Tetra­kis[μ-N,N′-bis­(4-bromo­phen­yl)formamidinato-κ2N:N′]dimolyb­denum(II) tetra­hydro­furan solvate

Han, L.-J.

doi:10.1107/S1600536811011202

metal-organic compounds

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Volume 67| Part 4| April 2011| Page m514

doi:10.1107/S1600536811011202

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Tetrakis[μ-N,N′-bis(4-bromophenyl)formamidinato-κ²N:N′]dimolybdenum(II) tetrahydrofuran solvate

L.-J. Han ^a ^*

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

(Received 15 February 2011; accepted 25 March 2011; online 31 March 2011)

The title complex, [Mo₂(C₁₃H₉N₂Br₂)₄]·C₄H₈O, contains a quadruply bonded Mo₂⁴⁺ unit equatorially coordinated by four N,N′-bis(4-bromophenyl)formamidinate ligands, forming a dimetal paddlewheel complex. The centroid of the Mo—Mo bond is located on a special position with 2/m symmetry. In the crystal, complex molecules are linked by Br⋯Br interactions [3.7049 (10) Å]. The disordered solvent molecule could not be satisfactorily modelled and was therefore eliminated from the final refinement.

Related literature

For the nature of halogen–halogen interactions, see: Domercq et al. (2001 ); Espallargas et al. (2006 ). For Br⋯Br interactions, see: Fujiwara et al. (2006 ); Reddy et al. (1996 ). For the use of intermolecular interactions in supramolecular synthesis, see: Brammer (2004 ); Desiraju (1995 , 2001 ).

Experimental

Crystal data

[Mo₂(C₁₃H₉N₂Br₂)₄]·C₄H₈O
M_r = 1604.05
Monoclinic, C 2/c
a = 21.795 (4) Å
b = 10.077 (2) Å
c = 29.967 (6) Å
β = 110.67 (3)°
V = 6158 (2) Å³
Z = 4
Mo Kα radiation
μ = 5.64 mm⁻¹
T = 293 K
0.15 × 0.13 × 0.10 mm

Data collection

BRUKER SMART 1000 diffractometer
Absorption correction: multi-scan (SADABS; Sheldrick, 2004 ) T_min = 0.429, T_max = 0.569
25098 measured reflections
5995 independent reflections
3563 reflections with I > 2σ(I)
R_int = 0.119

Refinement

R[F² > 2σ(F²)] = 0.055
wR(F²) = 0.151
S = 1.01
5995 reflections
317 parameters
H-atom parameters constrained
Δρ_max = 1.09 e Å⁻³
Δρ_min = −1.11 e Å⁻³

Table 1
Selected bond lengths (Å)

Mo1—Mo1ⁱ	2.1263 (13)
Mo1—N3	2.192 (5)
Mo1—N4ⁱ	2.195 (5)
Mo1—N1ⁱ	2.198 (5)
Mo1—N2	2.218 (5)
Symmetry code: (i) $[-x+{\script{1\over 2}}, -y+{\script{1\over 2}}, -z]$ .

Data collection: APEX2 (Bruker, 2004 ); cell refinement: SAINT-Plus (Bruker, 2001 ); data reduction: SAINT-Plus; program(s) used to solve structure: SHELXS97 (Sheldrick, 2008 ); program(s) used to refine structure: SHELXL97 (Sheldrick, 2008); molecular graphics: XP (Sheldrick, 2008); software used to prepare material for publication: SHELXL97 and PLATON (Spek, 2009 ).

Supporting information

Crystal structure: contains datablocks global, I. DOI: 10.1107/S1600536811011202/ff2002sup1.cif

Structure factors: contains datablock I. DOI: 10.1107/S1600536811011202/ff2002Isup2.hkl

checkCIF report

Comment top

One of the main interests of crystal engineering is the study of intermolecular interactions and their utilization in supramolecular synthesis (Desiraju 1995; Desiraju 2001; Brammer 2004). These interactions range from strong forces, e.g., classical hydrogen bonds, to weaker ones, e.g., halogen···halogen interactions. The nature of the halogen···halogen interactions has been studied both through extensive crystallographic investigation and using ab initio calculations(Domercq et al.,2001; Espallargas et al., 2006). Here we report intermolecular Br···Br interactions in the crystal structure Mo₂(C₁₃H₉N₂Br₂)₄.THF.

