Supporting information
Crystallographic Information File (CIF) https://doi.org/10.1107/S1600536804029010/rn6026sup1.cif | |
Structure factor file (CIF format) https://doi.org/10.1107/S1600536804029010/rn6026Isup2.hkl |
CCDC reference: 243544
Key indicators
- Single-crystal X-ray study
- T = 293 K
- Mean (C-C) = 0.003 Å
- R factor = 0.028
- wR factor = 0.075
- Data-to-parameter ratio = 22.6
checkCIF/PLATON results
No syntax errors found
Alert level B PLAT232_ALERT_2_B Hirshfeld Test Diff (M-X) Mo1 - Br1 .. 47.37 su PLAT232_ALERT_2_B Hirshfeld Test Diff (M-X) Mo1 - C2 .. 11.39 su PLAT232_ALERT_2_B Hirshfeld Test Diff (M-X) Mo2 - Br1 .. 12.88 su
Alert level C CRYSC01_ALERT_1_C The word below has not been recognised as a standard identifier. gray CRYSC01_ALERT_1_C No recognised colour has been given for crystal colour. PLAT063_ALERT_3_C Crystal Probably too Large for Beam Size ....... 0.70 mm PLAT125_ALERT_4_C No _symmetry_space_group_name_Hall Given ....... ? PLAT164_ALERT_4_C Nr. of Refined C-H H-Atoms in Heavy-At Struct... 1 PLAT220_ALERT_2_C Large Non-Solvent O Ueq(max)/Ueq(min) ... 2.63 Ratio PLAT222_ALERT_3_C Large Non-Solvent H Ueq(max)/Ueq(min) ... 3.04 Ratio PLAT230_ALERT_2_C Hirshfeld Test Diff for O2 - C2 .. 5.07 su PLAT232_ALERT_2_C Hirshfeld Test Diff (M-X) Mo1 - S1 .. 8.20 su PLAT232_ALERT_2_C Hirshfeld Test Diff (M-X) Mo1 - S2 .. 7.20 su PLAT232_ALERT_2_C Hirshfeld Test Diff (M-X) Mo1 - C1 .. 7.65 su PLAT232_ALERT_2_C Hirshfeld Test Diff (M-X) Mo1 - C3 .. 9.47 su PLAT232_ALERT_2_C Hirshfeld Test Diff (M-X) Mo2 - S1 .. 6.92 su PLAT232_ALERT_2_C Hirshfeld Test Diff (M-X) Mo2 - S2 .. 7.84 su PLAT232_ALERT_2_C Hirshfeld Test Diff (M-X) Mo2 - C4 .. 8.94 su PLAT232_ALERT_2_C Hirshfeld Test Diff (M-X) Mo2 - C5 .. 5.44 su PLAT232_ALERT_2_C Hirshfeld Test Diff (M-X) Mo2 - C6 .. 8.82 su PLAT320_ALERT_2_C Check Hybridisation of C23 in Main Residue . ? PLAT322_ALERT_2_C Check Hybridisation of H23A in Main Residue . ? PLAT322_ALERT_2_C Check Hybridisation of H23B in Main Residue . ? PLAT732_ALERT_1_C Angle Calc 75.90(1), Rep 75.90(4) ...... 4.00 su-Rat S1 -MO1 -BR1 1.555 1.555 1.555 PLAT732_ALERT_1_C Angle Calc 76.69(1), Rep 76.69(3) ...... 3.00 su-Rat S2 -MO1 -BR1 1.555 1.555 1.555 PLAT732_ALERT_1_C Angle Calc 54.30(1), Rep 54.30(3) ...... 3.00 su-Rat S2 -MO1 -MO2 1.555 1.555 1.555 PLAT732_ALERT_1_C Angle Calc 77.23(1), Rep 77.23(3) ...... 3.00 su-Rat S2 -MO2 -BR1 1.555 1.555 1.555 PLAT732_ALERT_1_C Angle Calc 76.09(1), Rep 76.09(4) ...... 4.00 su-Rat S1 -MO2 -BR1 1.555 1.555 1.555 PLAT732_ALERT_1_C Angle Calc 62.14(1), Rep 62.14(3) ...... 3.00 su-Rat MO2 -BR1 -MO1 1.555 1.555 1.555 PLAT732_ALERT_1_C Angle Calc 71.01(1), Rep 71.01(3) ...... 3.00 su-Rat MO1 -S1 -MO2 1.555 1.555 1.555 PLAT732_ALERT_1_C Angle Calc 71.00(1), Rep 71.00(3) ...... 3.00 su-Rat MO2 -S2 -MO1 1.555 1.555 1.555
0 ALERT level A = In general: serious problem 3 ALERT level B = Potentially serious problem 28 ALERT level C = Check and explain 0 ALERT level G = General alerts; check 10 ALERT type 1 CIF construction/syntax error, inconsistent or missing data 17 ALERT type 2 Indicator that the structure model may be wrong or deficient 2 ALERT type 3 Indicator that the structure quality may be low 2 ALERT type 4 Improvement, methodology, query or suggestion
Data collection: CrystalClear (Rigaku/MSC, 2004); cell refinement: CrystalClear; data reduction: CrystalClear; program(s) used to solve structure: SHELXTL (Siemens, 1994); program(s) used to refine structure: SHELXTL; molecular graphics: SHELXTL; software used to prepare material for publication: SHELXTL.
