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metal-organic compounds\(\def\hfill{\hskip 5em}\def\hfil{\hskip 3em}\def\eqno#1{\hfil {#1}}\)

Journal logoIUCrDATA
ISSN: 2414-3146
Volume 10| Part 7| July 2025| x250632
https://doi.org/10.1107/S2414314625006327

Bis­[N,N-bis­­(di­phenyl­phosphan­yl)cyclo­hexa­namine-κ2P,P′]di­chlorido­cobalt(III) tris­­(μ-di­phenyl­phos­phinato-κ2O:O′)bis­­[chloridocobaltate(II)]–di­chloro­methane–di­ethyl ether (1/1.189/0.811)

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Sizwe J. Zamisa,a* Adesola A. Adeleke,a Dunesha Naicker,a Holger B. Friedricha and Bernard Omondia

aSchool of Chemistry and Physics, University of KwaZulu-Natal, Private Bag X54001, Durban, 4000, Republic of South Africa
*Correspondence e-mail: [email protected]

Edited by M. Zeller, Purdue University, USA (Received 1 July 2025; accepted 16 July 2025; online 29 July 2025)

The DCM-Et2O solvated title compound, [CoCl2(C30H31NP2)2][Co2(C12H10O2P)3Cl2]·1.189CH2Cl2·0.811C4H10O or [CoCl2{Ph2PN(C6H11)PPh2}2][Co2{Ph2PO2}3Cl2]·1.189DCM·0.811Et2O, is a combination of a cationic CoIII-amino­diphosphine and a dimetallic CoII-di­phenyl­phospho­nate anionic species. The asymmetric unit features one half of the cationic and anionic species with solvent mol­ecules in the outer coordination sphere. The metal centre of the cation is located on an inversion center, while the anion is disordered around an inversion center. The cyclo­hexa­nyl moiety of the amino­diphosphine ligand exhibits two-component rotational disorder along the N—C bond, the moiety's major component occupancy refined to 71.1 (7)%. The di­chloro­methane and diethyl ether solvate mol­ecules are disordered with each other and were modelled with 59.4 (3)% and 40.6 (3)% site occupancies in the asymmetric unit, respectively. Inter­molecular C—H⋯π hydrogen-bonding patterns form infinite supra­molecular sheets extending parallel to (110). C—H⋯Cl and C—H⋯O hydrogen bonds were also found in the crystal packing of the title compound.

CCDC reference: 2473254

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[Scheme 3D1]
Chemical scheme
[Scheme 1]

Structure description

Nitro­gen-containing polyphosphines are known for their diverse structural motifs, versatile donating ability, and wide applications, especially in homogeneous catalysis (Parisel et al., 2004[Parisel, S. L., Moorcroft, N. D., Jutand, A., Aldous, D. J. & Hii, K. K. M. (2004). Org. Biomol. Chem. 2, 301-306.]; Wang et al., 2013[Wang, Y., Pan, J., Chen, Z., Sun, X. & Wang, Z. (2013). Mini Rev. Med. Chem. 13, 836-844.]) and supra­molecular chemistry (Wang et al., 2013[Wang, Y., Pan, J., Chen, Z., Sun, X. & Wang, Z. (2013). Mini Rev. Med. Chem. 13, 836-844.]). A commonly used ligand in this group is the flexible ‘PNP' amino­diphosphine ligand, which has a nitro­gen atom that does not coordinate to the metal centre. Over the years, various derivatives of their transition-metal complexes have been synthesized (Benito-Garagorri & Kirchner, 2008[Benito-Garagorri, D. & Kirchner, K. (2008). Acc. Chem. Res. 41, 201-213.]; Merz et al., 2020[Merz, L. S., Ballmann, J. & Gade, L. H. (2020). Eur. J. Inorg. Chem. pp. 2023-2042.]; Xiao et al., 2020[Xiao, Z., Natarajan, M., Zhong, W. & Liu, X. (2020). Electrochim. Acta 340, 135998.]) where the substituents on the phospho­rus and nitro­gen atoms were derivatized, thus encouraging fine-tuning of their steric and electronic properties. Such modifications influence their catalytic activity, including the electrolytic activities (Xiao et al., 2020[Xiao, Z., Natarajan, M., Zhong, W. & Liu, X. (2020). Electrochim. Acta 340, 135998.]) and promoting proton-coupled electron transfer in the catalytic reduction of protons (DuBois, 2014[DuBois, D. L. (2014). Inorg. Chem. 53, 3935-3960.]). Consequently, the ‘PNP' ligand framework continues to gain attention when designing efficient catalysts with broad applications. In an effort to grow a crystal of a cobalt amino­diphosphine complex having a cyclo­hexyl ring on its nitro­gen atom as related to the continuation of our research on cobalt amino­diphosphine complexes as catalysts in the oxidation of n-octane (Naicker et al., 2015[Naicker, D., Friedrich, H. B. & Omondi, B. (2015). RSC Adv. 5, 63123-63129.]), we determined the crystal structure of the title compound. It is suspected that the partial oxidation of the diphosphine ligand could have occurred during our crystal growth attempt, thus leading to the formation of the title compound.

In the asymmetric unit of the title compound, there is half of a cationic cobalt(III) amino­diphosphine complex and one half of the dimetallic cobalt(II)-diphosphinite anionic complex, with di­chloro­methane and diethyl ether solvent mol­ecules. Moreover, the metal centre of the cation is located on an inversion center (symmetry operation: 1 − x, −y, −z), while the anion is disordered around an inversion center (symmetry operation: 1 − x, −y, 1 − z). In the structure of the cationic cobalt(III) amino­diphosphine species, the Co1 atom adopts a distorted octa­hedral geometry in which the Cl atoms occupy the axial positions of the octa­hedral vertices (Fig. 1[link]). Two amino­diphosphine ligands, through the four P atoms, occupy the equatorial positions with acute P1—Co1—P2 bite angles [70.50 (2)°], which engender a short P1⋯P2 contact [2.6243 (8) Å] compared to the uncoordinated N-cyclo­hexyl-N-(di­phenyl­phosphan­yl)-1,1-di­phenyl­phosphanamine [P⋯P = 2.9750 (6) Å; Naicker et al., 2016[Naicker, D., Pansuriya, P. B. & Friedrich, H. B. (2016). Z. Kristallogr. New Cryst. Struct. 231, 653-656.]]. The coordination mode exhibited by the amino­diphosphine ligand is bidentate and forms an almost planar four-membered metallacycle defined by Co1—P1—N1—P2. In the anionic cobalt(II) diphosphinite complex, the Co2 and Co3 metal centres are each coordinated to separate Cl atoms, Cl2 and Cl3, respectively, and are bridged by three diphosphinite ligands via their oxygen atoms as shown in Fig. 2[link]. Moreover, the Co2 and Co3 atoms exhibit a distorted tetra­hedral geometry with O—Co—O and O—Co—Cl bond angles of 103.4 (2)–109.5 (2)° to 108.75 (2)–114.3 (2)°, respectively. The geometric bond parameters around the metal centres in both the cationic and anionic species are comparable with those of closely related structures reported in the literature (Naktode et al., 2014[Naktode, K., Kottalanka, R. K., Adimulam, H. & Panda, T. K. (2014). J. Coord. Chem. 67, 3042-3053.]; Fliedel et al., 2016[Fliedel, C., Rosa, V., Vileno, B., Parizel, N., Choua, S., Gourlaouen, C., Rosa, P., Turek, P. & Braunstein, P. (2016). Inorg. Chem. 55, 4183-4198.]).

[Figure 1]
Figure 1
Molecular structure of the cationic species of the title compound with displacement ellipsoids drawn at the 50% probability level. The disordered cyclohexanyl moieties are drawn in a faded grey colour and the disordered solvent molecules have been omitted for clarity.
[Figure 2]
Figure 2
Molecular structure of the anionic species of the title compound with displacement ellipsoids drawn at the 50% probability level. The disordered second anionic moiety is drawn in a faded grey colour and the disordered solvent molecules have been omitted for clarity.

No π–π stacking inter­actions are observed in the crystal packing of the title compound. However, C—H⋯O hydrogen bonds are found between the H17 atom of the phenyl ring and the O7 atom of the diethyl ether mol­ecule, as well as C—H⋯Cl inter­actions between the H6 atom of the phenyl moiety and Cl4 of the di­chloro­methane mol­ecule (Table 1[link]). Intra­molecular C—H⋯Cl hydrogen-bonding patterns with a S(6) graph-set motif are found between the H2 and Cl1 atoms of the cationic complex (Table 1[link]). Conversely, inter­molecular C24—H24⋯Cl2 hydrogen bonds link together neighbouring cationic and anionic complexes to form a supra­molecular chain along the crystallographic c-axis direction. The crystal packing is further consolidated by inter­molecular C—H⋯π hydrogen bonds between the phenyl rings of neighbouring amino­diphosphine and phosphinite moieties (Table 1[link]), which form two-dimensional supra­molecular structures along the crystallographic ac plane (Fig. 3[link]).

