Crystal structure of [Th3(Cp*)3(O)(OH)3]2Cl2(N3)6: a discrete mol­ecular capsule built from multinuclear organothorium cluster cations

Kelley, S.P.; Rungthanaphatsophon, P.; Walensky, J.R.

doi:10.1107/S2056989021008914

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ISSN: 2056-9890

Volume 77| Part 10| October 2021| Pages 971-974

https://doi.org/10.1107/S2056989021008914

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Crystal structure of [Th₃(Cp*)₃(O)(OH)₃]₂Cl₂(N₃)₆: a discrete molecular capsule built from multinuclear organothorium cluster cations

Steven P. Kelley,^a ^* Pokpong Rungthanaphatsophon ^a and Justin R. Walensky ^a ^*

^aDepartment of Chemistry, University of Missouri-Columbia, Columbia, MO 65211, USA
^*Correspondence e-mail: kelleysp@missouri.edu, walenskyj@missouri.edu

Edited by M. Zeller, Purdue University, USA (Received 19 August 2021; accepted 25 August 2021; online 3 September 2021)

An unusually large and structurally complex charge-neutral polynuclear cluster, hexa-μ₂-azido-di-μ₃-chlorido-hexa-μ₂-hydroxido-di-μ₃-oxido-hexakis(pentamethylcyclopentadienyl)hexathorium–diethyl ether–tetrahydrofuran (1/0.56/1.44), [Th₃(C₁₀H₁₅)₆Cl₃(N₃)₆(OH)₆O₂]·0.56C₄H₁₀O·1.44C₄H₈O or [Th₃(Cp*)₃(O)(OH)₃]₂Cl₂(N₃)₆·0.56C₄H₁₀O·1.44C₄H₈O (Cp* = [pentamethylcyclopentadienyl])⁻, has been crystallized as a mixed tetrahydrofuran/diethyl ether solvate and structurally characterized. The molecule contains a number of unusual features, the most notable being a finite yet exceptionally long cyclic metal-azido chain. These rare features are the consequence of both sterically protecting Cp* ligands and highly bridging oxide and hydroxide ligands in the same system and illustrate the interesting new possibilities that can arise from combining organometallic and solvothermal f-block element chemistry.

Keywords: actinide; thorium; cyclopentadienyl; polynuclear; sandwich complex; crystal structure.

CCDC reference: 2105511

1. Chemical context

Pentamethylcyclopentadienyl (Cp*) ligands have become almost ubiquitous in the organometallic chemistry of the f-block elements (Evans & Davis, 2002 ). These ligands protect the reactive metal center and allow the solubilization and recrystallization of metal complexes in non-coordinating organic solvents. The actinides in particular have unique chemical properties owing to the participation of f-orbital electrons in chemical bonding (Neidig et al., 2013 ) and the breakdown of periodic trends in the elements due to relativistic electron motion (Cary et al., 2015 ), making organoactinide chemistry an important frontier in fundamental chemistry. However, the general instability of f-element organometallic complexes towards air, moisture, and protic solvents has prevented them from being applied in other areas where f-elements have been successfully applied, such as the formation of unique extended structures driven by their unusual coordination polyhedra (Burns & Nyman, 2018 , Li et al., 2017 ; Rocha et al., 2011 ).

Compared to uranium and the lanthanides, the coordination chemistry of thorium has been surprisingly under-investigated. Of the 55,423 entries in the Cambridge Structural Database [Version 2020.3.0 (November 2020); Groom et al., 2016 ] containing an f-element, only 1,241 contain thorium, and over two-thirds of these have only been reported since 2010. The increased number of Th-containing structures coincides with a renewed interest in actinide chemistry in general, and these studies have revealed interesting structural features unique to Th-containing compounds such as a strong tendency of Th⁴⁺ to form high-nuclearity yet discrete molecular complexes and ions (Wilson et al., 2007 ; Knope et al., 2011 ; Wacker et al., 2019 .)

The title compound of this study was isolated during research using {Th(Cp*)₂}-based complexes to study novel organic transformations (Tarlton et al., 2020 ; Tarlton, Fajen et al., 2021 ) and actinide–main-group bonding involving Th⁴⁺ (Tarlton, Yang et al. 2021 ; Rungthanaphatsophon et al., 2018 ; Vilanova et al., 2017 ). It represents an unprecedented case of overlap between organothorium chemistry and the formation of polynuclear oxo-bridged clusters. Spontaneous cluster formation in other, oxygen-free complexes of Th⁴⁺ with tetrel group elements is explored in a second publication as part of this joint special issue (Kelley et al., 2021 ).

2. Structural commentary

The molecule is a charge-neutral polynuclear metal complex of unusual size and complexity. It can be conceived as being built from two polyatomic cations with the formula [Th₃(Cp*)₃(O)(OH)₃]⁴⁺, each of which is sandwiched between two terminal Cl⁻ ions at either end of the molecule and a ring of 6 N₃⁻ anions in the center (Fig. 1). The structure crystallizes in the monoclinic space group C2/m with Z = 2. The molecule resides on a crystallographic mirror plane perpendicular to b, a crystallographic twofold proper axis parallel to b, and the inversion center where the axis and plane coincide, giving the entire molecule exact C_2h symmetry. All Th⁴⁺ centers in the structure are chemically equivalent, and the {[Th₃(Cp*)₃(O)(OH)₃]Cl} units have approximate C_3v symmetry. The symmetry of the overall molecule is lowered by the arrangements of the N₃⁻ ions, which tilt to differing degrees relative to the twofold axis.

Figure 1
50% probability ellipsoid plot of a single molecule of [Th₃(Cp*)₃(O)(OH)₃]₂Cl₂(N₃)_6. A tetrahydrofuran molecule of crystallization is shown to illustrate hydrogen bonding, all other solvents of crystallization are omitted. Hydrogen atoms with the exception of hydroxyl H atoms have been omitted for clarity. Light dashes indicate hydrogen bonding. Unlabeled atoms are symmetry equivalents of labeled atoms.

