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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.

Supporting information

cif

Crystallographic Information File (CIF) https://doi.org/10.1107/S2414314620009396/pk4027sup1.cif
Contains datablocks I, global

hkl

Structure factor file (CIF format) https://doi.org/10.1107/S2414314620009396/pk4027Isup3.hkl
Contains datablock I

CCDC reference: 2015330

Key indicators

  • Single-crystal X-ray study
  • T = 150 K
  • Mean [sigma](C-C) = 0.012 Å
  • Disorder in main residue
  • R factor = 0.037
  • wR factor = 0.104
  • Data-to-parameter ratio = 21.2

checkCIF/PLATON results

No syntax errors found



Alert level A PLAT431_ALERT_2_A Short Inter HL..A Contact I1 ..S2 . 3.17 Ang. x,y,z = 1_555 Check
Author Response: As noted in the discussion, the short iodide-sulfur contact is typical for this type of cluster and arises from a pronounced electrophilic character to the axial sulfur atoms of the bridging disulfide ligands. As noted, some covalency is implied but not easily quantified in this context. The close contact is not a spurious observation and has been treated appropriately.
PLAT431_ALERT_2_A Short Inter HL..A Contact  I1       ..S2       .       3.17 Ang.
                                                1-y,1+x-y,z  =      2_665 Check
Author Response: As noted in the discussion, the short iodide-sulfur contact is typical for this type of cluster and arises from a pronounced electrophilic character to the axial sulfur atoms of the bridging disulfide ligands. As noted, some covalency is implied but not easily quantified in this context. The close contact is not a spurious observation and has been treated appropriately.
PLAT431_ALERT_2_A Short Inter HL..A Contact  I1       ..S2       .       3.17 Ang.
                                                 -x+y,1-x,z  =      3_565 Check
Author Response: As noted in the discussion, the short iodide-sulfur contact is typical for this type of cluster and arises from a pronounced electrophilic character to the axial sulfur atoms of the bridging disulfide ligands. As noted, some covalency is implied but not easily quantified in this context. The close contact is not a spurious observation and has been treated appropriately.

Alert level C PLAT220_ALERT_2_C NonSolvent Resd 1 C Ueq(max)/Ueq(min) Range 4.8 Ratio PLAT222_ALERT_3_C NonSolvent Resd 1 H Uiso(max)/Uiso(min) Range 5.9 Ratio PLAT242_ALERT_2_C Low 'MainMol' Ueq as Compared to Neighbors of C9 Check PLAT342_ALERT_3_C Low Bond Precision on C-C Bonds ............... 0.01191 Ang. PLAT911_ALERT_3_C Missing FCF Refl Between Thmin & STh/L= 0.600 2 Report PLAT978_ALERT_2_C Number C-C Bonds with Positive Residual Density. 0 Info
