The title compound, [Mo
3(C
31H
46NS
2)
3S
7]I, crystallizes on a threefold rotational axis in
P31
c (space group No. 159). The [Mo
3S
7(S
2CN(CH
2C
6H
3-3,5-
tBu
2)
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 Mo
3 centroids. On the underside of the cluster, opposite the μ
3-S
2− ligand, the iodide counteranion forms close contacts of 3.166 (2) Å with the sulfur atoms of the μ
2-S
22− 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 [Mo
3S
7(S
2CN(CH
2C
6H
3-3,5-
tBu
2)
2)
3]
+
I
− interactions.
Supporting information
CCDC reference: 2015330
Key indicators
- Single-crystal X-ray study
- T = 150 K
- Mean
(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
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']-µ
3-sulfido-tris-µ
2-disulfido-
triangulo-trimolybdenum(IV) iodide
top
Crystal data top
[Mo3(C31H46NS2)3S7]I | Dx = 1.328 Mg m−3 |
Mr = 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 | Rint = 0.043 |
Detector resolution: 8.3333 pixels mm-1 | θmax = 27.1°, θmin = 1.7° |
φ and ω scans | h = −30→30 |
Absorption correction: multi-scan (SADABS; Krause et al., 2015) | k = −30→30 |
Tmin = 0.799, Tmax = 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(Fo2) + (0.0543P)2 + 6.2404P] where P = (Fo2 + 2Fc2)/3 |
S = 1.06 | (Δ/σ)max < 0.001 |
7810 reflections | Δρmax = 1.08 e Å−3 |
369 parameters | Δρmin = −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 | Uiso*/Ueq | 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. |