The molecular structure of the title compound is shown in Fig.1. The molecule of Mo₂(C₁₃H₉N₂Br₂)₄ (I) occupies a special position on an inversion center, and the Mo—Mo distance is 2.1263 (13) Å, which is in the range of dimolybdenum quadruple bonds. Bromine atoms participate in short contacts (3.7049 (10) Å) linking the molecules of (I) into planes. This value is significantly shorter than van der Waals contact distance (3.90 Å) (Reddy et al., 1996; Fujiwara et al., 2006).

Related literature top

For the nature of halogen–halogen interactions, see: Domercq et al. (2001); Espallargas et al. (2006). For Br···Br interactions, see: Fujiwara et al. (2006); Reddy et al. (1996). For the use of intermolecular interactions in supramolecular synthesis, see: Brammer (2004); Desiraju (1995, 2001).

Experimental top

A mixture yellow Mo₂(OOCCH₃)₄ (0.128 g, 0.300 mmol) and N,N'-bis(4-bromophenyl)formamidinate (0.425 g, 1.20 mmol) was suspended in 20 ml of THF. While stirring, 2.4 ml NaOCH₂CH₃ solution (0.5 M in ethanol) was added slowly. The colour turned first to red and then to dark red. The reaction was stirred for 5 h at room temperature, and then the volume of the solvent was reduced to about 3 ml under reduced pressure. The residue was washed with distilled water(3×10 ml) and ethanol (8 ml) and dried under vacuum. The yellow solid was dissolved in THF (15 ml) and the solution was layered with hexanes. Yellow block-shaped crystals formed after several days. Yield: 0.342 g (71%). ¹HNMR(CDCl₃, p.p.m.): 8.41(s, 4H, –NCHN–), 7.10(d, 16H, aromatic), 6.06(d, 16H, aromatic). Anal. Calcd. C₅₂H₃₆Mo₂N₈Br₈: C, 38.94; H, 2.26; N, 6.99; Found: C, 38.78; H, 2.17; N, 7.08.

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 (Sheldrick, 2008); software used to prepare material for publication: SHELXL97 (Sheldrick, 2008) and PLATON (Spek, 20098).

Figures top

	Fig. 1. Molecular structure of the title compound drawn with displacement ellipsoids at the 30% probability level. All hydrogen atoms have been omitted for clarity. Atoms with suffix A are generated by the symmetry operation(-x + 1/2, -y + 1/2, -z).
	Fig. 2. Part of a two-dimensional plane of the title compound. Br···Br interactions are drawn with blue dashed lines.

Tetrakis[µ-N,N'-bis(4-bromophenyl) formamidinato-κ²N:N']dimolybdenum(II) tetrahydrofuran solvate top

Crystal data top

[Mo₂(C₁₃H₉N₂Br₂)₄]·C₄H₈O	F(000) = 3072
M_r = 1604.05	D_x = 1.730 Mg m⁻³
Monoclinic, C2/c	Mo Kα radiation, λ = 0.71073 Å
Hall symbol: -C 2yc	Cell parameters from 3824 reflections
a = 21.795 (4) Å	θ = 2.6–27.4°
b = 10.077 (2) Å	µ = 5.64 mm⁻¹
c = 29.967 (6) Å	T = 293 K
β = 110.67 (3)°	Block, yellow
V = 6158 (2) Å³	0.15 × 0.13 × 0.10 mm
Z = 4