Alert level G CHEMS02_ALERT_1_G Please check that you have entered the correct _publ_requested_category classification of your compound; FI or CI or EI for inorganic; FM or CM or EM for metal-organic; FO or CO or EO for organic. From the CIF: _publ_requested_category FI From the CIF: _chemical_formula_sum:C93 H138 I1 Mo3 N3 S13 PLAT002_ALERT_2_G Number of Distance or Angle Restraints on AtSite 22 Note PLAT083_ALERT_2_G SHELXL Second Parameter in WGHT Unusually Large 6.24 Why ? PLAT171_ALERT_4_G The CIF-Embedded .res File Contains EADP Records 8 Report PLAT172_ALERT_4_G The CIF-Embedded .res File Contains DFIX Records 11 Report PLAT301_ALERT_3_G Main Residue Disorder ..............(Resd 1 ) 21% Note PLAT304_ALERT_4_G Non-Integer Number of Atoms in ..... (Resd 2 ) 0.33 Check PLAT860_ALERT_3_G Number of Least-Squares Restraints ............. 35 Note PLAT910_ALERT_3_G Missing # of FCF Reflection(s) Below Theta(Min). 1 Note PLAT912_ALERT_4_G Missing # of FCF Reflections Above STh/L= 0.600 5 Note PLAT933_ALERT_2_G Number of OMIT Records in Embedded .res File ... 4 Note
3 ALERT level A = Most likely a serious problem - resolve or explain 0 ALERT level B = A potentially serious problem, consider carefully 6 ALERT level C = Check. Ensure it is not caused by an omission or oversight 11 ALERT level G = General information/check it is not something unexpected 1 ALERT type 1 CIF construction/syntax error, inconsistent or missing data 9 ALERT type 2 Indicator that the structure model may be wrong or deficient 6 ALERT type 3 Indicator that the structure quality may be low 4 ALERT type 4 Improvement, methodology, query or suggestion 0 ALERT type 5 Informative message, check

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]IDx = 1.328 Mg m3
Mr = 2129.56Mo Kα radiation, λ = 0.71073 Å
Trigonal, P31cCell parameters from 9927 reflections
a = 23.6627 (12) Åθ = 2.8–27.0°
c = 10.9815 (6) ŵ = 0.93 mm1
V = 5325.0 (6) Å3T = 150 K
Z = 2Column, yellow-orange
F(000) = 22080.38 × 0.16 × 0.13 mm
Data collection top
Bruker SMART APEX CCD
diffractometer
7810 independent reflections
Radiation source: fine-focus sealed tube7053 reflections with I > 2σ(I)
Graphite monochromatorRint = 0.043
Detector resolution: 8.3333 pixels mm-1θmax = 27.1°, θmin = 1.7°
φ and ω scansh = 3030
Absorption correction: multi-scan
(SADABS; Krause et al., 2015)
k = 3030
Tmin = 0.799, Tmax = 0.890l = 1414