(C16H36N)[Mo2Br(C6H11S)2(CO)6] | F(000) = 1872 |
Mr = 912.72 | Dx = 1.452 Mg m−3 |
Monoclinic, P21/n | Mo Kα radiation, λ = 0.71073 Å |
a = 10.738 (5) Å | Cell parameters from 9089 reflections |
b = 19.953 (10) Å | θ = 3.0–27.5° |
c = 19.498 (9) Å | µ = 1.70 mm−1 |
β = 91.863 (5)° | T = 293 K |
V = 4175 (3) Å3 | Prism, gray |
Z = 4 | 0.70 × 0.30 × 0.25 mm |
Rigaku Mercury CCD diffractometer | 9485 independent reflections |
Radiation source: rotating-anode generator | 8809 reflections with I > 2σ(I) |
Graphite monochromator | Rint = 0.019 |
ω scans and φ | θmax = 27.5°, θmin = 3.0° |
Absorption correction: multi-scan (CrystalClear; Rigaku/MSC, 2004) | h = −13→13 |
Tmin = 0.529, Tmax = 0.654 | k = −25→25 |
31610 measured reflections | l = −25→23 |
Refinement on F2 | Primary atom site location: structure-invariant direct methods |
Least-squares matrix: full | Secondary atom site location: difference Fourier map |
R[F2 > 2σ(F2)] = 0.028 | Hydrogen site location: inferred from neighbouring sites |
wR(F2) = 0.075 | H atoms treated by a mixture of independent and constrained refinement |
S = 1.04 | w = 1/[σ2(Fo2) + (0.0445P)2 + 2.1794P] where P = (Fo2 + 2Fc2)/3 |
9485 reflections | (Δ/σ)max = 0.003 |
419 parameters | Δρmax = 1.19 e Å−3 |
2 restraints | Δρmin = −0.78 e Å−3 |
Geometry. All e.s.d.'s (except the e.s.d. in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell e.s.d.'s are taken into account individually in the estimation of e.s.d.'s in distances, angles and torsion angles; correlations between e.s.d.'s in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell e.s.d.'s is used for estimating e.s.d.'s 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 > σ(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. |
x | y | z | Uiso*/Ueq | ||
Mo1 | 0.433032 (15) | 0.129191 (8) | 0.694598 (8) | 0.01657 (5) | |
Mo2 | 0.694062 (15) | 0.132085 (8) | 0.669002 (8) | 0.01716 (5) | |
N1 | 0.58727 (14) | 0.17065 (8) | 0.37122 (8) | 0.0174 (3) | |
Br1 | 0.53567 (2) | 0.047060 (10) | 0.595848 (10) | 0.02411 (6) | |
S1 | 0.53528 (4) | 0.20783 (2) | 0.61718 (2) | 0.01760 (9) | |
S2 | 0.59670 (5) | 0.06693 (2) | 0.75995 (2) | 0.01920 (10) | |
O1 | 0.17886 (16) | 0.18924 (9) | 0.63501 (10) | 0.0435 (4) | |
O2 | 0.39612 (15) | 0.23313 (8) | 0.80949 (8) | 0.0307 (3) | |
O3 | 0.24745 (16) | 0.02805 (8) | 0.76300 (9) | 0.0374 (4) | |
O4 | 0.80670 (15) | 0.23974 (8) | 0.76668 (8) | 0.0344 (4) | |
O5 | 0.9238 (2) | 0.03677 (14) | 0.70330 (13) | 0.0804 (9) | |
O6 | 0.86373 (16) | 0.19179 (10) | 0.55445 (9) | 0.0400 (4) | |
C1 | 0.2726 (2) | 0.16631 (11) | 0.65283 (11) | 0.0268 (4) | |
C2 | 0.40931 (18) | 0.19357 (10) | 0.76665 (10) | 0.0214 (4) | |
C3 | 0.3164 (2) | 0.06361 (10) | 0.73843 (11) | 0.0238 (4) | |
