Tris[N,N-bis­(3,5-di-tert-butyl­benz­yl)di­thio­carbamato-κ2S,S′]-μ3-sulfido-tris-μ2-disulfido-triangulo-trimolybdenum(IV) iodide

Chen, Y.; Wang, B.; Fontenot, P.; Donahue, J.P.

doi:10.1107/S2414314620009396

metal-organic compounds

IUCrDATA

ISSN: 2414-3146

Volume 5| Part 7| July 2020| x200939

https://doi.org/10.1107/S2414314620009396

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Tris[N,N-bis(3,5-di-tert-butylbenzyl)dithiocarbamato-κ²S,S′]-μ₃-sulfido-tris-μ₂-disulfido-triangulo-trimolybdenum(IV) iodide

Yueli Chen,^a Bo Wang,^b Patricia Fontenot ^b and James P. Donahue ^b ^*

^aDepartment of Chemistry, University of Pennsylvania, 231 S. 34 Street, Philadelphia, PA 19104-6323, USA, and ^bDepartment of Chemistry, Tulane University, 6400 Freret Street, New Orleans, Louisiana 70118-5698, USA
^*Correspondence e-mail: donahue@tulane.edu

Edited by S. Parkin, University of Kentucky, USA (Received 12 June 2020; accepted 9 July 2020; online 17 July 2020)

The title compound, [Mo₃(C₃₁H₄₆NS₂)₃S₇]I, crystallizes on a threefold rotational axis in P31c (space group No. 159). The [Mo₃S₇(S₂CN(CH₂C₆H₃-3,5-^tBu₂)₂)₃]⁺ cations are arrayed in sheets in the ab plane with interligand hydrophobic interactions between tert-butyl groups guiding the packing arrangement. These cations form stacks parallel to the c axis with a separating distance of 10.9815 (6) Å (the c axis length) between the Mo₃ centroids. On the underside of the cluster, opposite the μ₃-S²⁻ ligand, the iodide counteranion forms close contacts of 3.166 (2) Å with the sulfur atoms of the μ₂-S₂²⁻ ligands. These contacts are less than the sum of the van der Waals radii of the atoms (1.8 and 2.1 Å for S and I, respectively), thus indicating an appreciable degree of covalency to the [Mo₃S₇(S₂CN(CH₂C₆H₃-3,5-^tBu₂)₂)₃]⁺⋯I⁻ interactions.

Keywords: crystal structure; molybdenum-sulfide cluster; bulky dithiocarbamate anion; dispersion forces.

CCDC reference: 2015330

Structure description

In a recent report (Fontenot et al., 2019 ), we described photocatalytic H₂ evolution by [Mo₃S₇(S₂CNⁱBu₂)₃]I in a MeCN/H₂O mixture with [Ru(bipy)₃]²⁺ as photosensitizer and Et₃N as sacrificial electron donor. After a brief incubation period under photoylsis, the [Mo₃S₇(S₂CNⁱBu₂)₃]I cluster gives way to a charge-neutral asymmetric hexamolybdenum species, comprised of [Mo₃S₇]⁴⁺ and [Mo₃S₄]⁴⁺ fragments, that appears to be the operative H₂-evolution catalyst. As part of our efforts to understand solution speciation of [Mo₃S₇(S₂CNR₂)₃]I (R = alkyl) under photolysis, we endeavored to prepare and structurally characterize [Mo₃S₄(S₂CNR₂)₃]⁺ clusters. Although stable to air and moisture and protracted handling, [Mo₃S₄(S₂CNR₂)₃]⁺ clusters have proven to be surprisingly intractable to crystallization by typical methods. On the supposition that dithiocarbamate supporting ligands with sufficiently large substituents would decisively dictate the solubility and crystallinity of a cluster to which they coordinate, we have prepared [Mo₃S₇(S₂CN(CH₂C₆H₃-3,5-^tBu₂)₂)₃]I as a precursor to [Mo₃S₄(S₂CN(CH₂C₆H₃-3,5-^tBu₂)₂)₃]⁺. In this communication, we briefly describe the crystal structure of [Mo₃S₇(S₂CN(CH₂C₆H₃-3,5-^tBu₂)₂)₃]I.

The procedure implemented for the synthesis of [Mo₃S₇(S₂CN(CH₂C₆H₃-3,5-^tBu₂)₂)₃]I is similar to that reported for [Mo₃S₇(S₂CNⁱBu₂)₃]I (Fontenot et al., 2019). Although nominally an ion pair, [Mo₃S₇(S₂CN(CH₂C₆H₃-3,5-^tBu₂)₂)₃]I is so dominated by the hydrophobicity of the CH₂C₆H₃-3,5-^tBu₂ dithiocarbamate substituents that it is readily taken up into C₆H₆. Addition of MeOH to a C₆H₆ solution to the point of incipient precipitation, followed by slow cooling, produces well-formed orange column-shaped crystals of [Mo₃S₇(S₂CN(CH₂C₆H₃-3,5-^tBu₂)₂)₃]I with no interstitial solvent.

The triangular [Mo₃S₇(S₂CN(CH₂C₆H₃-3,5-^tBu₂)₂)₃]⁺ cation coincides with a crystallographic threefold rotational axis, defined by S5 and the center of the Mo₃ equilateral triangle (Fig. 1), in the non-centrosymmetric trigonal space group P31c (space group No. 159). Among the fair number of structural studies of [Mo₃S₇(S₂CNR₂)₃]⁺·X⁻ salts (X⁻ = halide anion) that have been described (Zimmermann et al., 1991 ; Fedin et al., 1992 , 1993 ; Lu et al., 1993 ; Wang et al., 1994 ; Mayor-López et al., 1998 ; Il'inchik et al., 2002 , 2007 ; Fontenot et al., 2019), in only one other instance (Fedin et al., 1993) has the cluster cation been found on a threefold special position: [Mo₃S₇(S₂CNEt₂)₃]I·1.5C₆H₆ in R $[\overline{3}]$ c (space group No. 167). The 3,5-^tBu₂C₆H₃CH₂ groups from each dithiocarbamate ligand that are syn to the μ₃-S²⁻ ligand (carbon atoms C1–C16) define a right-handed propeller when the cation is viewed from its `top', or from the direction of the μ₃-S²⁻ ligand toward the Mo₃ centroid (Fig. 1). The remaining three 3,5-^tBu₂C₆H₃CH₂ groups (C17–C31), one from each ligand, are situated just below the Mo₃ plane and define a left-handed propeller.

