metal-organic compounds\(\def\hfill{\hskip 5em}\def\hfil{\hskip 3em}\def\eqno#1{\hfil {#1}}\)

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ISSN: 2056-9890

(μ-Benzoato-κ2O:O′)tris­­[μ-N,N′-bis­­(4-meth­­oxy­phen­yl)formamidinato-κ2N:N′]dimolybdenum(II) di­chloro­methane monosolvate

aDepartment of Chemistry, Tongji University, Shanghai 200092, People's Republic of China
*Correspondence e-mail: 08hanlij@tongji.edu.cn

(Received 16 December 2010; accepted 19 January 2011; online 26 January 2011)

The title compound, [Mo2(C15H15N2O2)3(C7H5O2)]·CH2Cl2, has a quadruply bonded Mo24+ unit equatorially coordinated by three N,N′-bis­(4-μ-meth­oxy­phen­yl)formamidinate (DAniF) ligands and one benzoate anion. The Mo—Mo bond length of 2.0881 (8) Å is typical for quadruply bonded species. The phenyl ring and the connected dimetal chelating ring (Mo2O2C) are nearly co-planar, making a dihedral angle of 3.24 (13)°. The dichloromethane solvent molecule is disordered over four sets of sites with occupancies of 0.3:0.3:0.2:0.2.

Related literature

For Mo2(DAniF)3(OOCCH3), see: Cotton et al. (2003[Cotton, F. A., Liu, C. Y. & Murillo, C. A. (2003). J. Am. Chem. Soc. 125, 13564-13575.]). For Mo2(DAniF)4, see: Lin et al. (1996[Lin, C., Protasiewicz, J. D., Smith, E. T. & Ren, T. (1996). Inorg. Chem. 35, 6422-6428.]). For Mo2(OOCC6H5)4, see: Cotton et al. (1978[Cotton, F. A., Extine, M. & Gaga, L. D. (1978). Inorg. Chem. 17, 172-176.]).

[Scheme 1]

Experimental

Crystal data
  • [Mo2(C15H15N2O2)3(C7H5O2)]·CH2Cl2

  • Mr = 1163.79

  • Triclinic, [P \overline 1]

  • a = 12.025 (4) Å

  • b = 13.705 (4) Å

  • c = 17.727 (6) Å

  • α = 74.595 (4)°

  • β = 85.646 (4)°

  • γ = 67.238 (4)°

  • V = 2596.0 (14) Å3

  • Z = 2

  • Mo Kα radiation

  • μ = 0.65 mm−1

  • T = 293 K

  • 0.25 × 0.20 × 0.20 mm

Data collection
  • Bruker SMART 1000 diffractometer

  • Absorption correction: multi-scan (SADABS; Sheldrick, 2004[Sheldrick, G. M. (2004). SADABS. University of Göttingen, Germany.]) Tmin = 0.851, Tmax = 0.879

  • 10844 measured reflections

  • 8981 independent reflections

  • 6852 reflections with I > 2σ(I)

  • Rint = 0.018

Refinement
  • R[F2 > 2σ(F2)] = 0.036

  • wR(F2) = 0.107

  • S = 1.03

  • 8981 reflections

  • 652 parameters

  • 12 restraints

  • H-atom parameters constrained

  • Δρmax = 0.65 e Å−3

  • Δρmin = −0.59 e Å−3

Table 1
Selected bond lengths (Å)

Mo1—N3 2.117 (3)
Mo1—N5 2.142 (3)
Mo1—O1 2.144 (2)
Mo1—N1 2.156 (3)
Mo2—N4 2.120 (3)
Mo2—N2 2.132 (3)
Mo2—O2 2.133 (2)
Mo2—N6 2.144 (3)

Data collection: APEX2 (Bruker, 2004[Bruker (2004). APEX2. Bruker AXS Inc., Madison, Wisconsin, USA.]); cell refinement: SAINT-Plus (Bruker, 2001[Bruker (2001). SAINT-Plus. Bruker AXS Inc., Madison,Wisconsin, USA.]); data reduction: SAINT-Plus; program(s) used to solve structure: SHELXS97 (Sheldrick, 2008[Sheldrick, G. M. (2008). Acta Cryst. A64, 112-122.]); program(s) used to refine structure: SHELXL97 (Sheldrick, 2008[Sheldrick, G. M. (2008). Acta Cryst. A64, 112-122.]); molecular graphics: XP in SHELXTL (Sheldrick, 2008[Sheldrick, G. M. (2008). Acta Cryst. A64, 112-122.]); software used to prepare material for publication: SHELXL97.

Supporting information


Comment top

Research on the quadruply bonded compounds has became an active areas in the field of crystal engineering, supramolecular chemistry and electronic communication. Different from single metal coordination building blocks, a covalent dimetal Mo2 unit has four equatorial positions as three-atom bridging ligand is used and two axial positions. In order to create designed molecules, nitrogen-donor ligand N,N'-di-p-anisylformamidinate (referred to as DAniF) is used to selectively block part of the equatorial coordination sites. Upon replacement of acetate in Mo2(DAniF)3(OOCCH3) by a benzoate group, compound Mo2(DAniF)3(OOCC6H5) has been synthesized. Crystals Mo2(DAniF)3(OOCC6H5)(CH2Cl2) were obtained by crystallized from CH3CH2OH/CH2Cl2 solution. The single-crystal structure is shown in Fig. 1. The title compound crystalizes in the P-1 space group with molecules lying on general positions in the unit cell. The asymmetric unit contains one complex molecule and additionally one solvent molecule of dichloromethane.

The Mo—Mo bond length in title compound of 2.0881 (8) Å is quite similar to those in the Mo2(DAniF)4 and Mo2(OOCC6H5)4 which are 2.0964 (5) and 2.0960 (1) Å, respectively, and is typical for quadruply bonded species. As designed, this molecule is close to that of its precursor Mo2(DAniF)3(OOCCH3) by having the same coordination sphere and a similar Mo—Mo bond length (2.0888 (9) Å). The average Mo—N distance (2.135 Å) is also similar to that of Mo2(DAniF)3(OOCCH3)(2.140 Å), indicating that the Mo—N covalent bond is unperturbed by the inductive effect of the remote substituents.

Related literature top

For Mo2(DAniF)3(OOCCH3), see: Cotton et al. (2003). For Mo2(DAniF)4, see: Lin et al. (1996). For Mo2(OOCC6H5)4, see: Cotton et al. (1978).

Experimental top

The title compound was synthesized by following reaction. To the yellow solution of Mo2(DAniF)3(OOCCH3) (0.512 g, 0.500 mmol) in 15 ml of THF, was added 1.0 ml NaOCH3 solution (0.5 M in methanol). After stirring for about 2 h, a colorless microcrystalline material was removed by filtration. To the filtrate was added an excess of benzoic acid (0.080 g, 0.650 mmol). Upon stirring, the color of the mixture immediately changed from yellow to orange yellow. After stirring at room temperature for an additional 1 h, the solvent was removed under vacuum, and the residue was washed with ethanol (2×15 ml), and then dried under vacuum. The orange yellow solid was dissolved in dichloromethane (15 ml) and the solution was layered with ethanol. Yellow block-shaped crystals formed after three days. Yield: 0.420 g (78%). 1HNMR(CDCl3, p.p.m.): 8.47(s,1H, –NCHN–), 8.37(s, 2H, –NCHN–), 8.29(t, 2H, aromatic), 7.46(t, 3H, aromatic), 6.63(d, 8H, aromatic), 6.58(d, 8H, aromatic), 6.44(d, 4H, aromatic), 6.23(d, 4H, aromatic), 3.71(s, 12H, –OCH3), 3.67(s, 12H, –OCH3). Anal. Calcd. C52H50Mo2N6O8: C, 57.89; H, 4.67; N, 7.79; Found: C, 57.07; H, 4.76; N, 7.59.