C4 | 0.76612 (18) | 0.19845 (10) | 0.72964 (10) | 0.0224 (4) | |
C5 | 0.8400 (2) | 0.07007 (14) | 0.69029 (13) | 0.0411 (6) | |
C6 | 0.8015 (2) | 0.16914 (11) | 0.59459 (11) | 0.0254 (4) | |
C7 | 0.54608 (18) | 0.29252 (9) | 0.65473 (10) | 0.0198 (4) | |
H7A | 0.5639 | 0.2886 | 0.7042 | 0.024* | |
C8 | 0.6518 (2) | 0.33034 (10) | 0.62215 (13) | 0.0308 (5) | |
H8A | 0.6372 | 0.3322 | 0.5728 | 0.037* | |
H8B | 0.7296 | 0.3068 | 0.6312 | 0.037* | |
C9 | 0.6617 (2) | 0.40191 (11) | 0.65102 (18) | 0.0464 (7) | |
H9A | 0.6835 | 0.4000 | 0.6996 | 0.056* | |
H9B | 0.7273 | 0.4259 | 0.6283 | 0.056* | |
C10 | 0.5383 (2) | 0.43958 (11) | 0.64030 (16) | 0.0396 (6) | |
H10A | 0.5448 | 0.4834 | 0.6616 | 0.048* | |
H10B | 0.5210 | 0.4459 | 0.5916 | 0.048* | |
C11 | 0.4323 (2) | 0.40082 (11) | 0.67130 (13) | 0.0322 (5) | |
H11A | 0.3545 | 0.4242 | 0.6616 | 0.039* | |
H11B | 0.4453 | 0.3990 | 0.7207 | 0.039* | |
C12 | 0.42259 (19) | 0.32947 (10) | 0.64308 (12) | 0.0259 (4) | |
H12A | 0.3569 | 0.3056 | 0.6658 | 0.031* | |
H12B | 0.4014 | 0.3309 | 0.5944 | 0.031* | |
C13 | 0.62353 (18) | 0.10496 (10) | 0.84543 (10) | 0.0195 (4) | |
H13A | 0.6120 | 0.1536 | 0.8419 | 0.023* | |
C14 | 0.5279 (2) | 0.07637 (12) | 0.89380 (11) | 0.0291 (5) | |
H14A | 0.5343 | 0.0279 | 0.8946 | 0.035* | |
H14B | 0.4447 | 0.0881 | 0.8772 | 0.035* | |
C15 | 0.5497 (2) | 0.10391 (14) | 0.96664 (11) | 0.0374 (6) | |
H15A | 0.5348 | 0.1519 | 0.9665 | 0.045* | |
H15B | 0.4911 | 0.0833 | 0.9970 | 0.045* | |
C16 | 0.6820 (2) | 0.09008 (15) | 0.99336 (12) | 0.0407 (6) | |
H16A | 0.6944 | 0.1102 | 1.0383 | 0.049* | |
H16B | 0.6942 | 0.0421 | 0.9981 | 0.049* | |
C17 | 0.7770 (2) | 0.11818 (13) | 0.94511 (12) | 0.0322 (5) | |
H17A | 0.8602 | 0.1065 | 0.9618 | 0.039* | |
H17B | 0.7706 | 0.1667 | 0.9441 | 0.039* | |
C18 | 0.7556 (2) | 0.09040 (11) | 0.87215 (11) | 0.0261 (4) | |
H18A | 0.8148 | 0.1106 | 0.8418 | 0.031* | |
H18B | 0.7696 | 0.0424 | 0.8724 | 0.031* | |
C19 | 0.49736 (18) | 0.15693 (10) | 0.42810 (10) | 0.0211 (4) | |
H19A | 0.5258 | 0.1809 | 0.4690 | 0.025* | |
H19B | 0.4995 | 0.1094 | 0.4387 | 0.025* | |
C20 | 0.3628 (2) | 0.17712 (12) | 0.41103 (11) | 0.0286 (5) | |
H20A | 0.3606 | 0.2234 | 0.3958 | 0.034* | |
H20B | 0.3300 | 0.1494 | 0.3738 | 0.034* | |
C21 | 0.2822 (2) | 0.16942 (16) | 0.47210 (13) | 0.0418 (6) | |
H21A | 0.3089 | 0.2013 | 0.5071 | 0.050* | |
H21B | 0.2935 | 0.1248 | 0.4910 | 0.050* | |
C22 | 0.1453 (2) | 0.18033 (16) | 0.45476 (15) | 0.0470 (7) | |
H22A | 0.0982 | 0.1748 | 0.4954 | 0.070* | |
H22B | 0.1178 | 0.1483 | 0.4209 | 0.070* | |
H22C | 0.1332 | 0.2248 | 0.4370 | 0.070* | |
C23 | 0.59196 (19) | 0.24496 (9) | 0.35372 (10) | 0.0203 (4) | |
H23A | 0.5780 | 0.2601 | 0.3090 | 0.024* | |
C24 | 0.6204 (2) | 0.29340 (10) | 0.41247 (11) | 0.0243 (4) | |