Data collection top

BRUKER SMART 1000 diffractometer	5995 independent reflections
Radiation source: fine-focus sealed tube	3563 reflections with I > 2σ(I)
Graphite monochromator	R_int = 0.119
ω–scan	θ_max = 26.0°, θ_min = 3.4°
Absorption correction: multi-scan (SADABS; Sheldrick, 2004)	h = −26→26
T_min = 0.429, T_max = 0.569	k = −11→12
25098 measured reflections	l = −36→36

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)] = 0.055	H-atom parameters constrained
wR(F²) = 0.151	w = 1/[σ²(F_o²) + (0.0563P)²] where P = (F_o² + 2F_c²)/3
S = 1.01	(Δ/σ)_max < 0.001
5995 reflections	Δρ_max = 1.09 e Å⁻³
317 parameters	Δρ_min = −1.11 e Å⁻³
0 restraints	Extinction correction: SHELXL, Fc^*=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4
Primary atom site location: structure-invariant direct methods	Extinction coefficient: 0.00036 (7)

Crystal data top

[Mo₂(C₁₃H₉N₂Br₂)₄]·C₄H₈O	V = 6158 (2) Å³
M_r = 1604.05	Z = 4
Monoclinic, C2/c	Mo Kα radiation
a = 21.795 (4) Å	µ = 5.64 mm⁻¹
b = 10.077 (2) Å	T = 293 K
c = 29.967 (6) Å	0.15 × 0.13 × 0.10 mm
β = 110.67 (3)°

Data collection top

BRUKER SMART 1000 diffractometer	5995 independent reflections
Absorption correction: multi-scan (SADABS; Sheldrick, 2004)	3563 reflections with I > 2σ(I)
T_min = 0.429, T_max = 0.569	R_int = 0.119
25098 measured reflections

Refinement top

R[F² > 2σ(F²)] = 0.055	0 restraints
wR(F²) = 0.151	H-atom parameters constrained
S = 1.01	Δρ_max = 1.09 e Å⁻³
5995 reflections	Δρ_min = −1.11 e Å⁻³
317 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