Refinement top

H atoms were positioned geometrically with C—H = 0.93, 0.97 and 0.96 Å, for aromatic, methylene, and methyl H atoms, respectively, and constrained to ride on their parent atoms, with Uiso(H) = xUeq(C), where x = 1.5 for methyl H and x = 1.2 for aromatic H atoms. The dichloromethane solvent molecule exhibits high thermal motions and was refined as disordered over four sites with equivalent bonds from the disordered components restrained to have similar lengths. C—Cl and Cl—Cl distances were fixed to 1.78 and 2.85 Å, respectively. The same Uij parameters were used for atoms C1s/C2s/C3s/C4s, Cl1/Cl3/Cl5/Cl7, Cl2/Cl4/Cl6/Cl8, leading to refined site occupancies of 0.09: 0.17: 0.22.

Computing details top

Data collection: APEX2 (Bruker, 2004); cell refinement: SAINT-Plus (Bruker, 2001); data reduction: SAINT-Plus (Bruker, 2001); program(s) used to solve structure: SHELXS97 (Sheldrick, 2008); program(s) used to refine structure: SHELXL97 (Sheldrick, 2008); molecular graphics: XP in SHELXTL (Sheldrick, 2008); software used to prepare material for publication: SHELXL97 (Sheldrick, 2008).

Figures top
[Figure 1] Fig. 1. Molecular structure of the title compound drawn with displacement ellipsoids at the 30% probability level. The dichloromethane solvent molecule and hydrogen atoms have been omitted for clarity.
(µ-Benzoato-κ2O:O')tris[µ-N,N'-bis(4- methoxyphenyl)formamidinato-κ2N:N']dimolybdenum(II) dichloromethane monosolvate top
Crystal data top
[Mo2(C15H15N2O2)3(C7H5O2)]·CH2Cl2Z = 2
Mr = 1163.79F(000) = 1188
Triclinic, P1Dx = 1.489 Mg m3
Hall symbol: -P 1Mo Kα radiation, λ = 0.71073 Å
a = 12.025 (4) ÅCell parameters from 6372 reflections
b = 13.705 (4) Åθ = 2.4–26.3°
c = 17.727 (6) ŵ = 0.65 mm1
α = 74.595 (4)°T = 293 K
β = 85.646 (4)°Block, yellow
γ = 67.238 (4)°0.25 × 0.20 × 0.20 mm
V = 2596.0 (14) Å3
Data collection top
Bruker SMART 1000
diffractometer
8981 independent reflections
Radiation source: fine-focus sealed tube6852 reflections with I > 2σ(I)
Graphite monochromatorRint = 0.018
ω scansθmax = 25.0°, θmin = 1.7°
Absorption correction: multi-scan
(SADABS; Sheldrick, 2004)
h = 1414
Tmin = 0.851, Tmax = 0.879k = 1616
10844 measured reflectionsl = 1621
Refinement top
Refinement on F2Primary atom site location: structure-invariant direct methods
Least-squares matrix: fullSecondary atom site location: difference Fourier map
R[F2 > 2σ(F2)] = 0.036Hydrogen site location: inferred from neighbouring sites
wR(F2) = 0.107H-atom parameters constrained
S = 1.03 w = 1/[σ2(Fo2) + (0.048P)2 + 2.2558P]
where P = (Fo2 + 2Fc2)/3
8981 reflections(Δ/σ)max = 0.001
652 parametersΔρmax = 0.65 e Å3
12 restraintsΔρmin = 0.59 e Å3
Crystal data top
[Mo2(C15H15N2O2)3(C7H5O2)]·CH2Cl2γ = 67.238 (4)°
Mr = 1163.79V = 2596.0 (14) Å3
Triclinic, P1Z = 2
a = 12.025 (4) ÅMo Kα radiation
b = 13.705 (4) ŵ = 0.65 mm1
c = 17.727 (6) ÅT = 293 K
α = 74.595 (4)°0.25 × 0.20 × 0.20 mm
β = 85.646 (4)°
Data collection top
Bruker SMART 1000
diffractometer
8981 independent reflections
Absorption correction: multi-scan
(SADABS; Sheldrick, 2004)
6852 reflections with I > 2σ(I)
Tmin = 0.851, Tmax = 0.879Rint = 0.018
10844 measured reflections
Refinement top
R[F2 > 2σ(F2)] = 0.03612 restraints
wR(F2) = 0.107H-atom parameters constrained
S = 1.03Δρmax = 0.65 e Å3
8981 reflectionsΔρmin = 0.59 e Å3
652 parameters
Special details top

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.

Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top
xyzUiso*/UeqOcc. (<1)
Mo10.29773 (2)0.27398 (2)0.599717 (16)0.03700 (8)
Mo20.33531 (3)0.20914 (2)0.719867 (16)0.03797 (9)
O10.1144 (2)0.37048 (19)0.61915 (13)0.0433 (6)
O20.1550 (2)0.29894 (19)0.74747 (13)0.0430 (6)
O30.0341 (3)0.1526 (2)0.31737 (17)0.0688 (8)
O40.1310 (3)0.1329 (3)1.00562 (19)0.0998 (12)
O50.6233 (3)0.2150 (3)0.26384 (17)0.0873 (10)
O60.8253 (3)0.2027 (3)0.9482 (2)0.0927 (11)
O70.1843 (3)0.7823 (2)0.34264 (17)0.0756 (9)
O80.4791 (4)0.3747 (3)1.0234 (2)0.1021 (12)
N10.2318 (2)0.1509 (2)0.59293 (15)0.0389 (6)
N20.2713 (2)0.0826 (2)0.72517 (15)0.0403 (7)
N30.4753 (2)0.1823 (2)0.57165 (16)0.0412 (7)
N40.5168 (2)0.1112 (2)0.70350 (16)0.0432 (7)
N50.3333 (2)0.4157 (2)0.59902 (16)0.0421 (7)
N60.3733 (3)0.3454 (2)0.73067 (16)0.0435 (7)
C10.0832 (3)0.3611 (3)0.6901 (2)0.0426 (8)
C20.04220 (18)0.4275 (2)0.70731 (14)0.0478 (9)
C30.1242 (2)0.4981 (2)0.64675 (12)0.0542 (10)
H3A0.10170.50210.59500.065*
C40.2400 (2)0.5626 (2)0.66352 (16)0.0662 (12)
H4A0.29490.60980.62300.079*
C50.2737 (2)0.5565 (3)0.74086 (19)0.0862 (16)
H5A0.35120.59960.75210.103*
C60.1917 (3)0.4859 (3)0.80143 (13)0.114 (2)
H6A0.21420.48190.85320.137*
C70.0759 (2)0.4214 (3)0.78465 (13)0.0836 (16)
H7A0.02100.37420.82520.100*
C80.2241 (3)0.0832 (3)0.6604 (2)0.0415 (8)
H80.18510.03600.66190.050*
C90.1847 (3)0.1445 (3)0.52418 (19)0.0384 (8)
C100.1831 (3)0.0494 (3)0.5125 (2)0.0488 (9)
H100.21680.01570.55100.059*
C110.1329 (3)0.0480 (3)0.4454 (2)0.0530 (9)
H110.13030.01670.44000.064*
C120.0868 (3)0.1430 (3)0.3867 (2)0.0506 (9)
C130.0926 (3)0.2379 (3)0.3953 (2)0.0511 (9)
H130.06450.30160.35490.061*
C140.1396 (3)0.2391 (3)0.4633 (2)0.0470 (9)
H140.14140.30420.46870.056*
C150.0363 (5)0.0556 (4)0.3027 (3)0.0888 (16)
H15A0.11830.00470.30430.133*
H15B0.00040.07230.25190.133*
H15C0.00820.02380.34190.133*
C160.2377 (3)0.0263 (3)0.7972 (2)0.0436 (8)
C170.1183 (4)0.0429 (3)0.8126 (2)0.0559 (10)
H170.05890.09220.77530.067*
C180.0853 (4)0.0121 (4)0.8822 (2)0.0672 (12)
H180.00460.00130.89110.081*
C190.1727 (4)0.0829 (4)0.9381 (2)0.0631 (11)
C200.2916 (4)0.0983 (4)0.9253 (2)0.0645 (12)
H200.35030.14530.96370.077*
C210.3242 (4)0.0435 (3)0.8545 (2)0.0530 (10)
H210.40480.05410.84590.064*
C220.2169 (6)0.2152 (5)1.0604 (3)0.115 (2)
H22A0.26920.27011.03570.172*
H22B0.17700.24771.10250.172*
H22C0.26360.18421.08070.172*
C230.5519 (3)0.1167 (3)0.6304 (2)0.0456 (9)
H230.63040.07450.62030.055*
C240.5180 (3)0.1901 (3)0.49368 (19)0.0403 (8)
C250.5999 (3)0.2382 (3)0.4668 (2)0.0482 (9)
H250.63010.26450.50040.058*
C260.6380 (4)0.2482 (3)0.3903 (2)0.0539 (10)
H260.69370.28070.37300.065*
C270.5935 (4)0.2101 (3)0.3401 (2)0.0551 (10)
C280.5139 (4)0.1594 (4)0.3678 (2)0.0682 (12)
H280.48580.13080.33480.082*
C290.4754 (3)0.1502 (3)0.4434 (2)0.0561 (10)
H290.42040.11710.46070.067*
C300.7083 (5)0.2601 (4)0.2326 (3)0.0922 (17)
H30A0.67730.33600.23260.138*
H30B0.72420.25360.17990.138*
H30C0.78170.22170.26380.138*
C310.5973 (3)0.0305 (3)0.7652 (2)0.0459 (9)
C320.6731 (4)0.0721 (3)0.7584 (2)0.0573 (10)
H320.67380.09050.71150.069*
C330.7477 (4)0.1475 (4)0.8199 (3)0.0712 (13)
H330.79770.21650.81450.085*
C340.7482 (4)0.1208 (4)0.8895 (3)0.0657 (12)
C350.6727 (4)0.0204 (4)0.8979 (2)0.0653 (12)
H350.67150.00280.94520.078*
C360.5979 (4)0.0551 (3)0.8359 (2)0.0581 (10)
H360.54710.12360.84190.070*
C370.8501 (5)0.1717 (5)1.0130 (3)0.0993 (18)
H37A0.87810.11290.99480.149*
H37B0.91110.23311.04650.149*
H37C0.77790.14791.04170.149*
C380.3554 (3)0.4280 (3)0.6667 (2)0.0446 (8)
H380.35860.49350.66990.054*
C390.2985 (3)0.5108 (3)0.5337 (2)0.0413 (8)
C400.3649 (3)0.5121 (3)0.4674 (2)0.0509 (9)
H400.43510.45170.46590.061*
C410.3306 (3)0.6007 (3)0.4027 (2)0.0535 (10)
H410.37720.59950.35840.064*
C420.2273 (4)0.6906 (3)0.4040 (2)0.0522 (10)
C430.1598 (4)0.6910 (3)0.4702 (3)0.0635 (12)
H430.09010.75170.47170.076*
C440.1950 (4)0.6019 (3)0.5345 (2)0.0599 (11)
H440.14860.60310.57890.072*
C450.2434 (5)0.7782 (4)0.2708 (3)0.0832 (15)
H45A0.32620.76720.27790.125*
H45B0.20420.84580.23230.125*
H45C0.23990.71870.25350.125*
C460.3980 (3)0.3583 (3)0.8035 (2)0.0465 (9)
C470.3522 (4)0.3100 (4)0.8706 (2)0.0636 (11)
H470.30310.27360.86570.076*
C480.3765 (5)0.3138 (4)0.9441 (2)0.0733 (13)
H480.34520.27930.98790.088*
C490.4469 (5)0.3686 (4)0.9525 (3)0.0707 (13)
C500.4929 (4)0.4187 (4)0.8872 (3)0.0746 (13)
H500.53960.45720.89250.090*
C510.4704 (4)0.4122 (3)0.8137 (2)0.0609 (11)
H510.50430.44450.77030.073*
