate(–I) anthrancene(–I) top
Crystal data top
[K(C18H36N2O6)2][Fe(C10H8N2)3](C14H10)F(000) = 3264
Mr = 1533.79Dx = 1.277 Mg m3
Monoclinic, C2/cMo Kα radiation, λ = 0.71073 Å
a = 23.049 (4) ÅCell parameters from 2362 reflections
b = 17.067 (3) Åθ = 2.2–24.0°
c = 21.543 (3) ŵ = 0.36 mm1
β = 109.779 (3)°T = 173 K
V = 7975 (2) Å3Plate, purple–black
Z = 40.42 × 0.16 × 0.06 mm
Data collection top
Siemens SMART CCD platform
diffractometer
4398 reflections with I > 2σ(I)
Radiation source: normal-focus sealed tubeRint = 0.085
ω scansθmax = 25.1°, θmin = 1.5°
Absorption correction: multi-scan
(SADABS; Sheldrick, 2012)
h = 2727
Tmin = 0.637, Tmax = 0.745k = 2019
22943 measured reflectionsl = 2522
7069 independent reflections
Refinement top
Refinement on F20 restraints
Least-squares matrix: fullHydrogen site location: inferred from neighbouring sites
R[F2 > 2σ(F2)] = 0.057H-atom parameters constrained
wR(F2) = 0.122 w = 1/[σ2(Fo2) + (0.0515P)2]
where P = (Fo2 + 2Fc2)/3
S = 1.02(Δ/σ)max < 0.001
7069 reflectionsΔρmax = 0.27 e Å3
474 parametersΔρmin = 0.39 e Å3
Crystal data top
[K(C18H36N2O6)2][Fe(C10H8N2)3](C14H10)V = 7975 (2) Å3
Mr = 1533.79Z = 4
Monoclinic, C2/cMo Kα radiation
a = 23.049 (4) ŵ = 0.36 mm1
b = 17.067 (3) ÅT = 173 K
c = 21.543 (3) Å0.42 × 0.16 × 0.06 mm
β = 109.779 (3)°
Data collection top
Siemens SMART CCD platform
diffractometer
7069 independent reflections
Absorption correction: multi-scan
(SADABS; Sheldrick, 2012)
4398 reflections with I > 2σ(I)
Tmin = 0.637, Tmax = 0.745Rint = 0.085
22943 measured reflections
Refinement top
R[F2 > 2σ(F2)] = 0.0570 restraints
wR(F2) = 0.122H-atom parameters constrained
S = 1.02Δρmax = 0.27 e Å3
7069 reflectionsΔρmin = 0.39 e Å3
474 parameters
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. H atoms were placed geometrically and treated as riding atoms: methylene, C—H = 0.99 Å, and sp2, C—H = 0.95 Å, with Uiso(H) = 1.2Ueq(C).

Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top
xyzUiso*/Ueq
Fe11.00000.16987 (4)0.25000.02605 (18)
N10.92863 (11)0.17628 (14)0.27964 (12)0.0275 (6)
C10.91594 (15)0.13244 (19)0.32483 (16)0.0361 (8)
H1A0.94400.09180.34550.043*
C20.86458 (15)0.1424 (2)0.34346 (18)0.0422 (9)
H2A0.85810.10980.37630.051*
C30.82232 (15)0.2012 (2)0.31311 (18)0.0424 (9)
H3A0.78680.20980.32520.051*
C40.83313 (15)0.2458 (2)0.26593 (17)0.0388 (9)
H4A0.80480.28610.24510.047*
C50.88563 (14)0.23362 (18)0.24719 (15)0.0299 (8)
C60.89978 (14)0.27405 (18)0.19592 (16)0.0308 (8)
C70.86230 (16)0.33191 (19)0.15364 (17)0.0378 (8)
H7A0.82570.34940.16030.045*
C80.87866 (16)0.36215 (19)0.10376 (17)0.0412 (9)
H8A0.85310.40020.07520.049*
C90.93308 (16)0.33759 (19)0.09411 (17)0.0405 (9)
H9A0.94460.35780.05890.049*
C100.96930 (16)0.28303 (19)0.13744 (17)0.0376 (8)
H10A1.00680.26730.13180.045*
N20.95456 (11)0.25081 (14)0.18723 (13)0.0287 (6)
N31.03880 (11)0.08287 (14)0.30923 (12)0.0256 (6)
C111.08056 (14)0.0868 (2)0.37030 (16)0.0341 (8)
H11A1.09300.13740.38840.041*
C121.10648 (15)0.0231 (2)0.40843 (17)0.0384 (9)
H12A1.13580.02970.45140.046*
C131.08847 (15)0.0525 (2)0.38227 (17)0.0393 (9)
H13A1.10530.09790.40740.047*
C141.04672 (15)0.05885 (19)0.32081 (17)0.0372 (8)
H14A1.03390.10940.30300.045*
C151.02156 (13)0.00845 (17)0.28234 (15)0.0287 (7)
K10.62197 (3)0.19561 (4)0.16333 (3)0.03210 (19)
N40.61166 (13)0.35212 (16)0.09583 (14)0.0394 (7)
C160.59914 (17)0.4128 (2)0.13814 (18)0.0482 (10)
H16A0.55570.40810.13600.058*
H16B0.60410.46500.12040.058*
C170.64032 (17)0.40845 (19)0.20933 (18)0.0466 (10)
H17A0.68400.41260.21240.056*
H17B0.63100.45240.23440.056*
O10.63013 (10)0.33560 (12)0.23651 (11)0.0381 (6)
C180.66935 (15)0.3273 (2)0.30374 (16)0.0391 (9)
H18A0.66780.37540.32880.047*
H18B0.71250.31890.30590.047*
C190.64748 (15)0.25875 (19)0.33271 (16)0.0384 (9)
H19A0.67070.25550.38060.046*
H19B0.60320.26490.32660.046*
O20.65670 (10)0.18887 (12)0.30062 (11)0.0362 (6)
C200.63833 (16)0.12081 (19)0.32766 (17)0.0402 (9)
H20A0.59290.11950.31530.048*
H20B0.65650.12180.37640.048*
C210.66043 (17)0.0492 (2)0.30083 (17)0.0450 (10)
H21A0.70540.05370.31020.054*
H21B0.65320.00220.32420.054*
C220.67077 (16)0.3681 (2)0.08556 (18)0.0476 (10)
H22A0.70170.38370.12820.057*
H22B0.66510.41290.05490.057*
C230.69555 (17)0.2993 (2)0.05817 (19)0.0537 (11)
H23A0.66400.28050.01710.064*
H23B0.73240.31550.04760.064*
O30.71137 (10)0.23837 (14)0.10594 (11)0.0427 (6)
C240.73919 (17)0.1734 (2)0.0846 (2)0.0532 (11)
H24A0.77550.19180.07400.064*
H24B0.70930.15060.04410.064*
C250.75859 (16)0.1128 (2)0.1364 (2)0.0498 (10)
H25A0.77950.06940.12180.060*
H25B0.78800.13540.17720.060*
O40.70528 (10)0.08346 (13)0.14907 (12)0.0416 (6)
C260.72256 (18)0.0212 (2)0.1955 (2)0.0558 (11)
H26A0.74950.04150.23870.067*
H26B0.74590.01880.18040.067*
C270.66597 (18)0.0151 (2)0.20269 (19)0.0537 (11)
H27A0.63930.03420.15890.064*
H27B0.67850.06110.23220.064*
C280.56087 (16)0.3497 (2)0.03156 (18)0.0497 (10)
H28A0.57470.32010.00040.060*
H28B0.55140.40380.01470.060*
C290.50279 (16)0.3123 (2)0.03556 (19)0.0504 (10)
H29A0.48910.34030.06850.060*
H29B0.46950.31580.00780.060*
O50.51514 (9)0.23242 (14)0.05423 (11)0.0426 (6)
C300.46067 (17)0.1937 (2)0.0546 (2)0.0624 (12)
H30A0.42740.20160.01180.075*
H30B0.44690.21590.08980.075*
C310.47343 (17)0.1081 (2)0.0665 (2)0.0614 (12)
H31A0.43450.07980.06120.074*
H31B0.49100.08690.03390.074*
O60.51560 (10)0.09638 (13)0.13119 (12)0.0472 (7)
C320.52559 (18)0.0151 (2)0.1464 (2)0.0559 (11)
H32A0.54450.00970.11630.067*
H32B0.48570.01110.14020.067*
C330.56759 (17)0.0055 (2)0.21678 (18)0.0517 (10)
H33A0.54870.03160.24630.062*
H33B0.57140.05100.22790.062*
N50.62967 (13)0.03816 (16)0.22926 (14)0.0413 (7)
C340.68827 (14)0.1248 (2)0.53918 (16)0.0362 (8)
H34A0.66080.13560.56250.043*
C350.69764 (15)0.0479 (2)0.52524 (18)0.0420 (9)
H35A0.67620.00680.53790.050*
C360.73900 (15)0.0310 (2)0.49221 (17)0.0414 (9)
H36A0.74520.02170.48190.050*
C370.77079 (14)0.09053 (18)0.47444 (16)0.0346 (8)
H37A0.79940.07770.45300.041*
C380.76186 (13)0.17007 (19)0.48726 (15)0.0301 (7)
C390.79295 (13)0.23219 (18)0.46928 (15)0.0305 (8)
H39A0.82270.22020.44910.037*
C400.78204 (13)0.31163 (18)0.47990 (15)0.0285 (7)
