A binuclear molybdenum oxyfluoride: μ-oxido-bis-[(2,2'-bipyrid-yl)fluoridodioxidomolybdenum(VI)].

The title compound, [Mo(2)F(2)O(5)(C(10)H(8)N(2))(2)], is a centrosymmetric binuclear molybdenum(VI) species with the metal atoms in a distorted octa-hedral environment. The coordination geometries of the symmetry-equivalent molybdenum sites are defined by the cis-terminal oxide groups and the N-atom donors of the bipyridyl ligand in the equatorial plane with axial F and bridging O atoms. The bridging O atom occupies a center of symmetry. The mol-ecules stack in the a-axis direction, and the crystal packing is stabilized by weak intra- and inter-molecular C-H⋯O and C-H⋯F hydrogen bonds.

Related literature

For oxidofluoridomolybdates and n class="Chemical">-vanadates, see: Adil et al. (2010 ▶); Burkholder & Zubieta (2004 ▶); Jones et al. (2010 ▶); Michailovski et al. (2006 ▶, 2009 ▶).

Experimental

Crystal data

[Mo2F2O5(C10H8N2)2]

M = 622.25

Monoclinic,

a = 6.9180 (4) Å

b = 15.6494 (8) Å

c = 10.4544 (5) Å

β = 108.933 (1)°

V = 1070.59 (10) Å3

Z = 2

Mo Kα radiation

μ = 1.23 mm−1

T = 90 K

0.30 × 0.24 × 0.18 mm

Data collection

Bruker APEX CCD area-detector diffractometer

Absorption correction: multi-scan (SADABS; Sheldrick, 1996 ▶) T min = 0.709, T max = 0.809

10668 measured reflections

2647 independent reflections

2609 reflections with I > 2σ(I)

R int = 0.025

Refinement

R[F 2 > 2σ(F 2)] = 0.049

wR(F 2) = 0.094

S = 1.39

2647 reflections

183 parameters

All H-atom parameters refined

Δρmax = 0.81 e Å−3

Δρmin = −1.47 e Å−3

Data collection: SMART (Bruker, 1998 ▶); cell refinement: SAINT (Bruker, 1998 ▶); data reduction: SAIn class="Chemical">NT; program(s) used to solve structure: SHELXS97 (Sheldrick, 2008 ▶); program(s) used to refine structure: SHELXL97 (Sheldrick, 2008 ▶); molecular graphics: CrystalMaker (Palmer, 2005 ▶); software used to prepare material for publication: SHELXL97.

Crystal structure: contains datablocks I, global. DOI: 10.1107/S1600536810026383/om2344sup1.cif

Structure factors: contains datablocks I. DOI: 10.1107/S1600536810026383/om2344Isup2.hkl

Additional supplementary materials: crystallographic information; 3D view; checkCIF report

[Mo2F2O5(C10H8N2)2]	F(000) = 612
Mr = 622.25	Dx = 1.930 Mg m−3Dm = 1.91 (2) Mg m−3Dm measured by flotation
Monoclinic, P21/c	Mo Kα radiation, λ = 0.71073 Å
Hall symbol: -P 2ybc	Cell parameters from 5107 reflections
a = 6.9180 (4) Å	θ = 2.4–28.3°
b = 15.6494 (8) Å	µ = 1.23 mm−1
c = 10.4544 (5) Å	T = 90 K
β = 108.933 (1)°	Block, pink
V = 1070.59 (10) Å3	0.30 × 0.24 × 0.18 mm
Z = 2

Bruker APEX CCD area-detector diffractometer	2647 independent reflections
Radiation source: fine-focus sealed tube	2609 reflections with I > 2σ(I)
graphite	Rint = 0.025
Detector resolution: 512 pixels mm-1	θmax = 28.3°, θmin = 2.4°
Phi and ω scans	h = −9→9
Absorption correction: multi-scan (SADABS; Sheldrick, 1996)	k = −20→20
Tmin = 0.709, Tmax = 0.809	l = −13→13
10668 measured reflections