There are no published structures containing a moiety exactly analogous to the [Th₃(Cp*)₃(O)(OH)₃]⁴⁺ cluster, and published Th—O distances vary extremely widely due to the highly variable coordination geometry of Th⁴⁺. Another neutral hexanuclear Th⁴⁺ complex with the formula Th₆(O)₄(OH)₄(CHO₂)₁₂(OH₂)₁₂ has been reported and shows comparable Th—O²⁻ distances, although the OH⁻ ligands in this structure bridge three metal centers and have significantly longer bond distances (Takao et al., 2009 ). A polyatomic anion with the formula [Th₃Cl₁₀(OH)₅(OH₂)₂]³⁻ is reported, which has the same six-membered cycle of Th⁴⁺ and μ²-OH⁻ ligands (but no O²⁻ ligands), and the Th—O distances for these ligands are very similar to those in [Th₃(Cp*)₃(O)(OH)₃]⁴⁺ (Wacker et al., 2019).

The six Th⁴⁺ atoms and six azido ligands are bridged into what is essentially a linear chain that has cyclized to form a 24-membered ring, which is the longest non-polymeric metal–azido chain reported. However, cycles with three or four repeat units are quite common, and one example is known for Th⁴⁺ and has Th—N and azide N—N distances that overlap with those in this structure (Du et al. 2019 ). It is clear that while most of the individual building blocks within this structure have been observed previously, the unusual features arise from the termination of growth of a Th⁴⁺ cluster ion by Cp* ligands, leading to very intricate interconnectivity between the metal centers.

3. Supramolecular features

The molecules pack through a herringbone arrangement of the Cp* ligands so that the methyl groups of one Cp* point towards the aromatic ring plane of the neighboring molecules, leading to infinite two-dimensional layers parallel to the ab face (Fig. 2, left). These layers stack along c such that the molecules in each layer reside over holes in the neighboring layer, analogous to cubic close packing of spheres (Fig. 2, right); this arrangement most likely reduces repulsion between the like-charged anionic groups at either end of the molecule. For each molecule of the main moiety there are two solvent molecules of crystallization, which are located in the holes in each layer on the crystallographic mirror planes. These solvent molecules were found to be either tetrahydrofuran (THF) or diethyl ether (Et₂O) and are substitutionally disordered across the same site; their relative occupancies refined to 72%:28% THF:Et₂O. Both molecules are positioned such that the ether oxygen atom accepts a hydrogen bond from one of the bridging OH⁻ ions (Table 1, Fig. 1).

Table 1
Hydrogen-bond geometry (Å, °)

D—H⋯A	D—H	H⋯A	D⋯A	D—H⋯A
O2—H2⋯O1S	0.84 (2)	1.93 (3)	2.762 (10)	170 (8)

Figure 2
Left: Packing diagram showing a single two-dimensional layer of molecules, elements are color coded as in Fig. 1

. Right: Packing diagram showing the CCP-like arrangement of one molecule (red) over the hole formed by four neighboring molecules in the adjacent layer (yellow/blue, all atoms drawn as spheres of vdW radii).

4. Synthesis and crystallization

The title compound was the byproduct of the reaction of (C₅Me₅)₂Th(CH₃)[P(Mes)(SiMe₃)], Mes = 2,4,6-Me₃C₆H₂, (Rungthanaphatsophon et al., 2018) with two equivalents of Me₃SiN₃ in dimethoxyethane (DME) at room temperature. After stirring overnight, the resulting solution was allowed to crystallize inside an N₂-filled glove box at ambient temperature (∼3 days). Crystals suitable for SCXRD were obtained by recrystallization of these solids from diethyl ether/tetrahydrofuran. The chloride is presumably due to the starting material, (C₅Me₅)₂Th(CH₃)(Cl), which is used to make (C₅Me₅)₂Th(CH₃)[P(Mes)(SiMe₃)], while the oxo- and hydroxide ligands are due to an adventitious source of oxygen present in the solvent or glove box.

5. Refinement

Crystal data, data collection and structure refinement details are summarized in Table 2. The crystal structure was solved by an iterative dual space approach as implemented in SHELXT (Sheldrick, 2015a ). All atoms could be refined anisotropically. The residual difference map contained large, chemically non-reasonable peaks near the Th atoms which could not be modeled but could be reduced by truncating some of the high-angle data during reduction. The disordered THF and Et₂O molecules were located from the difference map. For the THF molecule, the oxygen atom and carbon atom C1S had their y coordinates fixed to reside on the crystallographic mirror plane; the other atoms were refined as additionally disordered across both positions related by the mirror plane. All non-hydrogen atoms of the Et₂O molecule had their y coordinates fixed to lie on the mirror plane. The chemical occupancy of the THF molecule was fixed to a free variable, which refined to 72 (1)%, and the chemical occupancies of the THF and Et₂O molecules were constrained to sum to 100%. The fractional occupancies of all atoms in both solvent molecules were set to 50% of the chemical occupancies due to their residence on or disorder across a crystallographic mirror plane. Both solvent molecules were also refined with C—C distances restrained to 1.54 (2) Å, C—O distances restrained to 1.41 (2) Å, and all anisotropic displacement parameters among bonded atoms restrained to be equal within an e.s.d. of 0.01 Å². A hydrogen atom was located from the difference map for the non-hydrogen bonding –OH group, and its coordinates were refined with the O—H distance restrained to 0.84 (2) Å. For the –OH group engaged in the strong hydrogen bond with THF, a hydrogen atom was placed along the ideal O—H⋯O hydrogen bond vector and restrained to a distance of 0.84 Å from the covalently bonded O atom. The identities of the –OH groups are established on the basis of charge-balance considerations and consistency with Th—O distances in the literature for –OH vs O²⁻ ligands, rather than the location of H atoms from the difference map. All other hydrogen atoms were placed in calculated positions, and were constrained to ride on their carrier atoms. Methyl group hydrogen atoms were refined with a riding-rotating model (except for disordered Et₂O methyl groups which were fixed in idealized staggered geometries). For all H atoms, displacement parameters were constrained to be multiples of U_iso for the bonded non-hydrogen atom.