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
Fe10.0223 (3)0.0244 (4)0.0320 (4)0.0000.0099 (3)0.000
N10.0262 (14)0.0241 (15)0.0332 (15)0.0015 (12)0.0116 (12)0.0017 (12)
C10.037 (2)0.0302 (19)0.044 (2)0.0042 (15)0.0175 (17)0.0025 (17)
C20.041 (2)0.043 (2)0.052 (2)0.0015 (17)0.0284 (19)0.0028 (18)
C30.034 (2)0.052 (2)0.049 (2)0.0055 (18)0.0234 (18)0.005 (2)
C40.0317 (19)0.037 (2)0.046 (2)0.0071 (16)0.0111 (17)0.0081 (18)
C50.0279 (18)0.0292 (19)0.0315 (19)0.0020 (15)0.0086 (15)0.0032 (15)
C60.0317 (18)0.0244 (18)0.0324 (19)0.0020 (14)0.0058 (16)0.0084 (15)
C70.038 (2)0.0318 (19)0.039 (2)0.0078 (17)0.0071 (17)0.0017 (17)
C80.045 (2)0.030 (2)0.038 (2)0.0065 (17)0.0004 (18)0.0030 (17)
C90.052 (2)0.0299 (19)0.038 (2)0.0054 (18)0.0131 (18)0.0062 (17)
C100.039 (2)0.035 (2)0.041 (2)0.0055 (16)0.0166 (18)0.0003 (18)
N20.0271 (14)0.0225 (14)0.0355 (16)0.0007 (12)0.0093 (13)0.0003 (12)
N30.0203 (13)0.0270 (15)0.0297 (16)0.0027 (11)0.0086 (12)0.0012 (12)
C110.0305 (19)0.036 (2)0.035 (2)0.0019 (16)0.0110 (17)0.0052 (16)
C120.0335 (19)0.046 (2)0.031 (2)0.0083 (17)0.0053 (16)0.0021 (17)
C130.039 (2)0.042 (2)0.036 (2)0.0118 (17)0.0113 (18)0.0075 (17)
C140.042 (2)0.0253 (19)0.043 (2)0.0049 (15)0.0126 (18)0.0011 (16)
C150.0275 (18)0.0259 (18)0.0351 (18)0.0030 (14)0.0136 (14)0.0007 (15)
K10.0299 (4)0.0327 (4)0.0340 (4)0.0013 (3)0.0113 (3)0.0015 (3)
N40.0429 (17)0.0379 (18)0.0377 (17)0.0051 (14)0.0140 (15)0.0075 (14)
C160.054 (2)0.034 (2)0.055 (3)0.0016 (18)0.018 (2)0.0121 (19)
C170.061 (3)0.031 (2)0.050 (3)0.0123 (18)0.022 (2)0.0044 (18)
O10.0413 (14)0.0304 (13)0.0378 (14)0.0031 (11)0.0072 (11)0.0001 (11)
C180.0331 (19)0.040 (2)0.041 (2)0.0035 (16)0.0080 (17)0.0089 (18)
C190.037 (2)0.042 (2)0.032 (2)0.0061 (17)0.0064 (16)0.0046 (17)
O20.0427 (14)0.0311 (13)0.0367 (14)0.0031 (10)0.0158 (11)0.0005 (11)
C200.041 (2)0.043 (2)0.035 (2)0.0011 (18)0.0117 (17)0.0061 (18)
C210.055 (2)0.035 (2)0.041 (2)0.0043 (18)0.012 (2)0.0048 (18)
C220.050 (2)0.052 (2)0.043 (2)0.0163 (19)0.0172 (19)0.0092 (19)
C230.043 (2)0.079 (3)0.044 (2)0.019 (2)0.022 (2)0.000 (2)
O30.0427 (14)0.0531 (16)0.0388 (14)0.0025 (12)0.0221 (12)0.0014 (13)
C240.044 (2)0.072 (3)0.055 (3)0.014 (2)0.031 (2)0.025 (2)
C250.034 (2)0.059 (3)0.058 (3)0.0026 (19)0.017 (2)0.023 (2)
O40.0344 (14)0.0445 (15)0.0473 (15)0.0062 (11)0.0155 (12)0.0059 (12)
C260.054 (3)0.057 (3)0.054 (3)0.028 (2)0.015 (2)0.002 (2)
C270.071 (3)0.031 (2)0.056 (3)0.007 (2)0.017 (2)0.0034 (19)
C280.050 (2)0.049 (2)0.043 (2)0.0008 (19)0.0074 (19)0.0137 (19)
C290.039 (2)0.051 (3)0.052 (2)0.0021 (18)0.0030 (19)0.010 (2)
O50.0295 (13)0.0450 (15)0.0489 (15)0.0031 (11)0.0075 (11)0.0040 (12)
C300.031 (2)0.063 (3)0.076 (3)0.008 (2)0.003 (2)0.010 (2)
C310.044 (2)0.058 (3)0.065 (3)0.021 (2)0.004 (2)0.005 (2)
O60.0393 (14)0.0421 (15)0.0501 (17)0.0111 (12)0.0021 (13)0.0006 (12)
C320.054 (3)0.042 (2)0.064 (3)0.0148 (19)0.010 (2)0.000 (2)
C330.057 (3)0.038 (2)0.058 (3)0.0153 (19)0.017 (2)0.005 (2)
N50.0468 (18)0.0312 (16)0.0440 (19)0.0014 (14)0.0131 (15)0.0018 (14)
C340.0230 (18)0.044 (2)0.039 (2)0.0001 (16)0.0067 (16)0.0086 (18)
C350.033 (2)0.029 (2)0.056 (2)0.0039 (16)0.0038 (19)0.0148 (18)
C360.036 (2)0.029 (2)0.049 (2)0.0069 (16)0.0022 (18)0.0010 (17)
C370.0312 (19)0.031 (2)0.039 (2)0.0040 (15)0.0085 (16)0.0006 (16)
C380.0241 (17)0.0350 (19)0.0259 (18)0.0010 (15)0.0015 (14)0.0037 (15)
C390.0252 (17)0.037 (2)0.0305 (19)0.0028 (15)0.0107 (15)0.0002 (15)
C400.0215 (16)0.0313 (19)0.0266 (18)0.0010 (14)0.0004 (14)0.0051 (14)
Geometric parameters (Å, º) top
Fe1—N11.959 (2)O2—C201.426 (4)
Fe1—N1i1.959 (2)C20—C211.512 (4)
Fe1—N3i1.965 (2)C20—H20A0.9900
Fe1—N31.965 (2)C20—H20B0.9900
Fe1—N2i1.969 (2)C21—N51.475 (4)
Fe1—N21.969 (2)C21—H21A0.9900
N1—C11.336 (4)C21—H21B0.9900
N1—C51.400 (4)C22—C231.510 (5)
C1—C21.383 (4)C22—H22A0.9900
C1—H1A0.9500C22—H22B0.9900
C2—C31.398 (5)C23—O31.422 (4)
C2—H2A0.9500C23—H23A0.9900
C3—C41.359 (5)C23—H23B0.9900
C3—H3A0.9500O3—C241.432 (4)
C4—C51.415 (4)C24—C251.475 (5)
C4—H4A0.9500C24—H24A0.9900
C5—C61.431 (4)C24—H24B0.9900
C6—N21.395 (4)C25—O41.436 (4)
C6—C71.421 (4)C25—H25A0.9900
C7—C81.356 (5)C25—H25B0.9900
C7—H7A0.9500O4—C261.421 (4)
C8—C91.403 (5)C26—C271.499 (5)
C8—H8A0.9500C26—H26A0.9900
C9—C101.381 (4)C26—H26B0.9900
C9—H9A0.9500C27—N51.476 (4)
C10—N21.347 (4)C27—H27A0.9900
C10—H10A0.9500C27—H27B0.9900
N3—C111.344 (4)C28—C291.511 (5)
N3—C151.397 (4)C28—H28A0.9900
C11—C121.372 (4)C28—H28B0.9900
C11—H11A0.9500C29—O51.423 (4)
C12—C131.414 (5)C29—H29A0.9900
C12—H12A0.9500C29—H29B0.9900
C13—C141.352 (4)O5—C301.422 (4)
C13—H13A0.9500C30—C311.495 (5)
C14—C151.420 (4)C30—H30A0.9900
C14—H14A0.9500C30—H30B0.9900
C15—C15i1.411 (6)C31—O61.417 (4)
K1—O22.793 (2)C31—H31A0.9900
K1—O42.801 (2)C31—H31B0.9900
K1—O12.833 (2)O6—C321.426 (4)
K1—O32.834 (2)C32—C331.507 (5)
K1—O52.840 (2)C32—H32A0.9900
K1—O62.865 (2)C32—H32B0.9900
K1—N43.012 (3)C33—N51.473 (4)
K1—N53.016 (3)C33—H33A0.9900
N4—C161.472 (4)C33—H33B0.9900
N4—C221.478 (4)C34—C351.380 (5)
N4—C281.481 (4)C34—C40ii1.415 (4)
C16—C171.508 (5)C34—H34A0.9500
C16—H16A0.9900C35—C361.399 (5)
C16—H16B0.9900C35—H35A0.9500
C17—O11.427 (4)C36—C371.380 (4)
C17—H17A0.9900C36—H36A0.9500
C17—H17B0.9900C37—C381.414 (4)
O1—C181.431 (4)C37—H37A0.9500
C18—C191.491 (4)C38—C391.406 (4)
C18—H18A0.9900C38—C40ii1.451 (4)
C18—H18B0.9900C39—C401.412 (4)
C19—O21.430 (4)C39—H39A0.9500
C19—H19A0.9900C40—C34ii1.415 (4)
C19—H19B0.9900C40—C38ii1.451 (4)
N1—Fe1—N1i173.60 (14)C18—C19—H19B109.9
N1—Fe1—N3i90.34 (10)H19A—C19—H19B108.3
N1i—Fe1—N3i94.49 (10)C20—O2—C19111.6 (2)
N1—Fe1—N394.49 (10)C20—O2—K1116.60 (18)
N1i—Fe1—N390.35 (10)C19—O2—K1116.19 (17)
N3i—Fe1—N381.82 (15)O2—C20—C21108.5 (3)
N1—Fe1—N2i92.71 (10)O2—C20—H20A110.0
N1i—Fe1—N2i82.79 (10)C21—C20—H20A110.0
N3i—Fe1—N2i174.78 (10)O2—C20—H20B110.0
N3—Fe1—N2i93.71 (10)C21—C20—H20B110.0
N1—Fe1—N282.79 (10)H20A—C20—H20B108.4
N1i—Fe1—N292.71 (10)N5—C21—C20113.4 (3)
N3i—Fe1—N293.71 (10)N5—C21—H21A108.9
N3—Fe1—N2174.78 (10)C20—C21—H21A108.9
N2i—Fe1—N290.87 (14)N5—C21—H21B108.9
C1—N1—C5117.6 (3)C20—C21—H21B108.9
C1—N1—Fe1128.4 (2)H21A—C21—H21B107.7
C5—N1—Fe1114.0 (2)N4—C22—C23113.9 (3)
N1—C1—C2124.2 (3)N4—C22—H22A108.8
N1—C1—H1A117.9C23—C22—H22A108.8