Figure 1
Displacement ellipsoid plot of [Mo₃S₇(S₂CN(CH₂C₆H₃-3,5-^tBu₂)₂)₃]I at the 50% probability level with view along the threefold symmetry axis. All hydrogen atoms are omitted for clarity. tert-Butyl groups C13–C16 and C28–C31 are edited to show one of two positional variants in a split-atom model for the disorder. Symmetry codes: A = 1 − y, 1 + x − y, z; B = −x + y, 1 − x, z.

The occurrence of the trigonal space group for [Mo₃S₇(S₂CN(CH₂C₆H₃-3,5-^tBu₂)₂)₃]I is guided by hydrophobic interactions among the ^tBu groups of adjoining (3,5-^tBu₂C₆H₃CH₂)₂NCS₂^1– ligands from neighboring [Mo₃S₇(S₂CN(CH₂C₆H₃-3,5-^tBu₂)₂)₃]⁺ cations (Fig. 2). The dispersion forces between these numerous hydrocarbon groups enforce an arrangement of [Mo₃S₇(S₂CN(CH₂C₆H₃-3,5-^tBu₂)₂)₃]⁺ cations into sheets in the ab plane and stacking of these cations, one upon another, along the c axis with a separation equal to the c-axis length of 10.9815 (6) Å between adjacent Mo₃ triangles. Interligand π-stacking interactions with the benzyl groups are not effectively made due to the encumbering steric profile of the ^tBu groups.

Figure 2
Cell packing diagram for the [Mo₃S₇(S₂CN(CH₂C₆H₃-3,5-^tBu₂)₂)₃]⁺ cations showing the numerous interligand hydrophobic interactions. The view is down the c axis. All hydrogen atoms are omitted for clarity.

The I⁻ counteranion is positioned on the underside of the [Mo₃S₇(S₂CN(CH₂C₆H₃-3,5-^tBu₂)₂)₃]⁺ cation opposite the μ₃-S²⁻ ligand (S5) (Fig. 3). A pronounced soft, electrophilic character to the S_axial atoms (Fig. 3) provides for close S_ax⋯I⁻ contacts of 3.166 (2) Å, which are considerably below the sum of the van der Waals radii of the two atoms, 1.8 and 2.1 Å, respectively (Batsanov, 2001 ). Other distinctive structural features of [Mo₃S₇(S₂CN(CH₂C₆H₃-3,5-^tBu₂)₂)₃]I are Mo—S_eq bond lengths [2.4847 (16) Å] that are appreciably longer by ∼0.080 Å than the Mo—S_ax [2.4056 (16) Å] bond lengths (Fig. 3), a longer Mo—S_{dithiocarbamate} bond length for the sulfur atom that is anti to the μ₃-S²⁻ ligand [2.5123 (16) Å] compared to the one that is syn [2.4816 (17) Å], and near orthogonality between the Mo₃ plane and the S₂CN chelate of the dithiocarbamate ligand. These parameters are quite similar to those observed in related compounds (Fontenot et al., 2019).

Figure 3
Side view of [Mo₃S₇(S₂CN(CH₂C₆H₃-3,5-^tBu₂)₂)₃]I (50% probability for the displacement ellipsoids) showing the proximity of the I⁻ anion to the S_ax atoms of the μ₂-S₂²⁻ ligands.

In continuing work, we target the deliberate synthesis of hexamolybdenum sulfide clusters by fusion of separate [Mo₃S₇]⁴⁺ and [Mo₃S₄]⁴⁺ fragments.

Synthesis and crystallization

[NH₄]₂[Mo₃S₁₃] and (3,5-^tBu₂–C₆H₃CH₂)₂NC(S)S–SC(S)N(CH₂C₆H₃-3,5-^tBu₂)₂ were reacted in a 1:3 ratio following a procedure detailed earlier (Fontenot et al., 2019). Crystallization was accomplished by layering MeOH onto a solution of the title compound in C₆H₆ and cooling the set-up to −20°C for 48 h.

Refinement

Crystal data, data collection and structure refinement details are summarized in Table 1. The tert-butyl groups defined by C13–C16 and C28–C31 are disordered and were treated with independent, floating site occupancy variables that identified 0.687 (13):0.313 (13) and 0.623 (11):0.377 (11) optimal partitioning, respectively, for the two groups.

Table 1
Experimental details

Crystal data
Chemical formula	[Mo₃(C₃₁H₄₆NS₂)₃S₇]I
M_r	2129.56
Crystal system, space group	Trigonal, P31c
Temperature (K)	150
a, c (Å)	23.6627 (12), 10.9815 (6)
V (Å³)	5325.0 (6)
Z	2
Radiation type	Mo Kα
μ (mm⁻¹)	0.93
Crystal size (mm)	0.38 × 0.16 × 0.13

Data collection
Diffractometer	Bruker SMART APEX CCD
Absorption correction	Multi-scan (SADABS; Krause et al., 2015 )
T_min, T_max	0.799, 0.890
No. of measured, independent and observed [I > 2σ(I)] reflections	89878, 7810, 7053
R_int	0.043
(sin θ/λ)_max (Å⁻¹)	0.641

Refinement
R[F² > 2σ(F²)], wR(F²), S	0.037, 0.104, 1.06
No. of reflections	7810
No. of parameters	369
No. of restraints	35
H-atom treatment	H-atom parameters constrained
Δρ_max, Δρ_min (e Å⁻³)	1.08, −0.54
Absolute structure	Flack x determined using 3209 quotients [(I⁺)−(I⁻)]/[(I⁺)+(I⁻)] (Parsons et al., 2013 )
Absolute structure parameter	0.014 (8)
Computer programs: APEX3 and SAINT (Bruker, 2016 ), SHELXT/5 (Sheldrick, 2015a ), SHELXL2018/3 (Sheldrick, 2015b ) and SHELXTL (Sheldrick, 2008 ).