Table 2
Experimental details

Crystal data
Chemical formula	[Th₆(C₁₀H₁₅)₆Cl₂(N₃)₆(OH)₆O₂]·0.56C₄H₁₀O·1.44C₄H₈O
M_r	2804.00
Crystal system, space group	Monoclinic, C2/m
Temperature (K)	100
a, b, c (Å)	17.6783 (14), 17.2647 (14), 16.383 (2)
β (°)	121.867 (3)
V (Å³)	4246.6 (7)
Z	2
Radiation type	Mo Kα
μ (mm⁻¹)	10.59
Crystal size (mm)	0.17 × 0.13 × 0.04

Data collection
Diffractometer	Bruker VENTURE CMOS area detector
Absorption correction	Multi-scan (AXScale; Bruker, 2017 )
T_min, T_max	0.333, 0.431
No. of measured, independent and observed [I > 2σ(I)] reflections	64622, 5050, 4393
R_int	0.071
(sin θ/λ)_max (Å⁻¹)	0.650

Refinement
R[F² > 2σ(F²)], wR(F²), S	0.027, 0.056, 1.03
No. of reflections	5050
No. of parameters	307
No. of restraints	155
H-atom treatment	H atoms treated by a mixture of independent and constrained refinement

Δρ_max, Δρ_min (e Å⁻³)	3.14, −0.91
Computer programs: APEX3 and SAINT (Bruker, 2017), SHELXT (Sheldrick, 2015a), SHELXL (Sheldrick, 2015b ), and OLEX2 (Dolomanov et al., 2009 ).

Supporting information

CCDC reference: 2105511

Crystal structure: contains datablock I. DOI: https://doi.org/10.1107/S2056989021008914/zl5025sup1.cif

Structure factors: contains datablock I. DOI: https://doi.org/10.1107/S2056989021008914/zl5025Isup2.hkl

checkCIF report

Computing details top

Data collection: APEX3 (Bruker, 2017); cell refinement: APEX3 and SAINT (Bruker, 2017); data reduction: APEX3 and SAINT (Bruker, 2017); program(s) used to refine structure: SHELXL (Sheldrick, 2015b); molecular graphics: OLEX2 (Dolomanov et al., 2009); software used to prepare material for publication: OLEX2 (Dolomanov et al., 2009).

Hexa-µ₂-azido-di-µ₃-chlorido-hexa-µ₂-hydroxido-di-µ₃-oxido-hexakis(pentamethylcyclopentadienyl)hexathorium–diethyl ether–tetrahydrofuran (1/0.56/1.44) top

Crystal data top

[Th₆(C₁₀H₁₅)₆Cl₂(N₃)₆(OH)₆O₂]·0.56C₄H₁₀O·1.44C₄H₈O	F(000) = 2598
M_r = 2804.00	D_x = 2.193 Mg m⁻³
Monoclinic, C2/m	Mo Kα radiation, λ = 0.71073 Å
a = 17.6783 (14) Å	Cell parameters from 9971 reflections
b = 17.2647 (14) Å	θ = 2.4–27.5°
c = 16.383 (2) Å	µ = 10.59 mm⁻¹
β = 121.867 (3)°	T = 100 K
V = 4246.6 (7) Å³	Irregular, colorless
Z = 2	0.17 × 0.13 × 0.04 mm

Data collection top

Bruker VENTURE CMOS area detector diffractometer	4393 reflections with I > 2σ(I)
Radiation source: Incoatec IMuS microfocus Mo tube	R_int = 0.071
shutterless ω and phi scans	θ_max = 27.5°, θ_min = 2.4°
Absorption correction: multi-scan (AXScale; Bruker, 2017)	h = −22→22
T_min = 0.333, T_max = 0.431	k = −22→22
64622 measured reflections	l = −21→21
5050 independent reflections

Refinement top

Refinement on F²	Primary atom site location: dual
Least-squares matrix: full	Secondary atom site location: difference Fourier map
R[F² > 2σ(F²)] = 0.027	Hydrogen site location: mixed
wR(F²) = 0.056	H atoms treated by a mixture of independent and constrained refinement
S = 1.03	w = 1/[σ²(F_o²) + (0.0229P)² + 34.2882P] where P = (F_o² + 2F_c²)/3
5050 reflections	(Δ/σ)_max = 0.003
307 parameters	Δρ_max = 3.14 e Å⁻³
155 restraints	Δρ_min = −0.90 e Å⁻³