C2—C1—H1A117.9N4—C22—H22B108.8
C1—C2—C3118.8 (3)C23—C22—H22B108.8
C1—C2—H2A120.6H22A—C22—H22B107.7
C3—C2—H2A120.6O3—C23—C22108.9 (3)
C4—C3—C2118.5 (3)O3—C23—H23A109.9
C4—C3—H3A120.7C22—C23—H23A109.9
C2—C3—H3A120.7O3—C23—H23B109.9
C3—C4—C5121.5 (3)C22—C23—H23B109.9
C3—C4—H4A119.3H23A—C23—H23B108.3
C5—C4—H4A119.3C23—O3—C24111.6 (3)
N1—C5—C4119.3 (3)C23—O3—K1117.26 (19)
N1—C5—C6114.5 (3)C24—O3—K1114.3 (2)
C4—C5—C6126.1 (3)O3—C24—C25110.8 (3)
N2—C6—C7119.6 (3)O3—C24—H24A109.5
N2—C6—C5114.8 (3)C25—C24—H24A109.5
C7—C6—C5125.6 (3)O3—C24—H24B109.5
C8—C7—C6120.1 (3)C25—C24—H24B109.5
C8—C7—H7A120.0H24A—C24—H24B108.1
C6—C7—H7A120.0O4—C25—C24109.2 (3)
C7—C8—C9120.4 (3)O4—C25—H25A109.8
C7—C8—H8A119.8C24—C25—H25A109.8
C9—C8—H8A119.8O4—C25—H25B109.8
C10—C9—C8117.9 (3)C24—C25—H25B109.8
C10—C9—H9A121.1H25A—C25—H25B108.3
C8—C9—H9A121.1C26—O4—C25109.9 (3)
N2—C10—C9123.7 (3)C26—O4—K1118.24 (19)
N2—C10—H10A118.1C25—O4—K1116.4 (2)
C9—C10—H10A118.1O4—C26—C27109.6 (3)
C10—N2—C6118.3 (3)O4—C26—H26A109.7
C10—N2—Fe1127.9 (2)C27—C26—H26A109.7
C6—N2—Fe1113.7 (2)O4—C26—H26B109.7
C11—N3—C15117.5 (3)C27—C26—H26B109.7
C11—N3—Fe1128.0 (2)H26A—C26—H26B108.2
C15—N3—Fe1114.50 (19)N5—C27—C26114.4 (3)
N3—C11—C12124.7 (3)N5—C27—H27A108.7
N3—C11—H11A117.7C26—C27—H27A108.7
C12—C11—H11A117.7N5—C27—H27B108.7
C11—C12—C13118.4 (3)C26—C27—H27B108.7
C11—C12—H12A120.8H27A—C27—H27B107.6
C13—C12—H12A120.8N4—C28—C29113.2 (3)
C14—C13—C12118.6 (3)N4—C28—H28A108.9
C14—C13—H13A120.7C29—C28—H28A108.9
C12—C13—H13A120.7N4—C28—H28B108.9
C13—C14—C15121.4 (3)C29—C28—H28B108.9
C13—C14—H14A119.3H28A—C28—H28B107.8
C15—C14—H14A119.3O5—C29—C28108.9 (3)
N3—C15—C15i114.58 (16)O5—C29—H29A109.9
N3—C15—C14119.4 (3)C28—C29—H29A109.9
C15i—C15—C14126.03 (19)O5—C29—H29B109.9
O2—K1—O497.27 (7)C28—C29—H29B109.9
O2—K1—O160.28 (6)H29A—C29—H29B108.3
O4—K1—O1135.92 (7)C30—O5—C29110.8 (3)
O2—K1—O3118.85 (7)C30—O5—K1114.3 (2)
O4—K1—O360.09 (7)C29—O5—K1118.71 (19)
O1—K1—O396.00 (7)O5—C30—C31109.4 (3)
O2—K1—O5138.00 (7)O5—C30—H30A109.8
O4—K1—O5119.67 (7)C31—C30—H30A109.8
O1—K1—O598.61 (7)O5—C30—H30B109.8
O3—K1—O597.86 (7)C31—C30—H30B109.8
O2—K1—O698.44 (7)H30A—C30—H30B108.2
O4—K1—O697.58 (7)O6—C31—C30109.6 (3)
O1—K1—O6121.54 (7)O6—C31—H31A109.8
O3—K1—O6137.37 (7)C30—C31—H31A109.8
O5—K1—O659.96 (7)O6—C31—H31B109.8
O2—K1—N4119.69 (7)C30—C31—H31B109.8
O4—K1—N4119.88 (8)H31A—C31—H31B108.2
O1—K1—N460.02 (7)C31—O6—C32111.5 (3)
O3—K1—N460.74 (7)C31—O6—K1113.6 (2)
O5—K1—N459.97 (7)C32—O6—K1117.4 (2)
O6—K1—N4119.09 (7)O6—C32—C33109.6 (3)
O2—K1—N560.96 (7)O6—C32—H32A109.7
O4—K1—N560.63 (8)C33—C32—H32A109.7
O1—K1—N5120.46 (8)O6—C32—H32B109.7
O3—K1—N5119.95 (8)C33—C32—H32B109.7
O5—K1—N5118.89 (7)H32A—C32—H32B108.2
O6—K1—N559.77 (7)N5—C33—C32113.3 (3)
N4—K1—N5178.86 (8)N5—C33—H33A108.9
C16—N4—C22110.3 (3)C32—C33—H33A108.9
C16—N4—C28109.9 (3)N5—C33—H33B108.9
C22—N4—C28110.0 (3)C32—C33—H33B108.9
C16—N4—K1108.99 (19)H33A—C33—H33B107.7
C22—N4—K1108.1 (2)C33—N5—C21109.4 (3)
C28—N4—K1109.57 (19)C33—N5—C27109.8 (3)
N4—C16—C17114.0 (3)C21—N5—C27110.4 (3)
N4—C16—H16A108.7C33—N5—K1110.6 (2)
C17—C16—H16A108.7C21—N5—K1108.03 (19)
N4—C16—H16B108.7C27—N5—K1108.5 (2)
C17—C16—H16B108.7C35—C34—C40ii122.6 (3)
H16A—C16—H16B107.6C35—C34—H34A118.7
O1—C17—C16109.0 (3)C40ii—C34—H34A118.7
O1—C17—H17A109.9C34—C35—C36119.4 (3)
C16—C17—H17A109.9C34—C35—H35A120.3
O1—C17—H17B109.9C36—C35—H35A120.3
C16—C17—H17B109.9C37—C36—C35120.5 (3)
H17A—C17—H17B108.3C37—C36—H36A119.8
C17—O1—C18111.5 (2)C35—C36—H36A119.8
C17—O1—K1119.70 (19)C36—C37—C38121.7 (3)
C18—O1—K1112.31 (17)C36—C37—H37A119.1
O1—C18—C19108.3 (3)C38—C37—H37A119.1
O1—C18—H18A110.0C39—C38—C37123.3 (3)
C19—C18—H18A110.0C39—C38—C40ii118.5 (3)
O1—C18—H18B110.0C37—C38—C40ii118.3 (3)
C19—C18—H18B110.0C38—C39—C40123.0 (3)
H18A—C18—H18B108.4C38—C39—H39A118.5
O2—C19—C18109.0 (3)C40—C39—H39A118.5
O2—C19—H19A109.9C39—C40—C34ii124.0 (3)
C18—C19—H19A109.9C39—C40—C38ii118.5 (3)
O2—C19—H19B109.9C34ii—C40—C38ii117.5 (3)
C5—N1—C1—C22.9 (5)K1—O2—C20—C2153.8 (3)
Fe1—N1—C1—C2178.7 (2)O2—C20—C21—N566.6 (4)
N1—C1—C2—C30.7 (5)C16—N4—C22—C23165.0 (3)
C1—C2—C3—C40.7 (5)C28—N4—C22—C2373.7 (4)
C2—C3—C4—C50.2 (5)K1—N4—C22—C2345.9 (3)
C1—N1—C5—C43.7 (4)N4—C22—C23—O366.0 (4)
Fe1—N1—C5—C4177.7 (2)C22—C23—O3—C24176.0 (3)
C1—N1—C5—C6175.3 (3)C22—C23—O3—K149.5 (3)
Fe1—N1—C5—C63.3 (3)C23—O3—C24—C25176.7 (3)
C3—C4—C5—N12.4 (5)K1—O3—C24—C2547.4 (3)
C3—C4—C5—C6176.4 (3)O3—C24—C25—O462.1 (4)
N1—C5—C6—N21.0 (4)C24—C25—O4—C26176.0 (3)
C4—C5—C6—N2179.9 (3)C24—C25—O4—K146.1 (3)
N1—C5—C6—C7176.8 (3)C25—O4—C26—C27173.6 (3)
C4—C5—C6—C72.1 (5)K1—O4—C26—C2749.4 (4)
N2—C6—C7—C82.4 (5)O4—C26—C27—N563.2 (4)
C5—C6—C7—C8175.4 (3)C16—N4—C28—C2974.2 (4)
C6—C7—C8—C91.0 (5)C22—N4—C28—C29164.2 (3)
C7—C8—C9—C101.0 (5)K1—N4—C28—C2945.5 (3)
C8—C9—C10—N21.7 (5)N4—C28—C29—O563.8 (4)
C9—C10—N2—C60.4 (5)C28—C29—O5—C30176.4 (3)
C9—C10—N2—Fe1177.3 (2)C28—C29—O5—K148.3 (4)
C7—C6—N2—C101.6 (4)C29—O5—C30—C31173.3 (3)
C5—C6—N2—C10176.3 (3)K1—O5—C30—C3149.3 (4)
C7—C6—N2—Fe1179.7 (2)O5—C30—C31—O666.5 (5)
C5—C6—N2—Fe11.7 (3)C30—C31—O6—C32175.7 (3)
C15—N3—C11—C121.3 (5)C30—C31—O6—K148.9 (4)
Fe1—N3—C11—C12178.8 (2)C31—O6—C32—C33176.6 (3)
N3—C11—C12—C130.1 (5)K1—O6—C32—C3349.8 (4)
C11—C12—C13—C140.2 (5)O6—C32—C33—N563.4 (4)
C12—C13—C14—C150.8 (5)C32—C33—N5—C21162.2 (3)
C11—N3—C15—C15i178.9 (3)C32—C33—N5—C2776.5 (4)
Fe1—N3—C15—C15i1.0 (4)C32—C33—N5—K143.3 (4)
C11—N3—C15—C142.2 (4)C20—C21—N5—C3377.4 (4)
Fe1—N3—C15—C14179.9 (2)C20—C21—N5—C27161.6 (3)
C13—C14—C15—N32.0 (5)C20—C21—N5—K143.1 (3)
C13—C14—C15—C15i179.2 (4)C26—C27—N5—C33163.9 (3)
C22—N4—C16—C1771.3 (4)C26—C27—N5—C2175.3 (4)
C28—N4—C16—C17167.2 (3)C26—C27—N5—K142.9 (3)
K1—N4—C16—C1747.2 (3)C40ii—C34—C35—C361.4 (5)
N4—C16—C17—O162.5 (4)C34—C35—C36—C370.8 (5)
C16—C17—O1—C18178.4 (3)C35—C36—C37—C381.6 (5)
C16—C17—O1—K144.5 (3)C36—C37—C38—C39179.3 (3)
C17—O1—C18—C19168.5 (3)C36—C37—C38—C40ii0.1 (5)
K1—O1—C18—C1954.0 (3)C37—C38—C39—C40177.4 (3)
O1—C18—C19—O266.2 (3)C40ii—C38—C39—C402.0 (5)
C18—C19—O2—C20178.2 (3)C38—C39—C40—C34ii178.5 (3)
C18—C19—O2—K144.7 (3)C38—C39—C40—C38ii2.0 (5)
C19—O2—C20—C21169.3 (3)
Symmetry codes: (i) x+2, y, z+1/2; (ii) x+3/2, y+1/2, z+1.