C520.4277 (6)0.3290 (5)1.0907 (3)0.107 (2)
H52A0.34170.36731.08750.161*
H52B0.45950.33541.13650.161*
H52C0.44690.25311.09410.161*
Cl10.0625 (11)0.6320 (9)0.8223 (8)0.212 (3)0.30
Cl20.1659 (16)0.6005 (13)0.9619 (8)0.201 (3)0.30
C1S0.087 (2)0.7044 (19)0.8855 (14)0.231 (14)0.30
H1S0.00960.73290.90900.278*0.30
H2S0.11400.76380.86260.278*0.30
Cl30.0397 (10)0.5605 (9)0.8530 (8)0.212 (3)0.30
Cl40.1674 (16)0.6251 (13)0.9421 (9)0.201 (3)0.30
C2S0.1004 (11)0.5307 (9)0.9493 (7)0.231 (14)0.30
H3S0.16210.45730.96290.278*0.30
H4S0.03680.53470.98690.278*0.30
Cl50.1180 (11)0.5692 (9)0.7925 (7)0.212 (3)0.20
Cl60.0177 (11)0.5259 (9)0.9404 (7)0.201 (3)0.20
C3S0.1202 (11)0.5839 (9)0.8918 (7)0.231 (14)0.20
H5S0.09370.66030.89200.278*0.20
H6S0.20040.54440.91600.278*0.20
Cl70.1116 (16)0.5654 (14)0.9890 (10)0.212 (3)0.20
Cl80.106 (2)0.5768 (15)0.8222 (10)0.201 (3)0.20
C4S0.061 (4)0.646 (3)0.8957 (14)0.231 (14)0.20
H7S0.02210.69630.88990.278*0.20
H8S0.11020.68950.88700.278*0.20
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
Mo10.03930 (16)0.04008 (17)0.03241 (15)0.01679 (13)0.00142 (12)0.00815 (12)
Mo20.04070 (17)0.04118 (17)0.03255 (15)0.01694 (13)0.00125 (12)0.00835 (12)
O10.0418 (13)0.0437 (13)0.0410 (13)0.0134 (11)0.0021 (10)0.0101 (11)
O20.0425 (13)0.0430 (13)0.0390 (13)0.0123 (11)0.0022 (10)0.0095 (10)
O30.0794 (19)0.0722 (19)0.0598 (17)0.0247 (16)0.0177 (15)0.0260 (15)
O40.105 (3)0.118 (3)0.0529 (19)0.042 (2)0.0234 (18)0.0085 (19)
O50.106 (2)0.125 (3)0.0418 (16)0.055 (2)0.0204 (16)0.0279 (17)
O60.094 (2)0.081 (2)0.071 (2)0.010 (2)0.0320 (19)0.0046 (18)
O70.086 (2)0.0577 (18)0.0575 (18)0.0157 (16)0.0073 (16)0.0073 (14)
O80.156 (3)0.104 (3)0.059 (2)0.054 (3)0.028 (2)0.0257 (19)
N10.0428 (15)0.0406 (15)0.0341 (14)0.0180 (13)0.0009 (12)0.0075 (12)
N20.0452 (15)0.0416 (16)0.0350 (15)0.0200 (13)0.0022 (12)0.0060 (12)
N30.0400 (15)0.0493 (17)0.0353 (15)0.0165 (13)0.0029 (12)0.0136 (13)
N40.0401 (15)0.0471 (17)0.0374 (15)0.0126 (13)0.0022 (12)0.0083 (13)
N50.0468 (16)0.0466 (16)0.0366 (15)0.0239 (14)0.0008 (12)0.0071 (13)
N60.0491 (16)0.0468 (17)0.0385 (15)0.0219 (14)0.0001 (13)0.0115 (13)
C10.0450 (19)0.0376 (18)0.047 (2)0.0168 (16)0.0060 (16)0.0132 (16)
C20.048 (2)0.044 (2)0.047 (2)0.0151 (17)0.0056 (17)0.0103 (16)
C30.056 (2)0.048 (2)0.059 (2)0.0171 (19)0.0017 (19)0.0184 (19)
C40.056 (2)0.061 (3)0.073 (3)0.017 (2)0.003 (2)0.011 (2)
C50.059 (3)0.094 (4)0.084 (4)0.007 (3)0.013 (3)0.023 (3)
C60.076 (3)0.141 (5)0.065 (3)0.013 (4)0.020 (3)0.016 (3)
C70.069 (3)0.092 (4)0.055 (3)0.001 (3)0.005 (2)0.011 (3)
C80.0455 (19)0.0405 (19)0.0441 (19)0.0219 (16)0.0029 (15)0.0119 (15)
C90.0341 (16)0.0404 (18)0.0409 (18)0.0140 (14)0.0043 (14)0.0121 (15)
C100.056 (2)0.042 (2)0.047 (2)0.0174 (17)0.0045 (17)0.0087 (16)
C110.063 (2)0.050 (2)0.056 (2)0.0261 (19)0.0000 (19)0.0227 (18)
C120.047 (2)0.063 (2)0.045 (2)0.0196 (18)0.0015 (16)0.0212 (18)
C130.058 (2)0.046 (2)0.046 (2)0.0159 (18)0.0047 (17)0.0095 (17)
C140.054 (2)0.046 (2)0.042 (2)0.0203 (17)0.0006 (16)0.0095 (16)
C150.110 (4)0.096 (4)0.084 (3)0.050 (3)0.017 (3)0.040 (3)
C160.055 (2)0.0409 (19)0.0387 (18)0.0223 (17)0.0074 (16)0.0128 (15)
C170.056 (2)0.067 (3)0.044 (2)0.025 (2)0.0016 (18)0.0084 (19)
C180.061 (3)0.084 (3)0.056 (3)0.032 (2)0.016 (2)0.014 (2)
C190.080 (3)0.065 (3)0.043 (2)0.031 (2)0.016 (2)0.0087 (19)
C200.073 (3)0.063 (3)0.043 (2)0.018 (2)0.002 (2)0.0013 (19)
C210.059 (2)0.051 (2)0.044 (2)0.0214 (19)0.0063 (18)0.0057 (17)
C220.155 (6)0.126 (5)0.055 (3)0.073 (4)0.003 (3)0.020 (3)
C230.0365 (18)0.053 (2)0.046 (2)0.0158 (16)0.0017 (16)0.0129 (17)
C240.0383 (17)0.0429 (19)0.0375 (18)0.0121 (15)0.0029 (14)0.0126 (15)
C250.055 (2)0.052 (2)0.046 (2)0.0241 (18)0.0062 (17)0.0213 (17)
C260.061 (2)0.050 (2)0.054 (2)0.0254 (19)0.0149 (19)0.0165 (18)
C270.058 (2)0.062 (2)0.038 (2)0.016 (2)0.0058 (17)0.0142 (18)
C280.067 (3)0.108 (4)0.051 (2)0.046 (3)0.003 (2)0.037 (2)
C290.052 (2)0.073 (3)0.056 (2)0.033 (2)0.0093 (18)0.026 (2)
C300.116 (4)0.100 (4)0.056 (3)0.042 (3)0.034 (3)0.019 (3)
C310.0392 (18)0.053 (2)0.043 (2)0.0190 (17)0.0004 (15)0.0066 (17)
C320.059 (2)0.056 (2)0.052 (2)0.015 (2)0.0056 (19)0.0140 (19)
C330.066 (3)0.057 (3)0.071 (3)0.004 (2)0.007 (2)0.014 (2)
C340.060 (3)0.067 (3)0.057 (3)0.017 (2)0.016 (2)0.001 (2)
C350.073 (3)0.073 (3)0.044 (2)0.024 (2)0.010 (2)0.008 (2)
C360.068 (3)0.053 (2)0.046 (2)0.017 (2)0.0026 (19)0.0095 (18)
C370.106 (4)0.105 (4)0.068 (3)0.032 (3)0.042 (3)0.009 (3)
C380.051 (2)0.0424 (19)0.047 (2)0.0237 (17)0.0032 (16)0.0131 (16)