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)] = 0.049	Hydrogen site location: inferred from neighbouring sites
wR(F2) = 0.094	All H-atom parameters refined
S = 1.39	w = 1/[σ2(Fo2) + 5.6215P] where P = (Fo2 + 2Fc2)/3
2647 reflections	(Δ/σ)max < 0.001
183 parameters	Δρmax = 0.81 e Å−3
0 restraints	Δρmin = −1.47 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	0.17273 (6)	0.44676 (2)	0.15590 (4)	0.01481 (11)
F1	0.3489 (4)	0.44354 (17)	0.3426 (3)	0.0209 (5)
O1	0.0243 (6)	0.3616 (2)	0.1657 (4)	0.0291 (8)
O2	0.3584 (6)	0.4088 (2)	0.0957 (4)	0.0286 (8)
O3	0.0000	0.5000	0.0000	0.0239 (10)
N1	−0.0007 (5)	0.5318 (2)	0.2675 (3)	0.0137 (7)
N2	0.2982 (5)	0.5853 (2)	0.1807 (3)	0.0129 (7)
C1	−0.1496 (6)	0.5004 (3)	0.3104 (4)	0.0151 (8)
C2	−0.2287 (7)	0.5437 (3)	0.3968 (4)	0.0192 (9)
C3	−0.1536 (7)	0.6243 (3)	0.4397 (5)	0.0211 (9)
C4	−0.0038 (7)	0.6590 (3)	0.3931 (4)	0.0177 (8)
C5	0.0695 (6)	0.6111 (3)	0.3071 (4)	0.0127 (7)
C6	0.2238 (6)	0.6437 (3)	0.2474 (4)	0.0142 (8)
C7	0.2838 (7)	0.7292 (3)	0.2557 (5)	0.0189 (9)
C8	0.4185 (7)	0.7546 (3)	0.1895 (5)	0.0205 (9)
C9	0.4902 (7)	0.6952 (3)	0.1185 (4)	0.0189 (9)
C10	0.4269 (7)	0.6112 (3)	0.1168 (4)	0.0167 (8)
H1	−0.197 (7)	0.445 (3)	0.277 (5)	0.011 (11)*
H2	−0.333 (8)	0.519 (3)	0.420 (5)	0.014 (12)*
H3	−0.194 (9)	0.653 (4)	0.499 (6)	0.032 (16)*
H4	0.046 (7)	0.710 (3)	0.420 (5)	0.008 (11)*
H7	0.234 (8)	0.767 (4)	0.302 (6)	0.026 (14)*
H8	0.463 (9)	0.809 (4)	0.193 (6)	0.031 (15)*
H9	0.573 (8)	0.710 (4)	0.073 (5)	0.025 (14)*
H10	0.472 (8)	0.571 (4)	0.077 (5)	0.023 (14)*

	U11	U22	U33	U12	U13	U23
Mo1	0.02326 (19)	0.00943 (16)	0.01567 (18)	−0.00208 (14)	0.01173 (14)	−0.00183 (14)
F1	0.0205 (13)	0.0233 (13)	0.0216 (12)	0.0055 (11)	0.0105 (10)	0.0058 (11)
O1	0.042 (2)	0.0135 (15)	0.039 (2)	−0.0115 (14)	0.0229 (18)	−0.0069 (14)
O2	0.046 (2)	0.0189 (16)	0.0340 (19)	0.0046 (15)	0.0316 (18)	−0.0013 (14)
O3	0.033 (3)	0.022 (2)	0.014 (2)	−0.006 (2)	0.0024 (19)	−0.0039 (18)
N1	0.0144 (16)	0.0139 (16)	0.0122 (16)	0.0008 (13)	0.0036 (13)	0.0006 (13)
N2	0.0158 (16)	0.0108 (15)	0.0123 (16)	0.0032 (13)	0.0048 (13)	0.0014 (12)
C1	0.016 (2)	0.016 (2)	0.0116 (19)	−0.0026 (16)	0.0028 (15)	0.0050 (15)
C2	0.0159 (19)	0.025 (2)	0.019 (2)	0.0019 (17)	0.0089 (16)	0.0024 (18)
C3	0.026 (2)	0.023 (2)	0.018 (2)	0.0085 (19)	0.0124 (18)	0.0020 (18)
C4	0.022 (2)	0.0133 (19)	0.018 (2)	0.0006 (17)	0.0069 (17)	−0.0006 (16)
C5	0.0139 (18)	0.0119 (18)	0.0115 (18)	0.0024 (15)	0.0031 (15)	0.0021 (14)
C6	0.0143 (19)	0.0116 (18)	0.0168 (19)	−0.0007 (15)	0.0051 (16)	−0.0022 (15)
C7	0.023 (2)	0.0126 (19)	0.022 (2)	−0.0015 (17)	0.0085 (18)	−0.0035 (17)
C8	0.023 (2)	0.015 (2)	0.023 (2)	−0.0050 (17)	0.0061 (18)	−0.0029 (17)
C9	0.020 (2)	0.022 (2)	0.017 (2)	−0.0019 (17)	0.0091 (17)	0.0043 (17)
C10	0.020 (2)	0.0145 (19)	0.017 (2)	0.0005 (16)	0.0085 (17)	−0.0023 (16)