89878 measured reflections
Refinement top
Refinement on F2Secondary atom site location: difference Fourier map
Least-squares matrix: fullHydrogen site location: inferred from neighbouring sites
R[F2 > 2σ(F2)] = 0.037H-atom parameters constrained
wR(F2) = 0.104 w = 1/[σ2(Fo2) + (0.0543P)2 + 6.2404P]
where P = (Fo2 + 2Fc2)/3
S = 1.06(Δ/σ)max < 0.001
7810 reflectionsΔρmax = 1.08 e Å3
369 parametersΔρmin = 0.54 e Å3
35 restraintsAbsolute structure: Flack x determined using 3209 quotients [(I+)-(I-)]/[(I+)+(I-)] (Parsons et al., 2013)
Primary atom site location: structure-invariant direct methodsAbsolute 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
xyzUiso*/UeqOcc. (<1)
I10.3333330.6666670.90377 (7)0.04082 (19)
Mo10.26950 (2)0.59847 (2)0.52052 (5)0.02818 (12)
S10.34151 (8)0.55022 (7)0.50720 (16)0.0357 (3)
S20.33840 (7)0.58992 (7)0.67175 (15)0.0319 (3)
S30.20057 (8)0.51946 (8)0.36144 (15)0.0376 (3)
S40.17377 (8)0.50221 (8)0.61825 (15)0.0367 (3)
S50.3333330.6666670.3562 (3)0.0324 (6)
N10.0983 (2)0.4120 (2)0.4549 (5)0.0313 (10)
C10.1493 (3)0.4695 (3)0.4762 (6)0.0329 (13)
C20.0818 (3)0.3809 (3)0.3340 (6)0.0349 (13)
H2A0.1066060.4139430.2707050.042*
H2B0.0347140.3628670.3180520.042*
C30.0980 (3)0.3270 (3)0.3274 (6)0.0359 (13)
C40.0558 (3)0.2684 (3)0.2686 (6)0.0387 (14)
H40.0158010.2621030.2362420.046*
C50.0710 (4)0.2194 (3)0.2564 (7)0.0448 (16)
C60.1312 (4)0.2316 (4)0.3071 (7)0.0500 (18)
H60.1434340.1992430.2979890.060*
C70.1722 (3)0.2870 (4)0.3679 (7)0.0490 (17)
C80.1555 (3)0.3358 (3)0.3757 (6)0.0409 (15)
H80.1843600.3758260.4150630.049*
C90.0279 (4)0.1560 (4)0.1908 (7)0.059 (2)
C100.0007 (7)0.1002 (5)0.2846 (11)0.158 (9)
H10A0.0287350.0587660.2429890.237*
H10B0.0349780.0980410.3257270.237*
H10C0.0263640.1082710.3448560.237*
C110.0264 (5)0.1557 (5)0.1227 (11)0.096 (4)
H11A0.0524210.1134490.0823520.144*
H11B0.0541240.1630120.1794410.144*
H11C0.0085840.1904950.0614910.144*
C120.0675 (6)0.1397 (6)0.1009 (11)0.108 (5)
H12A0.0384260.0984790.0596660.161*
H12B0.0882150.1747040.0403980.161*
H12C0.1012380.1356730.1453550.161*
C13A0.2382 (5)0.3013 (7)0.4211 (12)0.063 (3)0.687 (13)
C14A0.2939 (7)0.3563 (8)0.3491 (15)0.089 (5)0.687 (13)
H14A0.2910890.3433260.2636230.133*0.687 (13)
H14B0.2904580.3958480.3545800.133*0.687 (13)
H14C0.3358190.3650890.3830720.133*0.687 (13)
C15A0.2454 (9)0.2409 (8)0.4133 (18)0.114 (7)0.687 (13)
H15A0.2422880.2274030.3280660.171*0.687 (13)
H15B0.2878760.2509290.4463770.171*0.687 (13)
H15C0.2105610.2053880.4605660.171*0.687 (13)
C16A0.2430 (10)0.3218 (10)0.5527 (12)0.109 (9)0.687 (13)