	x	y	z	U_iso*/U_eq
Mo1	0.28396 (3)	0.20871 (5)	0.031782 (19)	0.0376 (2)
N1	0.2149 (3)	0.1089 (5)	−0.07230 (18)	0.0397 (13)
N2	0.2911 (3)	0.0167 (4)	−0.00225 (18)	0.0385 (13)
N3	0.3695 (3)	0.2759 (5)	0.01561 (19)	0.0404 (13)
N4	0.2950 (3)	0.3690 (5)	−0.05383 (18)	0.0405 (13)
Br1	0.05852 (5)	0.01976 (10)	−0.28619 (3)	0.0768 (3)
Br2	0.49853 (4)	−0.41859 (7)	0.08672 (3)	0.0659 (3)
Br3	0.64761 (5)	0.06765 (10)	0.13147 (4)	0.0836 (3)
Br4	0.23690 (6)	0.65632 (11)	−0.24584 (3)	0.0954 (4)
C1	0.2551 (4)	0.0100 (6)	−0.0494 (2)	0.0425 (16)
H1A	0.2583	−0.0652	−0.0664	0.051*
C2	0.3574 (4)	0.3392 (6)	−0.0260 (2)	0.0438 (16)
H2A	0.3919	0.3628	−0.0357	0.053*
C11	0.1773 (3)	0.0879 (6)	−0.1214 (2)	0.0380 (15)
C12	0.1655 (4)	0.1926 (7)	−0.1543 (2)	0.0535 (19)
H12A	0.1805	0.2772	−0.1434	0.064*
C13	0.1316 (4)	0.1730 (7)	−0.2030 (3)	0.061 (2)
H13A	0.1260	0.2429	−0.2243	0.073*
C14	0.1062 (4)	0.0477 (8)	−0.2194 (3)	0.057 (2)
C15	0.1144 (4)	−0.0577 (7)	−0.1874 (3)	0.058 (2)
H15A	0.0977	−0.1413	−0.1983	0.070*
C16	0.1481 (4)	−0.0353 (7)	−0.1390 (3)	0.0530 (19)
H16A	0.1515	−0.1041	−0.1176	0.064*
C21	0.3353 (3)	−0.0897 (5)	0.0191 (2)	0.0360 (14)
C22	0.3289 (4)	−0.2199 (6)	−0.0001 (2)	0.0482 (18)
H22A	0.2927	−0.2411	−0.0268	0.058*
C23	0.3763 (4)	−0.3170 (6)	0.0208 (3)	0.0543 (19)
H23A	0.3713	−0.4021	0.0080	0.065*
C24	0.4313 (4)	−0.2864 (6)	0.0608 (3)	0.0467 (17)
C25	0.4366 (3)	−0.1634 (6)	0.0815 (2)	0.0451 (17)
H25A	0.4722	−0.1442	0.1089	0.054*
C26	0.3889 (4)	−0.0670 (6)	0.0615 (2)	0.0472 (18)
H26A	0.3925	0.0147	0.0767	0.057*
C31	0.4360 (3)	0.2377 (6)	0.0422 (2)	0.0401 (15)
C32	0.4763 (4)	0.1811 (6)	0.0178 (2)	0.0462 (17)
H32A	0.4607	0.1762	−0.0153	0.055*
C33	0.5399 (4)	0.1330 (7)	0.0446 (3)	0.0512 (18)
H33A	0.5662	0.0970	0.0291	0.061*
C34	0.5629 (4)	0.1401 (7)	0.0945 (3)	0.0513 (18)
C35	0.5243 (4)	0.1974 (6)	0.1187 (3)	0.0514 (19)
H35A	0.5403	0.2040	0.1518	0.062*
C36	0.4613 (4)	0.2443 (6)	0.0918 (2)	0.0490 (18)
H36A	0.4357	0.2810	0.1077	0.059*
C41	0.2845 (3)	0.4385 (6)	−0.0982 (2)	0.0406 (16)
C42	0.2423 (4)	0.5467 (6)	−0.1095 (2)	0.0527 (19)
H42A	0.2231	0.5759	−0.0881	0.063*
C43	0.2285 (4)	0.6121 (7)	−0.1536 (3)	0.064 (2)
H43A	0.2004	0.6848	−0.1612	0.077*
C44	0.2570 (4)	0.5676 (7)	−0.1857 (3)	0.060 (2)
C45	0.2992 (4)	0.4573 (7)	−0.1745 (3)	0.060 (2)
H45A	0.3176	0.4271	−0.1963	0.072*
C46	0.3135 (4)	0.3926 (7)	−0.1302 (2)	0.0509 (18)
H46A	0.3419	0.3204	−0.1224	0.061*