Structural data

CCDC reference: 2015330

Crystal structure: contains datablocks I, global. DOI: https://doi.org/10.1107/S2414314620009396/pk4027sup1.cif

Structure factors: contains datablock I. DOI: https://doi.org/10.1107/S2414314620009396/pk4027Isup3.hkl

checkCIF report

Computing details top

Data collection: APEX3 (Bruker, 2016); cell refinement: SAINT (Bruker, 2016); data reduction: SAINT (Bruker, 2016); program(s) used to solve structure: SHELXT/5 (Sheldrick, 2015a); program(s) used to refine structure: SHELXL2018/3 (Sheldrick, 2015b); molecular graphics: SHELXTL (Sheldrick, 2008); software used to prepare material for publication: SHELXTL (Sheldrick, 2008).

Tris[N,N-bis(3,5-di-tert-butylbenzyl)dithiocarbamato-κ²S,S']-µ₃-sulfido-tris-µ₂-disulfido-triangulo-trimolybdenum(IV) iodide top

Crystal data top

[Mo₃(C₃₁H₄₆NS₂)₃S₇]I	D_x = 1.328 Mg m⁻³
M_r = 2129.56	Mo Kα radiation, λ = 0.71073 Å
Trigonal, P31c	Cell parameters from 9927 reflections
a = 23.6627 (12) Å	θ = 2.8–27.0°
c = 10.9815 (6) Å	µ = 0.93 mm⁻¹
V = 5325.0 (6) Å³	T = 150 K
Z = 2	Column, yellow-orange
F(000) = 2208	0.38 × 0.16 × 0.13 mm

Data collection top

Bruker SMART APEX CCD diffractometer	7810 independent reflections
Radiation source: fine-focus sealed tube	7053 reflections with I > 2σ(I)
Graphite monochromator	R_int = 0.043
Detector resolution: 8.3333 pixels mm^-1	θ_max = 27.1°, θ_min = 1.7°
φ and ω scans	h = −30→30
Absorption correction: multi-scan (SADABS; Krause et al., 2015)	k = −30→30
T_min = 0.799, T_max = 0.890	l = −14→14
89878 measured reflections

Refinement top

Refinement on F²	Secondary atom site location: difference Fourier map
Least-squares matrix: full	Hydrogen site location: inferred from neighbouring sites
R[F² > 2σ(F²)] = 0.037	H-atom parameters constrained
wR(F²) = 0.104	w = 1/[σ²(F_o²) + (0.0543P)² + 6.2404P] where P = (F_o² + 2F_c²)/3
S = 1.06	(Δ/σ)_max < 0.001
7810 reflections	Δρ_max = 1.08 e Å⁻³
369 parameters	Δρ_min = −0.54 e Å⁻³
35 restraints	Absolute structure: Flack x determined using 3209 quotients [(I⁺)-(I^-)]/[(I⁺)+(I^-)] (Parsons et al., 2013)
Primary atom site location: structure-invariant direct methods	Absolute structure parameter: 0.014 (8)

Special details top

Experimental. The diffraction data were obtained from 3 sets of 400 frames, each of width 0.5° in ω, collected at φ = 0.00, 90.00 and 180.00° and 2 sets of 800 frames, each of width 0.45° in φ, collected at ω = –30.00 and 210.00°. The scan time was 60 sec/frame.

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.

Refinement. Refinement of F² against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F², conventional R-factors R are based on F, with F set to zero for negative F². The threshold expression of F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F² are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. H-atoms attached to carbon were placed in calculated positions (C—H = 0.95 - 0.99 Å). All were included as riding contributions with isotropic displacement parameters 1.2 - 1.5 times those of the attached atoms.