H16A0.2074060.2867580.5993180.163*0.687 (13)
H16B0.2849640.3306170.5862540.163*0.687 (13)
H16C0.2396020.3613760.5577620.163*0.687 (13)
C13B0.2345 (10)0.2935 (16)0.426 (2)0.063 (3)0.313 (13)
C14B0.2834 (15)0.298 (2)0.330 (3)0.089 (5)0.313 (13)
H14D0.2630690.2581440.2796770.133*0.313 (13)
H14E0.2962540.3359550.2784450.133*0.313 (13)
H14F0.3220460.3014060.3704740.133*0.313 (13)
C15B0.2197 (17)0.2363 (18)0.510 (3)0.114 (7)0.313 (13)
H15D0.1975410.1955060.4637290.171*0.313 (13)
H15E0.2606380.2419050.5434130.171*0.313 (13)
H15F0.1915620.2348370.5768520.171*0.313 (13)
C16B0.269 (2)0.3560 (18)0.501 (4)0.109 (9)0.313 (13)
H16D0.2392410.3553620.5641610.163*0.313 (13)
H16E0.3077680.3592130.5398690.163*0.313 (13)
H16F0.2819760.3937620.4478410.163*0.313 (13)
C170.0557 (3)0.3703 (3)0.5544 (6)0.0347 (13)
H17A0.0748820.3906680.6337950.042*
H17B0.0529600.3272000.5512640.042*
C180.0116 (3)0.3613 (3)0.5439 (6)0.0342 (13)
C190.0634 (3)0.3013 (3)0.5099 (6)0.0332 (12)
H190.0564480.2655240.4967370.040*
C200.1259 (3)0.2928 (3)0.4947 (7)0.0412 (15)
C210.1349 (3)0.3460 (4)0.5215 (9)0.055 (2)
H210.1773920.3404900.5154710.066*
C220.0829 (4)0.4066 (3)0.5568 (11)0.066 (3)
C230.0215 (3)0.4128 (3)0.5669 (8)0.0485 (18)
H230.0145340.4536480.5901860.058*
C240.1834 (3)0.2258 (4)0.4600 (7)0.0456 (17)
C250.2046 (4)0.1810 (4)0.5663 (8)0.057 (2)
H25A0.2203520.1982090.6308690.085*
H25B0.1675450.1773730.5967360.085*
H25C0.2397140.1377790.5415740.085*
C260.2412 (4)0.2316 (5)0.4121 (9)0.065 (2)
H26A0.2723340.1908320.3716040.098*
H26B0.2253670.2677170.3538490.098*
H26C0.2627580.2399120.4802750.098*
C270.1633 (5)0.1952 (5)0.3569 (9)0.065 (2)
H27A0.1290550.1868340.3863170.097*
H27B0.1467080.2253650.2876300.097*
H27C0.2012200.1540790.3310810.097*
C28A0.0935 (6)0.4631 (6)0.6020 (13)0.067 (5)0.623 (11)
C29A0.0620 (8)0.4899 (8)0.7275 (13)0.093 (6)0.623 (11)
H29A0.0158270.5023990.7249290.139*0.623 (11)
H29B0.0658530.5282400.7476140.139*0.623 (11)
H29C0.0844410.4562220.7896490.139*0.623 (11)
C30A0.0590 (8)0.5175 (8)0.5091 (15)0.089 (6)0.623 (11)
H30A0.0131430.5289040.5027180.133*0.623 (11)
H30B0.0801660.5027160.4296080.133*0.623 (11)
H30C0.0613500.5558390.5351130.133*0.623 (11)
C31A0.1645 (6)0.4449 (10)0.6127 (17)0.075 (5)0.623 (11)
H31A0.1863930.4098480.6727070.113*0.623 (11)
H31B0.1671450.4831170.6389560.113*0.623 (11)
H31C0.1859620.4299940.5334510.113*0.623 (11)
C28B0.0926 (11)0.4657 (8)0.5325 (19)0.067 (5)0.377 (11)
C29B0.1503 (13)0.4527 (18)0.613 (2)0.093 (6)0.377 (11)
H29D0.1416020.4449730.6971970.139*0.377 (11)
H29E0.1565630.4906350.6114920.139*0.377 (11)