C390.0439 (18)0.0410 (19)0.0441 (19)0.0221 (16)0.0012 (15)0.0096 (15)
C400.053 (2)0.049 (2)0.047 (2)0.0148 (18)0.0020 (17)0.0124 (17)
C410.059 (2)0.060 (2)0.041 (2)0.025 (2)0.0095 (17)0.0110 (18)
C420.061 (2)0.045 (2)0.049 (2)0.0236 (19)0.0028 (18)0.0022 (17)
C430.056 (2)0.049 (2)0.067 (3)0.010 (2)0.011 (2)0.003 (2)
C440.054 (2)0.058 (2)0.056 (2)0.019 (2)0.0154 (19)0.0033 (19)
C450.114 (4)0.064 (3)0.055 (3)0.029 (3)0.004 (3)0.003 (2)
C460.058 (2)0.0415 (19)0.044 (2)0.0195 (17)0.0005 (17)0.0141 (16)
C470.086 (3)0.070 (3)0.050 (2)0.041 (2)0.004 (2)0.022 (2)
C480.104 (4)0.080 (3)0.043 (2)0.039 (3)0.008 (2)0.022 (2)
C490.097 (3)0.066 (3)0.051 (2)0.025 (3)0.019 (2)0.021 (2)
C500.097 (3)0.071 (3)0.069 (3)0.043 (3)0.025 (3)0.017 (2)
C510.074 (3)0.067 (3)0.051 (2)0.038 (2)0.009 (2)0.008 (2)
C520.139 (5)0.111 (4)0.052 (3)0.014 (4)0.013 (3)0.037 (3)
Cl10.174 (6)0.163 (6)0.279 (9)0.059 (5)0.030 (5)0.025 (6)
Cl20.225 (5)0.196 (6)0.188 (6)0.102 (4)0.033 (4)0.034 (4)
C1S0.096 (13)0.27 (3)0.38 (4)0.106 (17)0.026 (17)0.11 (3)
Cl30.174 (6)0.163 (6)0.279 (9)0.059 (5)0.030 (5)0.025 (6)
Cl40.225 (5)0.196 (6)0.188 (6)0.102 (4)0.033 (4)0.034 (4)
C2S0.096 (13)0.27 (3)0.38 (4)0.106 (17)0.026 (17)0.11 (3)
Cl50.174 (6)0.163 (6)0.279 (9)0.059 (5)0.030 (5)0.025 (6)
Cl60.225 (5)0.196 (6)0.188 (6)0.102 (4)0.033 (4)0.034 (4)
C3S0.096 (13)0.27 (3)0.38 (4)0.106 (17)0.026 (17)0.11 (3)
Cl70.174 (6)0.163 (6)0.279 (9)0.059 (5)0.030 (5)0.025 (6)
Cl80.225 (5)0.196 (6)0.188 (6)0.102 (4)0.033 (4)0.034 (4)
C4S0.096 (13)0.27 (3)0.38 (4)0.106 (17)0.026 (17)0.11 (3)
Geometric parameters (Å, º) top
Mo1—Mo22.0881 (8)C28—C291.374 (5)
Mo1—N32.117 (3)C28—H280.9300
Mo1—N52.142 (3)C29—H290.9300
Mo1—O12.144 (2)C30—H30A0.9600
Mo1—N12.156 (3)C30—H30B0.9600
Mo2—N42.120 (3)C30—H30C0.9600
Mo2—N22.132 (3)C31—C321.380 (5)
Mo2—O22.133 (2)C31—C361.382 (5)
Mo2—N62.144 (3)C32—C331.377 (5)
O1—C11.272 (4)C32—H320.9300
O2—C11.269 (4)C33—C341.378 (6)
O3—C121.378 (4)C33—H330.9300
O3—C151.411 (5)C34—C351.365 (6)
O4—C191.376 (5)C35—C361.384 (5)
O4—C221.397 (6)C35—H350.9300
O5—C271.362 (4)C36—H360.9300
O5—C301.399 (6)C37—H37A0.9600
O6—C341.387 (5)C37—H37B0.9600
O6—C371.414 (6)C37—H37C0.9600
O7—C421.373 (4)C38—H380.9300
O7—C451.414 (5)C39—C401.370 (5)
O8—C491.375 (5)C39—C441.382 (5)
O8—C521.412 (7)C40—C411.379 (5)
N1—C81.326 (4)C40—H400.9300
N1—C91.419 (4)C41—C421.374 (5)
N2—C81.315 (4)C41—H410.9300
N2—C161.424 (4)C42—C431.376 (5)
N3—C231.322 (4)C43—C441.379 (5)
N3—C241.429 (4)C43—H430.9300
N4—C231.324 (4)C44—H440.9300
N4—C311.431 (4)C45—H45A0.9600
N5—C381.314 (4)C45—H45B0.9600
N5—C391.437 (4)C45—H45C0.9600
N6—C381.334 (4)C46—C471.386 (5)
N6—C461.416 (4)C46—C511.388 (5)
C1—C21.487 (4)C47—C481.376 (6)
C2—C31.3900C47—H470.9300
C2—C71.3900C48—C491.369 (7)
C3—C41.3900C48—H480.9300
C3—H3A0.9300C49—C501.376 (6)
C4—C51.3900C50—C511.383 (6)
C4—H4A0.9300C50—H500.9300
C5—C61.3900C51—H510.9300
C5—H5A0.9300C52—H52A0.9600
C6—C71.3900C52—H52B0.9600
C6—H6A0.9300C52—H52C0.9600
C7—H7A0.9300Cl1—C1S1.786 (18)
C8—H80.9300Cl1—H5S1.5004
C9—C101.380 (5)Cl1—H7S1.7118
C9—C141.394 (5)Cl1—H8S1.7870
C10—C111.382 (5)Cl2—C1S1.699 (18)
C10—H100.9300Cl2—H5S1.4265
C11—C121.377 (5)Cl2—H6S1.2080
C11—H110.9300Cl2—H8S1.5302
C12—C131.377 (5)C1S—H1S0.9700
C13—C141.376 (5)C1S—H2S0.9699
C13—H130.9300C1S—H5S0.5593
C14—H140.9300C1S—H8S0.2721
C15—H15A0.9600Cl3—C2S1.790 (13)
C15—H15B0.9600Cl4—C2S1.745 (14)
C15—H15C0.9600Cl4—H5S1.1702
C16—C211.380 (5)Cl4—H6S1.2247
C16—C171.381 (5)Cl4—H8S1.1748
C17—C181.382 (5)C2S—H3S0.9699
C17—H170.9300C2S—H4S0.9701
C18—C191.374 (6)Cl5—C3S1.8275
C18—H180.9300Cl6—C3S1.7675
C19—C201.372 (6)Cl6—Cl6i2.11 (2)
C20—C211.394 (5)Cl6—H3S1.6434
C20—H200.9300Cl6—H4S0.9219
C21—H210.9300C3S—H5S0.9700
C22—H22A0.9600C3S—H6S0.9701
C22—H22B0.9600Cl7—C4S1.726 (19)
C22—H22C0.9600Cl7—H3S1.5497
C23—H230.9300Cl7—H4S1.1378
C24—C251.377 (5)Cl7—H6S1.6270
C24—C291.379 (5)Cl8—C4S1.74 (2)
C25—C261.387 (5)C4S—H1S1.1946
C25—H250.9300C4S—H5S0.4944
C26—C271.374 (6)C4S—H7S0.9700
C26—H260.9300C4S—H8S0.9701
C27—C281.381 (6)
Mo2—Mo1—N392.56 (7)C36—C31—N4118.7 (3)
Mo2—Mo1—N592.51 (7)C33—C32—C31121.0 (4)
N3—Mo1—N595.00 (11)C33—C32—H32119.5
Mo2—Mo1—O191.61 (6)C31—C32—H32119.5
N3—Mo1—O1175.79 (9)C32—C33—C34120.0 (4)
N5—Mo1—O185.37 (10)C32—C33—H33120.0
Mo2—Mo1—N192.50 (7)C34—C33—H33120.0
N3—Mo1—N193.12 (11)C35—C34—C33119.9 (4)
N5—Mo1—N1170.25 (10)C35—C34—O6124.4 (4)
O1—Mo1—N186.14 (10)C33—C34—O6115.7 (4)
Mo1—Mo2—N492.95 (8)C34—C35—C36119.8 (4)