(2) ([2.2.2]Cryptand)potassium(I) bis(2,2'-bipyridine)cobaltate(–I) anthrancene hemisolvate tetrahydrofuran disolvate top
Crystal data top
[K(C18H36N2O6)][Co(C10H8N2)2]·0.5C14H10·2C4H8OZ = 2
Mr = 1020.20F(000) = 1086
Triclinic, P1Dx = 1.289 Mg m3
a = 10.5981 (8) ÅMo Kα radiation, λ = 0.71073 Å
b = 14.4323 (11) ÅCell parameters from 3379 reflections
c = 18.4886 (15) Åθ = 2.3–25.0°
α = 99.1054 (13)°µ = 0.46 mm1
β = 90.8279 (14)°T = 173 K
γ = 109.2433 (13)°Rod, purple-black
V = 2629.5 (4) Å30.40 × 0.18 × 0.12 mm
Data collection top
Siemens SMART CCD platform
diffractometer
7616 reflections with I > 2σ(I)
Radiation source: normal-focus sealed tubeRint = 0.021
ω scansθmax = 25.0°, θmin = 1.1°
Absorption correction: multi-scan
(SADABS; Sheldrick, 2012)
h = 1212
Tmin = 0.684, Tmax = 0.745k = 1717
26404 measured reflectionsl = 2222
9299 independent reflections
Refinement top
Refinement on F2Primary atom site location: structure-invariant direct methods
Least-squares matrix: fullSecondary atom site location: difference Fourier map
R[F2 > 2σ(F2)] = 0.031Hydrogen site location: inferred from neighbouring sites
wR(F2) = 0.079H-atom parameters constrained
S = 1.03 w = 1/[σ2(Fo2) + (0.0385P)2 + 0.7396P]
where P = (Fo2 + 2Fc2)/3
9299 reflections(Δ/σ)max = 0.002
715 parametersΔρmax = 0.31 e Å3
257 restraintsΔρmin = 0.22 e Å3
Crystal data top
[K(C18H36N2O6)][Co(C10H8N2)2]·0.5C14H10·2C4H8Oγ = 109.2433 (13)°
Mr = 1020.20V = 2629.5 (4) Å3
Triclinic, P1Z = 2
a = 10.5981 (8) ÅMo Kα radiation
b = 14.4323 (11) ŵ = 0.46 mm1
c = 18.4886 (15) ÅT = 173 K
α = 99.1054 (13)°0.40 × 0.18 × 0.12 mm
β = 90.8279 (14)°
Data collection top
Siemens SMART CCD platform
diffractometer
9299 independent reflections
Absorption correction: multi-scan
(SADABS; Sheldrick, 2012)
7616 reflections with I > 2σ(I)
Tmin = 0.684, Tmax = 0.745Rint = 0.021
26404 measured reflections
Refinement top
R[F2 > 2σ(F2)] = 0.031257 restraints
wR(F2) = 0.079H-atom parameters constrained
S = 1.03Δρmax = 0.31 e Å3
9299 reflectionsΔρmin = 0.22 e Å3
715 parameters
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. Cocrystallized tetrahydrofuran (THF) solvent molecule O8—C43—C44—C45—C46 in (2) is located in a pocket that includes its inversion symmetry equivalent. After being modeled as disordered over two general positions, a third orientation could be found from the difference map. Thus the molecule was modeled as disordered over three positions, with a refined ratio of 0.412 (4):0.387 (3):0.201 (3).

Analogous bond lengths and angles among the three positions of the disordered THF molecule and both directions around the ring of the ordered THF molecule (O7—C39—C40—C41—C42) were restrained to be similar. Anistropic displacement parameters for pairs of near isopositional atoms were heavily restrained to be similar. Additionally, anisotropic displacement parameters for all atoms in the two major components of the disorder were restrained to be similar, and separately, the same for all the atoms in the ring of the third component.

H atoms were placed geometrically and treated as riding atoms: methylene, C—H = 0.99 Å, and sp2, C—H = 0.95 Å, with Uiso(H) = 1.2Ueq(C).

Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top
xyzUiso*/UeqOcc. (<1)
Co10.79825 (2)0.68786 (2)0.27461 (2)0.02917 (7)
N10.73827 (14)0.76779 (10)0.34643 (8)0.0316 (3)
N20.94887 (14)0.72689 (10)0.34143 (7)0.0303 (3)
N30.70742 (14)0.69375 (10)0.18865 (8)0.0327 (3)
N40.80414 (14)0.56819 (10)0.21983 (8)0.0327 (3)
C10.61916 (18)0.78591 (13)0.34510 (10)0.0363 (4)
H1A0.55600.75230.30450.044*
C20.5853 (2)0.84865 (14)0.39785 (11)0.0428 (5)
H2A0.50150.85860.39330.051*
C30.6766 (2)0.89921 (14)0.45989 (11)0.0467 (5)
H3A0.65600.94450.49700.056*
C40.7945 (2)0.88103 (14)0.46467 (10)0.0421 (5)
H4A0.85560.91290.50640.051*
C50.82746 (18)0.81573 (12)0.40890 (9)0.0328 (4)
C60.94642 (18)0.79272 (12)0.40590 (9)0.0327 (4)
C71.0599 (2)0.83344 (13)0.45681 (10)0.0406 (5)
H7A1.05630.87680.50050.049*
C81.1743 (2)0.81149 (14)0.44420 (11)0.0466 (5)
H8A1.25050.83970.47820.056*
C91.17644 (19)0.74547 (13)0.37890 (11)0.0407 (4)
H9A1.25460.72880.36840.049*
C101.06525 (17)0.70633 (12)0.33152 (10)0.0338 (4)
H10A1.06860.66160.28860.041*
C110.66737 (17)0.77004 (14)0.17334 (10)0.0380 (4)
H11A0.68490.82730.21030.046*
C120.60390 (19)0.76895 (16)0.10826 (11)0.0474 (5)
H12A0.57890.82440.10080.057*
C130.57571 (19)0.68474 (18)0.05212 (11)0.0505 (5)
H13A0.52860.68130.00710.061*
C140.61799 (18)0.60868 (16)0.06431 (10)0.0442 (5)
H14A0.60060.55170.02700.053*
C150.68694 (16)0.61284 (13)0.13113 (9)0.0350 (4)
C160.74272 (17)0.54251 (13)0.14845 (10)0.0355 (4)
C170.7434 (2)0.45519 (15)0.10176 (11)0.0470 (5)
H17A0.70400.44020.05300.056*
C180.7995 (2)0.39217 (15)0.12556 (12)0.0529 (6)
H18A0.80180.33440.09360.064*
C190.85409 (19)0.41464 (14)0.19876 (12)0.0459 (5)
H19A0.89010.37040.21760.055*
C200.85480 (17)0.50058 (12)0.24235 (11)0.0362 (4)
H20A0.89280.51440.29140.043*
K10.20912 (4)0.21094 (3)0.24133 (2)0.02954 (9)
N50.10809 (15)0.01034 (10)0.24458 (8)0.0347 (3)
N60.31118 (14)0.43454 (10)0.23696 (8)0.0332 (3)
O10.38212 (12)0.12138 (9)0.29969 (6)0.0385 (3)
O20.46266 (12)0.32999 (9)0.30661 (7)0.0390 (3)
O30.01121 (12)0.13026 (9)0.32558 (7)0.0398 (3)
O40.06812 (12)0.33387 (8)0.30799 (6)0.0368 (3)
O50.10657 (12)0.07044 (9)0.10631 (6)0.0359 (3)
O60.22491 (12)0.27768 (9)0.10430 (6)0.0368 (3)
C210.2210 (2)0.04156 (13)0.26402 (11)0.0421 (5)
H21A0.27120.04880.21990.051*
H21B0.18540.10770.27900.051*
C220.3162 (2)0.03021 (14)0.32510 (11)0.0451 (5)
H22A0.26620.04280.36820.054*
H22B0.38320.00140.34010.054*
C230.4818 (2)0.19048 (15)0.35253 (11)0.0468 (5)
H23A0.54620.15920.36720.056*
H23B0.43930.21060.39690.056*
C240.55316 (19)0.27983 (15)0.31909 (11)0.0449 (5)
H24A0.63010.32500.35260.054*
H24B0.58780.25880.27210.054*
C250.52743 (18)0.41829 (14)0.27688 (11)0.0407 (4)
H25A0.54470.40010.22500.049*
H25B0.61440.45630.30480.049*
C260.43881 (18)0.48103 (13)0.28178 (11)0.0417 (5)
H26A0.41950.49610.33370.050*
H26B0.48790.54510.26620.050*
C270.0074 (2)0.03195 (13)0.29957 (11)0.0426 (5)
H27A0.05450.01780.34880.051*
H27B0.04610.10380.28910.051*
C280.08581 (19)0.02676 (13)0.30119 (11)0.0438 (5)