H29F0.1898230.4142130.5834650.139*0.377 (11)
C30B0.0323 (12)0.5275 (12)0.577 (3)0.089 (6)0.377 (11)
H30D0.0052060.5364020.5261470.133*0.377 (11)
H30E0.0401570.5643480.5727350.133*0.377 (11)
H30F0.0231740.5214080.6619020.133*0.377 (11)
C31B0.1068 (12)0.4775 (12)0.4032 (18)0.075 (5)0.377 (11)
H31D0.0699290.4859060.3505280.113*0.377 (11)
H31E0.1463720.4389870.3737040.113*0.377 (11)
H31F0.1131120.5154100.4017300.113*0.377 (11)
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
I10.0389 (3)0.0389 (3)0.0447 (4)0.01945 (13)0.0000.000
Mo10.0219 (2)0.0211 (2)0.0392 (3)0.00897 (19)0.0007 (2)0.0010 (2)
S10.0356 (8)0.0283 (7)0.0477 (9)0.0192 (7)0.0003 (6)0.0037 (6)
S20.0279 (7)0.0260 (7)0.0432 (8)0.0145 (6)0.0011 (6)0.0024 (6)
S30.0318 (8)0.0290 (7)0.0398 (8)0.0060 (6)0.0003 (6)0.0005 (6)
S40.0302 (7)0.0291 (7)0.0381 (8)0.0054 (6)0.0006 (6)0.0001 (6)
S50.0296 (8)0.0296 (8)0.0380 (13)0.0148 (4)0.0000.000
N10.025 (2)0.027 (2)0.037 (3)0.009 (2)0.002 (2)0.002 (2)
C10.025 (3)0.028 (3)0.043 (3)0.012 (2)0.001 (2)0.000 (2)
C20.032 (3)0.028 (3)0.041 (3)0.012 (3)0.004 (2)0.002 (2)
C30.039 (3)0.035 (3)0.035 (3)0.019 (3)0.002 (3)0.000 (2)
C40.042 (4)0.034 (3)0.042 (4)0.020 (3)0.002 (3)0.000 (3)
C50.060 (4)0.033 (3)0.045 (4)0.026 (3)0.005 (3)0.005 (3)
C60.060 (5)0.048 (4)0.058 (4)0.039 (4)0.009 (4)0.008 (3)
C70.047 (4)0.056 (5)0.055 (4)0.033 (4)0.005 (3)0.007 (3)
C80.038 (4)0.043 (4)0.045 (4)0.022 (3)0.001 (3)0.002 (3)
C90.086 (6)0.034 (4)0.053 (4)0.027 (4)0.003 (4)0.000 (3)
C100.22 (2)0.050 (7)0.097 (10)0.007 (9)0.010 (11)0.009 (7)
C110.090 (8)0.057 (6)0.135 (10)0.032 (6)0.033 (8)0.046 (7)
C120.130 (11)0.124 (11)0.109 (9)0.095 (10)0.030 (8)0.056 (8)
C13A0.062 (6)0.092 (8)0.061 (5)0.058 (6)0.005 (4)0.003 (5)
C14A0.044 (7)0.111 (12)0.104 (11)0.033 (9)0.007 (7)0.025 (11)
C15A0.101 (14)0.144 (16)0.145 (19)0.097 (14)0.031 (13)0.001 (16)
C16A0.115 (18)0.20 (3)0.081 (14)0.13 (2)0.037 (12)0.038 (13)
C13B0.062 (6)0.092 (8)0.061 (5)0.058 (6)0.005 (4)0.003 (5)
C14B0.044 (7)0.111 (12)0.104 (11)0.033 (9)0.007 (7)0.025 (11)
C15B0.101 (14)0.144 (16)0.145 (19)0.097 (14)0.031 (13)0.001 (16)
C16B0.115 (18)0.20 (3)0.081 (14)0.13 (2)0.037 (12)0.038 (13)
C170.030 (3)0.025 (3)0.044 (3)0.010 (2)0.001 (2)0.004 (2)
C180.028 (3)0.030 (3)0.044 (3)0.014 (3)0.002 (2)0.007 (3)
C190.026 (3)0.030 (3)0.044 (3)0.015 (3)0.002 (2)0.001 (2)
C200.028 (3)0.035 (3)0.056 (4)0.012 (3)0.007 (3)0.009 (3)
C210.025 (3)0.038 (4)0.100 (7)0.015 (3)0.001 (4)0.010 (4)
C220.040 (4)0.031 (4)0.134 (8)0.024 (3)0.004 (5)0.008 (4)
C230.029 (3)0.032 (3)0.079 (5)0.011 (3)0.001 (3)0.004 (3)