Mo1—O1	1.705 (3)	C2—H2	0.92 (5)
Mo1—O2	1.710 (3)	C3—C4	1.391 (6)
Mo1—O3	1.8747 (4)	C3—H3	0.89 (6)
Mo1—F1	1.937 (3)	C4—C5	1.387 (6)
Mo1—N2	2.319 (3)	C4—H4	0.88 (5)
Mo1—N1	2.341 (3)	C5—C6	1.491 (6)
O3—Mo1i	1.8747 (4)	C6—C7	1.395 (6)
N1—C1	1.344 (5)	C7—C8	1.387 (6)
N1—C5	1.347 (5)	C7—H7	0.90 (6)
N2—C10	1.336 (5)	C8—C9	1.378 (6)
N2—C6	1.350 (5)	C8—H8	0.90 (6)
C1—C2	1.376 (6)	C9—C10	1.385 (6)
C1—H1	0.95 (5)	C9—H9	0.89 (6)
C2—C3	1.383 (7)	C10—H10	0.87 (6)
O1—Mo1—O2	106.83 (17)	C1—C2—H2	118 (3)
O1—Mo1—O3	99.97 (14)	C3—C2—H2	123 (3)
O2—Mo1—O3	100.21 (13)	C2—C3—C4	119.1 (4)
O1—Mo1—F1	96.52 (15)	C2—C3—H3	122 (4)
O2—Mo1—F1	93.42 (15)	C4—C3—H3	119 (4)
O3—Mo1—F1	154.49 (8)	C5—C4—C3	119.1 (4)
O1—Mo1—N2	159.21 (14)	C5—C4—H4	121 (3)
O2—Mo1—N2	93.84 (14)	C3—C4—H4	120 (3)
O3—Mo1—N2	77.95 (8)	N1—C5—C4	121.7 (4)
F1—Mo1—N2	79.72 (12)	N1—C5—C6	115.0 (3)
O1—Mo1—N1	89.94 (14)	C4—C5—C6	123.2 (4)
O2—Mo1—N1	161.53 (15)	N2—C6—C7	121.7 (4)
O3—Mo1—N1	84.00 (8)	N2—C6—C5	115.4 (4)
F1—Mo1—N1	76.66 (11)	C7—C6—C5	122.8 (4)
N2—Mo1—N1	69.28 (12)	C8—C7—C6	118.6 (4)
Mo1—O3—Mo1i	180.0	C8—C7—H7	121 (4)
C1—N1—C5	118.3 (4)	C6—C7—H7	121 (4)
C1—N1—Mo1	122.0 (3)	C9—C8—C7	119.6 (4)
C5—N1—Mo1	119.0 (3)	C9—C8—H8	119 (4)
C10—N2—C6	118.7 (4)	C7—C8—H8	122 (4)
C10—N2—Mo1	120.9 (3)	C8—C9—C10	118.6 (4)
C6—N2—Mo1	120.0 (3)	C8—C9—H9	122 (4)
N1—C1—C2	123.3 (4)	C10—C9—H9	120 (4)
N1—C1—H1	115 (3)	N2—C10—C9	122.7 (4)
C2—C1—H1	122 (3)	N2—C10—H10	115 (4)
C1—C2—C3	118.3 (4)	C9—C10—H10	122 (4)
O1—Mo1—N1—C1	1.4 (3)	C1—C2—C3—C4	0.8 (7)
O2—Mo1—N1—C1	−154.2 (4)	C2—C3—C4—C5	−1.4 (7)
O3—Mo1—N1—C1	101.4 (3)	C1—N1—C5—C4	1.9 (6)
F1—Mo1—N1—C1	−95.3 (3)	Mo1—N1—C5—C4	−168.8 (3)
N2—Mo1—N1—C1	−179.2 (3)	C1—N1—C5—C6	−175.8 (3)
O1—Mo1—N1—C5	171.7 (3)	Mo1—N1—C5—C6	13.5 (4)
O2—Mo1—N1—C5	16.1 (6)	C3—C4—C5—N1	0.0 (6)
O3—Mo1—N1—C5	−88.2 (3)	C3—C4—C5—C6	177.6 (4)
F1—Mo1—N1—C5	75.0 (3)	C10—N2—C6—C7	−2.5 (6)
N2—Mo1—N1—C5	−8.9 (3)	Mo1—N2—C6—C7	−175.0 (3)
O1—Mo1—N2—C10	−168.0 (4)	C10—N2—C6—C5	175.6 (4)
O2—Mo1—N2—C10	18.0 (3)	Mo1—N2—C6—C5	3.0 (5)
O3—Mo1—N2—C10	−81.7 (3)	N1—C5—C6—N2	−10.7 (5)
F1—Mo1—N2—C10	110.7 (3)	C4—C5—C6—N2	171.6 (4)
N1—Mo1—N2—C10	−169.7 (3)	N1—C5—C6—C7	167.3 (4)
O1—Mo1—N2—C6	4.3 (6)	C4—C5—C6—C7	−10.3 (7)
O2—Mo1—N2—C6	−169.7 (3)	N2—C6—C7—C8	2.1 (7)
O3—Mo1—N2—C6	90.7 (3)	C5—C6—C7—C8	−175.9 (4)
F1—Mo1—N2—C6	−76.9 (3)	C6—C7—C8—C9	−0.4 (7)
N1—Mo1—N2—C6	2.6 (3)	C7—C8—C9—C10	−0.8 (7)
C5—N1—C1—C2	−2.5 (6)	C6—N2—C10—C9	1.3 (6)
Mo1—N1—C1—C2	167.9 (3)	Mo1—N2—C10—C9	173.7 (3)
N1—C1—C2—C3	1.2 (7)	C8—C9—C10—N2	0.4 (7)