H28A0.12920.01710.25150.053*
H28B0.15670.00350.33500.053*
C290.09545 (19)0.18865 (14)0.33696 (11)0.0445 (5)
H29A0.16070.16370.37310.053*
H29B0.14590.18400.29030.053*
C300.0116 (2)0.29495 (14)0.36483 (11)0.0459 (5)
H30A0.07010.33470.37980.055*
H30B0.04690.29870.40820.055*
C310.14815 (19)0.43642 (13)0.33177 (10)0.0395 (4)
H31A0.21830.44170.36970.047*
H31B0.09130.47440.35350.047*
C320.21215 (19)0.47878 (13)0.26651 (10)0.0388 (4)
H32A0.14130.46750.22740.047*
H32B0.25650.55160.28120.047*
C330.0463 (2)0.06567 (13)0.17143 (10)0.0403 (4)
H33A0.04640.06480.16640.048*
H33B0.04120.13600.16780.048*
C340.12195 (19)0.02352 (13)0.10919 (10)0.0373 (4)
H34A0.21800.01490.11710.045*
H34B0.08640.06960.06230.045*
C350.16246 (18)0.11078 (13)0.04365 (9)0.0360 (4)
H35A0.11850.06430.00190.043*
H35B0.25940.12050.04480.043*
C360.14135 (18)0.20817 (13)0.04478 (10)0.0366 (4)
H36A0.16500.23200.00220.044*
H36B0.04620.20060.05150.044*
C370.21844 (19)0.37532 (13)0.10715 (10)0.0383 (4)
H37A0.13090.37730.12390.046*
H37B0.22790.39390.05770.046*
C380.33039 (19)0.44715 (13)0.15991 (10)0.0391 (4)
H38A0.41590.43780.14610.047*
H38B0.33750.51610.15540.047*
O70.13286 (14)0.74744 (10)0.04490 (8)0.0533 (4)
C390.0381 (2)0.65889 (16)0.06289 (14)0.0586 (6)
H39A0.00690.61240.01750.070*
H39B0.03090.67560.09260.070*
C400.1144 (2)0.61194 (16)0.10591 (13)0.0561 (6)
H40A0.14000.56050.07350.067*
H40B0.06100.58130.14480.067*
C410.2363 (2)0.69890 (16)0.13853 (12)0.0544 (5)
H41A0.21790.73490.18510.065*
H41B0.31350.67700.14750.065*
C420.26071 (19)0.76210 (14)0.07959 (12)0.0459 (5)
H42A0.30520.83320.10120.055*
H42B0.31880.74180.04350.055*
O80.6164 (13)0.0464 (13)0.1748 (6)0.122 (3)0.388 (3)
C430.5026 (11)0.0357 (14)0.1278 (10)0.076 (4)0.388 (3)
H43A0.43180.05160.15630.091*0.388 (3)
H43B0.46510.03290.09950.091*0.388 (3)
C440.5586 (9)0.1101 (9)0.0777 (9)0.085 (4)0.388 (3)
H44A0.57520.17930.10290.102*0.388 (3)
H44B0.49890.09620.03270.102*0.388 (3)
C450.6877 (8)0.0909 (7)0.0610 (4)0.0563 (19)0.388 (3)
H45A0.67210.03260.02150.068*0.388 (3)
H45B0.75440.14980.04610.068*0.388 (3)
C460.7330 (11)0.0711 (14)0.1325 (6)0.101 (5)0.388 (3)
H46A0.76840.01510.12380.121*0.388 (3)
H46B0.80440.13090.15880.121*0.388 (3)
O8'0.7052 (8)0.0335 (7)0.1470 (7)0.129 (3)0.413 (3)
C43'0.5802 (14)0.0279 (15)0.1804 (10)0.100 (4)0.413 (3)
H43C0.59780.06960.22990.120*0.413 (3)
H43D0.52900.04170.18500.120*0.413 (3)
C44'0.5049 (11)0.0654 (13)0.1309 (10)0.081 (4)0.413 (3)
H44C0.45230.10190.15930.098*0.413 (3)
H44D0.44290.00960.09550.098*0.413 (3)
C45'0.6087 (12)0.1335 (10)0.0917 (10)0.121 (5)0.413 (3)
H45C0.58160.12100.03860.146*0.413 (3)
H45D0.62180.20400.11200.146*0.413 (3)
C46'0.7346 (12)0.1109 (12)0.1037 (10)0.138 (5)0.413 (3)
H46C0.76610.08890.05600.166*0.413 (3)
H46D0.80580.17110.12960.166*0.413 (3)
O8"0.5137 (16)0.0635 (15)0.0627 (9)0.136 (7)0.199 (3)
C43"0.624 (2)0.0295 (16)0.0456 (8)0.105 (6)0.199 (3)
H43E0.65040.03930.00450.126*0.199 (3)
H43F0.59900.04230.04800.126*0.199 (3)
C44"0.7370 (17)0.089 (2)0.1009 (14)0.136 (6)0.199 (3)
H44E0.79870.14630.08180.163*0.199 (3)
H44F0.78830.04730.11480.163*0.199 (3)
C45"0.6685 (17)0.1233 (15)0.1652 (9)0.117 (7)0.199 (3)
H45E0.64510.07420.19890.140*0.199 (3)
H45F0.72620.18850.19290.140*0.199 (3)
C46"0.5447 (17)0.1318 (15)0.1305 (9)0.079 (5)0.199 (3)
H46E0.46970.11440.16280.095*0.199 (3)
H46F0.56120.20060.12180.095*0.199 (3)
C470.34197 (17)0.62250 (12)0.48693 (9)0.0306 (4)
H47A0.37720.68210.46730.037*
C480.21420 (17)0.59539 (13)0.50810 (9)0.0332 (4)
H48A0.16080.63560.50250.040*
C490.16054 (17)0.50724 (13)0.53843 (9)0.0334 (4)
H49A0.07190.48970.55390.040*
C500.23424 (16)0.44747 (13)0.54566 (9)0.0316 (4)
H50A0.19660.38880.56610.038*
C510.36826 (16)0.47229 (12)0.52272 (9)0.0268 (3)
C520.44457 (16)0.41122 (12)0.52806 (9)0.0290 (4)
H52A0.40690.35110.54680.035*
C530.57645 (16)0.43707 (12)0.50624 (9)0.0270 (4)
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
Co10.02942 (13)0.02400 (12)0.02744 (13)0.00157 (9)0.00143 (9)0.00138 (9)
N10.0342 (8)0.0256 (7)0.0299 (8)0.0028 (6)0.0049 (6)0.0054 (6)
N20.0357 (8)0.0218 (7)0.0281 (7)0.0018 (6)0.0021 (6)0.0060 (6)
N30.0276 (7)0.0314 (8)0.0315 (8)0.0009 (6)0.0021 (6)0.0029 (6)
N40.0266 (7)0.0300 (8)0.0329 (8)0.0002 (6)0.0048 (6)0.0014 (6)
C10.0360 (10)0.0288 (9)0.0389 (10)0.0034 (8)0.0063 (8)0.0070 (8)
C20.0432 (11)0.0374 (10)0.0478 (12)0.0114 (9)0.0144 (9)0.0108 (9)
C30.0640 (14)0.0376 (11)0.0374 (11)0.0173 (10)0.0151 (10)0.0020 (9)
C40.0582 (13)0.0340 (10)0.0285 (10)0.0092 (9)0.0048 (9)0.0027 (8)
C50.0444 (11)0.0223 (8)0.0251 (9)0.0016 (8)0.0045 (8)0.0056 (7)
C60.0428 (10)0.0230 (8)0.0274 (9)0.0031 (7)0.0012 (8)0.0079 (7)
C70.0556 (12)0.0294 (9)0.0300 (10)0.0056 (9)0.0081 (9)0.0049 (8)
C80.0472 (12)0.0368 (11)0.0485 (12)0.0045 (9)0.0170 (10)0.0093 (9)
C90.0397 (11)0.0324 (10)0.0481 (11)0.0078 (8)0.0041 (9)0.0114 (9)
C100.0360 (10)0.0250 (9)0.0375 (10)0.0045 (8)0.0021 (8)0.0097 (7)
C110.0304 (9)0.0391 (10)0.0392 (10)0.0049 (8)0.0017 (8)0.0069 (8)
C120.0344 (10)0.0600 (13)0.0470 (12)0.0109 (10)0.0012 (9)0.0178 (10)
C130.0330 (10)0.0757 (15)0.0326 (11)0.0048 (10)0.0024 (8)0.0101 (10)
C140.0303 (10)0.0563 (12)0.0322 (10)0.0008 (9)0.0034 (8)0.0007 (9)
C150.0245 (9)0.0390 (10)0.0285 (9)0.0041 (8)0.0045 (7)0.0003 (8)
C160.0280 (9)0.0331 (9)0.0334 (10)0.0021 (8)0.0057 (7)0.0020 (8)
C170.0408 (11)0.0441 (12)0.0404 (11)0.0010 (9)0.0059 (9)0.0099 (9)
C180.0484 (12)0.0348 (11)0.0628 (14)0.0062 (10)0.0110 (11)0.0124 (10)
C190.0368 (11)0.0327 (10)0.0621 (13)0.0056 (8)0.0109 (10)0.0026 (9)
C200.0303 (9)0.0272 (9)0.0451 (11)0.0023 (8)0.0073 (8)0.0045 (8)
K10.02985 (19)0.02562 (18)0.0305 (2)0.00589 (15)0.00308 (15)0.00460 (15)
N50.0424 (9)0.0246 (7)0.0333 (8)0.0051 (6)0.0013 (7)0.0069 (6)
N60.0336 (8)0.0257 (7)0.0366 (8)0.0058 (6)0.0071 (6)0.0037 (6)
O10.0425 (7)0.0369 (7)0.0332 (7)0.0092 (6)0.0060 (6)0.0074 (5)
O20.0282 (6)0.0381 (7)0.0456 (8)0.0033 (5)0.0030 (6)0.0091 (6)
O30.0352 (7)0.0303 (7)0.0475 (8)0.0027 (5)0.0100 (6)0.0057 (6)
O40.0424 (7)0.0296 (6)0.0358 (7)0.0094 (6)0.0135 (6)0.0029 (5)
O50.0465 (7)0.0302 (6)0.0311 (7)0.0127 (6)0.0060 (6)0.0059 (5)
O60.0447 (7)0.0313 (7)0.0327 (7)0.0106 (6)0.0030 (6)0.0059 (5)