H24A | 0.6966 | 0.2801 | 0.4369 | 0.029* | |
H24B | 0.5531 | 0.2928 | 0.4445 | 0.029* | |
C25 | 0.6349 (2) | 0.36371 (10) | 0.38296 (12) | 0.0283 (5) | |
H25A | 0.6999 | 0.3630 | 0.3495 | 0.034* | |
H25B | 0.5578 | 0.3764 | 0.3592 | 0.034* | |
C26 | 0.6674 (2) | 0.41628 (11) | 0.43723 (13) | 0.0345 (5) | |
H26A | 0.6753 | 0.4593 | 0.4157 | 0.052* | |
H26B | 0.7448 | 0.4046 | 0.4602 | 0.052* | |
H26C | 0.6027 | 0.4181 | 0.4700 | 0.052* | |
C27 | 0.54186 (18) | 0.13304 (9) | 0.30684 (10) | 0.0189 (4) | |
H27A | 0.5196 | 0.0878 | 0.3199 | 0.023* | |
H27B | 0.4668 | 0.1547 | 0.2889 | 0.023* | |
C28 | 0.6348 (2) | 0.12913 (10) | 0.24977 (11) | 0.0245 (4) | |
H28A | 0.7017 | 0.0985 | 0.2627 | 0.029* | |
H28B | 0.6707 | 0.1730 | 0.2421 | 0.029* | |
C29 | 0.5673 (2) | 0.10435 (11) | 0.18366 (10) | 0.0260 (4) | |
H29A | 0.6281 | 0.0854 | 0.1534 | 0.031* | |
H29B | 0.5096 | 0.0690 | 0.1952 | 0.031* | |
C30 | 0.4965 (2) | 0.15972 (14) | 0.14602 (12) | 0.0380 (6) | |
H30A | 0.4563 | 0.1418 | 0.1053 | 0.057* | |
H30B | 0.5535 | 0.1944 | 0.1336 | 0.057* | |
H30C | 0.4349 | 0.1780 | 0.1753 | 0.057* | |
C31 | 0.71743 (18) | 0.14790 (10) | 0.39434 (10) | 0.0213 (4) | |
H31A | 0.7432 | 0.1736 | 0.4346 | 0.026* | |
H31B | 0.7745 | 0.1584 | 0.3583 | 0.026* | |
C32 | 0.72985 (19) | 0.07366 (10) | 0.41149 (11) | 0.0242 (4) | |
H32A | 0.6871 | 0.0473 | 0.3762 | 0.029* | |
H32B | 0.6913 | 0.0646 | 0.4548 | 0.029* | |
C33 | 0.8670 (2) | 0.05365 (11) | 0.41629 (12) | 0.0288 (5) | |
H33A | 0.9043 | 0.0615 | 0.3724 | 0.035* | |
H33B | 0.9101 | 0.0815 | 0.4502 | 0.035* | |
C34 | 0.8834 (2) | −0.01980 (12) | 0.43608 (14) | 0.0403 (6) | |
H34A | 0.9705 | −0.0306 | 0.4387 | 0.060* | |
H34B | 0.8422 | −0.0476 | 0.4021 | 0.060* | |
H34C | 0.8477 | −0.0275 | 0.4799 | 0.060* | |
H23B | 0.6630 (18) | 0.2472 (12) | 0.3244 (11) | 0.026 (6)* |
U11 | U22 | U33 | U12 | U13 | U23 | |
Mo1 | 0.01770 (9) | 0.01561 (8) | 0.01653 (9) | −0.00204 (5) | 0.00255 (6) | −0.00102 (5) |
Mo2 | 0.01834 (9) | 0.01815 (9) | 0.01522 (9) | 0.00153 (6) | 0.00409 (6) | −0.00053 (5) |
N1 | 0.0163 (8) | 0.0191 (7) | 0.0168 (7) | −0.0022 (6) | 0.0010 (6) | 0.0014 (6) |
Br1 | 0.03326 (12) | 0.01952 (10) | 0.01971 (10) | −0.00608 (8) | 0.00322 (8) | −0.00406 (7) |
S1 | 0.0197 (2) | 0.0163 (2) | 0.0168 (2) | −0.00157 (16) | 0.00129 (17) | −0.00077 (16) |
S2 | 0.0237 (2) | 0.0177 (2) | 0.0164 (2) | 0.00151 (17) | 0.00384 (18) | −0.00030 (16) |
O1 | 0.0280 (9) | 0.0460 (10) | 0.0559 (12) | 0.0072 (8) | −0.0061 (8) | 0.0033 (9) |
O2 | 0.0305 (8) | 0.0291 (8) | 0.0327 (8) | 0.0036 (6) | 0.0069 (6) | −0.0099 (6) |
O3 | 0.0393 (9) | 0.0270 (8) | 0.0469 (10) | −0.0078 (7) | 0.0167 (8) | 0.0034 (7) |
O4 | 0.0351 (9) | 0.0403 (9) | 0.0275 (8) | −0.0117 (7) | −0.0040 (7) | −0.0047 (7) |