D—H···A	D—H	H···A	D···A	D—H···A
C1—H1···O1	0.95 (5)	2.56 (5)	3.104 (6)	117 (3)
C2—H2···F1ii	0.92 (5)	2.39 (5)	3.201 (5)	146 (4)
C2—H2···F1iii	0.92 (5)	2.59 (5)	3.103 (5)	116 (4)
C3—H3···F1iii	0.89 (6)	2.71 (6)	3.183 (5)	115 (5)
C4—H4···O1iv	0.88 (5)	2.52 (5)	3.224 (5)	137 (4)
C7—H7···O1iv	0.90 (6)	2.42 (6)	3.263 (6)	155 (5)
C8—H8···F1v	0.90 (6)	2.57 (6)	3.435 (5)	162 (5)
C8—H8···O2v	0.90 (6)	2.66 (6)	3.317 (6)	130 (5)
C9—H9···O2vi	0.89 (6)	2.70 (6)	3.207 (6)	117 (4)
C10—H10···O2vi	0.87 (6)	2.47 (5)	3.063 (5)	126 (4)
C10—H10···O2	0.87 (6)	2.68 (5)	3.199 (6)	120 (4)

Table 1

Hydrogen-bond geometry (Å, °)

D—H⋯A	D—H	H⋯A	D⋯A	D—H⋯A
C1—H1⋯O1	0.95 (5)	2.56 (5)	3.104 (6)	117 (3)
C2—H2⋯F1i	0.92 (5)	2.39 (5)	3.201 (5)	146 (4)
C2—H2⋯F1ii	0.92 (5)	2.59 (5)	3.103 (5)	116 (4)
C3—H3⋯F1ii	0.89 (6)	2.71 (6)	3.183 (5)	115 (5)
C4—H4⋯O1iii	0.88 (5)	2.52 (5)	3.224 (5)	137 (4)
C7—H7⋯O1iii	0.90 (6)	2.42 (6)	3.263 (6)	155 (5)
C8—H8⋯F1iv	0.90 (6)	2.57 (6)	3.435 (5)	162 (5)
C8—H8⋯O2iv	0.90 (6)	2.66 (6)	3.317 (6)	130 (5)
C9—H9⋯O2v	0.89 (6)	2.70 (6)	3.207 (6)	117 (4)
C10—H10⋯O2v	0.87 (6)	2.47 (5)	3.063 (5)	126 (4)
C10—H10⋯O2	0.87 (6)	2.68 (5)	3.199 (6)	120 (4)

Symmetry codes: (i) ; (ii) ; (iii) ; (iv) ; (v) .