Atomic displacement parameters (Å²) top

	U¹¹	U²²	U³³	U¹²	U¹³	U²³
Mo1	0.0420 (4)	0.0429 (3)	0.0298 (3)	0.0039 (2)	0.0151 (3)	−0.0015 (2)
N1	0.042 (4)	0.046 (3)	0.034 (3)	0.001 (2)	0.016 (3)	−0.004 (2)
N2	0.042 (4)	0.039 (3)	0.037 (3)	0.003 (2)	0.016 (3)	−0.002 (2)
N3	0.035 (3)	0.049 (3)	0.039 (3)	0.004 (2)	0.015 (3)	−0.001 (2)
N4	0.045 (4)	0.046 (3)	0.031 (3)	0.006 (2)	0.014 (3)	0.006 (2)
Br1	0.0584 (6)	0.1298 (8)	0.0361 (5)	−0.0046 (5)	0.0089 (4)	−0.0152 (4)
Br2	0.0648 (6)	0.0618 (5)	0.0715 (6)	0.0196 (4)	0.0245 (5)	0.0237 (4)
Br3	0.0522 (6)	0.1145 (8)	0.0780 (7)	0.0227 (5)	0.0152 (5)	0.0185 (5)
Br4	0.1135 (10)	0.1272 (8)	0.0507 (6)	0.0062 (7)	0.0352 (6)	0.0316 (5)
C1	0.051 (5)	0.040 (3)	0.038 (4)	−0.001 (3)	0.017 (3)	−0.011 (3)
C2	0.052 (5)	0.045 (3)	0.035 (4)	0.005 (3)	0.017 (4)	0.000 (3)
C11	0.037 (4)	0.052 (4)	0.028 (3)	0.000 (3)	0.014 (3)	−0.009 (3)
C12	0.060 (5)	0.049 (4)	0.044 (4)	−0.008 (3)	0.010 (4)	0.000 (3)
C13	0.069 (6)	0.065 (5)	0.045 (4)	−0.011 (4)	0.017 (4)	0.006 (4)
C14	0.042 (5)	0.095 (6)	0.033 (4)	0.003 (4)	0.011 (4)	−0.005 (4)
C15	0.056 (6)	0.057 (4)	0.052 (5)	0.002 (4)	0.006 (4)	−0.012 (4)
C16	0.051 (5)	0.059 (4)	0.044 (4)	0.002 (3)	0.011 (4)	0.001 (3)
C21	0.035 (4)	0.042 (3)	0.033 (3)	0.003 (3)	0.015 (3)	0.000 (3)
C22	0.046 (5)	0.044 (4)	0.048 (4)	0.000 (3)	0.008 (4)	−0.003 (3)
C23	0.053 (5)	0.045 (4)	0.066 (5)	0.002 (3)	0.023 (4)	−0.005 (4)
C24	0.049 (5)	0.044 (4)	0.050 (4)	−0.003 (3)	0.022 (4)	0.010 (3)
C25	0.041 (5)	0.046 (4)	0.039 (4)	−0.004 (3)	0.003 (3)	−0.001 (3)
C26	0.057 (5)	0.038 (3)	0.044 (4)	−0.001 (3)	0.015 (4)	−0.004 (3)
C31	0.037 (4)	0.049 (4)	0.041 (4)	0.001 (3)	0.022 (3)	−0.001 (3)
C32	0.045 (5)	0.056 (4)	0.038 (4)	0.004 (3)	0.014 (4)	−0.002 (3)
C33	0.055 (5)	0.057 (4)	0.048 (4)	−0.005 (3)	0.026 (4)	0.000 (3)
C34	0.040 (5)	0.059 (4)	0.060 (5)	−0.002 (3)	0.023 (4)	0.002 (4)
C35	0.057 (5)	0.051 (4)	0.043 (4)	0.001 (3)	0.013 (4)	0.000 (3)
C36	0.052 (5)	0.050 (4)	0.048 (4)	0.004 (3)	0.021 (4)	−0.010 (3)
C41	0.040 (4)	0.052 (4)	0.033 (4)	−0.004 (3)	0.016 (3)	0.005 (3)
C42	0.065 (6)	0.058 (4)	0.041 (4)	0.006 (4)	0.028 (4)	0.002 (3)
C43	0.078 (7)	0.056 (4)	0.053 (5)	0.006 (4)	0.018 (5)	0.008 (4)
C44	0.071 (6)	0.064 (5)	0.042 (4)	−0.012 (4)	0.015 (4)	0.001 (4)
C45	0.072 (6)	0.073 (5)	0.049 (5)	−0.008 (4)	0.039 (5)	−0.009 (4)
C46	0.054 (5)	0.064 (4)	0.041 (4)	0.008 (4)	0.025 (4)	0.005 (3)