Table 1
Hydrogen-bond geometry (Å, °)

Cg1, Cg2 and Cg3 are the centroids of the C37–C41/C65, C42/C61–C64/C66 and C19–C24 rings, respectively.
D—H⋯A D—H H⋯A D⋯A D—H⋯A
C2—H2⋯Cl1i 0.95 2.66 3.174 (2) 114
C6—H6⋯Cl4i 0.95 2.95 3.668 (4) 133
C17—H17⋯O7 0.95 2.48 3.314 (8) 146
C24—H24⋯Cl2ii 0.95 2.96 3.682 (5) 133
C27—H27B⋯Cg1 0.99 2.97 3.834 (11) 147
C53—H53⋯Cg2iii 0.95 2.98 3.787 (8) 143
C60—H60⋯Cg3ii 0.95 2.72 3.626 (8) 159
C29A—H29C⋯Cg2ii 0.99 2.69 3.57 (2) 148
Symmetry codes: (i) Mathematical equation; (ii) Mathematical equation; (iii) Mathematical equation.
[Figure 3]
Figure 3
Representation of C—H⋯π hydrogen-bonding patterns in the crystal packing of the title compound.

Synthesis and crystallization

The title compound was synthesized following a literature procedure (Naicker et al., 2015[Naicker, D., Friedrich, H. B. & Omondi, B. (2015). RSC Adv. 5, 63123-63129.]). The crude product was recrystallized via vapour diffusion of diethyl ether into a di­chloro­methane solution of the crude product to obtain green plate-like single crystals suitable for X-ray diffraction.

Refinement

Crystallographic data and structure refinement details are summarized in Table 2[link]. The cyclo­hexa­nyl moiety of the amino­diphosphine ligand exhibits a two-component rotational disorder along the N—C bond, while the di­phenyl­phospho­nate ligands in the anionic complex shows disorder around the inversion centre located between the two Co(II) atoms. The whole anionic species was modelled using PART −1 instruction with 50% site occupancy in the asymmetric unit, while the disordered cyclo­hexa­nyl moiety's major component was modelled using PART 1 and 2 instructions with 71.1 (7)% site occupancy. The di­chloro­methane and diether ether mol­ecules were modelled using PART 1 and 2 instructions with 59.4 (3)% and 40.6 (3)% site occupancies in the asymmetric unit, respectively.

Table 2
Experimental details

Crystal data
Chemical formula [CoCl2(C30H31NP2)2][Co2(C12H10O2P)3Cl2]·1.189CH2Cl2·0.811C4H10O
Mr 2066.26
Crystal system, space group Monoclinic, P21/c
Temperature (K) 100
a, b, c (Å) 10.365 (6), 23.0516 (5), 19.9984 (6)
β (°) 96.641 (1)
V (Å3) 4746 (3)
Z 2
Radiation type Cu Kα
μ (mm−1) 7.28
Crystal size (mm) 0.18 × 0.06 × 0.06
 
Data collection
Diffractometer Bruker SMART APEXII area detector
Absorption correction Multi-scan (SADABS; Krause et al., 2015[Krause, L., Herbst-Irmer, R., Sheldrick, G. M. & Stalke, D. (2015). J. Appl. Cryst. 48, 3-10.])
Tmin, Tmax 0.359, 0.674
No. of measured, independent and observed [I > 2σ(I)] reflections 18724, 9405, 8330
Rint 0.021
(sin θ/λ)max (Å−1) 0.624
 
Refinement
R[F2 > 2σ(F2)], wR(F2), S 0.038, 0.093, 1.03
No. of reflections 9405
No. of parameters 848
No. of restraints 297
H-atom treatment H-atom parameters constrained
Δρmax, Δρmin (e Å−3) 0.50, −0.49
Computer programs: COSMO and SAINT (Bruker, 2009[Bruker (2009). COSMO and SAINT. Bruker AXS Inc., Madison, Wisconsin, USA.]), SHELXT2018/2 (Sheldrick, 2015a[Sheldrick, G. M. (2015a). Acta Cryst. A71, 3-8.]), SHELX2018/3 (Sheldrick, 2015b[Sheldrick, G. M. (2015b). Acta Cryst. C71, 3-8.]), OLEX2 (Dolomanov et al., 2009[Dolomanov, O. V., Bourhis, L. J., Gildea, R. J., Howard, J. A. K. & Puschmann, H. (2009). J. Appl. Cryst. 42, 339-341.]).

The geometry of the ether mol­ecule was restrained. The two C—O bond distances were restrained to be similar (s.u. 0.02 Å) and 1,3 distances were restrained to target values of 2.36 (1) for the O—C—C angles, and 2.359 (1) for the C—O—C angle. Uij components of ADPs for disordered ether and DCM atoms closer to each other than 2.0 Å were restrained to be similar with an s.u. of 0.01 Å2. The two disordered cyclo­hexyl moieties were restrained to have similar geometries (SAME restraint with s.u. 0.02 Å. The two N—C bond lengths were restrained to be similar in length (SADI restraint with s.u. 0.02 Angstrom). Uij components of ADPs for disordered ether and DCM atoms closer to each other than 2.0 Å were restrained to be similar with an s.u. of 0.01 Å2. The Co and Cl atoms in the anion are related by pseudo-inversion and the ADPs of cobalt and chlorine atoms were each constrained to be identical (EADP constraint). The Co—Cl bonds as well as all Co—O bonds were each restrained to be similar (SADI restraints with s.u. 0.02 Å). Half of the phenyl rings of the anion (which overlap with their counterparts from inversion) were constrained to resemble ideal hexa­gons with 1.39 A C—C bonds (AFIX 66 constraint). Constrained were C31—C36 and C49—C54.

Structural data

CCDC reference: 2473254

Crystal structure: contains datablock I. DOI: https://doi.org/10.1107/S2414314625006327/zl4085sup1.cif

Structure factors: contains datablock I. DOI: https://doi.org/10.1107/S2414314625006327/zl4085Isup2.hkl

checkCIF report


Computing details top

Bis[N,N-bis(diphenylphosphanyl)cyclohexanamine-κ2P,P']dichloridocobalt(III) tris(µ-diphenylphosphinato-κ2O:O')bis[chloridocobaltate(II)]–dichloromethane–diethyl ether (1/1.189/0.811) top
Crystal data top
[CoCl2(C30H31NP2)2][Co2(C12H10O2P)3Cl2]·1.189CH2Cl2·0.811C4H10OF(000) = 2136
Mr = 2066.26Dx = 1.446 Mg m−3
Monoclinic, P21/cCu Kα radiation, λ = 1.54184 Å
a = 10.365 (6) ÅCell parameters from 9277 reflections
b = 23.0516 (5) Åθ = 2.5–28.4°
c = 19.9984 (6) ŵ = 7.28 mm−1
β = 96.641 (1)°T = 100 K
V = 4746 (3) Å3Plate, green
Z = 20.18 × 0.06 × 0.06 mm
Data collection top
Bruker SMART APEXII area detector
diffractometer		8330 reflections with I > 2σ(I)
Detector resolution: 7.9 pixels mm-1Rint = 0.021
ω and φ scansθmax = 74.2°, θmin = 3.8°
Absorption correction: multi-scan
(SADABS; Krause et al., 2015)		h = −12→12
Tmin = 0.359, Tmax = 0.674k = −28→25
18724 measured reflectionsl = −24→20
9405 independent reflections
Refinement top
Refinement on F2Primary atom site location: dual
Least-squares matrix: fullHydrogen site location: inferred from neighbouring sites
R[F2 > 2σ(F2)] = 0.038H-atom parameters constrained
wR(F2) = 0.093 w = 1/[σ2(Fo2) + (0.0371P)2 + 3.8871P]
where P = (Fo2 + 2Fc2)/3
S = 1.03(Δ/σ)max = 0.001
9405 reflectionsΔρmax = 0.50 e Å−3
848 parametersΔρmin = −0.49 e Å−3
297 restraints
Special details top

Geometry. All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes.

Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top
xyzUiso*/UeqOcc. (<1)
Co10.5000000.0000000.0000000.01898 (10)
Cl10.69903 (4)0.01872 (2)0.04848 (2)0.02301 (10)
P10.51415 (5)−0.08972 (2)0.04709 (3)0.02132 (11)
P20.42620 (5)0.00310 (2)0.10286 (3)0.02095 (11)
N10.43784 (17)−0.07018 (8)0.11469 (9)0.0233 (4)
C10.4307 (2)−0.15243 (9)0.00676 (11)0.0269 (4)
C20.2955 (2)−0.15165 (10)−0.00755 (11)0.0297 (5)
H20.247538−0.1197990.0068380.036*
C30.2306 (3)−0.19715 (11)−0.04272 (12)0.0364 (6)
H30.138606−0.196392−0.0519540.044*
C40.3000 (3)−0.24342 (11)−0.06419 (13)0.0415 (6)
H40.255504−0.274252−0.0885270.050*
C50.4332 (3)−0.24503 (11)−0.05047 (13)0.0424 (6)
H50.480583−0.276835−0.0654800.051*
C60.4985 (3)−0.19995 (10)−0.01453 (12)0.0338 (5)
H60.590296−0.201616−0.0044270.041*
C70.6792 (2)−0.11345 (9)0.07478 (11)0.0258 (4)
C80.7311 (2)−0.11461 (10)0.14218 (12)0.0313 (5)
H80.677558−0.1057660.1763040.038*
C90.8610 (2)−0.12868 (11)0.15962 (14)0.0381 (6)
H90.895754−0.1296820.2056890.046*
C100.9402 (2)−0.14127 (11)0.11022 (15)0.0404 (6)
H101.028565−0.1515190.1224100.048*
C110.8901 (2)−0.13883 (11)0.04320 (14)0.0387 (6)
H110.944492−0.1468350.0092170.046*
C120.7608 (2)−0.12477 (10)0.02543 (12)0.0319 (5)
H120.727317−0.122795−0.0207820.038*
C130.2620 (2)0.02661 (9)0.11248 (10)0.0239 (4)
C140.1548 (2)−0.00558 (10)0.08462 (11)0.0251 (4)
H140.167735−0.0410480.0621480.030*
C150.0297 (2)0.01382 (10)0.08950 (11)0.0289 (5)
H15−0.042443−0.0088660.0713340.035*
C160.0093 (2)0.06633 (11)0.12084 (12)0.0345 (5)
H16−0.0765370.0798790.1234070.041*
C170.1147 (2)0.09870 (11)0.14825 (13)0.0355 (5)
H170.1010600.1346520.1695760.043*
C180.2403 (2)0.07895 (10)0.14477 (12)0.0300 (5)
H180.3119960.1011500.1644880.036*
C190.5293 (2)0.04136 (10)0.16797 (11)0.0265 (4)
C200.5585 (3)0.09922 (11)0.15560 (12)0.0350 (5)
H200.5202290.1176130.1156520.042*
C210.6434 (3)0.13005 (13)0.20139 (14)0.0446 (7)
H210.6617270.1696010.1930650.053*
C220.7010 (3)0.10325 (13)0.25895 (15)0.0477 (7)
H220.7606970.1240730.2896550.057*
C230.6720 (3)0.04630 (13)0.27193 (14)0.0440 (7)
H230.7106910.0282380.3120120.053*
C240.5864 (2)0.01507 (11)0.22681 (12)0.0338 (5)
H240.566859−0.0241770.2361020.041*
C250.4157 (5)−0.10776 (17)0.1757 (2)0.0265 (8)0.711 (7)
H250.492899−0.1024600.2100980.032*0.711 (7)
C260.2969 (5)−0.0881 (2)0.2078 (3)0.0319 (10)0.711 (7)
H26A0.218794−0.0914400.1744790.038*0.711 (7)
H26B0.307164−0.0467790.2209850.038*0.711 (7)
C270.2784 (6)−0.1249 (3)0.2702 (3)0.0363 (12)0.711 (7)
H27A0.351404−0.1176560.3056960.044*0.711 (7)
H27B0.196991−0.1132050.2879430.044*0.711 (7)
C280.2726 (5)−0.18899 (19)0.2531 (2)0.0419 (10)0.711 (7)
H28A0.194786−0.1969350.2208550.050*0.711 (7)
H28B0.265411−0.2118270.2944340.050*0.711 (7)
C290.3946 (6)−0.2074 (3)0.2222 (3)0.0397 (13)0.711 (7)
H29A0.389416−0.2491880.2108780.048*0.711 (7)
H29B0.472228−0.2011880.2552340.048*0.711 (7)
C300.4071 (5)−0.17186 (19)0.1585 (2)0.0332 (10)0.711 (7)
H30A0.485875−0.1840030.1385730.040*0.711 (7)
H30B0.330734−0.1789930.1249970.040*0.711 (7)
C25A0.3675 (11)−0.1071 (4)0.1588 (5)0.0288 (18)0.289 (7)
H25A0.284683−0.1192530.1317900.035*0.289 (7)
C26A0.4445 (12)−0.1622 (5)0.1769 (6)0.035 (2)0.289 (7)
H26C0.523762−0.1529690.2076340.042*0.289 (7)
H26D0.471048−0.1803420.1357850.042*0.289 (7)
C27A0.3558 (14)−0.2047 (7)0.2122 (7)0.038 (2)0.289 (7)
H27C0.276008−0.2133700.1816120.046*0.289 (7)
H27D0.402344−0.2415990.2231370.046*0.289 (7)
C28A0.3205 (12)−0.1767 (5)0.2758 (5)0.0409 (19)0.289 (7)
H28C0.400238−0.1696050.3070430.049*0.289 (7)
H28D0.263465−0.2028990.2982870.049*0.289 (7)
C29A0.2504 (15)−0.1190 (7)0.2588 (8)0.036 (2)0.289 (7)
H29C0.167031−0.1268490.2308720.043*0.289 (7)
H29D0.230529−0.1003820.3010440.043*0.289 (7)
C30A0.3306 (12)−0.0776 (5)0.2213 (6)0.031 (2)0.289 (7)
H30C0.279692−0.0421030.2086510.037*0.289 (7)
H30D0.409995−0.0660920.2507110.037*0.289 (7)
Co20.4494 (3)0.04230 (11)0.56458 (15)0.0252 (3)0.5
Co30.5664 (3)−0.05433 (11)0.42347 (15)0.0252 (3)0.5
Cl20.3763 (4)0.09917 (13)0.64369 (18)0.0339 (4)0.5
Cl30.6335 (4)−0.11390 (13)0.34402 (18)0.0339 (4)0.5
P40.72920 (11)0.04486 (5)0.50884 (6)0.0282 (2)0.5
O20.7141 (3)−0.01107 (14)0.46919 (17)0.0315 (7)0.5
O40.6061 (3)0.07130 (15)0.52968 (18)0.0366 (8)0.5
C420.879 (3)−0.0231 (12)0.6915 (16)0.033 (4)0.5
H420.851949−0.0523020.7202850.039*0.5
C430.8018 (5)0.0997 (2)0.4607 (3)0.0322 (12)0.5
C440.7422 (6)0.1531 (2)0.4505 (3)0.0401 (12)0.5
H440.6610270.1600960.4666670.048*0.5
C450.8015 (11)0.1968 (4)0.4161 (5)0.050 (2)0.5
H450.7604760.2335140.4089000.061*0.5
C460.9196 (8)0.1865 (4)0.3929 (4)0.0419 (19)0.5
H460.9607920.2166710.3709240.050*0.5
C470.9783 (7)0.1332 (3)0.4012 (3)0.0427 (13)0.5
H471.0588170.1265250.3841150.051*0.5
C480.9206 (8)0.0893 (3)0.4344 (4)0.0397 (18)0.5
H480.9607060.0522070.4393950.048*0.5
C610.8380 (6)0.0314 (3)0.5845 (3)0.0289 (13)0.5
C620.9576 (7)0.0596 (3)0.6001 (4)0.0329 (13)0.5
H620.9860180.0874840.5699610.039*0.5
C631.0331 (12)0.0468 (6)0.6590 (6)0.043 (3)0.5
H631.1165100.0640430.6681680.052*0.5
C640.990 (3)0.0093 (11)0.7053 (11)0.043 (4)0.5