C210.0590 (13)0.0278 (9)0.0415 (11)0.0154 (9)0.0008 (9)0.0102 (8)
C220.0585 (13)0.0405 (11)0.0397 (11)0.0178 (10)0.0043 (9)0.0149 (9)
C230.0460 (12)0.0491 (12)0.0421 (11)0.0129 (10)0.0117 (9)0.0064 (9)
C240.0325 (10)0.0503 (12)0.0465 (12)0.0083 (9)0.0064 (9)0.0051 (9)
C250.0305 (10)0.0386 (10)0.0432 (11)0.0019 (8)0.0044 (8)0.0077 (9)
C260.0389 (11)0.0272 (9)0.0472 (11)0.0018 (8)0.0038 (9)0.0001 (8)
C270.0524 (12)0.0278 (9)0.0402 (11)0.0006 (9)0.0073 (9)0.0121 (8)
C280.0415 (11)0.0323 (10)0.0464 (11)0.0037 (8)0.0104 (9)0.0085 (8)
C290.0384 (11)0.0434 (11)0.0491 (12)0.0092 (9)0.0177 (9)0.0089 (9)
C300.0507 (12)0.0405 (11)0.0449 (11)0.0135 (9)0.0235 (10)0.0051 (9)
C310.0437 (11)0.0294 (9)0.0423 (11)0.0118 (8)0.0104 (9)0.0024 (8)
C320.0448 (11)0.0249 (9)0.0468 (11)0.0125 (8)0.0105 (9)0.0040 (8)
C330.0483 (11)0.0237 (9)0.0404 (11)0.0024 (8)0.0029 (9)0.0027 (8)
C340.0469 (11)0.0287 (9)0.0335 (10)0.0120 (8)0.0038 (8)0.0008 (8)
C350.0385 (10)0.0385 (10)0.0273 (9)0.0095 (8)0.0007 (8)0.0027 (8)
C360.0374 (10)0.0409 (10)0.0296 (9)0.0092 (8)0.0004 (8)0.0099 (8)
C370.0487 (11)0.0353 (10)0.0365 (10)0.0170 (9)0.0100 (9)0.0152 (8)
C380.0437 (11)0.0274 (9)0.0461 (11)0.0083 (8)0.0143 (9)0.0134 (8)
O70.0459 (8)0.0471 (8)0.0723 (10)0.0155 (7)0.0048 (7)0.0263 (7)
C390.0455 (12)0.0457 (12)0.0814 (17)0.0064 (10)0.0015 (11)0.0217 (12)
C400.0538 (13)0.0462 (12)0.0670 (15)0.0093 (10)0.0034 (11)0.0226 (11)
C410.0518 (13)0.0528 (13)0.0578 (14)0.0132 (11)0.0011 (11)0.0169 (11)
C420.0409 (11)0.0364 (10)0.0591 (13)0.0100 (9)0.0045 (10)0.0107 (9)
O80.142 (8)0.128 (7)0.086 (4)0.025 (7)0.049 (5)0.024 (4)
C430.060 (4)0.094 (9)0.071 (5)0.019 (4)0.019 (4)0.017 (6)
C440.050 (7)0.076 (8)0.114 (10)0.008 (6)0.005 (6)0.003 (7)
C450.071 (5)0.060 (4)0.044 (4)0.031 (4)0.007 (4)0.007 (4)
C460.113 (10)0.142 (12)0.064 (6)0.041 (8)0.038 (6)0.063 (6)
O8'0.079 (5)0.129 (7)0.179 (9)0.042 (5)0.035 (5)0.012 (6)
C43'0.079 (6)0.109 (7)0.102 (6)0.020 (6)0.053 (5)0.014 (5)
C44'0.070 (5)0.095 (10)0.065 (5)0.005 (5)0.030 (4)0.018 (6)
C45'0.105 (10)0.082 (7)0.150 (11)0.019 (8)0.036 (10)0.049 (8)
C46'0.105 (7)0.147 (9)0.144 (10)0.012 (6)0.080 (7)0.029 (8)
O8"0.105 (13)0.149 (15)0.132 (13)0.034 (11)0.009 (10)0.022 (12)
C43"0.141 (17)0.117 (14)0.075 (11)0.073 (13)0.036 (11)0.002 (11)
C44"0.106 (9)0.144 (12)0.142 (12)0.016 (9)0.087 (9)0.024 (10)
C45"0.087 (12)0.084 (12)0.137 (16)0.014 (10)0.018 (12)0.014 (12)
C46"0.074 (11)0.074 (11)0.061 (10)0.008 (9)0.001 (8)0.000 (9)
C470.0324 (9)0.0273 (9)0.0308 (9)0.0084 (7)0.0009 (7)0.0051 (7)
C480.0333 (10)0.0349 (10)0.0329 (9)0.0152 (8)0.0004 (8)0.0023 (8)
C490.0243 (9)0.0411 (10)0.0325 (9)0.0091 (8)0.0053 (7)0.0034 (8)
C500.0287 (9)0.0306 (9)0.0320 (9)0.0038 (7)0.0053 (7)0.0083 (7)
C510.0261 (8)0.0268 (8)0.0247 (8)0.0049 (7)0.0021 (7)0.0048 (7)
C520.0304 (9)0.0261 (8)0.0293 (9)0.0060 (7)0.0035 (7)0.0082 (7)
C530.0276 (9)0.0262 (8)0.0252 (8)0.0062 (7)0.0012 (7)0.0046 (7)
Geometric parameters (Å, º) top
Co1—N31.8742 (14)C29—C301.499 (3)
Co1—N11.8764 (14)C29—H29A0.9900
Co1—N21.8767 (14)C29—H29B0.9900
Co1—N41.8794 (14)C30—H30A0.9900
N1—C11.372 (2)C30—H30B0.9900
N1—C51.411 (2)C31—C321.508 (3)
N2—C101.369 (2)C31—H31A0.9900
N2—C61.408 (2)C31—H31B0.9900
N3—C111.370 (2)C32—H32A0.9900
N3—C151.405 (2)C32—H32B0.9900
N4—C201.372 (2)C33—C341.505 (3)
N4—C161.401 (2)C33—H33A0.9900
C1—C21.358 (3)C33—H33B0.9900
C1—H1A0.9500C34—H34A0.9900
C2—C31.422 (3)C34—H34B0.9900
C2—H2A0.9500C35—C361.491 (3)
C3—C41.363 (3)C35—H35A0.9900
C3—H3A0.9500C35—H35B0.9900
C4—C51.412 (2)C36—H36A0.9900
C4—H4A0.9500C36—H36B0.9900
C5—C61.405 (3)C37—C381.507 (3)
C6—C71.415 (2)C37—H37A0.9900
C7—C81.365 (3)C37—H37B0.9900
C7—H7A0.9500C38—H38A0.9900
C8—C91.420 (3)C38—H38B0.9900
C8—H8A0.9500O7—C421.426 (2)
C9—C101.360 (2)O7—C391.432 (2)
C9—H9A0.9500C39—C401.503 (3)
C10—H10A0.9500C39—H39A0.9900
C11—C121.365 (3)C39—H39B0.9900
C11—H11A0.9500C40—C411.509 (3)
C12—C131.413 (3)C40—H40A0.9900
C12—H12A0.9500C40—H40B0.9900
C13—C141.363 (3)C41—C421.501 (3)
C13—H13A0.9500C41—H41A0.9900
C14—C151.409 (3)C41—H41B0.9900
C14—H14A0.9500C42—H42A0.9900
C15—C161.405 (3)C42—H42B0.9900
C16—C171.413 (3)O8—C431.428 (9)
C17—C181.360 (3)O8—C461.446 (8)
C17—H17A0.9500C43—C441.508 (9)
C18—C191.409 (3)C43—H43A0.9900
C18—H18A0.9500C43—H43B0.9900
C19—C201.366 (3)C44—C451.509 (9)
C19—H19A0.9500C44—H44A0.9900
C20—H20A0.9500C44—H44B0.9900
K1—O22.7993 (12)C45—C461.501 (8)
K1—O42.8300 (12)C45—H45A0.9900
K1—O62.8377 (12)C45—H45B0.9900
K1—O32.8499 (12)C46—H46A0.9900
K1—O12.8536 (13)C46—H46B0.9900
K1—O52.8968 (12)O8'—C46'1.430 (9)
K1—N53.0262 (14)O8'—C43'1.453 (9)
K1—N63.0618 (14)C43'—C44'1.479 (9)
N5—C211.469 (2)C43'—H43C0.9900
N5—C271.477 (2)C43'—H43D0.9900
N5—C331.478 (2)C44'—C45'1.496 (8)
N6—C321.468 (2)C44'—H44C0.9900
N6—C261.470 (2)C44'—H44D0.9900
N6—C381.473 (2)C45'—C46'1.495 (9)
O1—C231.425 (2)C45'—H45C0.9900
O1—C221.428 (2)C45'—H45D0.9900
O2—C241.415 (2)C46'—H46C0.9900
O2—C251.433 (2)C46'—H46D0.9900
O3—C291.413 (2)O8"—C46"1.427 (9)
O3—C281.434 (2)O8"—C43"1.432 (9)
O4—C301.426 (2)C43"—C44"1.492 (10)
O4—C311.435 (2)C43"—H43E0.9900
O5—C341.427 (2)C43"—H43F0.9900
O5—C351.428 (2)C44"—C45"1.504 (9)
O6—C371.426 (2)C44"—H44E0.9900
O6—C361.428 (2)C44"—H44F0.9900
C21—C221.508 (3)C45"—C46"1.502 (9)
C21—H21A0.9900C45"—H45E0.9900
C21—H21B0.9900C45"—H45F0.9900
C22—H22A0.9900C46"—H46E0.9900
C22—H22B0.9900C46"—H46F0.9900
C23—C241.497 (3)C47—C481.362 (2)
C23—H23A0.9900C47—C53i1.423 (2)
C23—H23B0.9900C47—H47A0.9500
C24—H24A0.9900C48—C491.419 (2)
C24—H24B0.9900C48—H48A0.9500
C25—C261.499 (3)C49—C501.360 (2)
C25—H25A0.9900C49—H49A0.9500
C25—H25B0.9900C50—C511.434 (2)
C26—H26A0.9900C50—H50A0.9500
C26—H26B0.9900C51—C521.391 (2)
C27—C281.496 (3)C51—C53i1.438 (2)
C27—H27A0.9900C52—C531.406 (2)
C27—H27B0.9900C52—H52A0.9500
C28—H28A0.9900C53—C47i1.423 (2)
C28—H28B0.9900C53—C51i1.438 (2)
N3—Co1—N1102.15 (6)H28A—C28—H28B108.3
N3—Co1—N2153.20 (6)O3—C29—C30109.21 (16)
N1—Co1—N283.09 (6)O3—C29—H29A109.8
N3—Co1—N483.16 (6)C30—C29—H29A109.8
N1—Co1—N4156.15 (6)O3—C29—H29B109.8
N2—Co1—N4102.73 (6)C30—C29—H29B109.8
C1—N1—C5116.32 (15)H29A—C29—H29B108.3
C1—N1—Co1127.86 (12)O4—C30—C29109.00 (15)
C5—N1—Co1115.81 (12)O4—C30—H30A109.9
C10—N2—C6116.46 (15)C29—C30—H30A109.9