C240.023 (3)0.044 (4)0.062 (4)0.011 (3)0.006 (3)0.012 (3)
C250.049 (4)0.043 (4)0.057 (5)0.007 (4)0.005 (3)0.009 (3)
C260.037 (4)0.064 (5)0.077 (6)0.012 (4)0.016 (4)0.019 (4)
C270.053 (5)0.054 (5)0.067 (6)0.011 (4)0.008 (4)0.009 (4)
C28A0.052 (6)0.039 (5)0.123 (17)0.034 (5)0.009 (10)0.011 (9)
C29A0.084 (11)0.069 (9)0.144 (17)0.051 (9)0.014 (10)0.041 (10)
C30A0.096 (14)0.055 (8)0.131 (19)0.049 (10)0.012 (11)0.028 (11)
C31A0.091 (11)0.077 (10)0.095 (11)0.070 (10)0.027 (9)0.044 (8)
C28B0.052 (6)0.039 (5)0.123 (17)0.034 (5)0.009 (10)0.011 (9)
C29B0.084 (11)0.069 (9)0.144 (17)0.051 (9)0.014 (10)0.041 (10)
C30B0.096 (14)0.055 (8)0.131 (19)0.049 (10)0.012 (11)0.028 (11)
C31B0.091 (11)0.077 (10)0.095 (11)0.070 (10)0.027 (9)0.044 (8)
Geometric parameters (Å, º) top
I1—S23.1657 (17)C14B—H14E0.9800
Mo1—S52.389 (2)C14B—H14F0.9800
Mo1—S22.4056 (16)C15B—H15D0.9800
Mo1—S2i2.4096 (16)C15B—H15E0.9800
Mo1—S1i2.4801 (16)C15B—H15F0.9800
Mo1—S32.4816 (17)C16B—H16D0.9800
Mo1—S12.4847 (16)C16B—H16E0.9800
Mo1—S42.5123 (16)C16B—H16F0.9800
Mo1—Mo1ii2.7100 (8)C17—C181.501 (9)
Mo1—Mo1i2.7100 (8)C17—H17A0.9900
S1—S22.055 (2)C17—H17B0.9900
S3—C11.738 (7)C18—C231.375 (10)
S4—C11.708 (7)C18—C191.385 (9)
N1—C11.313 (8)C19—C201.399 (9)
N1—C21.472 (8)C19—H190.9500
N1—C171.479 (8)C20—C211.407 (11)
C2—C31.505 (9)C20—C241.535 (10)
C2—H2A0.9900C21—C221.399 (11)
C2—H2B0.9900C21—H210.9500
C3—C81.376 (10)C22—C231.391 (10)
C3—C41.397 (9)C22—C28A1.558 (11)
C4—C51.381 (9)C22—C28B1.548 (12)
C4—H40.9500C23—H230.9500
C5—C61.419 (11)C24—C251.486 (10)
C5—C91.510 (10)C24—C261.533 (10)
C6—C71.354 (11)C24—C271.542 (12)
C6—H60.9500C25—H25A0.9800
C7—C81.397 (10)C25—H25B0.9800
C7—C13A1.539 (11)C25—H25C0.9800
C7—C13B1.545 (13)C26—H26A0.9800
C8—H80.9500C26—H26B0.9800
C9—C111.483 (10)C26—H26C0.9800
C9—C101.540 (9)C27—H27A0.9800
C9—C121.538 (10)C27—H27B0.9800
C10—H10A0.9800C27—H27C0.9800
C10—H10B0.9800C28A—C31A1.518 (11)
C10—H10C0.9800C28A—C30A1.520 (11)
C11—H11A0.9800C28A—C29A1.544 (12)
C11—H11B0.9800C29A—H29A0.9800
C11—H11C0.9800C29A—H29B0.9800
C12—H12A0.9800C29A—H29C0.9800
C12—H12B0.9800C30A—H30A0.9800
C12—H12C0.9800C30A—H30B0.9800
C13A—C16A1.510 (12)C30A—H30C0.9800
C13A—C14A1.531 (12)C31A—H31A0.9800
C13A—C15A1.524 (12)C31A—H31B0.9800
C14A—H14A0.9800C31A—H31C0.9800
C14A—H14B0.9800C28B—C29B1.526 (13)
C14A—H14C0.9800C28B—C31B1.518 (13)
C15A—H15A0.9800C28B—C30B1.527 (13)
C15A—H15B0.9800C29B—H29D0.9800
C15A—H15C0.9800C29B—H29E0.9800
C16A—H16A0.9800C29B—H29F0.9800
C16A—H16B0.9800C30B—H30D0.9800
C16A—H16C0.9800C30B—H30E0.9800
C13B—C16B1.525 (14)C30B—H30F0.9800