H641.0393180.0056220.7482490.052*0.5
C660.817 (3)−0.0089 (14)0.6352 (15)0.035 (5)0.5
H660.738772−0.0302550.6251130.042*0.5
P30.32535 (11)0.03429 (5)0.41031 (6)0.0303 (2)0.5
O10.3194 (3)0.03453 (17)0.48573 (17)0.0381 (8)0.5
O60.4343 (3)0.00087 (15)0.38402 (16)0.0344 (7)0.5
C310.3333 (3)0.10843 (13)0.38094 (19)0.0331 (10)0.5
C320.2854 (4)0.15319 (17)0.41756 (17)0.0403 (12)0.5
H320.2539760.1452090.4593860.048*0.5
C330.2834 (5)0.20962 (14)0.3930 (2)0.049 (4)0.5
H330.2506170.2402140.4180020.058*0.5
C340.3294 (5)0.22130 (14)0.3318 (3)0.0479 (15)0.5
H340.3279870.2598660.3149760.057*0.5
C350.3773 (5)0.1765 (2)0.2952 (2)0.0455 (19)0.5
H350.4087170.1845150.2533330.055*0.5
C360.3793 (4)0.12010 (17)0.3197 (2)0.0383 (17)0.5
H360.4120770.0895100.2947150.046*0.5
C370.187 (3)0.0052 (15)0.3781 (17)0.036 (4)0.5
C380.0971 (9)−0.0264 (4)0.4134 (4)0.0493 (18)0.5
H380.121877−0.0324500.4600790.059*0.5
C39−0.0217 (10)−0.0492 (3)0.3872 (5)0.0517 (19)0.5
H39−0.073444−0.0693060.4158990.062*0.5
C40−0.0651 (10)−0.0431 (6)0.3202 (6)0.035 (2)0.5
H40−0.142491−0.0619830.3017320.043*0.5
C410.004 (2)−0.0091 (11)0.2794 (12)0.041 (4)0.5
H41−0.0300500.0004670.2346560.049*0.5
C650.129 (3)0.0106 (11)0.3079 (15)0.031 (4)0.5
H650.1807600.0294050.2780280.038*0.5
P50.46798 (11)−0.09748 (5)0.56283 (6)0.0266 (2)0.5
O30.4792 (3)−0.03785 (13)0.59485 (16)0.0309 (7)0.5
O50.4873 (3)−0.10143 (14)0.48930 (16)0.0329 (7)0.5
C490.3095 (3)−0.12660 (16)0.57327 (18)0.0302 (10)0.5
C500.2919 (4)−0.18605 (15)0.5795 (2)0.0363 (11)0.5
H500.363768−0.2116050.5794990.044*0.5
C510.1691 (6)−0.20810 (16)0.5859 (3)0.047 (3)0.5
H510.157019−0.2487320.5901510.056*0.5
C520.0639 (4)−0.1707 (3)0.5859 (4)0.047 (2)0.5
H52−0.020075−0.1857860.5902470.056*0.5
C530.0815 (3)−0.1113 (2)0.5797 (3)0.043 (2)0.5
H530.009577−0.0857130.5796910.052*0.5
C540.2043 (4)−0.08921 (14)0.5733 (2)0.0341 (12)0.5
H540.216326−0.0485850.5690390.041*0.5
C550.5828 (4)−0.14520 (19)0.6097 (2)0.0290 (9)0.5
C560.6535 (6)−0.1851 (3)0.5763 (3)0.0344 (10)0.5
H560.646478−0.1851480.5285190.041*0.5
C570.7337 (11)−0.2247 (5)0.6126 (5)0.0400 (17)0.5
H570.781222−0.2519050.5895560.048*0.5
C580.7453 (6)−0.2249 (2)0.6816 (3)0.0404 (13)0.5
H580.799933−0.2525430.7060610.048*0.5
C590.6776 (6)−0.1851 (3)0.7156 (4)0.0407 (17)0.5
H590.686093−0.1852870.7634130.049*0.5
C600.5967 (7)−0.1444 (3)0.6798 (3)0.0351 (15)0.5
H600.551617−0.1163890.7031220.042*0.5
Cl40.2005 (4)0.24516 (9)0.07969 (18)0.1402 (15)0.595 (3)
Cl50.01892 (14)0.28376 (9)0.16786 (9)0.0713 (6)0.595 (3)
C710.1010 (7)0.3014 (3)0.0968 (4)0.0688 (16)0.595 (3)
H71A0.0366100.3088670.0572320.083*0.595 (3)
H71B0.1532580.3370140.1063190.083*0.595 (3)
O70.0675 (8)0.2407 (3)0.1545 (3)0.0861 (19)0.405 (3)
C67−0.0431 (14)0.2098 (6)0.2436 (6)0.125 (5)0.405 (3)
H67A−0.0708510.2240260.2858470.187*0.405 (3)
H67B0.0189740.1779390.2532400.187*0.405 (3)
H67C−0.1188060.1957820.2141660.187*0.405 (3)
C680.0181 (10)0.2563 (4)0.2106 (5)0.073 (2)0.405 (3)
H68A−0.0466740.2874010.1992890.088*0.405 (3)
H68B0.0887410.2727650.2425830.088*0.405 (3)
C690.1534 (13)0.2818 (6)0.1287 (7)0.101 (3)0.405 (3)
H69A0.2447150.2754920.1478970.122*0.405 (3)
H69B0.1279370.3222320.1375010.122*0.405 (3)
C700.1330 (12)0.2676 (6)0.0540 (4)0.081 (3)0.405 (3)
H70A0.0416570.2739260.0367150.122*0.405 (3)
H70B0.1558370.2269250.0472140.122*0.405 (3)
H70C0.1881660.2927340.0298490.122*0.405 (3)
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
Co10.0164 (2)0.0190 (2)0.0205 (2)−0.00092 (17)−0.00225 (17)−0.00228 (17)
Cl10.0173 (2)0.0249 (2)0.0254 (2)−0.00158 (18)−0.00343 (17)−0.00280 (18)
P10.0215 (2)0.0196 (2)0.0217 (2)0.00004 (19)−0.00208 (19)−0.00153 (19)
P20.0189 (2)0.0220 (2)0.0211 (2)−0.00144 (19)−0.00101 (18)−0.00325 (19)
N10.0235 (9)0.0225 (9)0.0233 (9)−0.0007 (7)−0.0006 (7)0.0002 (7)
C10.0360 (12)0.0215 (10)0.0221 (10)−0.0032 (9)−0.0011 (9)−0.0006 (8)
C20.0354 (12)0.0256 (11)0.0274 (11)−0.0064 (9)0.0003 (9)0.0003 (9)
C30.0402 (14)0.0363 (13)0.0310 (12)−0.0134 (11)−0.0033 (10)−0.0020 (10)
C40.0588 (17)0.0314 (13)0.0318 (13)−0.0146 (12)−0.0059 (11)−0.0052 (10)
C50.0598 (18)0.0254 (12)0.0401 (14)−0.0009 (12)−0.0025 (12)−0.0078 (10)
C60.0408 (14)0.0246 (11)0.0341 (12)0.0016 (10)−0.0040 (10)−0.0032 (9)
C70.0249 (11)0.0181 (10)0.0327 (11)0.0034 (8)−0.0031 (8)0.0012 (8)
C80.0327 (12)0.0255 (11)0.0337 (12)0.0006 (9)−0.0049 (9)−0.0023 (9)
C90.0349 (13)0.0320 (12)0.0431 (14)0.0037 (10)−0.0135 (11)−0.0015 (10)
C100.0252 (12)0.0303 (13)0.0634 (17)0.0057 (10)−0.0049 (11)0.0015 (12)
C110.0332 (13)0.0297 (12)0.0543 (16)0.0067 (10)0.0096 (11)0.0031 (11)
C120.0341 (12)0.0268 (11)0.0343 (12)0.0069 (9)0.0026 (10)0.0035 (9)
C130.0230 (10)0.0251 (10)0.0229 (10)0.0007 (8)−0.0001 (8)−0.0002 (8)
C140.0241 (11)0.0273 (11)0.0232 (10)−0.0001 (8)0.0000 (8)−0.0002 (8)
C150.0211 (10)0.0353 (12)0.0293 (11)0.0013 (9)−0.0015 (8)0.0007 (9)
C160.0256 (12)0.0419 (14)0.0354 (13)0.0091 (10)0.0014 (9)0.0002 (10)
C170.0345 (13)0.0329 (12)0.0383 (13)0.0095 (10)0.0008 (10)−0.0068 (10)
C180.0296 (12)0.0285 (11)0.0312 (12)−0.0005 (9)0.0001 (9)−0.0047 (9)