Mo1—Mo2—N292.96 (7)C34—C35—H35120.1
N4—Mo2—N293.97 (11)C36—C35—H35120.1
Mo1—Mo2—O292.27 (6)C31—C36—C35121.2 (4)
N4—Mo2—O2174.64 (10)C31—C36—H36119.4
N2—Mo2—O284.56 (10)C35—C36—H36119.4
Mo1—Mo2—N692.77 (8)O6—C37—H37A109.5
N4—Mo2—N695.24 (11)O6—C37—H37B109.5
N2—Mo2—N6168.88 (11)H37A—C37—H37B109.5
O2—Mo2—N685.70 (10)O6—C37—H37C109.5
C1—O1—Mo1116.5 (2)H37A—C37—H37C109.5
C1—O2—Mo2116.6 (2)H37B—C37—H37C109.5
C12—O3—C15117.3 (3)N5—C38—N6119.3 (3)
C19—O4—C22117.3 (4)N5—C38—H38120.4
C27—O5—C30118.7 (4)N6—C38—H38120.4
C34—O6—C37117.2 (4)C40—C39—C44118.0 (3)
C42—O7—C45117.1 (3)C40—C39—N5120.7 (3)
C49—O8—C52117.2 (4)C44—C39—N5121.3 (3)
C8—N1—C9118.2 (3)C39—C40—C41121.8 (4)
C8—N1—Mo1116.2 (2)C39—C40—H40119.1
C9—N1—Mo1125.3 (2)C41—C40—H40119.1
C8—N2—C16117.3 (3)C42—C41—C40119.8 (3)
C8—N2—Mo2117.2 (2)C42—C41—H41120.1
C16—N2—Mo2121.4 (2)C40—C41—H41120.1
C23—N3—C24118.4 (3)O7—C42—C41124.5 (4)
C23—N3—Mo1117.5 (2)O7—C42—C43116.3 (4)
C24—N3—Mo1124.0 (2)C41—C42—C43119.2 (3)
C23—N4—C31118.5 (3)C42—C43—C44120.4 (4)
C23—N4—Mo2117.0 (2)C42—C43—H43119.8
C31—N4—Mo2124.1 (2)C44—C43—H43119.8
C38—N5—C39117.5 (3)C43—C44—C39120.8 (4)
C38—N5—Mo1117.7 (2)C43—C44—H44119.6
C39—N5—Mo1121.9 (2)C39—C44—H44119.6
C38—N6—C46119.3 (3)O7—C45—H45A109.5
C38—N6—Mo2116.9 (2)O7—C45—H45B109.5
C46—N6—Mo2123.1 (2)H45A—C45—H45B109.5
O2—C1—O1123.0 (3)O7—C45—H45C109.5
O2—C1—C2118.0 (3)H45A—C45—H45C109.5
O1—C1—C2119.0 (3)H45B—C45—H45C109.5
C3—C2—C7120.0C47—C46—C51116.5 (4)
C3—C2—C1120.4 (2)C47—C46—N6118.7 (3)
C7—C2—C1119.5 (2)C51—C46—N6124.7 (3)
C4—C3—C2120.0C48—C47—C46122.6 (4)
C4—C3—H3A120.0C48—C47—H47118.7
C2—C3—H3A120.0C46—C47—H47118.7
C3—C4—C5120.0C49—C48—C47119.7 (4)
C3—C4—H4A120.0C49—C48—H48120.2
C5—C4—H4A120.0C47—C48—H48120.2
C6—C5—C4120.0C48—C49—O8124.2 (5)
C6—C5—H5A120.0C48—C49—C50119.4 (4)
C4—C5—H5A120.0O8—C49—C50116.4 (4)
C5—C6—C7120.0C49—C50—C51120.5 (4)
C5—C6—H6A120.0C49—C50—H50119.8
C7—C6—H6A120.0C51—C50—H50119.8
C6—C7—C2120.0C50—C51—C46121.2 (4)
C6—C7—H7A120.0C50—C51—H51119.4
C2—C7—H7A120.0C46—C51—H51119.4
N2—C8—N1120.5 (3)O8—C52—H52A109.5
N2—C8—H8119.8O8—C52—H52B109.5
N1—C8—H8119.8H52A—C52—H52B109.5
C10—C9—C14117.3 (3)O8—C52—H52C109.5
C10—C9—N1124.2 (3)H52A—C52—H52C109.5
C14—C9—N1118.6 (3)H52B—C52—H52C109.5
C9—C10—C11122.0 (3)C1S—Cl1—H7S45.5
C9—C10—H10119.0H5S—Cl1—H7S46.6
C11—C10—H10119.0H7S—Cl1—H8S52.7
C12—C11—C10119.6 (4)C1S—Cl2—H6S87.0
C12—C11—H11120.2H5S—Cl2—H6S73.2
C10—C11—H11120.2H6S—Cl2—H8S81.7
C11—C12—C13119.5 (3)Cl2—C1S—Cl1102.0 (12)
C11—C12—O3125.2 (4)Cl2—C1S—H1S100.5
C13—C12—O3115.3 (3)Cl1—C1S—H1S104.0
C14—C13—C12120.4 (3)Cl2—C1S—H2S120.3
C14—C13—H13119.8Cl1—C1S—H2S118.3
C12—C13—H13119.8H1S—C1S—H2S109.3
C13—C14—C9121.1 (4)Cl2—C1S—H5S52.2
C13—C14—H14119.4Cl1—C1S—H5S51.2
C9—C14—H14119.4H1S—C1S—H5S99.8
O3—C15—H15A109.5H2S—C1S—H5S151.0
O3—C15—H15B109.5Cl2—C1S—H7S102.4
H15A—C15—H15B109.5Cl1—C1S—H7S64.3
O3—C15—H15C109.5H2S—C1S—H7S133.4
H15A—C15—H15C109.5H5S—C1S—H7S70.8
H15B—C15—H15C109.5Cl2—C1S—H8S47.9
C21—C16—C17118.5 (3)Cl1—C1S—H8S85.8
C21—C16—N2120.3 (3)H1S—C1S—H8S148.5
C17—C16—N2121.2 (3)H2S—C1S—H8S91.1
C16—C17—C18121.4 (4)H5S—C1S—H8S63.0
C16—C17—H17119.3H7S—C1S—H8S133.7
C18—C17—H17119.3C2S—Cl4—H5S71.8
C19—C18—C17119.3 (4)C2S—Cl4—H6S50.7
C19—C18—H18120.3H5S—Cl4—H6S82.5
C17—C18—H18120.3C2S—Cl4—H8S96.3
C20—C19—C18120.4 (4)H6S—Cl4—H8S97.8
C20—C19—O4124.5 (4)Cl4—C2S—Cl3104.4 (7)
C18—C19—O4115.1 (4)Cl4—C2S—H3S109.0
C19—C20—C21119.8 (4)Cl3—C2S—H3S109.9
C19—C20—H20120.1Cl4—C2S—H4S115.2
C21—C20—H20120.1Cl3—C2S—H4S109.6
C16—C21—C20120.5 (4)H3S—C2S—H4S108.6
C16—C21—H21119.8Cl3—C2S—H6S88.3
C20—C21—H21119.8H3S—C2S—H6S76.5
O4—C22—H22A109.5H4S—C2S—H6S157.3
O4—C22—H22B109.5C3S—Cl6—Cl6i133.0 (7)
H22A—C22—H22B109.5C3S—Cl6—H3S62.1
O4—C22—H22C109.5Cl6i—Cl6—H3S88.1
H22A—C22—H22C109.5C3S—Cl6—H4S89.8
H22B—C22—H22C109.5H3S—Cl6—H4S69.3
N3—C23—N4120.0 (3)Cl6—C3S—Cl5103.1
N3—C23—H23120.0Cl6—C3S—H5S111.1
N4—C23—H23120.0Cl5—C3S—H5S111.2
C25—C24—C29118.8 (3)Cl6—C3S—H6S111.1
C25—C24—N3121.6 (3)Cl5—C3S—H6S111.2
C29—C24—N3119.6 (3)H5S—C3S—H6S109.1
C24—C25—C26121.1 (4)Cl6—C3S—H8S124.3
C24—C25—H25119.5Cl5—C3S—H8S108.4
C26—C25—H25119.5H6S—C3S—H8S98.8
C27—C26—C25119.9 (4)C4S—Cl7—H3S93.5
C27—C26—H26120.1C4S—Cl7—H4S85.7
C25—C26—H26120.1H3S—Cl7—H4S69.8
O5—C27—C26125.7 (4)C4S—Cl7—H6S60.7
O5—C27—C28115.3 (4)H3S—Cl7—H6S55.1
C26—C27—C28118.9 (4)H4S—Cl7—H6S110.0
C29—C28—C27121.2 (4)Cl7—C4S—Cl8115.0 (17)
C29—C28—H28119.4Cl7—C4S—H1S100.2
C27—C28—H28119.4Cl8—C4S—H1S144.7
C28—C29—C24120.1 (4)Cl7—C4S—H5S94.0
C28—C29—H29119.9Cl8—C4S—H5S96.0