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

	x	y	z	U_iso*/U_eq	Occ. (<1)
I1	0.333333	0.666667	0.90377 (7)	0.04082 (19)
Mo1	0.26950 (2)	0.59847 (2)	0.52052 (5)	0.02818 (12)
S1	0.34151 (8)	0.55022 (7)	0.50720 (16)	0.0357 (3)
S2	0.33840 (7)	0.58992 (7)	0.67175 (15)	0.0319 (3)
S3	0.20057 (8)	0.51946 (8)	0.36144 (15)	0.0376 (3)
S4	0.17377 (8)	0.50221 (8)	0.61825 (15)	0.0367 (3)
S5	0.333333	0.666667	0.3562 (3)	0.0324 (6)
N1	0.0983 (2)	0.4120 (2)	0.4549 (5)	0.0313 (10)
C1	0.1493 (3)	0.4695 (3)	0.4762 (6)	0.0329 (13)
C2	0.0818 (3)	0.3809 (3)	0.3340 (6)	0.0349 (13)
H2A	0.106606	0.413943	0.270705	0.042*
H2B	0.034714	0.362867	0.318052	0.042*
C3	0.0980 (3)	0.3270 (3)	0.3274 (6)	0.0359 (13)
C4	0.0558 (3)	0.2684 (3)	0.2686 (6)	0.0387 (14)
H4	0.015801	0.262103	0.236242	0.046*
C5	0.0710 (4)	0.2194 (3)	0.2564 (7)	0.0448 (16)
C6	0.1312 (4)	0.2316 (4)	0.3071 (7)	0.0500 (18)
H6	0.143434	0.199243	0.297989	0.060*
C7	0.1722 (3)	0.2870 (4)	0.3679 (7)	0.0490 (17)
C8	0.1555 (3)	0.3358 (3)	0.3757 (6)	0.0409 (15)
H8	0.184360	0.375826	0.415063	0.049*
C9	0.0279 (4)	0.1560 (4)	0.1908 (7)	0.059 (2)
C10	−0.0007 (7)	0.1002 (5)	0.2846 (11)	0.158 (9)
H10A	−0.028735	0.058766	0.242989	0.237*
H10B	0.034978	0.098041	0.325727	0.237*
H10C	−0.026364	0.108271	0.344856	0.237*
C11	−0.0264 (5)	0.1557 (5)	0.1227 (11)	0.096 (4)
H11A	−0.052421	0.113449	0.082352	0.144*
H11B	−0.054124	0.163012	0.179441	0.144*
H11C	−0.008584	0.190495	0.061491	0.144*
C12	0.0675 (6)	0.1397 (6)	0.1009 (11)	0.108 (5)
H12A	0.038426	0.098479	0.059666	0.161*
H12B	0.088215	0.174704	0.040398	0.161*
H12C	0.101238	0.135673	0.145355	0.161*
C13A	0.2382 (5)	0.3013 (7)	0.4211 (12)	0.063 (3)	0.687 (13)
C14A	0.2939 (7)	0.3563 (8)	0.3491 (15)	0.089 (5)	0.687 (13)
H14A	0.291089	0.343326	0.263623	0.133*	0.687 (13)
H14B	0.290458	0.395848	0.354580	0.133*	0.687 (13)
H14C	0.335819	0.365089	0.383072	0.133*	0.687 (13)
C15A	0.2454 (9)	0.2409 (8)	0.4133 (18)	0.114 (7)	0.687 (13)
H15A	0.242288	0.227403	0.328066	0.171*	0.687 (13)
H15B	0.287876	0.250929	0.446377	0.171*	0.687 (13)
H15C	0.210561	0.205388	0.460566	0.171*	0.687 (13)
C16A	0.2430 (10)	0.3218 (10)	0.5527 (12)	0.109 (9)	0.687 (13)
H16A	0.207406	0.286758	0.599318	0.163*	0.687 (13)
H16B	0.284964	0.330617	0.586254	0.163*	0.687 (13)
H16C	0.239602	0.361376	0.557762	0.163*	0.687 (13)
C13B	0.2345 (10)	0.2935 (16)	0.426 (2)	0.063 (3)	0.313 (13)
C14B	0.2834 (15)	0.298 (2)	0.330 (3)	0.089 (5)	0.313 (13)
H14D	0.263069	0.258144	0.279677	0.133*	0.313 (13)
H14E	0.296254	0.335955	0.278445	0.133*	0.313 (13)
H14F	0.322046	0.301406	0.370474	0.133*	0.313 (13)
C15B	0.2197 (17)	0.2363 (18)	0.510 (3)	0.114 (7)	0.313 (13)
H15D	0.197541	0.195506	0.463729	0.171*	0.313 (13)
H15E	0.260638	0.241905	0.543413	0.171*	0.313 (13)
H15F	0.191562	0.234837	0.576852	0.171*	0.313 (13)
C16B	0.269 (2)	0.3560 (18)	0.501 (4)	0.109 (9)	0.313 (13)
H16D	0.239241	0.355362	0.564161	0.163*	0.313 (13)
H16E	0.307768	0.359213	0.539869	0.163*	0.313 (13)
H16F	0.281976	0.393762	0.447841	0.163*	0.313 (13)
C17	0.0557 (3)	0.3703 (3)	0.5544 (6)	0.0347 (13)
H17A	0.074882	0.390668	0.633795	0.042*
H17B	0.052960	0.327200	0.551264	0.042*
C18	−0.0116 (3)	0.3613 (3)	0.5439 (6)	0.0342 (13)
C19	−0.0634 (3)	0.3013 (3)	0.5099 (6)	0.0332 (12)
H19	−0.056448	0.265524	0.496737	0.040*
C20	−0.1259 (3)	0.2928 (3)	0.4947 (7)	0.0412 (15)
C21	−0.1349 (3)	0.3460 (4)	0.5215 (9)	0.055 (2)
H21	−0.177392	0.340490	0.515471	0.066*
C22	−0.0829 (4)	0.4066 (3)	0.5568 (11)	0.066 (3)
C23	−0.0215 (3)	0.4128 (3)	0.5669 (8)	0.0485 (18)
H23	0.014534	0.453648	0.590186	0.058*
C24	−0.1834 (3)	0.2258 (4)	0.4600 (7)	0.0456 (17)
C25	−0.2046 (4)	0.1810 (4)	0.5663 (8)	0.057 (2)
H25A	−0.220352	0.198209	0.630869	0.085*
H25B	−0.167545	0.177373	0.596736	0.085*
H25C	−0.239714	0.137779	0.541574	0.085*
C26	−0.2412 (4)	0.2316 (5)	0.4121 (9)	0.065 (2)
H26A	−0.272334	0.190832	0.371604	0.098*
H26B	−0.225367	0.267717	0.353849	0.098*
H26C	−0.262758	0.239912	0.480275	0.098*
C27	−0.1633 (5)	0.1952 (5)	0.3569 (9)	0.065 (2)
H27A	−0.129055	0.186834	0.386317	0.097*
H27B	−0.146708	0.225365	0.287630	0.097*
H27C	−0.201220	0.154079	0.331081	0.097*
C28A	−0.0935 (6)	0.4631 (6)	0.6020 (13)	0.067 (5)	0.623 (11)
C29A	−0.0620 (8)	0.4899 (8)	0.7275 (13)	0.093 (6)	0.623 (11)
H29A	−0.015827	0.502399	0.724929	0.139*	0.623 (11)
H29B	−0.065853	0.528240	0.747614	0.139*	0.623 (11)
H29C	−0.084441	0.456222	0.789649	0.139*	0.623 (11)
C30A	−0.0590 (8)	0.5175 (8)	0.5091 (15)	0.089 (6)	0.623 (11)
H30A	−0.013143	0.528904	0.502718	0.133*	0.623 (11)
H30B	−0.080166	0.502716	0.429608	0.133*	0.623 (11)
H30C	−0.061350	0.555839	0.535113	0.133*	0.623 (11)
C31A	−0.1645 (6)	0.4449 (10)	0.6127 (17)	0.075 (5)	0.623 (11)
H31A	−0.186393	0.409848	0.672707	0.113*	0.623 (11)
H31B	−0.167145	0.483117	0.638956	0.113*	0.623 (11)
H31C	−0.185962	0.429994	0.533451	0.113*	0.623 (11)
C28B	−0.0926 (11)	0.4657 (8)	0.5325 (19)	0.067 (5)	0.377 (11)
C29B	−0.1503 (13)	0.4527 (18)	0.613 (2)	0.093 (6)	0.377 (11)
H29D	−0.141602	0.444973	0.697197	0.139*	0.377 (11)
H29E	−0.156563	0.490635	0.611492	0.139*	0.377 (11)
H29F	−0.189823	0.414213	0.583465	0.139*	0.377 (11)
C30B	−0.0323 (12)	0.5275 (12)	0.577 (3)	0.089 (6)	0.377 (11)
H30D	0.005206	0.536402	0.526147	0.133*	0.377 (11)
H30E	−0.040157	0.564348	0.572735	0.133*	0.377 (11)
H30F	−0.023174	0.521408	0.661902	0.133*	0.377 (11)
C31B	−0.1068 (12)	0.4775 (12)	0.4032 (18)	0.075 (5)	0.377 (11)
H31D	−0.069929	0.485906	0.350528	0.113*	0.377 (11)
H31E	−0.146372	0.438987	0.373704	0.113*	0.377 (11)
H31F	−0.113112	0.515410	0.401730	0.113*	0.377 (11)