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

	x	y	z	U_iso*/U_eq	Occ. (<1)
Th1	0.68056 (2)	0.60822 (2)	0.69358 (2)	0.01292 (5)
Th2	0.53556 (2)	0.500000	0.75710 (2)	0.01168 (6)
Cl1	0.73648 (11)	0.500000	0.86411 (11)	0.0174 (3)
O1	0.5917 (3)	0.500000	0.6566 (3)	0.0147 (9)
O2	0.7638 (3)	0.500000	0.6957 (3)	0.0169 (10)
H2	0.809 (3)	0.500000	0.691 (6)	0.025*
O3	0.5971 (2)	0.62494 (18)	0.7689 (2)	0.0168 (7)
H3	0.563 (6)	0.663 (4)	0.748 (7)	0.025*	0.5
N1	0.4076 (3)	0.5858 (3)	0.6357 (3)	0.0233 (9)
N2	0.3749 (3)	0.5981 (2)	0.5529 (3)	0.0153 (8)
N3	0.3402 (3)	0.6128 (2)	0.4715 (3)	0.0228 (9)
N4	0.5440 (3)	0.6925 (2)	0.5842 (3)	0.0198 (9)
N5	0.500000	0.6919 (3)	0.500000	0.0168 (12)
C1	0.8493 (3)	0.6738 (3)	0.8077 (4)	0.0204 (10)
C2	0.8168 (3)	0.7073 (3)	0.7160 (3)	0.0211 (11)
C3	0.7461 (4)	0.7577 (3)	0.6962 (4)	0.0236 (11)
C4	0.7349 (3)	0.7564 (3)	0.7756 (3)	0.0208 (10)
C5	0.7987 (3)	0.7044 (3)	0.8442 (3)	0.0187 (10)
C6	0.9278 (4)	0.6209 (3)	0.8601 (4)	0.0307 (13)
H6A	0.918535	0.585471	0.900768	0.046*
H6B	0.981731	0.651592	0.900265	0.046*
H6C	0.934610	0.590903	0.813530	0.046*
C7	0.8561 (4)	0.6980 (4)	0.6544 (4)	0.0332 (14)
H7A	0.884053	0.646886	0.665711	0.050*
H7B	0.901031	0.738296	0.670865	0.050*
H7C	0.808905	0.702819	0.586503	0.050*
C8	0.6968 (4)	0.8088 (3)	0.6087 (4)	0.0314 (13)
H8A	0.675395	0.777497	0.550602	0.047*
H8B	0.736905	0.849200	0.611231	0.047*
H8C	0.645907	0.832931	0.607281	0.047*
C9	0.6695 (4)	0.8042 (3)	0.7866 (4)	0.0276 (12)
H9A	0.611609	0.803876	0.726080	0.041*
H9B	0.691318	0.857577	0.803166	0.041*
H9C	0.663160	0.782241	0.837851	0.041*
C10	0.8162 (4)	0.6901 (3)	0.9437 (4)	0.0260 (12)
H10A	0.762198	0.701260	0.944310	0.039*
H10B	0.864643	0.723791	0.989868	0.039*
H10C	0.833217	0.635783	0.961429	0.039*
C11	0.4835 (3)	0.4335 (3)	0.8752 (3)	0.0154 (9)
C12	0.4289 (4)	0.500000	0.8363 (5)	0.0171 (14)
C13	0.5718 (3)	0.4589 (3)	0.9384 (3)	0.0154 (9)
C14	0.4549 (4)	0.3503 (3)	0.8574 (4)	0.0260 (12)
H14A	0.395664	0.346319	0.798828	0.039*
H14B	0.452683	0.330173	0.912070	0.039*
H14C	0.497535	0.319910	0.849670	0.039*
C15	0.3290 (5)	0.500000	0.7689 (5)	0.0279 (17)
H15A	0.312567	0.464474	0.715426	0.042*	0.5
H15B	0.308772	0.552425	0.743913	0.042*	0.5
H15C	0.300794	0.483101	0.803799	0.042*	0.5
C16	0.6503 (4)	0.4080 (3)	0.9991 (3)	0.0222 (11)
H16A	0.705180	0.436174	1.017657	0.033*
H16B	0.646369	0.361634	0.962550	0.033*
H16C	0.650705	0.392683	1.056974	0.033*
O2S	0.962 (2)	0.500000	0.674 (2)	0.061 (4)	0.280 (11)
C5S	1.055 (2)	0.500000	0.720 (2)	0.065 (5)	0.280 (11)
H5SA	1.075920	0.546619	0.701666	0.078*	0.140 (5)
H5SB	1.075920	0.453381	0.701666	0.078*	0.140 (5)
C6S	1.091 (3)	0.500000	0.828 (3)	0.064 (6)	0.280 (11)
H6SA	1.156583	0.500000	0.864533	0.097*	0.280 (11)
H6SB	1.070092	0.546347	0.844821	0.097*	0.140 (5)
H6SC	1.070092	0.453653	0.844821	0.097*	0.140 (5)
C7S	0.923 (2)	0.500000	0.573 (2)	0.058 (4)	0.280 (11)
H7SA	0.942803	0.453573	0.554259	0.069*	0.140 (5)
H7SB	0.942803	0.546427	0.554259	0.069*	0.140 (5)
C8S	0.822 (2)	0.500000	0.522 (3)	0.054 (4)	0.280 (11)
H8SA	0.795779	0.500000	0.452448	0.081*	0.280 (11)
H8SB	0.802133	0.453653	0.540462	0.081*	0.140 (5)
H8SC	0.802133	0.546347	0.540462	0.081*	0.140 (5)
O1S	0.8969 (7)	0.500000	0.6553 (7)	0.050 (2)	0.360 (5)
C1S	0.8526 (10)	0.500000	0.5515 (11)	0.055 (3)	0.360 (5)
H1SA	0.805267	0.539887	0.523128	0.066*	0.360 (5)
H1SB	0.825386	0.448814	0.525057	0.066*	0.360 (5)
C2S	0.9243 (12)	0.5179 (12)	0.5292 (15)	0.066 (4)	0.360 (5)
H2SA	0.934339	0.574303	0.528668	0.079*	0.360 (5)
H2SB	0.910796	0.494664	0.467676	0.079*	0.360 (5)
C3S	1.0042 (13)	0.4768 (12)	0.6179 (14)	0.067 (4)	0.360 (5)
H3SA	0.998454	0.419714	0.613336	0.080*	0.360 (5)
H3SB	1.062238	0.492263	0.627273	0.080*	0.360 (5)
C4S	0.9910 (10)	0.510 (2)	0.6976 (15)	0.061 (3)	0.360 (5)
H4SA	1.025462	0.480111	0.758113	0.073*	0.360 (5)
H4SB	1.008272	0.565129	0.710357	0.073*	0.360 (5)