Geometric parameters (Å, º) top

Mo1—Mo1ⁱ	2.1263 (13)	C21—C26	1.410 (9)
Mo1—N3	2.192 (5)	C21—C22	1.419 (8)
Mo1—N4ⁱ	2.195 (5)	C22—C23	1.400 (9)
Mo1—N1ⁱ	2.198 (5)	C22—H22A	0.9300
Mo1—N2	2.218 (5)	C23—C24	1.398 (10)
N1—C1	1.345 (8)	C23—H23A	0.9300
N1—C11	1.424 (7)	C24—C25	1.372 (9)
N1—Mo1ⁱ	2.198 (5)	C25—C26	1.395 (9)
N2—C1	1.353 (8)	C25—H25A	0.9300
N2—C21	1.432 (7)	C26—H26A	0.9300
N3—C2	1.341 (8)	C31—C36	1.393 (9)
N3—C31	1.439 (8)	C31—C32	1.444 (9)
N4—C2	1.353 (8)	C32—C33	1.419 (9)
N4—C41	1.448 (7)	C32—H32A	0.9300
N4—Mo1ⁱ	2.195 (5)	C33—C34	1.401 (9)
Br1—C14	1.924 (7)	C33—H33A	0.9300
Br2—C24	1.929 (7)	C34—C35	1.413 (10)
Br3—C34	1.930 (7)	C35—C36	1.406 (9)
Br4—C44	1.919 (7)	C35—H35A	0.9300
C1—H1A	0.9300	C36—H36A	0.9300
C2—H2A	0.9300	C41—C42	1.389 (9)
C11—C12	1.404 (8)	C41—C46	1.402 (8)
C11—C16	1.410 (9)	C42—C43	1.411 (9)
C12—C13	1.398 (9)	C42—H42A	0.9300
C12—H12A	0.9300	C43—C44	1.390 (10)
C13—C14	1.396 (10)	C43—H43A	0.9300
C13—H13A	0.9300	C44—C45	1.405 (11)
C14—C15	1.399 (10)	C45—C46	1.412 (9)
C15—C16	1.393 (9)	C45—H45A	0.9300
C15—H15A	0.9300	C46—H46A	0.9300
C16—H16A	0.9300

Mo1ⁱ—Mo1—N3	93.36 (14)	C23—C22—H22A	119.5
Mo1ⁱ—Mo1—N4ⁱ	92.14 (14)	C21—C22—H22A	119.5
N3—Mo1—N4ⁱ	174.47 (19)	C24—C23—C22	120.2 (6)
Mo1ⁱ—Mo1—N1ⁱ	92.07 (14)	C24—C23—H23A	119.9
N3—Mo1—N1ⁱ	91.09 (19)	C22—C23—H23A	119.9
N4ⁱ—Mo1—N1ⁱ	89.39 (19)	C25—C24—C23	119.8 (6)
Mo1ⁱ—Mo1—N2	93.96 (14)	C25—C24—Br2	120.7 (5)
N3—Mo1—N2	87.97 (18)	C23—C24—Br2	119.5 (5)
N4ⁱ—Mo1—N2	90.97 (18)	C24—C25—C26	120.3 (6)
N1ⁱ—Mo1—N2	173.9 (2)	C24—C25—H25A	119.9
C1—N1—C11	116.9 (5)	C26—C25—H25A	119.9
C1—N1—Mo1ⁱ	117.3 (4)	C25—C26—C21	121.9 (6)
C11—N1—Mo1ⁱ	125.8 (4)	C25—C26—H26A	119.0
C1—N2—C21	118.6 (5)	C21—C26—H26A	119.0
C1—N2—Mo1	114.5 (4)	C36—C31—N3	121.4 (6)
C21—N2—Mo1	126.4 (4)	C36—C31—C32	118.4 (6)
C2—N3—C31	118.2 (6)	N3—C31—C32	120.0 (6)
C2—N3—Mo1	116.6 (5)	C33—C32—C31	119.7 (6)
C31—N3—Mo1	124.4 (4)	C33—C32—H32A	120.1
C2—N4—C41	118.2 (6)	C31—C32—H32A	120.1
C2—N4—Mo1ⁱ	117.3 (4)	C34—C33—C32	119.7 (7)
C41—N4—Mo1ⁱ	124.2 (4)	C34—C33—H33A	120.1
N1—C1—N2	122.0 (5)	C32—C33—H33A	120.1
N1—C1—H1A	119.0	C33—C34—C35	121.0 (7)
N2—C1—H1A	119.0	C33—C34—Br3	120.1 (6)
N3—C2—N4	120.3 (6)	C35—C34—Br3	118.8 (6)
N3—C2—H2A	119.9	C36—C35—C34	118.7 (7)
N4—C2—H2A	119.9	C36—C35—H35A	120.6
C12—C11—C16	116.8 (6)	C34—C35—H35A	120.6
C12—C11—N1	120.7 (6)	C31—C36—C35	122.3 (7)
C16—C11—N1	122.5 (6)	C31—C36—H36A	118.9
C13—C12—C11	121.7 (6)	C35—C36—H36A	118.9
C13—C12—H12A	119.2	C42—C41—C46	120.8 (6)
C11—C12—H12A	119.2	C42—C41—N4	118.7 (6)
C14—C13—C12	119.5 (7)	C46—C41—N4	120.3 (6)
C14—C13—H13A	120.2	C41—C42—C43	119.9 (6)
C12—C13—H13A	120.2	C41—C42—H42A	120.0
C13—C14—C15	120.5 (7)	C43—C42—H42A	120.0
C13—C14—Br1	120.0 (6)	C44—C43—C42	119.8 (7)
C15—C14—Br1	119.5 (6)	C44—C43—H43A	120.1
C16—C15—C14	118.8 (7)	C42—C43—H43A	120.1
C16—C15—H15A	120.6	C43—C44—C45	120.4 (7)
C14—C15—H15A	120.6	C43—C44—Br4	119.3 (6)
C15—C16—C11	122.4 (7)	C45—C44—Br4	120.3 (6)
C15—C16—H16A	118.8	C44—C45—C46	119.9 (7)
C11—C16—H16A	118.8	C44—C45—H45A	120.1
C26—C21—C22	116.5 (6)	C46—C45—H45A	120.1
C26—C21—N2	119.6 (5)	C41—C46—C45	119.2 (6)
C22—C21—N2	123.9 (6)	C41—C46—H46A	120.4
C23—C22—C21	120.9 (7)	C45—C46—H46A	120.4