Atomic displacement parameters (Å²) top

	U¹¹	U²²	U³³	U¹²	U¹³	U²³
I1	0.0389 (3)	0.0389 (3)	0.0447 (4)	0.01945 (13)	0.000	0.000
Mo1	0.0219 (2)	0.0211 (2)	0.0392 (3)	0.00897 (19)	−0.0007 (2)	−0.0010 (2)
S1	0.0356 (8)	0.0283 (7)	0.0477 (9)	0.0192 (7)	0.0003 (6)	−0.0037 (6)
S2	0.0279 (7)	0.0260 (7)	0.0432 (8)	0.0145 (6)	0.0011 (6)	0.0024 (6)
S3	0.0318 (8)	0.0290 (7)	0.0398 (8)	0.0060 (6)	0.0003 (6)	−0.0005 (6)
S4	0.0302 (7)	0.0291 (7)	0.0381 (8)	0.0054 (6)	−0.0006 (6)	0.0001 (6)
S5	0.0296 (8)	0.0296 (8)	0.0380 (13)	0.0148 (4)	0.000	0.000
N1	0.025 (2)	0.027 (2)	0.037 (3)	0.009 (2)	0.002 (2)	0.002 (2)
C1	0.025 (3)	0.028 (3)	0.043 (3)	0.012 (2)	−0.001 (2)	0.000 (2)
C2	0.032 (3)	0.028 (3)	0.041 (3)	0.012 (3)	−0.004 (2)	−0.002 (2)
C3	0.039 (3)	0.035 (3)	0.035 (3)	0.019 (3)	−0.002 (3)	0.000 (2)
C4	0.042 (4)	0.034 (3)	0.042 (4)	0.020 (3)	−0.002 (3)	0.000 (3)
C5	0.060 (4)	0.033 (3)	0.045 (4)	0.026 (3)	0.005 (3)	0.005 (3)
C6	0.060 (5)	0.048 (4)	0.058 (4)	0.039 (4)	0.009 (4)	0.008 (3)
C7	0.047 (4)	0.056 (5)	0.055 (4)	0.033 (4)	0.005 (3)	0.007 (3)
C8	0.038 (4)	0.043 (4)	0.045 (4)	0.022 (3)	−0.001 (3)	−0.002 (3)
C9	0.086 (6)	0.034 (4)	0.053 (4)	0.027 (4)	0.003 (4)	0.000 (3)
C10	0.22 (2)	0.050 (7)	0.097 (10)	−0.007 (9)	−0.010 (11)	0.009 (7)
C11	0.090 (8)	0.057 (6)	0.135 (10)	0.032 (6)	−0.033 (8)	−0.046 (7)
C12	0.130 (11)	0.124 (11)	0.109 (9)	0.095 (10)	−0.030 (8)	−0.056 (8)
C13A	0.062 (6)	0.092 (8)	0.061 (5)	0.058 (6)	−0.005 (4)	0.003 (5)
C14A	0.044 (7)	0.111 (12)	0.104 (11)	0.033 (9)	0.007 (7)	0.025 (11)
C15A	0.101 (14)	0.144 (16)	0.145 (19)	0.097 (14)	−0.031 (13)	0.001 (16)
C16A	0.115 (18)	0.20 (3)	0.081 (14)	0.13 (2)	−0.037 (12)	−0.038 (13)
C13B	0.062 (6)	0.092 (8)	0.061 (5)	0.058 (6)	−0.005 (4)	0.003 (5)
C14B	0.044 (7)	0.111 (12)	0.104 (11)	0.033 (9)	0.007 (7)	0.025 (11)
C15B	0.101 (14)	0.144 (16)	0.145 (19)	0.097 (14)	−0.031 (13)	0.001 (16)
C16B	0.115 (18)	0.20 (3)	0.081 (14)	0.13 (2)	−0.037 (12)	−0.038 (13)
C17	0.030 (3)	0.025 (3)	0.044 (3)	0.010 (2)	−0.001 (2)	0.004 (2)
C18	0.028 (3)	0.030 (3)	0.044 (3)	0.014 (3)	0.002 (2)	0.007 (3)
C19	0.026 (3)	0.030 (3)	0.044 (3)	0.015 (3)	−0.002 (2)	0.001 (2)
C20	0.028 (3)	0.035 (3)	0.056 (4)	0.012 (3)	−0.007 (3)	0.009 (3)
C21	0.025 (3)	0.038 (4)	0.100 (7)	0.015 (3)	0.001 (4)	0.010 (4)
C22	0.040 (4)	0.031 (4)	0.134 (8)	0.024 (3)	0.004 (5)	0.008 (4)
C23	0.029 (3)	0.032 (3)	0.079 (5)	0.011 (3)	0.001 (3)	0.004 (3)
C24	0.023 (3)	0.044 (4)	0.062 (4)	0.011 (3)	−0.006 (3)	0.012 (3)
C25	0.049 (4)	0.043 (4)	0.057 (5)	0.007 (4)	−0.005 (3)	0.009 (3)
C26	0.037 (4)	0.064 (5)	0.077 (6)	0.012 (4)	−0.016 (4)	0.019 (4)
C27	0.053 (5)	0.054 (5)	0.067 (6)	0.011 (4)	−0.008 (4)	−0.009 (4)
C28A	0.052 (6)	0.039 (5)	0.123 (17)	0.034 (5)	0.009 (10)	0.011 (9)
C29A	0.084 (11)	0.069 (9)	0.144 (17)	0.051 (9)	−0.014 (10)	−0.041 (10)
C30A	0.096 (14)	0.055 (8)	0.131 (19)	0.049 (10)	0.012 (11)	0.028 (11)
C31A	0.091 (11)	0.077 (10)	0.095 (11)	0.070 (10)	0.027 (9)	0.044 (8)
C28B	0.052 (6)	0.039 (5)	0.123 (17)	0.034 (5)	0.009 (10)	0.011 (9)
C29B	0.084 (11)	0.069 (9)	0.144 (17)	0.051 (9)	−0.014 (10)	−0.041 (10)
C30B	0.096 (14)	0.055 (8)	0.131 (19)	0.049 (10)	0.012 (11)	0.028 (11)
C31B	0.091 (11)	0.077 (10)	0.095 (11)	0.070 (10)	0.027 (9)	0.044 (8)