Atomic displacement parameters (Å²) top

	U¹¹	U²²	U³³	U¹²	U¹³	U²³
Th1	0.01355 (9)	0.01211 (8)	0.01065 (8)	−0.00232 (6)	0.00472 (7)	−0.00054 (6)
Th2	0.01279 (12)	0.01143 (11)	0.01021 (11)	0.000	0.00567 (9)	0.000
Cl1	0.0168 (8)	0.0177 (8)	0.0122 (7)	0.000	0.0039 (6)	0.000
O1	0.015 (2)	0.014 (2)	0.010 (2)	0.000	0.0034 (19)	0.000
O2	0.014 (2)	0.019 (2)	0.017 (2)	0.000	0.008 (2)	0.000
O3	0.0188 (18)	0.0151 (16)	0.0162 (17)	0.0004 (13)	0.0090 (15)	0.0016 (13)
N1	0.021 (2)	0.033 (2)	0.015 (2)	0.0078 (19)	0.0086 (18)	0.0078 (18)
N2	0.014 (2)	0.0136 (18)	0.017 (2)	0.0046 (16)	0.0073 (17)	0.0007 (15)
N3	0.024 (2)	0.029 (2)	0.012 (2)	0.0009 (19)	0.0074 (18)	−0.0004 (17)
N4	0.019 (2)	0.021 (2)	0.011 (2)	0.0002 (17)	0.0022 (18)	0.0013 (16)
N5	0.018 (3)	0.012 (3)	0.019 (3)	0.000	0.008 (3)	0.000
C1	0.019 (3)	0.018 (2)	0.022 (3)	−0.007 (2)	0.009 (2)	−0.0013 (19)
C2	0.024 (3)	0.021 (2)	0.019 (2)	−0.014 (2)	0.011 (2)	−0.007 (2)
C3	0.027 (3)	0.017 (2)	0.022 (3)	−0.009 (2)	0.010 (2)	−0.002 (2)
C4	0.022 (3)	0.017 (2)	0.017 (2)	−0.007 (2)	0.007 (2)	−0.0037 (19)
C5	0.018 (2)	0.019 (2)	0.014 (2)	−0.010 (2)	0.005 (2)	−0.0050 (19)
C6	0.020 (3)	0.037 (3)	0.028 (3)	0.002 (2)	0.008 (2)	−0.005 (2)
C7	0.035 (3)	0.040 (3)	0.029 (3)	−0.017 (3)	0.020 (3)	−0.013 (3)
C8	0.039 (3)	0.025 (3)	0.021 (3)	−0.010 (3)	0.010 (3)	0.003 (2)
C9	0.031 (3)	0.019 (3)	0.027 (3)	−0.003 (2)	0.012 (3)	−0.008 (2)
C10	0.029 (3)	0.026 (3)	0.018 (3)	−0.006 (2)	0.009 (2)	−0.002 (2)
C11	0.018 (2)	0.018 (2)	0.015 (2)	−0.0038 (19)	0.012 (2)	−0.0010 (18)
C12	0.014 (3)	0.027 (4)	0.015 (3)	0.000	0.010 (3)	0.000
C13	0.022 (3)	0.014 (2)	0.012 (2)	0.0000 (19)	0.010 (2)	0.0008 (17)
C14	0.035 (3)	0.022 (3)	0.028 (3)	−0.008 (2)	0.021 (3)	−0.003 (2)
C15	0.017 (4)	0.045 (5)	0.020 (4)	0.000	0.008 (3)	0.000
C16	0.028 (3)	0.021 (2)	0.017 (2)	0.006 (2)	0.011 (2)	0.007 (2)
O2S	0.059 (6)	0.055 (6)	0.085 (6)	0.000	0.050 (6)	0.000
C5S	0.058 (7)	0.057 (7)	0.090 (7)	0.000	0.046 (7)	0.000
C6S	0.055 (9)	0.058 (9)	0.091 (9)	0.000	0.046 (8)	0.000
C7S	0.058 (6)	0.055 (5)	0.084 (6)	0.000	0.053 (6)	0.000
C8S	0.057 (7)	0.051 (6)	0.081 (7)	0.000	0.054 (6)	0.000
O1S	0.052 (5)	0.049 (4)	0.079 (5)	0.001 (5)	0.054 (5)	0.000
C1S	0.058 (6)	0.051 (5)	0.083 (6)	0.003 (5)	0.054 (5)	0.000
C2S	0.063 (6)	0.059 (6)	0.089 (7)	0.012 (5)	0.050 (6)	0.006 (5)
C3S	0.062 (6)	0.062 (6)	0.090 (7)	0.010 (4)	0.050 (6)	0.009 (4)
C4S	0.056 (6)	0.057 (6)	0.088 (6)	0.001 (4)	0.051 (6)	0.002 (4)