C24—C29—H29119.9H1S—C4S—H5S78.6
O5—C30—H30A109.5Cl7—C4S—H7S116.4
O5—C30—H30B109.5Cl8—C4S—H7S113.6
H30A—C30—H30B109.5H1S—C4S—H7S46.3
O5—C30—H30C109.5Cl7—C4S—H8S100.1
H30A—C30—H30C109.5Cl8—C4S—H8S102.8
H30B—C30—H30C109.5H1S—C4S—H8S67.1
C32—C31—C36118.0 (3)H7S—C4S—H8S106.6
C32—C31—N4123.3 (3)
N3—Mo1—Mo2—N40.09 (11)O3—C12—C13—C14177.8 (3)
N5—Mo1—Mo2—N495.03 (11)C12—C13—C14—C91.4 (6)
O1—Mo1—Mo2—N4179.53 (10)C10—C9—C14—C131.7 (5)
N1—Mo1—Mo2—N493.33 (11)N1—C9—C14—C13179.8 (3)
N3—Mo1—Mo2—N294.05 (11)C8—N2—C16—C21134.2 (4)
N5—Mo1—Mo2—N2170.83 (10)Mo2—N2—C16—C2169.0 (4)
O1—Mo1—Mo2—N285.40 (10)C8—N2—C16—C1748.0 (5)
N1—Mo1—Mo2—N20.81 (10)Mo2—N2—C16—C17108.8 (4)
N3—Mo1—Mo2—O2178.71 (10)C21—C16—C17—C182.7 (6)
N5—Mo1—Mo2—O286.17 (10)N2—C16—C17—C18179.5 (4)
O1—Mo1—Mo2—O20.73 (9)C16—C17—C18—C191.6 (7)
N1—Mo1—Mo2—O285.47 (10)C17—C18—C19—C200.4 (7)
N3—Mo1—Mo2—N695.49 (11)C17—C18—C19—O4179.4 (4)
N5—Mo1—Mo2—N60.37 (10)C22—O4—C19—C208.5 (8)
O1—Mo1—Mo2—N685.07 (10)C22—O4—C19—C18172.6 (5)
N1—Mo1—Mo2—N6171.27 (10)C18—C19—C20—C211.2 (7)
Mo2—Mo1—O1—C10.9 (2)O4—C19—C20—C21179.9 (4)
N5—Mo1—O1—C193.3 (2)C17—C16—C21—C201.9 (6)
N1—Mo1—O1—C191.5 (2)N2—C16—C21—C20179.7 (4)
Mo1—Mo2—O2—C10.9 (2)C19—C20—C21—C160.1 (7)
N2—Mo2—O2—C193.6 (2)C24—N3—C23—N4177.0 (3)
N6—Mo2—O2—C191.7 (2)Mo1—N3—C23—N40.8 (5)
Mo2—Mo1—N1—C85.5 (2)C31—N4—C23—N3172.9 (3)
N3—Mo1—N1—C898.2 (2)Mo2—N4—C23—N30.9 (5)
O1—Mo1—N1—C885.9 (2)C23—N3—C24—C2568.3 (5)
Mo2—Mo1—N1—C9178.4 (2)Mo1—N3—C24—C25109.3 (3)
N3—Mo1—N1—C988.9 (2)C23—N3—C24—C29112.7 (4)
O1—Mo1—N1—C986.9 (2)Mo1—N3—C24—C2969.7 (4)
Mo1—Mo2—N2—C83.7 (2)C29—C24—C25—C260.9 (5)
N4—Mo2—N2—C896.9 (2)N3—C24—C25—C26178.1 (3)
O2—Mo2—N2—C888.3 (2)C24—C25—C26—C270.3 (6)
N6—Mo2—N2—C8117.2 (5)C30—O5—C27—C261.5 (7)
Mo1—Mo2—N2—C16160.4 (2)C30—O5—C27—C28176.7 (4)
N4—Mo2—N2—C16106.4 (3)C25—C26—C27—O5179.9 (4)
O2—Mo2—N2—C1668.4 (2)C25—C26—C27—C281.9 (6)
N6—Mo2—N2—C1639.5 (7)O5—C27—C28—C29179.2 (4)
Mo2—Mo1—N3—C230.3 (3)C26—C27—C28—C292.5 (7)
N5—Mo1—N3—C2393.1 (3)C27—C28—C29—C241.3 (7)
N1—Mo1—N3—C2392.3 (3)C25—C24—C29—C280.4 (6)
Mo2—Mo1—N3—C24177.3 (3)N3—C24—C29—C28178.6 (4)
N5—Mo1—N3—C2484.6 (3)C23—N4—C31—C3235.2 (5)
N1—Mo1—N3—C2490.0 (3)Mo2—N4—C31—C32136.2 (3)
Mo1—Mo2—N4—C230.5 (3)C23—N4—C31—C36146.2 (4)
N2—Mo2—N4—C2392.7 (3)Mo2—N4—C31—C3642.4 (4)
N6—Mo2—N4—C2393.6 (3)C36—C31—C32—C330.4 (6)
Mo1—Mo2—N4—C31172.0 (3)N4—C31—C32—C33179.0 (4)
N2—Mo2—N4—C3178.9 (3)C31—C32—C33—C340.6 (7)
N6—Mo2—N4—C3194.9 (3)C32—C33—C34—C351.5 (7)
Mo2—Mo1—N5—C385.5 (2)C32—C33—C34—O6179.2 (4)
N3—Mo1—N5—C3898.3 (3)C37—O6—C34—C3516.9 (7)
O1—Mo1—N5—C3885.9 (3)C37—O6—C34—C33165.5 (5)
Mo2—Mo1—N5—C39166.2 (2)C33—C34—C35—C361.5 (7)
N3—Mo1—N5—C39101.1 (3)O6—C34—C35—C36179.0 (4)
O1—Mo1—N5—C3974.7 (2)C32—C31—C36—C350.5 (6)
Mo1—Mo2—N6—C384.6 (2)N4—C31—C36—C35179.1 (4)
N4—Mo2—N6—C3897.8 (3)C34—C35—C36—C310.5 (7)
N2—Mo2—N6—C38116.4 (5)C39—N5—C38—N6171.7 (3)
O2—Mo2—N6—C3887.5 (2)Mo1—N5—C38—N610.2 (4)
Mo1—Mo2—N6—C46174.9 (3)C46—N6—C38—N5179.5 (3)
N4—Mo2—N6—C4691.9 (3)Mo2—N6—C38—N59.8 (4)
N2—Mo2—N6—C4653.9 (6)C38—N5—C39—C40121.3 (4)
O2—Mo2—N6—C4682.8 (3)Mo1—N5—C39—C4078.1 (4)
Mo2—O2—C1—O10.4 (4)C38—N5—C39—C4461.1 (5)
Mo2—O2—C1—C2178.1 (2)Mo1—N5—C39—C4499.5 (4)
Mo1—O1—C1—O20.4 (4)C44—C39—C40—C410.4 (6)
Mo1—O1—C1—C2178.9 (2)N5—C39—C40—C41177.3 (3)
O2—C1—C2—C3179.1 (2)C39—C40—C41—C420.1 (6)
O1—C1—C2—C30.6 (4)C45—O7—C42—C417.4 (6)
O2—C1—C2—C71.3 (4)C45—O7—C42—C43172.2 (4)
O1—C1—C2—C7177.3 (3)C40—C41—C42—O7179.2 (4)
C7—C2—C3—C40.0C40—C41—C42—C430.3 (6)
C1—C2—C3—C4177.8 (3)O7—C42—C43—C44179.2 (4)
C2—C3—C4—C50.0C41—C42—C43—C440.4 (7)
C3—C4—C5—C60.0C42—C43—C44—C390.1 (7)
C4—C5—C6—C70.0C40—C39—C44—C430.3 (6)
C5—C6—C7—C20.0N5—C39—C44—C43177.4 (4)
C3—C2—C7—C60.0C38—N6—C46—C47144.1 (4)
C1—C2—C7—C6177.8 (3)Mo2—N6—C46—C4726.0 (5)
C16—N2—C8—N1166.7 (3)C38—N6—C46—C5139.0 (5)
Mo2—N2—C8—N19.0 (4)Mo2—N6—C46—C51150.9 (3)
C9—N1—C8—N2176.9 (3)C51—C46—C47—C480.3 (6)
Mo1—N1—C8—N29.7 (4)N6—C46—C47—C48176.8 (4)
C8—N1—C9—C1031.5 (5)C46—C47—C48—C491.1 (7)
Mo1—N1—C9—C10155.8 (3)C47—C48—C49—O8178.1 (4)
C8—N1—C9—C14150.2 (3)C47—C48—C49—C500.4 (7)
Mo1—N1—C9—C1422.5 (4)C52—O8—C49—C485.4 (7)
C14—C9—C10—C113.6 (5)C52—O8—C49—C50176.7 (5)
N1—C9—C10—C11178.0 (3)C48—C49—C50—C511.2 (7)
C9—C10—C11—C122.5 (6)O8—C49—C50—C51176.8 (4)
C10—C11—C12—C130.7 (6)C49—C50—C51—C462.0 (7)
C10—C11—C12—O3179.7 (3)C47—C46—C51—C501.3 (6)
C15—O3—C12—C115.4 (6)N6—C46—C51—C50178.2 (4)
C15—O3—C12—C13174.2 (4)Cl6i—Cl6—C3S—Cl5165.5 (8)
C11—C12—C13—C142.6 (6)
Symmetry code: (i) x, y+1, z+2.