Geometric parameters (Å, º) top

I1—S2	3.1657 (17)	C14B—H14E	0.9800
Mo1—S5	2.389 (2)	C14B—H14F	0.9800
Mo1—S2	2.4056 (16)	C15B—H15D	0.9800
Mo1—S2ⁱ	2.4096 (16)	C15B—H15E	0.9800
Mo1—S1ⁱ	2.4801 (16)	C15B—H15F	0.9800
Mo1—S3	2.4816 (17)	C16B—H16D	0.9800
Mo1—S1	2.4847 (16)	C16B—H16E	0.9800
Mo1—S4	2.5123 (16)	C16B—H16F	0.9800
Mo1—Mo1ⁱⁱ	2.7100 (8)	C17—C18	1.501 (9)
Mo1—Mo1ⁱ	2.7100 (8)	C17—H17A	0.9900
S1—S2	2.055 (2)	C17—H17B	0.9900
S3—C1	1.738 (7)	C18—C23	1.375 (10)
S4—C1	1.708 (7)	C18—C19	1.385 (9)
N1—C1	1.313 (8)	C19—C20	1.399 (9)
N1—C2	1.472 (8)	C19—H19	0.9500
N1—C17	1.479 (8)	C20—C21	1.407 (11)
C2—C3	1.505 (9)	C20—C24	1.535 (10)
C2—H2A	0.9900	C21—C22	1.399 (11)
C2—H2B	0.9900	C21—H21	0.9500
C3—C8	1.376 (10)	C22—C23	1.391 (10)
C3—C4	1.397 (9)	C22—C28A	1.558 (11)
C4—C5	1.381 (9)	C22—C28B	1.548 (12)
C4—H4	0.9500	C23—H23	0.9500
C5—C6	1.419 (11)	C24—C25	1.486 (10)
C5—C9	1.510 (10)	C24—C26	1.533 (10)
C6—C7	1.354 (11)	C24—C27	1.542 (12)
C6—H6	0.9500	C25—H25A	0.9800
C7—C8	1.397 (10)	C25—H25B	0.9800
C7—C13A	1.539 (11)	C25—H25C	0.9800
C7—C13B	1.545 (13)	C26—H26A	0.9800
C8—H8	0.9500	C26—H26B	0.9800
C9—C11	1.483 (10)	C26—H26C	0.9800
C9—C10	1.540 (9)	C27—H27A	0.9800
C9—C12	1.538 (10)	C27—H27B	0.9800
C10—H10A	0.9800	C27—H27C	0.9800
C10—H10B	0.9800	C28A—C31A	1.518 (11)
C10—H10C	0.9800	C28A—C30A	1.520 (11)
C11—H11A	0.9800	C28A—C29A	1.544 (12)
C11—H11B	0.9800	C29A—H29A	0.9800
C11—H11C	0.9800	C29A—H29B	0.9800
C12—H12A	0.9800	C29A—H29C	0.9800
C12—H12B	0.9800	C30A—H30A	0.9800
C12—H12C	0.9800	C30A—H30B	0.9800
C13A—C16A	1.510 (12)	C30A—H30C	0.9800
C13A—C14A	1.531 (12)	C31A—H31A	0.9800
C13A—C15A	1.524 (12)	C31A—H31B	0.9800
C14A—H14A	0.9800	C31A—H31C	0.9800
C14A—H14B	0.9800	C28B—C29B	1.526 (13)
C14A—H14C	0.9800	C28B—C31B	1.518 (13)
C15A—H15A	0.9800	C28B—C30B	1.527 (13)
C15A—H15B	0.9800	C29B—H29D	0.9800
C15A—H15C	0.9800	C29B—H29E	0.9800
C16A—H16A	0.9800	C29B—H29F	0.9800
C16A—H16B	0.9800	C30B—H30D	0.9800
C16A—H16C	0.9800	C30B—H30E	0.9800
C13B—C16B	1.525 (14)	C30B—H30F	0.9800
C13B—C14B	1.534 (14)	C31B—H31D	0.9800
C13B—C15B	1.524 (14)	C31B—H31E	0.9800
C14B—H14D	0.9800	C31B—H31F	0.9800