Geometric parameters (Å, º) top

Th1—Cl1	3.0589 (12)	C10—H10A	0.9800
Th1—O1	2.307 (3)	C10—H10B	0.9800
Th1—O2	2.367 (3)	C10—H10C	0.9800
Th1—O3	2.388 (3)	C11—C12	1.417 (6)
Th1—N3ⁱ	2.530 (4)	C11—C13	1.413 (7)
Th1—N4	2.567 (4)	C11—C14	1.500 (7)
Th1—C1	2.791 (5)	C12—C15	1.510 (10)
Th1—C2	2.816 (5)	C13—C13ⁱⁱ	1.417 (9)
Th1—C3	2.820 (5)	C13—C16	1.493 (7)
Th1—C4	2.813 (5)	C14—H14A	0.9800
Th1—C5	2.787 (5)	C14—H14B	0.9800
Th2—Cl1	3.0190 (17)	C14—H14C	0.9800
Th2—O1	2.329 (4)	C15—H15Aⁱⁱ	0.98 (6)
Th2—O3	2.378 (3)	C15—H15A	0.9800
Th2—O3ⁱⁱ	2.378 (3)	C15—H15B	0.9800
Th2—N1	2.553 (4)	C15—H15Bⁱⁱ	0.98 (2)
Th2—N1ⁱⁱ	2.553 (4)	C15—H15C	0.9800
Th2—C11	2.791 (4)	C15—H15Cⁱⁱ	0.98 (4)
Th2—C11ⁱⁱ	2.791 (4)	C16—H16A	0.9800
Th2—C12	2.796 (6)	C16—H16B	0.9800
Th2—C13ⁱⁱ	2.780 (4)	C16—H16C	0.9800
Th2—C13	2.780 (4)	O2S—C5S	1.415 (19)
O2—H2	0.84 (2)	O2S—C7S	1.411 (19)
O3—H3	0.84 (2)	C5S—H5SA	0.9900
N1—N2	1.180 (5)	C5S—H5SB	0.9900
N2—N3	1.165 (5)	C5S—C6S	1.542 (19)
N4—N5	1.172 (4)	C6S—H6SA	0.9800
C1—C2	1.418 (7)	C6S—H6SB	0.9800
C1—C5	1.415 (7)	C6S—H6SC	0.9800
C1—C6	1.497 (7)	C7S—H7SA	0.9900
C2—C3	1.414 (8)	C7S—H7SB	0.9900
C2—C7	1.505 (7)	C7S—C8S	1.523 (19)
C3—C4	1.415 (7)	C8S—H8SA	0.9800
C3—C8	1.508 (7)	C8S—H8SB	0.9800
C4—C5	1.415 (7)	C8S—H8SC	0.9800
C4—C9	1.507 (7)	O1S—C1S	1.448 (15)
C5—C10	1.511 (7)	O1S—C4S	1.435 (15)
C6—H6A	0.9800	C1S—H1SA	0.9900
C6—H6B	0.9800	C1S—H1SB	0.9900
C6—H6C	0.9800	C1S—C2S	1.525 (16)
C7—H7A	0.9800	C2S—H2SA	0.9900
C7—H7B	0.9800	C2S—H2SB	0.9900
C7—H7C	0.9800	C2S—C3S	1.563 (17)
C8—H8A	0.9800	C3S—H3SA	0.9900
C8—H8B	0.9800	C3S—H3SB	0.9900
C8—H8C	0.9800	C3S—C4S	1.551 (17)
C9—H9A	0.9800	C4S—H4SA	0.9900
C9—H9B	0.9800	C4S—H4SB	0.9900
C9—H9C	0.9800