O5 | 0.0634 (15) | 0.105 (2) | 0.0747 (16) | 0.0590 (14) | 0.0318 (13) | 0.0421 (14) |
O6 | 0.0353 (9) | 0.0554 (11) | 0.0302 (9) | −0.0065 (8) | 0.0138 (7) | 0.0042 (8) |
C1 | 0.0259 (11) | 0.0249 (10) | 0.0295 (11) | −0.0042 (8) | 0.0005 (9) | 0.0007 (8) |
C2 | 0.0173 (9) | 0.0230 (9) | 0.0240 (10) | −0.0001 (7) | 0.0021 (7) | 0.0023 (8) |
C3 | 0.0256 (10) | 0.0209 (9) | 0.0250 (10) | 0.0007 (8) | 0.0044 (8) | −0.0031 (8) |
C4 | 0.0183 (9) | 0.0294 (10) | 0.0196 (9) | −0.0029 (8) | 0.0036 (7) | 0.0039 (8) |
C5 | 0.0391 (14) | 0.0486 (15) | 0.0366 (13) | 0.0194 (12) | 0.0152 (11) | 0.0129 (11) |
C6 | 0.0238 (10) | 0.0305 (11) | 0.0219 (10) | 0.0009 (8) | 0.0032 (8) | −0.0026 (8) |
C7 | 0.0220 (10) | 0.0155 (8) | 0.0219 (9) | −0.0013 (7) | 0.0010 (7) | −0.0009 (7) |
C8 | 0.0236 (11) | 0.0183 (10) | 0.0512 (14) | −0.0016 (8) | 0.0104 (10) | 0.0000 (9) |
C9 | 0.0314 (13) | 0.0193 (11) | 0.089 (2) | −0.0056 (9) | 0.0150 (13) | −0.0085 (12) |
C10 | 0.0369 (13) | 0.0173 (10) | 0.0656 (18) | −0.0010 (9) | 0.0177 (12) | −0.0014 (10) |
C11 | 0.0291 (12) | 0.0213 (10) | 0.0470 (14) | 0.0029 (8) | 0.0137 (10) | −0.0039 (9) |
C12 | 0.0205 (10) | 0.0210 (10) | 0.0365 (12) | 0.0009 (8) | 0.0051 (9) | 0.0007 (8) |
C13 | 0.0216 (10) | 0.0202 (9) | 0.0168 (9) | 0.0027 (7) | 0.0042 (7) | −0.0008 (7) |
C14 | 0.0298 (11) | 0.0389 (12) | 0.0190 (10) | −0.0075 (9) | 0.0060 (8) | −0.0002 (8) |
C15 | 0.0358 (13) | 0.0570 (16) | 0.0201 (11) | −0.0080 (11) | 0.0101 (9) | −0.0060 (10) |
C16 | 0.0456 (15) | 0.0575 (16) | 0.0189 (11) | −0.0071 (12) | −0.0014 (10) | 0.0035 (10) |
C17 | 0.0273 (11) | 0.0442 (13) | 0.0246 (11) | 0.0002 (10) | −0.0041 (9) | 0.0005 (9) |
C18 | 0.0243 (10) | 0.0313 (11) | 0.0227 (10) | 0.0063 (8) | 0.0016 (8) | 0.0032 (8) |
C19 | 0.0232 (10) | 0.0232 (9) | 0.0172 (9) | −0.0037 (8) | 0.0046 (7) | 0.0015 (7) |
C20 | 0.0232 (10) | 0.0371 (12) | 0.0259 (11) | 0.0008 (9) | 0.0080 (8) | 0.0065 (9) |
C21 | 0.0291 (12) | 0.0653 (18) | 0.0315 (13) | −0.0022 (12) | 0.0086 (10) | 0.0100 (12) |
C22 | 0.0305 (13) | 0.0600 (17) | 0.0512 (16) | −0.0048 (12) | 0.0137 (12) | 0.0048 (13) |
C23 | 0.0239 (10) | 0.0188 (9) | 0.0182 (9) | −0.0015 (7) | 0.0037 (7) | 0.0033 (7) |
C24 | 0.0303 (11) | 0.0186 (9) | 0.0242 (10) | −0.0029 (8) | 0.0035 (8) | −0.0013 (7) |
C25 | 0.0323 (12) | 0.0200 (10) | 0.0327 (12) | −0.0017 (8) | 0.0045 (9) | 0.0024 (8) |
C26 | 0.0398 (13) | 0.0207 (10) | 0.0433 (14) | −0.0036 (9) | 0.0044 (11) | −0.0025 (9) |
C27 | 0.0187 (9) | 0.0213 (9) | 0.0167 (9) | −0.0019 (7) | 0.0002 (7) | −0.0014 (7) |
C28 | 0.0228 (10) | 0.0296 (11) | 0.0212 (10) | 0.0005 (8) | 0.0044 (8) | −0.0022 (8) |
C29 | 0.0310 (12) | 0.0281 (11) | 0.0192 (10) | −0.0027 (8) | 0.0069 (8) | −0.0045 (7) |