C10—N2—Co1127.37 (12)O4—C30—H30B109.9
C6—N2—Co1115.85 (12)C29—C30—H30B109.9
C11—N3—C15116.26 (15)H30A—C30—H30B108.3
C11—N3—Co1128.00 (12)O4—C31—C32108.83 (14)
C15—N3—Co1115.56 (12)O4—C31—H31A109.9
C20—N4—C16116.13 (15)C32—C31—H31A109.9
C20—N4—Co1128.02 (12)O4—C31—H31B109.9
C16—N4—Co1115.76 (12)C32—C31—H31B109.9
C2—C1—N1124.48 (18)H31A—C31—H31B108.3
C2—C1—H1A117.8N6—C32—C31113.05 (15)
N1—C1—H1A117.8N6—C32—H32A109.0
C1—C2—C3119.28 (19)C31—C32—H32A109.0
C1—C2—H2A120.4N6—C32—H32B109.0
C3—C2—H2A120.4C31—C32—H32B109.0
C4—C3—C2118.26 (18)H32A—C32—H32B107.8
C4—C3—H3A120.9N5—C33—C34113.22 (14)
C2—C3—H3A120.9N5—C33—H33A108.9
C3—C4—C5121.29 (18)C34—C33—H33A108.9
C3—C4—H4A119.4N5—C33—H33B108.9
C5—C4—H4A119.4C34—C33—H33B108.9
C6—C5—N1112.55 (15)H33A—C33—H33B107.7
C6—C5—C4127.12 (17)O5—C34—C33108.46 (15)
N1—C5—C4120.31 (17)O5—C34—H34A110.0
C5—C6—N2112.67 (15)C33—C34—H34A110.0
C5—C6—C7126.90 (16)O5—C34—H34B110.0
N2—C6—C7120.28 (17)C33—C34—H34B110.0
C8—C7—C6121.15 (18)H34A—C34—H34B108.4
C8—C7—H7A119.4O5—C35—C36108.68 (14)
C6—C7—H7A119.4O5—C35—H35A110.0
C7—C8—C9118.33 (18)C36—C35—H35A110.0
C7—C8—H8A120.8O5—C35—H35B110.0
C9—C8—H8A120.8C36—C35—H35B110.0
C10—C9—C8119.21 (18)H35A—C35—H35B108.3
C10—C9—H9A120.4O6—C36—C35107.88 (14)
C8—C9—H9A120.4O6—C36—H36A110.1
C9—C10—N2124.56 (17)C35—C36—H36A110.1
C9—C10—H10A117.7O6—C36—H36B110.1
N2—C10—H10A117.7C35—C36—H36B110.1
C12—C11—N3124.14 (18)H36A—C36—H36B108.4
C12—C11—H11A117.9O6—C37—C38108.38 (15)
N3—C11—H11A117.9O6—C37—H37A110.0
C11—C12—C13119.5 (2)C38—C37—H37A110.0
C11—C12—H12A120.3O6—C37—H37B110.0
C13—C12—H12A120.3C38—C37—H37B110.0
C14—C13—C12118.16 (18)H37A—C37—H37B108.4
C14—C13—H13A120.9N6—C38—C37113.16 (14)
C12—C13—H13A120.9N6—C38—H38A108.9
C13—C14—C15121.31 (19)C37—C38—H38A108.9
C13—C14—H14A119.3N6—C38—H38B108.9
C15—C14—H14A119.3C37—C38—H38B108.9
N3—C15—C16112.94 (15)H38A—C38—H38B107.8
N3—C15—C14120.45 (18)C42—O7—C39108.73 (15)
C16—C15—C14126.61 (17)O7—C39—C40107.27 (17)
N4—C16—C15112.57 (15)O7—C39—H39A110.3
N4—C16—C17120.69 (18)C40—C39—H39A110.3
C15—C16—C17126.73 (18)O7—C39—H39B110.3
C18—C17—C16121.03 (19)C40—C39—H39B110.3
C18—C17—H17A119.5H39A—C39—H39B108.5
C16—C17—H17A119.5C39—C40—C41103.07 (17)
C17—C18—C19118.39 (18)C39—C40—H40A111.1
C17—C18—H18A120.8C41—C40—H40A111.2
C19—C18—H18A120.8C39—C40—H40B111.1
C20—C19—C18119.4 (2)C41—C40—H40B111.1
C20—C19—H19A120.3H40A—C40—H40B109.1
C18—C19—H19A120.3C42—C41—C40102.07 (17)
C19—C20—N4124.13 (19)C42—C41—H41A111.4
C19—C20—H20A117.9C40—C41—H41A111.4
N4—C20—H20A117.9C42—C41—H41B111.4
O2—K1—O496.52 (4)C40—C41—H41B111.4
O2—K1—O699.43 (4)H41A—C41—H41B109.2
O4—K1—O695.87 (4)O7—C42—C41106.77 (16)
O2—K1—O3122.29 (4)O7—C42—H42A110.4
O4—K1—O360.26 (3)C41—C42—H42A110.4
O6—K1—O3132.34 (4)O7—C42—H42B110.4
O2—K1—O160.00 (4)C41—C42—H42B110.4
O4—K1—O1132.66 (4)H42A—C42—H42B108.6
O6—K1—O1126.36 (4)C43—O8—C46107.8 (8)
O3—K1—O196.17 (4)O8—C43—C44103.3 (9)
O2—K1—O5135.91 (4)O8—C43—H43A111.1
O4—K1—O5122.06 (4)C44—C43—H43A111.1
O6—K1—O559.44 (3)O8—C43—H43B111.1
O3—K1—O596.87 (4)C44—C43—H43B111.1
O1—K1—O599.64 (4)H43A—C43—H43B109.1
O2—K1—N5120.09 (4)C43—C44—C45100.2 (8)
O4—K1—N5120.23 (4)C43—C44—H44A111.7
O6—K1—N5119.44 (4)C45—C44—H44A111.7
O3—K1—N560.34 (4)C43—C44—H44B111.7
O1—K1—N560.32 (4)C45—C44—H44B111.7
O5—K1—N560.25 (4)H44A—C44—H44B109.5
O2—K1—N660.10 (4)C46—C45—C44103.3 (7)
O4—K1—N659.95 (4)C46—C45—H45A111.1
O6—K1—N660.19 (4)C44—C45—H45A111.1
O3—K1—N6119.89 (4)C46—C45—H45B111.1
O1—K1—N6119.84 (4)C44—C45—H45B111.1
O5—K1—N6119.39 (4)H45A—C45—H45B109.1
N5—K1—N6179.63 (4)O8—C46—C45106.3 (7)
C21—N5—C27109.62 (14)O8—C46—H46A110.5
C21—N5—C33109.29 (14)C45—C46—H46A110.5
C27—N5—C33109.38 (14)O8—C46—H46B110.5
C21—N5—K1109.31 (10)C45—C46—H46B110.5
C27—N5—K1109.60 (10)H46A—C46—H46B108.7
C33—N5—K1109.64 (10)C46'—O8'—C43'107.9 (8)
C32—N6—C26109.79 (14)O8'—C43'—C44'105.9 (9)
C32—N6—C38110.31 (14)O8'—C43'—H43C110.6
C26—N6—C38110.45 (14)C44'—C43'—H43C110.6
C32—N6—K1109.34 (10)O8'—C43'—H43D110.6
C26—N6—K1108.90 (10)C44'—C43'—H43D110.6
C38—N6—K1108.00 (10)H43C—C43'—H43D108.7
C23—O1—C22112.27 (14)C43'—C44'—C45'105.5 (8)
C23—O1—K1112.18 (11)C43'—C44'—H44C110.6
C22—O1—K1115.34 (11)C45'—C44'—H44C110.6
C24—O2—C25111.23 (14)C43'—C44'—H44D110.7
C24—O2—K1116.38 (10)C45'—C44'—H44D110.6
C25—O2—K1116.16 (10)H44C—C44'—H44D108.8
C29—O3—C28112.06 (14)C46'—C45'—C44'105.8 (7)
C29—O3—K1113.34 (10)C46'—C45'—H45C110.6
C28—O3—K1114.84 (10)C44'—C45'—H45C110.6
C30—O4—C31110.94 (13)C46'—C45'—H45D110.6
C30—O4—K1113.84 (10)C44'—C45'—H45D110.6
C31—O4—K1114.99 (10)H45C—C45'—H45D108.7
C34—O5—C35112.29 (13)O8'—C46'—C45'107.7 (8)
C34—O5—K1112.03 (9)O8'—C46'—H46C110.2
C35—O5—K1111.76 (9)C45'—C46'—H46C110.2
C37—O6—C36112.19 (13)O8'—C46'—H46D110.2
C37—O6—K1115.01 (10)C45'—C46'—H46D110.2
C36—O6—K1115.52 (9)H46C—C46'—H46D108.5
N5—C21—C22113.55 (15)C46"—O8"—C43"109.9 (8)
N5—C21—H21A108.9O8"—C43"—C44"107.1 (9)
C22—C21—H21A108.9O8"—C43"—H43E110.3
N5—C21—H21B108.9C44"—C43"—H43E110.3
C22—C21—H21B108.9O8"—C43"—H43F110.3
H21A—C21—H21B107.7C44"—C43"—H43F110.3
O1—C22—C21108.92 (15)H43E—C43"—H43F108.5
O1—C22—H22A109.9C43"—C44"—C45"103.6 (9)
C21—C22—H22A109.9C43"—C44"—H44E111.0
O1—C22—H22B109.9C45"—C44"—H44E111.0
C21—C22—H22B109.9C43"—C44"—H44F111.0
H22A—C22—H22B108.3C45"—C44"—H44F111.0
O1—C23—C24108.60 (15)H44E—C44"—H44F109.0
O1—C23—H23A110.0C46"—C45"—C44"103.8 (10)
C24—C23—H23A110.0C46"—C45"—H45E111.0
O1—C23—H23B110.0C44"—C45"—H45E111.0
C24—C23—H23B110.0C46"—C45"—H45F111.0
H23A—C23—H23B108.4C44"—C45"—H45F111.0
O2—C24—C23109.00 (16)H45E—C45"—H45F109.0
O2—C24—H24A109.9O8"—C46"—C45"106.2 (8)
C23—C24—H24A109.9O8"—C46"—H46E110.5
O2—C24—H24B109.9C45"—C46"—H46E110.5
C23—C24—H24B109.9O8"—C46"—H46F110.5
H24A—C24—H24B108.3C45"—C46"—H46F110.5
O2—C25—C26109.05 (14)H46E—C46"—H46F108.7
O2—C25—H25A109.9C48—C47—C53i121.03 (16)
C26—C25—H25A109.9C48—C47—H47A119.5
O2—C25—H25B109.9C53i—C47—H47A119.5
C26—C25—H25B109.9C47—C48—C49120.25 (16)
H25A—C25—H25B108.3C47—C48—H48A119.9
N6—C26—C25114.18 (15)C49—C48—H48A119.9
N6—C26—H26A108.7C50—C49—C48120.93 (16)
C25—C26—H26A108.7C50—C49—H49A119.5
N6—C26—H26B108.7C48—C49—H49A119.5
C25—C26—H26B108.7C49—C50—C51120.57 (16)
H26A—C26—H26B107.6C49—C50—H50A119.7
N5—C27—C28113.94 (15)C51—C50—H50A119.7