O1—Th1—Cl1	65.94 (10)	C8—C3—Th1	119.6 (3)
O1—Th1—O2	72.32 (13)	C3—C4—Th1	75.7 (3)
O1—Th1—O3	73.33 (13)	C3—C4—C9	126.1 (5)
O1—Th1—N3ⁱ	92.85 (14)	C5—C4—Th1	74.3 (3)
O1—Th1—N4	90.95 (13)	C5—C4—C3	107.5 (4)
O1—Th1—C1	147.52 (14)	C5—C4—C9	126.3 (5)
O1—Th1—C2	160.60 (14)	C9—C4—Th1	117.7 (3)
O1—Th1—C3	164.27 (14)	C1—C5—Th1	75.4 (3)
O1—Th1—C4	151.16 (15)	C1—C5—C4	108.5 (4)
O1—Th1—C5	143.48 (14)	C1—C5—C10	125.4 (5)
O2—Th1—Cl1	66.77 (11)	C4—C5—Th1	76.4 (3)
O2—Th1—O3	129.52 (12)	C4—C5—C10	125.8 (5)
O2—Th1—N3ⁱ	77.23 (15)	C10—C5—Th1	119.2 (3)
O2—Th1—N4	143.70 (14)	C1—C6—H6A	109.5
O2—Th1—C1	82.76 (14)	C1—C6—H6B	109.5
O2—Th1—C2	89.72 (14)	C1—C6—H6C	109.5
O2—Th1—C3	118.37 (14)	H6A—C6—H6B	109.5
O2—Th1—C4	131.14 (14)	H6A—C6—H6C	109.5
O2—Th1—C5	106.72 (15)	H6B—C6—H6C	109.5
O3—Th1—Cl1	65.92 (8)	C2—C7—H7A	109.5
O3—Th1—N3ⁱ	140.13 (13)	C2—C7—H7B	109.5
O3—Th1—N4	71.49 (12)	C2—C7—H7C	109.5
O3—Th1—C1	109.77 (13)	H7A—C7—H7B	109.5
O3—Th1—C2	125.35 (13)	H7A—C7—H7C	109.5
O3—Th1—C3	104.02 (14)	H7B—C7—H7C	109.5
O3—Th1—C4	77.98 (13)	C3—C8—H8A	109.5
O3—Th1—C5	81.33 (13)	C3—C8—H8B	109.5
N3ⁱ—Th1—Cl1	142.14 (10)	C3—C8—H8C	109.5
N3ⁱ—Th1—N4	71.56 (13)	H8A—C8—H8B	109.5
N3ⁱ—Th1—C1	101.77 (14)	H8A—C8—H8C	109.5
N3ⁱ—Th1—C2	75.63 (14)	H8B—C8—H8C	109.5
N3ⁱ—Th1—C3	79.31 (14)	C4—C9—H9A	109.5
N3ⁱ—Th1—C4	107.60 (14)	C4—C9—H9B	109.5
N3ⁱ—Th1—C5	123.06 (14)	C4—C9—H9C	109.5
N4—Th1—Cl1	135.67 (10)	H9A—C9—H9B	109.5
N4—Th1—C1	121.10 (14)	H9A—C9—H9C	109.5
N4—Th1—C2	99.86 (15)	H9B—C9—H9C	109.5
N4—Th1—C3	73.69 (14)	C5—C10—H10A	109.5
N4—Th1—C4	77.07 (14)	C5—C10—H10B	109.5
N4—Th1—C5	105.63 (14)	C5—C10—H10C	109.5
C1—Th1—Cl1	85.43 (10)	H10A—C10—H10B	109.5
C1—Th1—C2	29.29 (14)	H10A—C10—H10C	109.5
C1—Th1—C3	48.19 (15)	H10B—C10—H10C	109.5
C1—Th1—C4	48.40 (15)	C12—C11—Th2	75.5 (3)
C2—Th1—Cl1	114.22 (11)	C12—C11—C14	127.5 (5)
C2—Th1—C3	29.07 (15)	C13—C11—Th2	74.9 (2)
C3—Th1—Cl1	127.82 (11)	C13—C11—C12	107.7 (4)
C4—Th1—Cl1	104.78 (10)	C13—C11—C14	124.7 (4)
C4—Th1—C2	48.11 (15)	C14—C11—Th2	117.4 (3)
C4—Th1—C3	29.10 (14)	C11ⁱⁱ—C12—Th2	75.1 (3)
C5—Th1—Cl1	79.97 (10)	C11—C12—Th2	75.1 (3)
C5—Th1—C1	29.39 (15)	C11ⁱⁱ—C12—C11	108.3 (6)
C5—Th1—C2	48.16 (14)	C11—C12—C15	125.8 (3)
C5—Th1—C3	48.03 (14)	C11ⁱⁱ—C12—C15	125.8 (3)
C5—Th1—C4	29.26 (14)	C15—C12—Th2	118.5 (4)
O1—Th2—Cl1	66.47 (11)	C11—C13—Th2	75.7 (3)
O1—Th2—O3	73.12 (9)	C11—C13—C13ⁱⁱ	108.1 (3)
O1—Th2—O3ⁱⁱ	73.12 (9)	C11—C13—C16	125.7 (4)
O1—Th2—N1	88.99 (13)	C13ⁱⁱ—C13—Th2	75.23 (9)
O1—Th2—N1ⁱⁱ	88.99 (13)	C13ⁱⁱ—C13—C16	126.1 (3)
O1—Th2—C11	155.49 (10)	C16—C13—Th2	118.1 (3)
O1—Th2—C11ⁱⁱ	155.49 (10)	C11—C14—H14A	109.5
O1—Th2—C12	166.28 (18)	C11—C14—H14B	109.5
O1—Th2—C13ⁱⁱ	144.28 (14)	C11—C14—H14C	109.5
O1—Th2—C13	144.28 (14)	H14A—C14—H14B	109.5
O3—Th2—Cl1	66.73 (8)	H14A—C14—H14C	109.5
O3ⁱⁱ—Th2—Cl1	66.73 (8)	H14B—C14—H14C	109.5
O3ⁱⁱ—Th2—O3	130.25 (16)	C12—C15—H15Aⁱⁱ	109.5 (13)
O3ⁱⁱ—Th2—N1ⁱⁱ	73.53 (13)	C12—C15—H15A	109.5
O3—Th2—N1ⁱⁱ	140.27 (13)	C12—C15—H15B	109.5
O3—Th2—N1	73.53 (13)	C12—C15—H15Bⁱⁱ	109.5 (5)
O3ⁱⁱ—Th2—N1	140.27 (13)	C12—C15—H15Cⁱⁱ	109.5 (9)
O3—Th2—C11	128.42 (12)	C12—C15—H15C	109.5
O3ⁱⁱ—Th2—C11	82.80 (12)	H15A—C15—H15Aⁱⁱ	77.5
O3—Th2—C11ⁱⁱ	82.80 (12)	H15A—C15—H15B	109.5
O3ⁱⁱ—Th2—C11ⁱⁱ	128.42 (12)	H15Aⁱⁱ—C15—H15Bⁱⁱ	109.5
O3—Th2—C12	110.75 (9)	H15A—C15—H15Bⁱⁱ	34.6
O3ⁱⁱ—Th2—C12	110.75 (9)	H15A—C15—H15C	109.5