Experimental details

Crystal data
Chemical formula[Mo2(C15H15N2O2)3(C7H5O2)]·CH2Cl2
Mr1163.79
Crystal system, space groupTriclinic, P1
Temperature (K)293
a, b, c (Å)12.025 (4), 13.705 (4), 17.727 (6)
α, β, γ (°)74.595 (4), 85.646 (4), 67.238 (4)
V3)2596.0 (14)
Z2
Radiation typeMo Kα
µ (mm1)0.65
Crystal size (mm)0.25 × 0.20 × 0.20
Data collection
DiffractometerBruker SMART 1000
diffractometer
Absorption correctionMulti-scan
(SADABS; Sheldrick, 2004)
Tmin, Tmax0.851, 0.879
No. of measured, independent and
observed [I > 2σ(I)] reflections
10844, 8981, 6852
Rint0.018
(sin θ/λ)max1)0.595
Refinement
R[F2 > 2σ(F2)], wR(F2), S 0.036, 0.107, 1.03
No. of reflections8981
No. of parameters652
No. of restraints12
H-atom treatmentH-atom parameters constrained
Δρmax, Δρmin (e Å3)0.65, 0.59

Computer programs: APEX2 (Bruker, 2004), SAINT-Plus (Bruker, 2001), SHELXS97 (Sheldrick, 2008), SHELXL97 (Sheldrick, 2008), XP in SHELXTL (Sheldrick, 2008).

Selected bond lengths (Å) top
Mo1—Mo22.0881 (8)Mo2—N42.120 (3)
Mo1—N32.117 (3)Mo2—N22.132 (3)
Mo1—N52.142 (3)Mo2—O22.133 (2)
Mo1—O12.144 (2)Mo2—N62.144 (3)
Mo1—N12.156 (3)
 

Acknowledgements

This work was supported by the National Natural Scientific Foundation of China (No. 20741004/B010303).

References

First citationBruker (2001). SAINT-Plus. Bruker AXS Inc., Madison,Wisconsin, USA.  Google Scholar
First citationBruker (2004). APEX2. Bruker AXS Inc., Madison, Wisconsin, USA.  Google Scholar
First citationCotton, F. A., Extine, M. & Gaga, L. D. (1978). Inorg. Chem. 17, 172–176.  CSD CrossRef CAS Web of Science Google Scholar
First citationCotton, F. A., Liu, C. Y. & Murillo, C. A. (2003). J. Am. Chem. Soc. 125, 13564–13575.  Web of Science CSD CrossRef PubMed CAS Google Scholar
First citationLin, C., Protasiewicz, J. D., Smith, E. T. & Ren, T. (1996). Inorg. Chem. 35, 6422–6428.  CSD CrossRef PubMed CAS Web of Science Google Scholar
First citationSheldrick, G. M. (2004). SADABS. University of Göttingen, Germany.  Google Scholar
First citationSheldrick, G. M. (2008). Acta Cryst. A64, 112–122.  Web of Science CrossRef CAS IUCr Journals Google Scholar

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