C190.0218 (10)0.0313 (11)0.0265 (11)−0.0028 (9)0.0028 (8)−0.0094 (9)
C200.0413 (14)0.0345 (13)0.0293 (12)−0.0102 (11)0.0045 (10)−0.0091 (10)
C210.0493 (16)0.0413 (15)0.0439 (15)−0.0196 (13)0.0093 (12)−0.0188 (12)
C220.0356 (14)0.0545 (17)0.0503 (16)−0.0089 (12)−0.0070 (12)−0.0288 (14)
C230.0349 (14)0.0486 (16)0.0439 (15)0.0063 (12)−0.0149 (11)−0.0192 (12)
C240.0302 (12)0.0339 (12)0.0348 (12)0.0043 (10)−0.0073 (9)−0.0102 (10)
C250.030 (2)0.0258 (16)0.0225 (18)−0.0020 (16)−0.0022 (15)0.0028 (13)
C260.033 (2)0.033 (2)0.029 (2)−0.0019 (17)0.0020 (17)0.0033 (16)
C270.037 (3)0.045 (2)0.027 (2)−0.0009 (19)0.0049 (19)0.0095 (17)
C280.054 (3)0.041 (2)0.030 (2)−0.0106 (18)0.0035 (18)0.0116 (16)
C290.056 (3)0.0320 (19)0.030 (2)−0.001 (2)0.003 (2)0.0074 (17)
C300.045 (2)0.0263 (19)0.027 (2)−0.0036 (16)0.0000 (16)0.0030 (15)
C25A0.029 (4)0.031 (3)0.025 (4)−0.003 (3)−0.002 (3)0.006 (3)
C26A0.044 (4)0.032 (4)0.029 (4)−0.001 (3)0.003 (3)0.003 (3)
C27A0.050 (5)0.032 (4)0.032 (4)−0.007 (4)0.000 (4)0.008 (3)
C28A0.049 (4)0.041 (4)0.032 (4)−0.009 (3)0.002 (3)0.010 (3)
C29A0.040 (5)0.042 (4)0.026 (4)−0.003 (4)0.000 (4)0.005 (3)
C30A0.033 (4)0.034 (4)0.025 (4)−0.001 (3)0.001 (3)0.004 (3)
Co20.0222 (6)0.0238 (9)0.0288 (9)0.0017 (6)−0.0004 (5)−0.0018 (6)
Co30.0222 (6)0.0238 (9)0.0288 (9)0.0017 (6)−0.0004 (5)−0.0018 (6)
Cl20.0334 (6)0.0350 (14)0.0327 (12)0.0061 (9)0.0014 (7)−0.0048 (8)
Cl30.0334 (6)0.0350 (14)0.0327 (12)0.0061 (9)0.0014 (7)−0.0048 (8)
P40.0247 (5)0.0247 (5)0.0343 (6)0.0002 (4)−0.0003 (4)−0.0019 (4)
O20.0297 (17)0.0246 (16)0.0387 (19)−0.0031 (13)−0.0015 (14)−0.0026 (14)
O40.0271 (17)0.0383 (19)0.045 (2)0.0057 (15)0.0063 (14)0.0046 (15)
C420.027 (4)0.028 (9)0.042 (6)0.005 (6)−0.003 (3)0.003 (6)
C430.033 (3)0.023 (2)0.039 (3)−0.0005 (19)−0.001 (2)−0.006 (2)
C440.045 (3)0.027 (3)0.048 (3)0.009 (3)0.006 (2)0.000 (3)
C450.081 (8)0.024 (3)0.044 (4)0.002 (4)0.001 (4)−0.001 (3)
C460.058 (4)0.029 (3)0.037 (4)−0.012 (3)0.002 (3)0.003 (3)
C470.043 (4)0.035 (3)0.050 (3)−0.007 (3)0.007 (3)0.000 (3)
C480.042 (4)0.033 (4)0.044 (4)0.002 (3)0.004 (3)−0.004 (3)
C610.018 (3)0.032 (3)0.035 (3)0.001 (3)0.002 (3)−0.007 (2)
C620.024 (3)0.034 (3)0.040 (4)−0.001 (3)−0.001 (3)0.000 (2)
C630.021 (5)0.053 (5)0.051 (9)−0.010 (4)−0.008 (4)−0.013 (6)
C640.037 (6)0.055 (6)0.034 (10)0.014 (5)−0.010 (5)−0.002 (5)
C660.052 (7)0.028 (5)0.022 (12)−0.001 (5)−0.004 (6)0.003 (6)
P30.0244 (6)0.0325 (6)0.0324 (6)0.0052 (5)−0.0033 (4)−0.0029 (5)
O10.0279 (17)0.051 (2)0.0337 (19)0.0033 (16)−0.0056 (14)−0.0054 (16)
O60.0308 (18)0.0386 (19)0.0330 (17)0.0078 (14)0.0003 (14)−0.0001 (14)
C310.020 (2)0.033 (2)0.044 (3)0.0022 (19)−0.0052 (19)−0.010 (2)
C320.028 (3)0.037 (3)0.055 (3)−0.001 (2)−0.002 (2)−0.017 (2)
C330.034 (5)0.037 (6)0.075 (7)−0.001 (4)0.006 (5)−0.021 (5)
C340.034 (3)0.028 (3)0.081 (5)−0.007 (3)0.004 (3)−0.004 (3)
C350.049 (5)0.034 (4)0.055 (5)−0.006 (4)0.010 (4)−0.008 (4)
C360.031 (3)0.035 (4)0.048 (3)−0.002 (3)−0.001 (2)−0.011 (3)
C370.059 (6)0.031 (5)0.015 (9)0.016 (4)−0.011 (5)0.004 (5)
C380.051 (5)0.054 (5)0.038 (3)−0.022 (5)−0.013 (4)0.020 (3)
C390.056 (6)0.051 (4)0.044 (5)−0.021 (4)−0.012 (5)0.014 (4)
C400.028 (6)0.038 (4)0.039 (6)−0.010 (4)−0.003 (4)−0.011 (4)
C410.032 (5)0.056 (5)0.033 (9)−0.012 (4)−0.007 (5)0.001 (5)
C650.036 (6)0.029 (10)0.031 (5)0.004 (5)0.008 (4)−0.001 (6)
P50.0263 (5)0.0251 (5)0.0282 (6)−0.0016 (4)0.0016 (4)−0.0017 (4)
O30.0331 (17)0.0260 (16)0.0325 (17)−0.0002 (13)−0.0006 (13)−0.0024 (13)
O50.0366 (18)0.0296 (17)0.0326 (17)−0.0058 (14)0.0049 (14)−0.0022 (13)
C490.032 (2)0.033 (3)0.025 (2)−0.006 (2)−0.0002 (18)−0.004 (2)
C500.037 (3)0.031 (3)0.040 (3)−0.009 (3)0.004 (2)−0.001 (2)
C510.037 (4)0.042 (5)0.062 (5)−0.011 (3)0.009 (3)−0.005 (4)
C520.031 (3)0.061 (7)0.048 (5)−0.012 (4)0.003 (3)0.002 (4)
C530.027 (3)0.058 (7)0.045 (4)0.009 (4)0.000 (3)−0.007 (4)
C540.031 (3)0.037 (3)0.033 (3)−0.002 (2)−0.001 (2)−0.002 (2)
C550.025 (2)0.023 (2)0.038 (2)−0.0041 (18)0.0008 (18)−0.0035 (18)
C560.033 (3)0.032 (3)0.038 (3)−0.001 (3)0.003 (2)−0.009 (2)
C570.034 (3)0.030 (4)0.054 (4)0.002 (3)−0.004 (3)−0.010 (3)
C580.042 (3)0.024 (2)0.052 (3)0.003 (2)−0.012 (3)−0.008 (2)
C590.049 (4)0.030 (3)0.040 (3)0.005 (3)−0.010 (3)−0.003 (2)
C600.039 (4)0.031 (4)0.034 (3)0.004 (3)0.000 (2)−0.008 (3)
Cl40.213 (3)0.0556 (11)0.183 (3)0.0045 (15)0.152 (3)−0.0170 (14)
Cl50.0467 (8)0.0986 (14)0.0709 (10)−0.0055 (8)0.0158 (7)−0.0365 (9)
C710.063 (4)0.063 (4)0.080 (4)−0.007 (3)0.008 (3)0.000 (3)
O70.106 (4)0.056 (3)0.104 (4)−0.021 (3)0.040 (4)−0.002 (3)
C670.141 (11)0.137 (11)0.109 (9)0.055 (9)0.068 (8)0.020 (8)
C680.084 (6)0.043 (4)0.095 (6)0.016 (4)0.019 (5)−0.013 (4)
C690.102 (6)0.085 (5)0.122 (6)−0.019 (5)0.033 (5)0.002 (5)
C700.082 (6)0.123 (8)0.042 (4)−0.079 (6)0.017 (4)−0.022 (5)
Geometric parameters (Å, º) top
Co1—Cl1i2.2179 (11)Co3—O61.966 (4)
Co1—Cl12.2179 (11)Co3—O51.958 (4)
Co1—P1i2.2701 (5)P4—O21.512 (3)
Co1—P12.2701 (5)P4—O41.516 (3)
Co1—P2i2.2770 (6)P4—C431.805 (6)
Co1—P22.2771 (6)P4—C611.807 (6)