N5—C27—H27A108.8C52—C51—C50121.63 (15)
C28—C27—H27A108.8C52—C51—C53i120.00 (14)
N5—C27—H27B108.8C50—C51—C53i118.37 (15)
C28—C27—H27B108.8C51—C52—C53121.06 (15)
H27A—C27—H27B107.7C51—C52—H52A119.5
O3—C28—C27109.10 (15)C53—C52—H52A119.5
O3—C28—H28A109.9C52—C53—C47i122.24 (15)
C27—C28—H28A109.9C52—C53—C51i118.94 (15)
O3—C28—H28B109.9C47i—C53—C51i118.81 (14)
C27—C28—H28B109.9
N3—Co1—N1—C127.24 (15)K1—N5—C21—C2242.36 (18)
N2—Co1—N1—C1179.42 (15)C23—O1—C22—C21175.37 (16)
N4—Co1—N1—C173.5 (2)K1—O1—C22—C2154.44 (18)
N3—Co1—N1—C5152.02 (11)N5—C21—C22—O166.8 (2)
N2—Co1—N1—C51.32 (11)C22—O1—C23—C24175.29 (16)
N4—Co1—N1—C5107.28 (17)K1—O1—C23—C2452.92 (18)
N3—Co1—N2—C1071.4 (2)C25—O2—C24—C23178.00 (15)
N1—Co1—N2—C10174.72 (14)K1—O2—C24—C2345.88 (18)
N4—Co1—N2—C1028.77 (14)O1—C23—C24—O266.5 (2)
N3—Co1—N2—C6101.88 (16)C24—O2—C25—C26166.36 (15)
N1—Co1—N2—C61.45 (11)K1—O2—C25—C2657.42 (17)
N4—Co1—N2—C6157.96 (11)C32—N6—C26—C25157.10 (15)
N1—Co1—N3—C1129.96 (15)C38—N6—C26—C2581.03 (19)
N2—Co1—N3—C1168.9 (2)K1—N6—C26—C2537.41 (17)
N4—Co1—N3—C11173.63 (15)O2—C25—C26—N664.4 (2)
N1—Co1—N3—C15155.13 (11)C21—N5—C27—C28159.76 (15)
N2—Co1—N3—C15106.04 (16)C33—N5—C27—C2880.43 (18)
N4—Co1—N3—C151.28 (11)K1—N5—C27—C2839.79 (17)
N3—Co1—N4—C20176.92 (15)C29—O3—C28—C27172.82 (15)
N1—Co1—N4—C2072.3 (2)K1—O3—C28—C2755.98 (17)
N2—Co1—N4—C2029.63 (15)N5—C27—C28—O365.9 (2)
N3—Co1—N4—C160.66 (11)C28—O3—C29—C30178.01 (15)
N1—Co1—N4—C16104.00 (18)K1—O3—C29—C3050.03 (18)
N2—Co1—N4—C16154.11 (11)C31—O4—C30—C29178.76 (16)
C5—N1—C1—C22.5 (2)K1—O4—C30—C2949.66 (19)
Co1—N1—C1—C2176.74 (14)O3—C29—C30—O467.7 (2)
N1—C1—C2—C30.8 (3)C30—O4—C31—C32170.51 (16)
C1—C2—C3—C41.3 (3)K1—O4—C31—C3258.51 (17)
C2—C3—C4—C51.6 (3)C26—N6—C32—C3180.24 (18)
C1—N1—C5—C6179.71 (14)C38—N6—C32—C31157.81 (15)
Co1—N1—C5—C60.94 (18)K1—N6—C32—C3139.18 (17)
C1—N1—C5—C42.1 (2)O4—C31—C32—N666.8 (2)
Co1—N1—C5—C4177.21 (12)C21—N5—C33—C3479.84 (18)
C3—C4—C5—C6178.02 (17)C27—N5—C33—C34160.15 (16)
C3—C4—C5—N10.2 (3)K1—N5—C33—C3439.95 (18)
N1—C5—C6—N20.2 (2)C35—O5—C34—C33173.34 (14)
C4—C5—C6—N2178.23 (16)K1—O5—C34—C3359.93 (15)
N1—C5—C6—C7175.24 (16)N5—C33—C34—O569.7 (2)
C4—C5—C6—C72.8 (3)C34—O5—C35—C36179.68 (14)
C10—N2—C6—C5175.33 (14)K1—O5—C35—C3653.44 (15)
Co1—N2—C6—C51.31 (17)C37—O6—C36—C35176.19 (14)
C10—N2—C6—C70.5 (2)K1—O6—C36—C3549.33 (16)
Co1—N2—C6—C7174.50 (12)O5—C35—C36—O669.47 (18)
C5—C6—C7—C8174.02 (17)C36—O6—C37—C38167.67 (14)
N2—C6—C7—C81.1 (3)K1—O6—C37—C3857.60 (16)
C6—C7—C8—C90.8 (3)C32—N6—C38—C3777.09 (18)
C7—C8—C9—C100.2 (3)C26—N6—C38—C37161.35 (15)
C8—C9—C10—N20.9 (3)K1—N6—C38—C3742.36 (17)
C6—N2—C10—C90.5 (2)O6—C37—C38—N669.15 (19)
Co1—N2—C10—C9172.69 (13)C42—O7—C39—C404.9 (2)
C15—N3—C11—C123.6 (2)O7—C39—C40—C4124.6 (3)
Co1—N3—C11—C12178.50 (14)C39—C40—C41—C4233.6 (2)
N3—C11—C12—C130.3 (3)C39—O7—C42—C4117.3 (2)
C11—C12—C13—C142.5 (3)C40—C41—C42—O731.9 (2)
C12—C13—C14—C150.6 (3)C46—O8—C43—C4433.0 (18)
C11—N3—C15—C16173.87 (15)O8—C43—C44—C4543.3 (14)
Co1—N3—C15—C161.65 (18)C43—C44—C45—C4637.3 (13)
C11—N3—C15—C145.4 (2)C43—O8—C46—C458.8 (19)
Co1—N3—C15—C14179.04 (12)C44—C45—C46—O818.8 (15)
C13—C14—C15—N33.5 (3)C46'—O8'—C43'—C44'26.7 (18)
C13—C14—C15—C16175.70 (18)O8'—C43'—C44'—C45'25.9 (19)
C20—N4—C16—C15176.64 (14)C43'—C44'—C45'—C46'16 (2)
Co1—N4—C16—C150.08 (18)C43'—O8'—C46'—C45'16.8 (19)
C20—N4—C16—C174.6 (2)C44'—C45'—C46'—O8'0 (2)
Co1—N4—C16—C17178.72 (13)C46"—O8"—C43"—C44"7 (3)
N3—C15—C16—N41.1 (2)O8"—C43"—C44"—C45"24 (3)
C14—C15—C16—N4179.66 (16)C43"—C44"—C45"—C46"30 (2)
N3—C15—C16—C17177.63 (16)C43"—O8"—C46"—C45"12 (3)
C14—C15—C16—C171.6 (3)C44"—C45"—C46"—O8"27 (2)
N4—C16—C17—C182.2 (3)C53i—C47—C48—C490.8 (3)
C15—C16—C17—C18179.15 (18)C47—C48—C49—C501.2 (3)
C16—C17—C18—C191.6 (3)C48—C49—C50—C510.0 (3)
C17—C18—C19—C203.0 (3)C49—C50—C51—C52178.57 (16)
C18—C19—C20—N40.5 (3)C49—C50—C51—C53i1.6 (2)
C16—N4—C20—C193.3 (2)C50—C51—C52—C53179.18 (15)
Co1—N4—C20—C19179.50 (13)C53i—C51—C52—C530.7 (3)
C27—N5—C21—C2277.79 (19)C51—C52—C53—C47i178.15 (15)
C33—N5—C21—C22162.34 (15)C51—C52—C53—C51i0.7 (3)
Symmetry code: (i) x+1, y+1, z+1.

Experimental details

(1)(2)
Crystal data
Chemical formula[K(C18H36N2O6)2][Fe(C10H8N2)3](C14H10)[K(C18H36N2O6)][Co(C10H8N2)2]·0.5C14H10·2C4H8O
Mr1533.791020.20
Crystal system, space groupMonoclinic, C2/cTriclinic, P1
Temperature (K)173173
a, b, c (Å)23.049 (4), 17.067 (3), 21.543 (3)10.5981 (8), 14.4323 (11), 18.4886 (15)
α, β, γ (°)90, 109.779 (3), 9099.1054 (13), 90.8279 (14), 109.2433 (13)
V3)7975 (2)2629.5 (4)
Z42
Radiation typeMo KαMo Kα
µ (mm1)0.360.46
Crystal size (mm)0.42 × 0.16 × 0.060.40 × 0.18 × 0.12
Data collection
DiffractometerSiemens SMART CCD platform
diffractometer
Siemens SMART CCD platform
diffractometer
Absorption correctionMulti-scan
(SADABS; Sheldrick, 2012)
Multi-scan
(SADABS; Sheldrick, 2012)
Tmin, Tmax0.637, 0.7450.684, 0.745
No. of measured, independent and
observed [I > 2σ(I)] reflections
22943, 7069, 4398 26404, 9299, 7616
Rint0.0850.021
(sin θ/λ)max1)0.5960.595
Refinement
R[F2 > 2σ(F2)], wR(F2), S 0.057, 0.122, 1.02 0.031, 0.079, 1.03
No. of reflections70699299
No. of parameters474715
No. of restraints0257
H-atom treatmentH-atom parameters constrainedH-atom parameters constrained
Δρmax, Δρmin (e Å3)0.27, 0.390.31, 0.22

Computer programs: SMART (Bruker, 2003), SAINT (Bruker, 2003), SIR97 (Altomare et al., 1999), SHELXL2014 (Sheldrick, 2014), SHELXTL (Sheldrick, 2008).

Selected bond lengths (Å) for (1) top
Fe1—N11.959 (2)C36—C371.380 (4)
Fe1—N31.965 (2)C37—C381.414 (4)
Fe1—N21.969 (2)C38—C391.406 (4)
C5—C61.431 (4)C38—C40ii1.451 (4)
C15—C15i1.411 (6)C39—C401.412 (4)
C34—C40ii1.415 (4)C40—C34ii1.415 (4)
C35—C361.399 (5)
Symmetry codes: (i) x+2, y, z+1/2; (ii) x+3/2, y+1/2, z+1.
Selected geometric parameters (Å, º) for (2) top
Co1—N31.8742 (14)C48—C491.419 (2)
Co1—N11.8764 (14)C49—C501.360 (2)
Co1—N21.8767 (14)C50—C511.434 (2)
Co1—N41.8794 (14)C51—C521.391 (2)
C5—C61.405 (3)C51—C53i1.438 (2)
C15—C161.405 (3)C52—C531.406 (2)
C47—C481.362 (2)C53—C47i1.423 (2)
C47—C53i1.423 (2)
N3—Co1—N2153.20 (6)N3—Co1—N483.16 (6)
N1—Co1—N283.09 (6)N1—Co1—N4156.15 (6)
Symmetry code: (i) x+1, y+1, z+1.
 

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