C13B—C14B1.534 (14)C31B—H31D0.9800
C13B—C15B1.524 (14)C31B—H31E0.9800
C14B—H14D0.9800C31B—H31F0.9800
S5—Mo1—S2110.63 (5)H16A—C16A—H16B109.5
S5—Mo1—S2i110.49 (5)C13A—C16A—H16C109.5
S2—Mo1—S2i85.04 (8)H16A—C16A—H16C109.5
S5—Mo1—S1i85.44 (4)H16B—C16A—H16C109.5
S2—Mo1—S1i134.46 (6)C16B—C13B—C14B106.8 (12)
S2i—Mo1—S1i49.68 (6)C16B—C13B—C15B108.1 (12)
S5—Mo1—S386.13 (6)C14B—C13B—C15B107.7 (12)
S2—Mo1—S3129.83 (6)C16B—C13B—C7110 (2)
S2i—Mo1—S3134.34 (6)C14B—C13B—C7111.9 (19)
S1i—Mo1—S392.23 (6)C15B—C13B—C7112 (2)
S5—Mo1—S185.33 (4)C13B—C14B—H14D109.5
S2—Mo1—S149.66 (6)C13B—C14B—H14E109.5
S2i—Mo1—S1134.40 (6)H14D—C14B—H14E109.5
S1i—Mo1—S1170.77 (7)C13B—C14B—H14F109.5
S3—Mo1—S187.47 (6)H14D—C14B—H14F109.5
S5—Mo1—S4156.09 (6)H14E—C14B—H14F109.5
S2—Mo1—S488.32 (5)C13B—C15B—H15D109.5
S2i—Mo1—S484.78 (5)C13B—C15B—H15E109.5
S1i—Mo1—S491.49 (6)H15D—C15B—H15E109.5
S3—Mo1—S470.28 (5)C13B—C15B—H15F109.5
S1—Mo1—S497.08 (5)H15D—C15B—H15F109.5
S5—Mo1—Mo1ii55.44 (4)H15E—C15B—H15F109.5
S2—Mo1—Mo1ii55.82 (4)C13B—C16B—H16D109.5
S2i—Mo1—Mo1ii96.44 (4)C13B—C16B—H16E109.5
S1i—Mo1—Mo1ii116.88 (4)H16D—C16B—H16E109.5
S3—Mo1—Mo1ii126.34 (4)C13B—C16B—H16F109.5
S1—Mo1—Mo1ii56.84 (4)H16D—C16B—H16F109.5
S4—Mo1—Mo1ii143.68 (4)H16E—C16B—H16F109.5
S5—Mo1—Mo1i55.44 (4)N1—C17—C18111.0 (5)
S2—Mo1—Mo1i96.54 (4)N1—C17—H17A109.4
S2i—Mo1—Mo1i55.68 (4)C18—C17—H17A109.4
S1i—Mo1—Mo1i57.00 (4)N1—C17—H17B109.4
S3—Mo1—Mo1i129.44 (4)C18—C17—H17B109.4
S1—Mo1—Mo1i116.72 (4)H17A—C17—H17B108.0
S4—Mo1—Mo1i139.31 (4)C23—C18—C19120.2 (6)
Mo1ii—Mo1—Mo1i60.0C23—C18—C17119.9 (6)
S2—S1—Mo1ii63.38 (6)C19—C18—C17119.9 (6)
S2—S1—Mo163.17 (6)C18—C19—C20120.6 (6)
Mo1ii—S1—Mo166.16 (4)C18—C19—H19119.7
S1—S2—Mo167.17 (6)C20—C19—H19119.7
S1—S2—Mo1ii66.95 (6)C19—C20—C21117.9 (6)
Mo1—S2—Mo1ii68.50 (5)C19—C20—C24120.4 (6)
S1—S2—I1172.02 (8)C21—C20—C24121.5 (6)
Mo1—S2—I1106.60 (5)C20—C21—C22121.8 (7)
Mo1ii—S2—I1106.50 (5)C20—C21—H21119.1
C1—S3—Mo188.5 (2)C22—C21—H21119.1
C1—S4—Mo188.2 (2)C23—C22—C21117.8 (6)
Mo1i—S5—Mo169.12 (7)C23—C22—C28A119.4 (8)
Mo1i—S5—Mo1ii69.12 (7)C21—C22—C28A122.2 (8)
Mo1—S5—Mo1ii69.12 (7)C23—C22—C28B122.5 (10)
C1—N1—C2123.7 (5)C21—C22—C28B115.3 (11)
C1—N1—C17121.8 (5)C18—C23—C22121.6 (7)
C2—N1—C17114.3 (5)C18—C23—H23119.2
N1—C1—S4124.1 (5)C22—C23—H23119.2
N1—C1—S3122.9 (5)C25—C24—C20110.5 (6)
S4—C1—S3113.0 (3)C25—C24—C26109.7 (6)
N1—C2—C3110.6 (5)C20—C24—C26111.3 (7)
N1—C2—H2A109.5C25—C24—C27108.4 (7)
C3—C2—H2A109.5C20—C24—C27110.1 (6)
N1—C2—H2B109.5C26—C24—C27106.8 (7)
C3—C2—H2B109.5C24—C25—H25A109.5
H2A—C2—H2B108.1C24—C25—H25B109.5