C30 | 0.0378 (13) | 0.0508 (15) | 0.0252 (11) | 0.0122 (11) | −0.0026 (10) | −0.0053 (10) |
C31 | 0.0186 (9) | 0.0220 (9) | 0.0230 (10) | −0.0025 (7) | −0.0014 (8) | 0.0022 (7) |
C32 | 0.0227 (10) | 0.0208 (9) | 0.0290 (11) | −0.0026 (8) | −0.0013 (8) | 0.0033 (8) |
C33 | 0.0240 (11) | 0.0251 (10) | 0.0368 (12) | 0.0015 (8) | −0.0046 (9) | 0.0034 (9) |
C34 | 0.0419 (14) | 0.0254 (11) | 0.0521 (15) | 0.0033 (10) | −0.0183 (12) | 0.0011 (10) |
Mo1—C2 | 1.927 (2) | C17—C18 | 1.537 (3) |
Mo1—C3 | 2.020 (2) | C17—H17A | 0.9700 |
Mo1—C1 | 2.022 (2) | C17—H17B | 0.9700 |
Mo1—S1 | 2.4605 (9) | C18—H18A | 0.9700 |
Mo1—S2 | 2.4718 (9) | C18—H18B | 0.9700 |
Mo1—Br1 | 2.7831 (9) | C19—C20 | 1.526 (3) |
Mo1—Mo2 | 2.8635 (13) | C19—H19A | 0.9700 |
Mo2—C4 | 1.921 (2) | C19—H19B | 0.9700 |
Mo2—C6 | 2.023 (2) | C20—C21 | 1.503 (3) |
Mo2—C5 | 2.029 (2) | C20—H20A | 0.9700 |
Mo2—S2 | 2.4593 (9) | C20—H20B | 0.9700 |
Mo2—S1 | 2.4699 (9) | C21—C22 | 1.513 (4) |
Mo2—Br1 | 2.7654 (8) | C21—H21A | 0.9700 |
N1—C19 | 1.519 (2) | C21—H21B | 0.9700 |
N1—C31 | 1.524 (2) | C22—H22A | 0.9600 |
N1—C23 | 1.523 (2) | C22—H22B | 0.9600 |
N1—C27 | 1.529 (2) | C22—H22C | 0.9600 |
S1—C7 | 1.844 (2) | C23—C24 | 1.522 (3) |
S2—C13 | 1.845 (2) | C23—H23A | 0.9300 |
O1—C1 | 1.149 (3) | C23—H23B | 0.969 (16) |
O2—C2 | 1.161 (2) | C24—C25 | 1.526 (3) |
O3—C3 | 1.142 (3) | C24—H24A | 0.9700 |
O4—C4 | 1.170 (3) | C24—H24B | 0.9700 |
O5—C5 | 1.140 (3) | C25—C26 | 1.522 (3) |
O6—C6 | 1.139 (3) | C25—H25A | 0.9700 |
C7—C8 | 1.519 (3) | C25—H25B | 0.9700 |
C7—C12 | 1.528 (3) | C26—H26A | 0.9600 |
C7—H7A | 0.9800 | C26—H26B | 0.9600 |
C8—C9 | 1.537 (3) | C26—H26C | 0.9600 |
C8—H8A | 0.9700 | C27—C28 | 1.521 (3) |
C8—H8B | 0.9700 | C27—H27A | 0.9700 |
C9—C10 | 1.532 (4) | C27—H27B | 0.9700 |
C9—H9A | 0.9700 | C28—C29 | 1.540 (3) |
C9—H9B | 0.9700 | C28—H28A | 0.9700 |
C10—C11 | 1.518 (3) | C28—H28B | 0.9700 |
C10—H10A | 0.9700 | C29—C30 | 1.517 (3) |
C10—H10B | 0.9700 | C29—H29A | 0.9700 |
C11—C12 | 1.529 (3) | C29—H29B | 0.9700 |
C11—H11A | 0.9700 | C30—H30A | 0.9600 |
C11—H11B | 0.9700 | C30—H30B | 0.9600 |
C12—H12A | 0.9700 | C30—H30C | 0.9600 |
C12—H12B | 0.9700 | C31—C32 | 1.524 (3) |
C13—C18 | 1.523 (3) | C31—H31A | 0.9700 |
C13—C14 | 1.527 (3) | C31—H31B | 0.9700 |
C13—H13A | 0.9800 | C32—C33 | 1.525 (3) |
C14—C15 | 1.534 (3) | C32—H32A | 0.9700 |
C14—H14A | 0.9700 | C32—H32B | 0.9700 |
C14—H14B | 0.9700 | C33—C34 | 1.524 (3) |
C15—C16 | 1.523 (4) | C33—H33A | 0.9700 |
C15—H15A | 0.9700 | C33—H33B | 0.9700 |
C15—H15B | 0.9700 | C34—H34A | 0.9600 |
C16—C17 | 1.517 (3) | C34—H34B | 0.9600 |
C16—H16A | 0.9700 | C34—H34C | 0.9600 |
C16—H16B | 0.9700 | ||
C2—Mo1—C3 | 91.43 (9) | C17—C16—C15 | 111.0 (2) |
C2—Mo1—C1 | 85.32 (9) | C17—C16—H16A | 109.4 |