P1—P22.6243 (8)C42—H420.9500
P1—N11.7038 (19)C42—C641.37 (5)
P1—C11.824 (2)C42—C661.27 (4)
P1—C71.820 (2)C43—C441.382 (7)
P2—N11.7080 (18)C43—C481.415 (10)
P2—C131.817 (2)C44—H440.9500
P2—C191.815 (2)C44—C451.402 (13)
N1—C251.536 (4)C45—H450.9500
N1—C25A1.478 (9)C45—C461.379 (13)
C1—C21.398 (3)C46—H460.9500
C1—C61.394 (3)C46—C471.372 (10)
C2—H20.9500C47—H470.9500
C2—C31.392 (3)C47—C481.385 (9)
C3—H30.9500C48—H480.9500
C3—C41.382 (4)C61—C621.402 (8)
C4—H40.9500C61—C661.41 (3)
C4—C51.378 (4)C62—H620.9500
C5—H50.9500C62—C631.370 (10)
C5—C61.393 (3)C63—H630.9500
C6—H60.9500C63—C641.38 (3)
C7—C81.393 (3)C64—H640.9500
C7—C121.397 (3)C66—H660.9500
C8—H80.9500P3—O11.517 (4)
C8—C91.390 (3)P3—O61.511 (3)
C9—H90.9500P3—C311.812 (3)
C9—C101.386 (4)P3—C371.65 (3)
C10—H100.9500C31—C321.3900
C10—C111.381 (4)C31—C361.3900
C11—H110.9500C32—H320.9500
C11—C121.384 (3)C32—C331.3900
C12—H120.9500C33—H330.9500
C13—C141.398 (3)C33—C341.3900
C13—C181.399 (3)C34—H340.9500
C14—H140.9500C34—C351.3900
C14—C151.385 (3)C35—H350.9500
C15—H150.9500C35—C361.3900
C15—C161.391 (3)C36—H360.9500
C16—H160.9500C37—C381.43 (3)
C16—C171.382 (4)C37—C651.47 (4)
C17—H170.9500C38—H380.9500
C17—C181.388 (3)C38—C391.385 (10)
C18—H180.9500C39—H390.9500
C19—C201.396 (3)C39—C401.370 (10)
C19—C241.393 (3)C40—H400.9500
C20—H200.9500C40—C411.39 (3)
C20—C211.389 (3)C41—H410.9500
C21—H210.9500C41—C651.43 (5)
C21—C221.380 (4)C65—H650.9500
C22—H220.9500P5—O31.515 (3)
C22—C231.378 (4)P5—O51.510 (3)
C23—H230.9500P5—C491.809 (3)
C23—C241.391 (3)P5—C551.801 (5)
C24—H240.9500C49—C501.3900
C25—H251.0000C49—C541.3900
C25—C261.521 (7)C50—H500.9500
C25—C301.518 (6)C50—C511.3900
C26—H26A0.9900C51—H510.9500
C26—H26B0.9900C51—C521.3900
C26—C271.540 (7)C52—H520.9500
C27—H27A0.9900C52—C531.3900
C27—H27B0.9900C53—H530.9500
C27—C281.516 (8)C53—C541.3900
C28—H28A0.9900C54—H540.9500
C28—H28B0.9900C55—C561.393 (7)
C28—C291.530 (8)C55—C601.393 (8)
C29—H29A0.9900C56—H560.9500
C29—H29B0.9900C56—C571.382 (12)
C29—C301.533 (7)C57—H570.9500
C30—H30A0.9900C57—C581.371 (11)
C30—H30B0.9900C58—H580.9500
C25A—H25A1.0000C58—C591.381 (9)
C25A—C26A1.520 (14)C59—H590.9500
C25A—C30A1.511 (15)C59—C601.399 (9)
C26A—H26C0.9900C60—H600.9500
C26A—H26D0.9900Cl4—C711.715 (7)
C26A—C27A1.566 (16)Cl5—C711.785 (7)
C27A—H27C0.9900C71—H71A0.9900
C27A—H27D0.9900C71—H71B0.9900
C27A—C28A1.509 (16)O7—C681.335 (9)
C28A—H28C0.9900O7—C691.436 (9)
C28A—H28D0.9900C67—H67A0.9800
C28A—C29A1.533 (15)C67—H67B0.9800
C29A—H29C0.9900C67—H67C0.9800
C29A—H29D0.9900C67—C681.445 (14)
C29A—C30A1.520 (17)C68—H68A0.9900
C30A—H30C0.9900C68—H68B0.9900
C30A—H30D0.9900C69—H69A0.9900
Co2—Cl22.252 (2)C69—H69B0.9900
Co2—O41.958 (5)C69—C701.520 (15)
Co2—O11.960 (4)C70—H70A0.9800
Co2—O31.958 (4)C70—H70B0.9800
Co3—Cl32.269 (2)C70—H70C0.9800
Co3—O21.962 (4)
Cl1i—Co1—Cl1180.00 (3)C25A—C30A—H30D109.8
Cl1—Co1—P189.065 (18)C29A—C30A—H30C109.8
Cl1i—Co1—P190.935 (18)C29A—C30A—H30D109.8
Cl1—Co1—P1i90.935 (18)H30C—C30A—H30D108.3
Cl1i—Co1—P1i89.065 (18)O4—Co2—Cl2114.3 (2)
Cl1—Co1—P2i90.48 (3)O4—Co2—O1105.4 (2)
Cl1i—Co1—P2i89.52 (3)O1—Co2—Cl2111.26 (19)
Cl1i—Co1—P290.48 (3)O3—Co2—Cl2112.7 (2)
Cl1—Co1—P289.52 (3)O3—Co2—O4108.94 (18)
P1i—Co1—P1180.0O3—Co2—O1103.41 (19)
P1i—Co1—P2109.501 (19)O2—Co3—Cl3110.34 (19)
P1i—Co1—P2i70.500 (19)O2—Co3—O6109.12 (19)
P1—Co1—P270.497 (19)O6—Co3—Cl3111.5 (2)
P1—Co1—P2i109.502 (19)O5—Co3—Cl3108.75 (19)
P2i—Co1—P2180.0O5—Co3—O2109.5 (2)
Co1—P1—P254.876 (16)O5—Co3—O6107.60 (19)
N1—P1—Co194.29 (6)O2—P4—O4116.6 (2)
N1—P1—P239.78 (6)O2—P4—C43110.0 (2)
N1—P1—C1108.69 (10)O2—P4—C61108.1 (2)
N1—P1—C7110.14 (10)O4—P4—C43106.4 (2)
C1—P1—Co1122.28 (7)O4—P4—C61107.6 (2)
C1—P1—P2131.60 (8)C43—P4—C61108.0 (3)
C7—P1—Co1114.42 (7)P4—O2—Co3134.9 (2)
C7—P1—P2118.44 (7)P4—O4—Co2136.1 (2)
C7—P1—C1106.08 (10)C64—C42—H42124.3
Co1—P2—P154.627 (17)C66—C42—H42124.3
N1—P2—Co193.92 (6)C66—C42—C64111 (3)
N1—P2—P139.66 (6)C44—C43—P4119.7 (5)
N1—P2—C13109.41 (10)C44—C43—C48119.3 (6)
N1—P2—C19110.79 (10)C48—C43—P4121.0 (4)
C13—P2—Co1121.43 (7)C43—C44—H44120.0
C13—P2—P1131.59 (7)C43—C44—C45120.0 (6)
C19—P2—Co1115.59 (8)C45—C44—H44120.0
C19—P2—P1119.77 (8)C44—C45—H45120.1
C19—P2—C13105.07 (10)C46—C45—C44119.8 (7)
P1—N1—P2100.56 (10)C46—C45—H45120.1
C25—N1—P1127.40 (19)C45—C46—H46119.6
C25—N1—P2130.79 (19)C47—C46—C45120.8 (8)
C25A—N1—P1128.9 (4)C47—C46—H46119.6
C25A—N1—P2128.4 (4)C46—C47—H47119.9
C2—C1—P1119.55 (17)C46—C47—C48120.2 (6)
C6—C1—P1121.86 (19)C48—C47—H47119.9
C6—C1—C2118.4 (2)C43—C48—H48120.1
C1—C2—H2119.7C47—C48—C43119.8 (6)
C3—C2—C1120.6 (2)C47—C48—H48120.1
C3—C2—H2119.7C62—C61—P4123.8 (5)
C2—C3—H3120.0C62—C61—C66110.6 (12)
C4—C3—C2120.0 (2)C66—C61—P4125.6 (12)
C4—C3—H3120.0C61—C62—H62120.2
C3—C4—H4119.8C63—C62—C61119.5 (8)
C5—C4—C3120.3 (2)C63—C62—H62120.2
C5—C4—H4119.8C62—C63—H63119.4
C4—C5—H5120.0C62—C63—C64121.2 (14)
C4—C5—C6119.9 (3)C64—C63—H63119.4
C6—C5—H5120.0C42—C64—C63122 (2)
C1—C6—H6119.6C42—C64—H64118.9
C5—C6—C1120.8 (2)C63—C64—H64118.9
C5—C6—H6119.6C42—C66—C61134 (3)
C8—C7—P1122.99 (18)C42—C66—H66112.8