S5—Mo1—S2	110.63 (5)	H16A—C16A—H16B	109.5
S5—Mo1—S2ⁱ	110.49 (5)	C13A—C16A—H16C	109.5
S2—Mo1—S2ⁱ	85.04 (8)	H16A—C16A—H16C	109.5
S5—Mo1—S1ⁱ	85.44 (4)	H16B—C16A—H16C	109.5
S2—Mo1—S1ⁱ	134.46 (6)	C16B—C13B—C14B	106.8 (12)
S2ⁱ—Mo1—S1ⁱ	49.68 (6)	C16B—C13B—C15B	108.1 (12)
S5—Mo1—S3	86.13 (6)	C14B—C13B—C15B	107.7 (12)
S2—Mo1—S3	129.83 (6)	C16B—C13B—C7	110 (2)
S2ⁱ—Mo1—S3	134.34 (6)	C14B—C13B—C7	111.9 (19)
S1ⁱ—Mo1—S3	92.23 (6)	C15B—C13B—C7	112 (2)
S5—Mo1—S1	85.33 (4)	C13B—C14B—H14D	109.5
S2—Mo1—S1	49.66 (6)	C13B—C14B—H14E	109.5
S2ⁱ—Mo1—S1	134.40 (6)	H14D—C14B—H14E	109.5
S1ⁱ—Mo1—S1	170.77 (7)	C13B—C14B—H14F	109.5
S3—Mo1—S1	87.47 (6)	H14D—C14B—H14F	109.5
S5—Mo1—S4	156.09 (6)	H14E—C14B—H14F	109.5
S2—Mo1—S4	88.32 (5)	C13B—C15B—H15D	109.5
S2ⁱ—Mo1—S4	84.78 (5)	C13B—C15B—H15E	109.5
S1ⁱ—Mo1—S4	91.49 (6)	H15D—C15B—H15E	109.5
S3—Mo1—S4	70.28 (5)	C13B—C15B—H15F	109.5
S1—Mo1—S4	97.08 (5)	H15D—C15B—H15F	109.5
S5—Mo1—Mo1ⁱⁱ	55.44 (4)	H15E—C15B—H15F	109.5
S2—Mo1—Mo1ⁱⁱ	55.82 (4)	C13B—C16B—H16D	109.5
S2ⁱ—Mo1—Mo1ⁱⁱ	96.44 (4)	C13B—C16B—H16E	109.5
S1ⁱ—Mo1—Mo1ⁱⁱ	116.88 (4)	H16D—C16B—H16E	109.5
S3—Mo1—Mo1ⁱⁱ	126.34 (4)	C13B—C16B—H16F	109.5
S1—Mo1—Mo1ⁱⁱ	56.84 (4)	H16D—C16B—H16F	109.5
S4—Mo1—Mo1ⁱⁱ	143.68 (4)	H16E—C16B—H16F	109.5
S5—Mo1—Mo1ⁱ	55.44 (4)	N1—C17—C18	111.0 (5)
S2—Mo1—Mo1ⁱ	96.54 (4)	N1—C17—H17A	109.4
S2ⁱ—Mo1—Mo1ⁱ	55.68 (4)	C18—C17—H17A	109.4
S1ⁱ—Mo1—Mo1ⁱ	57.00 (4)	N1—C17—H17B	109.4
S3—Mo1—Mo1ⁱ	129.44 (4)	C18—C17—H17B	109.4
S1—Mo1—Mo1ⁱ	116.72 (4)	H17A—C17—H17B	108.0
S4—Mo1—Mo1ⁱ	139.31 (4)	C23—C18—C19	120.2 (6)
Mo1ⁱⁱ—Mo1—Mo1ⁱ	60.0	C23—C18—C17	119.9 (6)
S2—S1—Mo1ⁱⁱ	63.38 (6)	C19—C18—C17	119.9 (6)
S2—S1—Mo1	63.17 (6)	C18—C19—C20	120.6 (6)
Mo1ⁱⁱ—S1—Mo1	66.16 (4)	C18—C19—H19	119.7
S1—S2—Mo1	67.17 (6)	C20—C19—H19	119.7
S1—S2—Mo1ⁱⁱ	66.95 (6)	C19—C20—C21	117.9 (6)
Mo1—S2—Mo1ⁱⁱ	68.50 (5)	C19—C20—C24	120.4 (6)
S1—S2—I1	172.02 (8)	C21—C20—C24	121.5 (6)
Mo1—S2—I1	106.60 (5)	C20—C21—C22	121.8 (7)
Mo1ⁱⁱ—S2—I1	106.50 (5)	C20—C21—H21	119.1
C1—S3—Mo1	88.5 (2)	C22—C21—H21	119.1
C1—S4—Mo1	88.2 (2)	C23—C22—C21	117.8 (6)
Mo1ⁱ—S5—Mo1	69.12 (7)	C23—C22—C28A	119.4 (8)
Mo1ⁱ—S5—Mo1ⁱⁱ	69.12 (7)	C21—C22—C28A	122.2 (8)
Mo1—S5—Mo1ⁱⁱ	69.12 (7)	C23—C22—C28B	122.5 (10)
C1—N1—C2	123.7 (5)	C21—C22—C28B	115.3 (11)
C1—N1—C17	121.8 (5)	C18—C23—C22	121.6 (7)
C2—N1—C17	114.3 (5)	C18—C23—H23	119.2
N1—C1—S4	124.1 (5)	C22—C23—H23	119.2
N1—C1—S3	122.9 (5)	C25—C24—C20	110.5 (6)
S4—C1—S3	113.0 (3)	C25—C24—C26	109.7 (6)
N1—C2—C3	110.6 (5)	C20—C24—C26	111.3 (7)
N1—C2—H2A	109.5	C25—C24—C27	108.4 (7)
C3—C2—H2A	109.5	C20—C24—C27	110.1 (6)
N1—C2—H2B	109.5	C26—C24—C27	106.8 (7)
C3—C2—H2B	109.5	C24—C25—H25A	109.5
H2A—C2—H2B	108.1	C24—C25—H25B	109.5
C8—C3—C4	119.4 (6)	H25A—C25—H25B	109.5
C8—C3—C2	120.2 (6)	C24—C25—H25C	109.5
C4—C3—C2	120.4 (6)	H25A—C25—H25C	109.5
C5—C4—C3	121.4 (7)	H25B—C25—H25C	109.5
C5—C4—H4	119.3	C24—C26—H26A	109.5
C3—C4—H4	119.3	C24—C26—H26B	109.5
C4—C5—C6	116.6 (7)	H26A—C26—H26B	109.5
C4—C5—C9	123.4 (7)	C24—C26—H26C	109.5
C6—C5—C9	120.0 (7)	H26A—C26—H26C	109.5
C7—C6—C5	123.4 (7)	H26B—C26—H26C	109.5