Symmetry code: (i) −x+1/2, −y+1/2, −z.

Experimental details

Crystal data
Chemical formula	[Mo₂(C₁₃H₉N₂Br₂)₄]·C₄H₈O
M_r	1604.05
Crystal system, space group	Monoclinic, C2/c
Temperature (K)	293
a, b, c (Å)	21.795 (4), 10.077 (2), 29.967 (6)
β (°)	110.67 (3)
V (Å³)	6158 (2)
Z	4
Radiation type	Mo Kα
µ (mm⁻¹)	5.64
Crystal size (mm)	0.15 × 0.13 × 0.10

Data collection
Diffractometer	BRUKER SMART 1000 diffractometer
Absorption correction	Multi-scan (SADABS; Sheldrick, 2004)
T_min, T_max	0.429, 0.569
No. of measured, independent and observed [I > 2σ(I)] reflections	25098, 5995, 3563
R_int	0.119
(sin θ/λ)_max (Å⁻¹)	0.617

Refinement
R[F² > 2σ(F²)], wR(F²), S	0.055, 0.151, 1.01
No. of reflections	5995
No. of parameters	317
H-atom treatment	H-atom parameters constrained
Δρ_max, Δρ_min (e Å⁻³)	1.09, −1.11

Computer programs: APEX2 (Bruker, 2004), SAINT-Plus (Bruker, 2001), SHELXS97 (Sheldrick, 2008), XP (Sheldrick, 2008), SHELXL97 (Sheldrick, 2008) and PLATON (Spek, 20098).

Selected bond lengths (Å) top

Mo1—Mo1ⁱ	2.1263 (13)	Mo1—N1ⁱ	2.198 (5)
Mo1—N3	2.192 (5)	Mo1—N2	2.218 (5)
Mo1—N4ⁱ	2.195 (5)

Symmetry code: (i) −x+1/2, −y+1/2, −z.

Acknowledgements

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

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