O3ⁱⁱ—Th2—C13ⁱⁱ	107.88 (12)	H15Aⁱⁱ—C15—H15Cⁱⁱ	109.5
O3—Th2—C13ⁱⁱ	81.05 (12)	H15A—C15—H15Cⁱⁱ	134.9
O3ⁱⁱ—Th2—C13	81.05 (12)	H15B—C15—H15Aⁱⁱ	34.6
O3—Th2—C13	107.88 (12)	H15B—C15—H15Bⁱⁱ	134.9
N1—Th2—Cl1	137.70 (10)	H15B—C15—H15C	109.5
N1ⁱⁱ—Th2—Cl1	137.70 (10)	H15Bⁱⁱ—C15—H15Cⁱⁱ	109.5
N1ⁱⁱ—Th2—N1	70.9 (2)	H15B—C15—H15Cⁱⁱ	77.5
N1—Th2—C11	107.32 (14)	H15C—C15—H15Aⁱⁱ	134.9
N1ⁱⁱ—Th2—C11ⁱⁱ	107.32 (14)	H15C—C15—H15Bⁱⁱ	77.5
N1—Th2—C11ⁱⁱ	79.65 (13)	H15C—C15—H15Cⁱⁱ	34.6
N1ⁱⁱ—Th2—C11	79.65 (13)	C13—C16—H16A	109.5
N1ⁱⁱ—Th2—C12	79.86 (15)	C13—C16—H16B	109.5
N1—Th2—C12	79.86 (15)	C13—C16—H16C	109.5
N1ⁱⁱ—Th2—C13	107.11 (14)	H16A—C16—H16B	109.5
N1—Th2—C13	126.15 (13)	H16A—C16—H16C	109.5
N1ⁱⁱ—Th2—C13ⁱⁱ	126.15 (13)	H16B—C16—H16C	109.5
N1—Th2—C13ⁱⁱ	107.11 (13)	C7S—O2S—C5S	109 (3)
C11—Th2—Cl1	108.35 (10)	O2S—C5S—H5SA	110.7
C11ⁱⁱ—Th2—Cl1	108.35 (10)	O2S—C5S—H5SB	110.7
C11—Th2—C11ⁱⁱ	48.60 (19)	O2S—C5S—C6S	105 (3)
C11ⁱⁱ—Th2—C12	29.38 (12)	H5SA—C5S—H5SB	108.8
C11—Th2—C12	29.38 (12)	C6S—C5S—H5SA	110.7
C12—Th2—Cl1	127.25 (14)	C6S—C5S—H5SB	110.7
C13ⁱⁱ—Th2—Cl1	80.94 (10)	C5S—C6S—H6SA	109.5
C13—Th2—Cl1	80.94 (10)	C5S—C6S—H6SB	109.5
C13—Th2—C11	29.39 (13)	C5S—C6S—H6SC	109.5
C13—Th2—C11ⁱⁱ	48.59 (13)	H6SA—C6S—H6SB	109.5
C13ⁱⁱ—Th2—C11	48.59 (13)	H6SA—C6S—H6SC	109.5
C13ⁱⁱ—Th2—C11ⁱⁱ	29.39 (13)	H6SB—C6S—H6SC	109.5
C13ⁱⁱ—Th2—C12	48.39 (16)	O2S—C7S—H7SA	109.6
C13—Th2—C12	48.39 (16)	O2S—C7S—H7SB	109.6
C13ⁱⁱ—Th2—C13	29.54 (18)	O2S—C7S—C8S	110 (3)
Th1ⁱⁱ—Cl1—Th1	75.30 (4)	H7SA—C7S—H7SB	108.1
Th2—Cl1—Th1ⁱⁱ	75.86 (3)	C8S—C7S—H7SA	109.6
Th2—Cl1—Th1	75.86 (3)	C8S—C7S—H7SB	109.6
Th1—O1—Th1ⁱⁱ	108.19 (18)	C7S—C8S—H8SA	109.5
Th1ⁱⁱ—O1—Th2	107.42 (12)	C7S—C8S—H8SB	109.5
Th1—O1—Th2	107.42 (12)	C7S—C8S—H8SC	109.5
Th1ⁱⁱ—O2—Th1	104.25 (18)	H8SA—C8S—H8SB	109.5
Th1—O2—H2	127.6 (5)	H8SA—C8S—H8SC	109.5
Th1ⁱⁱ—O2—H2	127.6 (5)	H8SB—C8S—H8SC	109.5
Th1—O3—H3	113 (8)	C4S—O1S—C1S	109.7 (12)
Th2—O3—Th1	103.27 (12)	O1S—C1S—H1SA	110.5
Th2—O3—H3	119 (8)	O1S—C1S—H1SB	110.5
N2—N1—Th2	134.0 (3)	O1S—C1S—C2S	106.2 (13)
N3—N2—N1	176.9 (5)	H1SA—C1S—H1SB	108.7
N2—N3—Th1ⁱ	155.4 (4)	C2S—C1S—H1SA	110.5
N5—N4—Th1	127.7 (3)	C2S—C1S—H1SB	110.5
N4—N5—N4ⁱ	179.0 (7)	C1S—C2S—H2SA	112.1
C2—C1—Th1	76.3 (3)	C1S—C2S—H2SB	112.1
C2—C1—C6	126.2 (5)	C1S—C2S—C3S	98.2 (15)
C5—C1—Th1	75.2 (3)	H2SA—C2S—H2SB	109.8
C5—C1—C2	107.6 (4)	C3S—C2S—H2SA	112.1
C5—C1—C6	126.0 (5)	C3S—C2S—H2SB	112.1
C6—C1—Th1	118.4 (3)	C2S—C3S—H3SA	112.0
C1—C2—Th1	74.4 (3)	C2S—C3S—H3SB	112.0
C1—C2—C7	126.5 (5)	C4S—C3S—C2S	98.7 (16)
C3—C2—Th1	75.6 (3)	C4S—C3S—H3SA	112.0
C3—C2—C1	107.9 (4)	C4S—C3S—H3SB	112.0
C3—C2—C7	125.3 (5)	O1S—C4S—C3S	101.6 (15)
C7—C2—Th1	120.9 (3)	O1S—C4S—H4SA	111.5
C2—C3—Th1	75.3 (3)	O1S—C4S—H4SB	111.5
C2—C3—C4	108.4 (4)	C3S—C4S—H4SA	111.5
C2—C3—C8	125.1 (5)	C3S—C4S—H4SB	111.5
C4—C3—Th1	75.2 (3)	H4SA—C4S—H4SB	109.3
C4—C3—C8	126.3 (5)

Symmetry codes: (i) −x+1, y, −z+1; (ii) x, −y+1, z.

Hydrogen-bond geometry (Å, º) top

D—H···A	D—H	H···A	D···A	D—H···A
O2—H2···O1S	0.84 (2)	1.93 (3)	2.762 (10)	170 (8)

Funding information

JRW gratefully acknowledges support for this work from the US Department of Energy, Office of Science under award No. DE-SC0021273. SPK thanks the University of Missouri Department of Chemistry for support of this work.

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