C8—C7—C12118.8 (2)C61—C66—H66112.8
C12—C7—P1117.78 (17)O1—P3—C31109.1 (2)
C7—C8—H8119.9O1—P3—C37104.9 (12)
C9—C8—C7120.1 (2)O6—P3—O1117.8 (2)
C9—C8—H8119.9O6—P3—C31107.70 (19)
C8—C9—H9119.8O6—P3—C37108.0 (13)
C10—C9—C8120.4 (2)C37—P3—C31109.2 (12)
C10—C9—H9119.8P3—O1—Co2134.2 (2)
C9—C10—H10120.1P3—O6—Co3134.8 (2)
C11—C10—C9119.7 (2)C32—C31—P3119.8 (2)
C11—C10—H10120.1C32—C31—C36120.0
C10—C11—H11119.9C36—C31—P3120.1 (2)
C10—C11—C12120.2 (2)C31—C32—H32120.0
C12—C11—H11119.9C33—C32—C31120.0
C7—C12—H12119.7C33—C32—H32120.0
C11—C12—C7120.7 (2)C32—C33—H33120.0
C11—C12—H12119.7C34—C33—C32120.0
C14—C13—P2120.72 (17)C34—C33—H33120.0
C14—C13—C18118.6 (2)C33—C34—H34120.0
C18—C13—P2120.61 (17)C33—C34—C35120.0
C13—C14—H14119.7C35—C34—H34120.0
C15—C14—C13120.5 (2)C34—C35—H35120.0
C15—C14—H14119.7C36—C35—C34120.0
C14—C15—H15119.8C36—C35—H35120.0
C14—C15—C16120.4 (2)C31—C36—H36120.0
C16—C15—H15119.8C35—C36—C31120.0
C15—C16—H16120.2C35—C36—H36120.0
C17—C16—C15119.6 (2)C38—C37—P3127 (2)
C17—C16—H16120.2C38—C37—C65108 (2)
C16—C17—H17119.8C65—C37—P3125 (2)
C16—C17—C18120.3 (2)C37—C38—H38116.3
C18—C17—H17119.8C39—C38—C37127.4 (14)
C13—C18—H18119.7C39—C38—H38116.3
C17—C18—C13120.5 (2)C38—C39—H39119.8
C17—C18—H18119.7C40—C39—C38120.5 (8)
C20—C19—P2117.33 (18)C40—C39—H39119.8
C24—C19—P2123.50 (18)C39—C40—H40120.0
C24—C19—C20119.0 (2)C39—C40—C41120.0 (13)
C19—C20—H20119.8C41—C40—H40120.0
C21—C20—C19120.4 (2)C40—C41—H41121.6
C21—C20—H20119.8C40—C41—C65117 (2)
C20—C21—H21120.0C65—C41—H41121.6
C22—C21—C20120.0 (3)C37—C65—H65116.4
C22—C21—H21120.0C41—C65—C37127 (2)
C21—C22—H22120.0C41—C65—H65116.4
C23—C22—C21120.0 (2)O3—P5—C49108.33 (19)
C23—C22—H22120.0O3—P5—C55108.69 (19)
C22—C23—H23119.7O5—P5—O3117.00 (19)
C22—C23—C24120.5 (3)O5—P5—C49108.31 (18)
C24—C23—H23119.7O5—P5—C55108.4 (2)
C19—C24—H24120.0C55—P5—C49105.51 (19)
C23—C24—C19120.0 (2)P5—O3—Co2136.4 (2)
C23—C24—H24120.0P5—O5—Co3137.3 (2)
N1—C25—H25107.2C50—C49—P5120.4 (2)
C26—C25—N1111.6 (3)C50—C49—C54120.0
C26—C25—H25107.2C54—C49—P5119.5 (2)
C30—C25—N1112.3 (3)C49—C50—H50120.0
C30—C25—H25107.2C49—C50—C51120.0
C30—C25—C26110.9 (4)C51—C50—H50120.0
C25—C26—H26A109.4C50—C51—H51120.0
C25—C26—H26B109.4C52—C51—C50120.0
C25—C26—C27111.1 (4)C52—C51—H51120.0
H26A—C26—H26B108.0C51—C52—H52120.0
C27—C26—H26A109.4C53—C52—C51120.0
C27—C26—H26B109.4C53—C52—H52120.0
C26—C27—H27A109.4C52—C53—H53120.0
C26—C27—H27B109.4C52—C53—C54120.0
H27A—C27—H27B108.0C54—C53—H53120.0
C28—C27—C26111.1 (5)C49—C54—H54120.0
C28—C27—H27A109.4C53—C54—C49120.0
C28—C27—H27B109.4C53—C54—H54120.0
C27—C28—H28A109.6C56—C55—P5120.4 (4)
C27—C28—H28B109.6C60—C55—P5120.0 (4)
C27—C28—C29110.4 (5)C60—C55—C56119.5 (5)
H28A—C28—H28B108.1C55—C56—H56119.9
C29—C28—H28A109.6C57—C56—C55120.1 (6)
C29—C28—H28B109.6C57—C56—H56119.9
C28—C29—H29A109.7C56—C57—H57119.7
C28—C29—H29B109.7C58—C57—C56120.6 (9)
C28—C29—C30109.9 (5)C58—C57—H57119.7
H29A—C29—H29B108.2C57—C58—H58119.9
C30—C29—H29A109.7C57—C58—C59120.2 (8)
C30—C29—H29B109.7C59—C58—H58119.9
C25—C30—C29109.9 (4)C58—C59—H59119.9
C25—C30—H30A109.7C58—C59—C60120.1 (7)
C25—C30—H30B109.7C60—C59—H59119.9
C29—C30—H30A109.7C55—C60—C59119.5 (6)
C29—C30—H30B109.7C55—C60—H60120.3
H30A—C30—H30B108.2C59—C60—H60120.3
N1—C25A—H25A106.8Cl4—C71—Cl5109.9 (4)
N1—C25A—C26A110.0 (8)Cl4—C71—H71A109.7
N1—C25A—C30A115.0 (8)Cl4—C71—H71B109.7
C26A—C25A—H25A106.8Cl5—C71—H71A109.7
C30A—C25A—H25A106.8Cl5—C71—H71B109.7
C30A—C25A—C26A110.8 (10)H71A—C71—H71B108.2
C25A—C26A—H26C110.1C68—O7—C69116.0 (8)
C25A—C26A—H26D110.1H67A—C67—H67B109.5
C25A—C26A—C27A108.0 (10)H67A—C67—H67C109.5
H26C—C26A—H26D108.4H67B—C67—H67C109.5
C27A—C26A—H26C110.1C68—C67—H67A109.5
C27A—C26A—H26D110.1C68—C67—H67B109.5
C26A—C27A—H27C109.9C68—C67—H67C109.5
C26A—C27A—H27D109.9O7—C68—C67114.5 (8)
H27C—C27A—H27D108.3O7—C68—H68A108.6
C28A—C27A—C26A108.9 (11)O7—C68—H68B108.6
C28A—C27A—H27C109.9C67—C68—H68A108.6
C28A—C27A—H27D109.9C67—C68—H68B108.6
C27A—C28A—H28C109.7H68A—C68—H68B107.6
C27A—C28A—H28D109.7O7—C69—H69A111.6
C27A—C28A—C29A109.8 (11)O7—C69—H69B111.6
H28C—C28A—H28D108.2O7—C69—C70100.9 (9)
C29A—C28A—H28C109.7H69A—C69—H69B109.4
C29A—C28A—H28D109.7C70—C69—H69A111.6
C28A—C29A—H29C109.1C70—C69—H69B111.6
C28A—C29A—H29D109.1C69—C70—H70A109.5
H29C—C29A—H29D107.9C69—C70—H70B109.5
C30A—C29A—C28A112.4 (12)C69—C70—H70C109.5
C30A—C29A—H29C109.1H70A—C70—H70B109.5
C30A—C29A—H29D109.1H70A—C70—H70C109.5
C25A—C30A—C29A109.2 (11)H70B—C70—H70C109.5
C25A—C30A—H30C109.8
Co1—P1—N1—P2−7.34 (8)C27A—C28A—C29A—C30A−56.8 (18)
Co1—P1—N1—C25−175.6 (3)C28A—C29A—C30A—C25A55.7 (18)
Co1—P1—N1—C25A156.7 (6)C30A—C25A—C26A—C27A61.9 (15)
Co1—P1—C1—C2−59.3 (2)P4—C43—C44—C45176.7 (6)
Co1—P1—C1—C6116.26 (18)P4—C43—C48—C47−176.0 (5)
Co1—P1—C7—C8104.65 (19)P4—C61—C62—C63179.6 (8)
Co1—P1—C7—C12−68.12 (19)P4—C61—C66—C42−178 (3)
Co1—P2—N1—P17.32 (8)O2—P4—O4—Co241.2 (4)
Co1—P2—N1—C25175.0 (3)O2—P4—C43—C44127.3 (5)
Co1—P2—N1—C25A−156.9 (6)O2—P4—C43—C48−54.0 (7)
Co1—P2—C13—C1465.15 (19)O2—P4—C61—C62118.3 (5)
Co1—P2—C13—C18−111.36 (17)O2—P4—C61—C66−60.6 (19)