C3—Mo1—C1 | 82.88 (9) | C15—C16—H16A | 109.4 |
C2—Mo1—S1 | 95.42 (7) | C17—C16—H16B | 109.4 |
C3—Mo1—S1 | 165.43 (6) | C15—C16—H16B | 109.4 |
C1—Mo1—S1 | 84.87 (7) | H16A—C16—H16B | 108.0 |
C2—Mo1—S2 | 93.89 (7) | C16—C17—C18 | 111.0 (2) |
C3—Mo1—S2 | 84.05 (7) | C16—C17—H17A | 109.4 |
C1—Mo1—S2 | 166.88 (6) | C18—C17—H17A | 109.4 |
S1—Mo1—S2 | 108.23 (3) | C16—C17—H17B | 109.4 |
C2—Mo1—Br1 | 164.11 (6) | C18—C17—H17B | 109.4 |
C3—Mo1—Br1 | 100.14 (6) | H17A—C17—H17B | 108.0 |
C1—Mo1—Br1 | 106.76 (7) | C13—C18—C17 | 110.92 (17) |
S1—Mo1—Br1 | 75.90 (4) | C13—C18—H18A | 109.5 |
S2—Mo1—Br1 | 76.69 (3) | C17—C18—H18A | 109.5 |
C2—Mo1—Mo2 | 105.49 (6) | C13—C18—H18B | 109.5 |
C3—Mo1—Mo2 | 135.28 (6) | C17—C18—H18B | 109.5 |
C1—Mo1—Mo2 | 138.45 (7) | H18A—C18—H18B | 108.0 |
S1—Mo1—Mo2 | 54.647 (16) | N1—C19—C20 | 114.39 (16) |
S2—Mo1—Mo2 | 54.30 (3) | N1—C19—H19A | 108.7 |
Br1—Mo1—Mo2 | 58.628 (12) | C20—C19—H19A | 108.7 |
C4—Mo2—C6 | 87.82 (9) | N1—C19—H19B | 108.7 |
C4—Mo2—C5 | 90.09 (11) | C20—C19—H19B | 108.7 |
C6—Mo2—C5 | 85.12 (10) | H19A—C19—H19B | 107.6 |
C4—Mo2—S2 | 95.32 (7) | C21—C20—C19 | 111.47 (18) |
C6—Mo2—S2 | 167.47 (6) | C21—C20—H20A | 109.3 |
C5—Mo2—S2 | 82.75 (8) | C19—C20—H20A | 109.3 |
C4—Mo2—S1 | 95.10 (7) | C21—C20—H20B | 109.3 |
C6—Mo2—S1 | 83.40 (7) | C19—C20—H20B | 109.3 |
C5—Mo2—S1 | 167.20 (7) | H20A—C20—H20B | 108.0 |
S2—Mo2—S1 | 108.33 (3) | C20—C21—C22 | 112.9 (2) |
C4—Mo2—Br1 | 165.68 (6) | C20—C21—H21A | 109.0 |
C6—Mo2—Br1 | 102.11 (7) | C22—C21—H21A | 109.0 |
C5—Mo2—Br1 | 100.92 (9) | C20—C21—H21B | 109.0 |
S2—Mo2—Br1 | 77.23 (3) | C22—C21—H21B | 109.0 |
S1—Mo2—Br1 | 76.09 (4) | H21A—C21—H21B | 107.8 |
C4—Mo2—Mo1 | 106.47 (6) | C21—C22—H22A | 109.5 |
C6—Mo2—Mo1 | 135.78 (6) | C21—C22—H22B | 109.5 |
C5—Mo2—Mo1 | 134.91 (8) | H22A—C22—H22B | 109.5 |
S2—Mo2—Mo1 | 54.703 (15) | C21—C22—H22C | 109.5 |
S1—Mo2—Mo1 | 54.34 (2) | H22A—C22—H22C | 109.5 |
Br1—Mo2—Mo1 | 59.23 (2) | H22B—C22—H22C | 109.5 |
C19—N1—C31 | 109.21 (15) | C24—C23—N1 | 117.19 (16) |
C19—N1—C23 | 111.44 (15) | C24—C23—H23A | 121.4 |
C31—N1—C23 | 108.65 (14) | N1—C23—H23A | 121.4 |
C19—N1—C27 | 108.53 (14) | C24—C23—H23B | 105.8 (14) |
C31—N1—C27 | 111.20 (15) | N1—C23—H23B | 102.1 (14) |
C23—N1—C27 | 107.82 (14) | H23A—C23—H23B | 62.4 |
Mo2—Br1—Mo1 | 62.14 (3) | C23—C24—C25 | 108.69 (17) |
C7—S1—Mo1 | 111.37 (7) | C23—C24—H24A | 110.0 |
C7—S1—Mo2 | 111.39 (7) | C25—C24—H24A | 110.0 |
Mo1—S1—Mo2 | 71.01 (3) | C23—C24—H24B | 110.0 |
C13—S2—Mo2 | 112.11 (7) | C25—C24—H24B | 110.0 |
C13—S2—Mo1 | 110.27 (7) | H24A—C24—H24B | 108.3 |
Mo2—S2—Mo1 | 71.00 (3) | C26—C25—C24 | 113.29 (19) |
O1—C1—Mo1 | 173.8 (2) | C26—C25—H25A | 108.9 |
O2—C2—Mo1 | 178.88 (18) | C24—C25—H25A | 108.9 |