C7—C6—H6	118.3	C24—C27—H27A	109.5
C5—C6—H6	118.3	C24—C27—H27B	109.5
C6—C7—C8	118.0 (7)	H27A—C27—H27B	109.5
C6—C7—C13A	123.8 (8)	C24—C27—H27C	109.5
C8—C7—C13A	118.1 (8)	H27A—C27—H27C	109.5
C6—C7—C13B	119.1 (14)	H27B—C27—H27C	109.5
C8—C7—C13B	122.9 (14)	C31A—C28A—C30A	110.0 (9)
C3—C8—C7	121.1 (6)	C31A—C28A—C29A	106.5 (10)
C3—C8—H8	119.4	C30A—C28A—C29A	107.8 (10)
C7—C8—H8	119.4	C31A—C28A—C22	114.3 (12)
C5—C9—C11	113.5 (7)	C30A—C28A—C22	105.3 (10)
C5—C9—C10	108.7 (7)	C29A—C28A—C22	112.7 (10)
C11—C9—C10	109.0 (8)	C28A—C29A—H29A	109.5
C5—C9—C12	111.2 (8)	C28A—C29A—H29B	109.5
C11—C9—C12	108.1 (7)	H29A—C29A—H29B	109.5
C10—C9—C12	106.0 (8)	C28A—C29A—H29C	109.5
C9—C10—H10A	109.5	H29A—C29A—H29C	109.5
C9—C10—H10B	109.5	H29B—C29A—H29C	109.5
H10A—C10—H10B	109.5	C28A—C30A—H30A	109.5
C9—C10—H10C	109.5	C28A—C30A—H30B	109.5
H10A—C10—H10C	109.5	H30A—C30A—H30B	109.5
H10B—C10—H10C	109.5	C28A—C30A—H30C	109.5
C9—C11—H11A	109.5	H30A—C30A—H30C	109.5
C9—C11—H11B	109.5	H30B—C30A—H30C	109.5
H11A—C11—H11B	109.5	C28A—C31A—H31A	109.5
C9—C11—H11C	109.5	C28A—C31A—H31B	109.5
H11A—C11—H11C	109.5	H31A—C31A—H31B	109.5
H11B—C11—H11C	109.5	C28A—C31A—H31C	109.5
C9—C12—H12A	109.5	H31A—C31A—H31C	109.5
C9—C12—H12B	109.5	H31B—C31A—H31C	109.5
H12A—C12—H12B	109.5	C29B—C28B—C31B	108.9 (12)
C9—C12—H12C	109.5	C29B—C28B—C30B	108.6 (12)
H12A—C12—H12C	109.5	C31B—C28B—C30B	108.1 (11)
H12B—C12—H12C	109.5	C29B—C28B—C22	104 (2)
C16A—C13A—C14A	109.0 (10)	C31B—C28B—C22	118.3 (15)
C16A—C13A—C15A	109.3 (10)	C30B—C28B—C22	108.7 (16)
C14A—C13A—C15A	108.5 (10)	C28B—C29B—H29D	109.5
C16A—C13A—C7	109.8 (11)	C28B—C29B—H29E	109.5
C14A—C13A—C7	109.7 (10)	H29D—C29B—H29E	109.5
C15A—C13A—C7	110.5 (11)	C28B—C29B—H29F	109.5
C13A—C14A—H14A	109.5	H29D—C29B—H29F	109.5
C13A—C14A—H14B	109.5	H29E—C29B—H29F	109.5
H14A—C14A—H14B	109.5	C28B—C30B—H30D	109.5
C13A—C14A—H14C	109.5	C28B—C30B—H30E	109.5
H14A—C14A—H14C	109.5	H30D—C30B—H30E	109.5
H14B—C14A—H14C	109.5	C28B—C30B—H30F	109.5
C13A—C15A—H15A	109.5	H30D—C30B—H30F	109.5
C13A—C15A—H15B	109.5	H30E—C30B—H30F	109.5
H15A—C15A—H15B	109.5	C28B—C31B—H31D	109.5
C13A—C15A—H15C	109.5	C28B—C31B—H31E	109.5
H15A—C15A—H15C	109.5	H31D—C31B—H31E	109.5
H15B—C15A—H15C	109.5	C28B—C31B—H31F	109.5
C13A—C16A—H16A	109.5	H31D—C31B—H31F	109.5
C13A—C16A—H16B	109.5	H31E—C31B—H31F	109.5

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

Acknowledgements

This work was supported in part by the NSF (DMR 1460637). The Louisiana Board of Regents is thanked for enhancement grant LEQSF–(2002–03)–ENH–TR–67 with which Tulane University's Bruker SMART APEX CCD X-ray diffractometer was purchased. Tulane University is acknowledged for its ongoing support with operational costs for the diffraction facility.

Funding information

Funding for this research was provided by: National Science Foundation, Directorate for Mathematical and Physical Sciences (grant No. DMR 1460637); Louisiana Board of Regents (grant No. LEQSF-(2002-03)-ENH-TR-67).

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