Co1—P2—C19—C2057.5 (2)O4—P4—O2—Co312.1 (4)
Co1—P2—C19—C24−118.31 (19)O4—P4—C43—C440.2 (5)
P1—P2—N1—C25167.7 (3)O4—P4—C43—C48178.9 (6)
P1—P2—N1—C25A−164.2 (6)O4—P4—C61—C62−115.0 (5)
P1—P2—C13—C14−3.5 (2)O4—P4—C61—C6666.1 (19)
P1—P2—C13—C18−179.98 (14)C43—P4—O2—Co3−109.1 (4)
P1—P2—C19—C20119.73 (17)C43—P4—O4—Co2164.3 (3)
P1—P2—C19—C24−56.1 (2)C43—P4—C61—C62−0.6 (6)
P1—N1—C25—C26−153.6 (3)C43—P4—C61—C66−179.5 (19)
P1—N1—C25—C30−28.3 (5)C43—C44—C45—C46−0.2 (11)
P1—N1—C25A—C26A44.1 (12)C44—C43—C48—C472.7 (12)
P1—N1—C25A—C30A170.1 (7)C44—C45—C46—C472.0 (12)
P1—C1—C2—C3175.25 (18)C45—C46—C47—C48−1.3 (12)
P1—C1—C6—C5−174.3 (2)C46—C47—C48—C43−1.0 (13)
P1—C7—C8—C9−174.76 (18)C48—C43—C44—C45−2.0 (10)
P1—C7—C12—C11175.24 (19)C61—P4—O2—Co3133.3 (4)
P2—P1—N1—C25−168.3 (3)C61—P4—O4—Co2−80.2 (4)
P2—P1—N1—C25A164.1 (6)C61—P4—C43—C44−115.0 (5)
P2—P1—C1—C210.2 (2)C61—P4—C43—C4863.7 (7)
P2—P1—C1—C6−174.18 (15)C61—C62—C63—C64−4.0 (19)
P2—P1—C7—C842.9 (2)C62—C61—C66—C423 (5)
P2—P1—C7—C12−129.91 (16)C62—C63—C64—C429 (3)
P2—N1—C25—C2641.7 (5)C64—C42—C66—C611 (5)
P2—N1—C25—C30167.0 (3)C66—C42—C64—C63−7 (4)
P2—N1—C25A—C26A−156.0 (6)C66—C61—C62—C63−1.4 (19)
P2—N1—C25A—C30A−30.0 (13)P3—C31—C32—C33−175.7 (3)
P2—C13—C14—C15−177.13 (17)P3—C31—C36—C35175.7 (3)
P2—C13—C18—C17175.80 (19)P3—C37—C38—C39177.5 (17)
P2—C19—C20—C21−176.0 (2)P3—C37—C65—C41−174 (2)
P2—C19—C24—C23175.2 (2)O1—P3—O6—Co310.3 (4)
N1—P1—C1—C248.6 (2)O1—P3—C31—C32−24.3 (3)
N1—P1—C1—C6−135.85 (19)O1—P3—C31—C36160.0 (2)
N1—P1—C7—C8−0.1 (2)O1—P3—C37—C38−15 (3)
N1—P1—C7—C12−172.83 (17)O1—P3—C37—C65161 (3)
N1—P2—C13—C14−42.3 (2)O6—P3—O1—Co242.2 (4)
N1—P2—C13—C18141.15 (18)O6—P3—C31—C32−153.2 (3)
N1—P2—C19—C20162.71 (18)O6—P3—C31—C3631.1 (3)
N1—P2—C19—C24−13.1 (2)O6—P3—C37—C38112 (3)
N1—C25—C26—C27−178.2 (4)O6—P3—C37—C65−73 (3)
N1—C25—C30—C29176.0 (3)C31—P3—O1—Co2−80.9 (3)
N1—C25A—C26A—C27A−169.7 (8)C31—P3—O6—Co3134.1 (3)
N1—C25A—C30A—C29A175.7 (9)C31—P3—C37—C38−131 (3)
C1—P1—N1—P2−133.55 (10)C31—P3—C37—C6544 (3)
C1—P1—N1—C2558.2 (3)C31—C32—C33—C340.0
C1—P1—N1—C25A30.5 (6)C32—C31—C36—C350.0
C1—P1—C7—C8−117.51 (19)C32—C33—C34—C350.0
C1—P1—C7—C1269.7 (2)C33—C34—C35—C360.0
C1—C2—C3—C4−0.4 (4)C34—C35—C36—C310.0
C2—C1—C6—C51.3 (4)C36—C31—C32—C330.0
C2—C3—C4—C50.6 (4)C37—P3—O1—Co2162.2 (13)
C3—C4—C5—C60.3 (4)C37—P3—O6—Co3−108.2 (12)
C4—C5—C6—C1−1.2 (4)C37—P3—C31—C3289.8 (14)
C6—C1—C2—C3−0.5 (3)C37—P3—C31—C36−86.0 (13)
C7—P1—N1—P2110.63 (10)C37—C38—C39—C400 (2)
C7—P1—N1—C25−57.7 (3)C38—C37—C65—C413 (4)
C7—P1—N1—C25A−85.3 (6)C38—C39—C40—C41−6 (2)
C7—P1—C1—C2166.97 (18)C39—C40—C41—C659 (3)
C7—P1—C1—C6−17.4 (2)C40—C41—C65—C37−8 (4)
C7—C8—C9—C100.5 (4)C65—C37—C38—C391 (3)
C8—C7—C12—C112.2 (3)P5—C49—C50—C51−178.4 (3)
C8—C9—C10—C111.1 (4)P5—C49—C54—C53178.4 (3)
C9—C10—C11—C12−1.0 (4)P5—C55—C56—C57−174.9 (6)
C10—C11—C12—C7−0.6 (4)P5—C55—C60—C59174.4 (5)
C12—C7—C8—C9−2.1 (3)O3—P5—O5—Co319.5 (4)
C13—P2—N1—P1132.65 (9)O3—P5—C49—C50−149.0 (3)
C13—P2—N1—C25−59.6 (3)O3—P5—C49—C5432.6 (3)
C13—P2—N1—C25A−31.5 (6)O3—P5—C55—C56−139.4 (4)
C13—P2—C19—C20−79.2 (2)O3—P5—C55—C6043.8 (5)
C13—P2—C19—C24105.0 (2)O5—P5—O3—Co228.7 (4)
C13—C14—C15—C161.5 (3)O5—P5—C49—C5083.2 (3)
C14—C13—C18—C17−0.8 (3)O5—P5—C49—C54−95.2 (3)
C14—C15—C16—C17−1.1 (4)O5—P5—C55—C56−11.2 (5)
C15—C16—C17—C18−0.2 (4)O5—P5—C55—C60171.9 (4)
C16—C17—C18—C131.2 (4)C49—P5—O3—Co2−94.0 (3)
C18—C13—C14—C15−0.6 (3)C49—P5—O5—Co3142.2 (3)
C19—P2—N1—P1−111.97 (11)C49—P5—C55—C56104.6 (4)
C19—P2—N1—C2555.7 (3)C49—P5—C55—C60−72.2 (5)
C19—P2—N1—C25A83.8 (6)C49—C50—C51—C520.0
C19—P2—C13—C14−161.32 (18)C50—C49—C54—C530.0
C19—P2—C13—C1822.2 (2)C50—C51—C52—C530.0
C19—C20—C21—C221.1 (4)C51—C52—C53—C540.0
C20—C19—C24—C23−0.5 (4)C52—C53—C54—C490.0
C20—C21—C22—C23−1.6 (4)C54—C49—C50—C510.0
C21—C22—C23—C241.1 (4)C55—P5—O3—Co2151.9 (3)
C22—C23—C24—C190.0 (4)C55—P5—O5—Co3−103.8 (3)
C24—C19—C20—C210.0 (4)C55—P5—C49—C50−32.7 (3)
C25—C26—C27—C28−54.8 (7)C55—P5—C49—C54148.8 (3)
C26—C25—C30—C29−58.3 (7)C55—C56—C57—C58−0.4 (12)
C26—C27—C28—C2956.3 (7)C56—C55—C60—C59−2.4 (9)
C27—C28—C29—C30−58.8 (7)C56—C57—C58—C59−0.7 (13)
C28—C29—C30—C2559.6 (7)C57—C58—C59—C600.2 (11)
C30—C25—C26—C2755.7 (7)C58—C59—C60—C551.4 (10)
C25A—C26A—C27A—C28A−61.6 (16)C60—C55—C56—C571.9 (9)
C26A—C25A—C30A—C29A−58.8 (16)C68—O7—C69—C70−151.7 (11)
C26A—C27A—C28A—C29A58.6 (16)C69—O7—C68—C67−166.6 (12)
Symmetry code: (i) −x+1, −y, −z.
Hydrogen-bond geometry (Å, º) top
Cg1, Cg2 and Cg3 are the centroids of the C37–C41/C65, C42/C61–C64/C66 and C19–C24 rings, respectively.
D—H···AD—HH···AD···AD—H···A
C2—H2···Cl1i0.952.663.174 (2)114
C6—H6···Cl4i0.952.953.668 (4)133
C17—H17···O70.952.483.314 (8)146
C24—H24···Cl2ii0.952.963.682 (5)133
C27—H27B···Cg10.992.973.834 (11)147
C53—H53···Cg2iii0.952.983.787 (8)143
C60—H60···Cg3ii0.952.723.626 (8)159
C29A—H29C···Cg2ii0.992.693.57 (2)148
Symmetry codes: (i) −x+1, −y, −z; (ii) −x+1, −y, −z+1; (iii) x−1, y, z.
 

Acknowledgements

We gratefully acknowledge the financial support from NRF, THRIP, and UKZN (URF).

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