O3—C3—Mo1 | 177.75 (19) | C26—C25—H25B | 108.9 |
O4—C4—Mo2 | 178.06 (19) | C24—C25—H25B | 108.9 |
O5—C5—Mo2 | 177.9 (3) | H25A—C25—H25B | 107.7 |
O6—C6—Mo2 | 177.34 (19) | C25—C26—H26A | 109.5 |
C8—C7—C12 | 110.79 (17) | C25—C26—H26B | 109.5 |
C8—C7—S1 | 109.11 (14) | H26A—C26—H26B | 109.5 |
C12—C7—S1 | 109.88 (14) | C25—C26—H26C | 109.5 |
C8—C7—H7A | 109.0 | H26A—C26—H26C | 109.5 |
C12—C7—H7A | 109.0 | H26B—C26—H26C | 109.5 |
S1—C7—H7A | 109.0 | C28—C27—N1 | 115.26 (16) |
C7—C8—C9 | 110.60 (19) | C28—C27—H27A | 108.5 |
C7—C8—H8A | 109.5 | N1—C27—H27A | 108.5 |
C9—C8—H8A | 109.5 | C28—C27—H27B | 108.5 |
C7—C8—H8B | 109.5 | N1—C27—H27B | 108.5 |
C9—C8—H8B | 109.5 | H27A—C27—H27B | 107.5 |
H8A—C8—H8B | 108.1 | C27—C28—C29 | 109.09 (17) |
C10—C9—C8 | 110.9 (2) | C27—C28—H28A | 109.9 |
C10—C9—H9A | 109.5 | C29—C28—H28A | 109.9 |
C8—C9—H9A | 109.5 | C27—C28—H28B | 109.9 |
C10—C9—H9B | 109.5 | C29—C28—H28B | 109.9 |
C8—C9—H9B | 109.5 | H28A—C28—H28B | 108.3 |
H9A—C9—H9B | 108.0 | C30—C29—C28 | 112.71 (19) |
C11—C10—C9 | 110.6 (2) | C30—C29—H29A | 109.0 |
C11—C10—H10A | 109.5 | C28—C29—H29A | 109.0 |
C9—C10—H10A | 109.5 | C30—C29—H29B | 109.0 |
C11—C10—H10B | 109.5 | C28—C29—H29B | 109.0 |
C9—C10—H10B | 109.5 | H29A—C29—H29B | 107.8 |
H10A—C10—H10B | 108.1 | C29—C30—H30A | 109.5 |
C10—C11—C12 | 111.99 (19) | C29—C30—H30B | 109.5 |
C10—C11—H11A | 109.2 | H30A—C30—H30B | 109.5 |
C12—C11—H11A | 109.2 | C29—C30—H30C | 109.5 |
C10—C11—H11B | 109.2 | H30A—C30—H30C | 109.5 |
C12—C11—H11B | 109.2 | H30B—C30—H30C | 109.5 |
H11A—C11—H11B | 107.9 | N1—C31—C32 | 115.31 (16) |
C7—C12—C11 | 110.31 (18) | N1—C31—H31A | 108.4 |
C7—C12—H12A | 109.6 | C32—C31—H31A | 108.4 |
C11—C12—H12A | 109.6 | N1—C31—H31B | 108.4 |
C7—C12—H12B | 109.6 | C32—C31—H31B | 108.4 |
C11—C12—H12B | 109.6 | H31A—C31—H31B | 107.5 |
H12A—C12—H12B | 108.1 | C31—C32—C33 | 110.20 (17) |
C18—C13—C14 | 110.77 (17) | C31—C32—H32A | 109.6 |
C18—C13—S2 | 110.30 (13) | C33—C32—H32A | 109.6 |
C14—C13—S2 | 108.41 (14) | C31—C32—H32B | 109.6 |
C18—C13—H13A | 109.1 | C33—C32—H32B | 109.6 |
C14—C13—H13A | 109.1 | H32A—C32—H32B | 108.1 |
S2—C13—H13A | 109.1 | C34—C33—C32 | 111.74 (19) |
C13—C14—C15 | 110.65 (18) | C34—C33—H33A | 109.3 |
C13—C14—H14A | 109.5 | C32—C33—H33A | 109.3 |
C15—C14—H14A | 109.5 | C34—C33—H33B | 109.3 |
C13—C14—H14B | 109.5 | C32—C33—H33B | 109.3 |
C15—C14—H14B | 109.5 | H33A—C33—H33B | 107.9 |
H14A—C14—H14B | 108.1 | C33—C34—H34A | 109.5 |
C16—C15—C14 | 111.4 (2) | C33—C34—H34B | 109.5 |
C16—C15—H15A | 109.4 | H34A—C34—H34B | 109.5 |
C14—C15—H15A | 109.4 | C33—C34—H34C | 109.5 |
C16—C15—H15B | 109.4 | H34A—C34—H34C | 109.5 |
C14—C15—H15B | 109.4 | H34B—C34—H34C | 109.5 |
H15A—C15—H15B | 108.0 |
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