C8—C3—C4119.4 (6)H25A—C25—H25B109.5
C8—C3—C2120.2 (6)C24—C25—H25C109.5
C4—C3—C2120.4 (6)H25A—C25—H25C109.5
C5—C4—C3121.4 (7)H25B—C25—H25C109.5
C5—C4—H4119.3C24—C26—H26A109.5
C3—C4—H4119.3C24—C26—H26B109.5
C4—C5—C6116.6 (7)H26A—C26—H26B109.5
C4—C5—C9123.4 (7)C24—C26—H26C109.5
C6—C5—C9120.0 (7)H26A—C26—H26C109.5
C7—C6—C5123.4 (7)H26B—C26—H26C109.5
C7—C6—H6118.3C24—C27—H27A109.5
C5—C6—H6118.3C24—C27—H27B109.5
C6—C7—C8118.0 (7)H27A—C27—H27B109.5
C6—C7—C13A123.8 (8)C24—C27—H27C109.5
C8—C7—C13A118.1 (8)H27A—C27—H27C109.5
C6—C7—C13B119.1 (14)H27B—C27—H27C109.5
C8—C7—C13B122.9 (14)C31A—C28A—C30A110.0 (9)
C3—C8—C7121.1 (6)C31A—C28A—C29A106.5 (10)
C3—C8—H8119.4C30A—C28A—C29A107.8 (10)
C7—C8—H8119.4C31A—C28A—C22114.3 (12)
C5—C9—C11113.5 (7)C30A—C28A—C22105.3 (10)
C5—C9—C10108.7 (7)C29A—C28A—C22112.7 (10)
C11—C9—C10109.0 (8)C28A—C29A—H29A109.5
C5—C9—C12111.2 (8)C28A—C29A—H29B109.5
C11—C9—C12108.1 (7)H29A—C29A—H29B109.5
C10—C9—C12106.0 (8)C28A—C29A—H29C109.5
C9—C10—H10A109.5H29A—C29A—H29C109.5
C9—C10—H10B109.5H29B—C29A—H29C109.5
H10A—C10—H10B109.5C28A—C30A—H30A109.5
C9—C10—H10C109.5C28A—C30A—H30B109.5
H10A—C10—H10C109.5H30A—C30A—H30B109.5
H10B—C10—H10C109.5C28A—C30A—H30C109.5
C9—C11—H11A109.5H30A—C30A—H30C109.5
C9—C11—H11B109.5H30B—C30A—H30C109.5
H11A—C11—H11B109.5C28A—C31A—H31A109.5
C9—C11—H11C109.5C28A—C31A—H31B109.5
H11A—C11—H11C109.5H31A—C31A—H31B109.5
H11B—C11—H11C109.5C28A—C31A—H31C109.5
C9—C12—H12A109.5H31A—C31A—H31C109.5
C9—C12—H12B109.5H31B—C31A—H31C109.5
H12A—C12—H12B109.5C29B—C28B—C31B108.9 (12)
C9—C12—H12C109.5C29B—C28B—C30B108.6 (12)
H12A—C12—H12C109.5C31B—C28B—C30B108.1 (11)
H12B—C12—H12C109.5C29B—C28B—C22104 (2)
C16A—C13A—C14A109.0 (10)C31B—C28B—C22118.3 (15)
C16A—C13A—C15A109.3 (10)C30B—C28B—C22108.7 (16)
C14A—C13A—C15A108.5 (10)C28B—C29B—H29D109.5
C16A—C13A—C7109.8 (11)C28B—C29B—H29E109.5
C14A—C13A—C7109.7 (10)H29D—C29B—H29E109.5
C15A—C13A—C7110.5 (11)C28B—C29B—H29F109.5
C13A—C14A—H14A109.5H29D—C29B—H29F109.5
C13A—C14A—H14B109.5H29E—C29B—H29F109.5
H14A—C14A—H14B109.5C28B—C30B—H30D109.5
C13A—C14A—H14C109.5C28B—C30B—H30E109.5
H14A—C14A—H14C109.5H30D—C30B—H30E109.5
H14B—C14A—H14C109.5C28B—C30B—H30F109.5
C13A—C15A—H15A109.5H30D—C30B—H30F109.5
C13A—C15A—H15B109.5H30E—C30B—H30F109.5
H15A—C15A—H15B109.5C28B—C31B—H31D109.5
C13A—C15A—H15C109.5C28B—C31B—H31E109.5
H15A—C15A—H15C109.5H31D—C31B—H31E109.5
H15B—C15A—H15C109.5C28B—C31B—H31F109.5
C13A—C16A—H16A109.5H31D—C31B—H31F109.5
C13A—C16A—H16B109.5H31E—C31B—H31F109.5
Symmetry codes: (i) x+y, x+1, z; (ii) y+1, xy+1, z.
 

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