Literature DB >> 22058859

catena-Poly[[tetra-kis-(μ-penta-fluoro-benzoato-κO:O')dimolybdenum(II)]-μ-4,4'-bipyridine-κN:N'].

Li-Juan Han1.   

Abstract

In the title compound, [Mo(2)(C(7)F(5)O(2))(4)(C(10)H(8)N(2))](n), the mol-ecule forms a paddle-wheel-type structure. Each Mo(2) (4+) unit is equatorially coordinated by four n class="Chemical">pentafluoro-benzoate groups, while the axial positions are occupied by two 4,4'-bipyridine mol-ecules. The Mo-Mo bond length of 2.1227 (4) Å is representative of a dimolybdenum quadruple bond. An infinite linear chain parallel to [110] is formed by the Mo(2) (4+) unit coordinating axially to the two N atoms of the 4,4'-bipyridine ligand [Mo-N = 2.594 (2) Å]. The crystal packing shows mol-ecules linked together into a three-dimensional network via Mo-N coordination inter-actions and weak π-π stacking inter-actions between perfluoro-phenyl rings [centroid-centroid distance = 3.7280 (3) Å and centroid-to-plane distance = 3.6103 (12) Å between two penta-fluoro-phenyl rings].

Entities:  

Year:  2011        PMID： 22058859      PMCID： PMC3200718          DOI： 10.1107/S1600536811031734

Source DB:  PubMed          Journal:  Acta Crystallogr Sect E Struct Rep Online        ISSN： 1600-5368


Related literature

For background to coordination polymers, see: Batten (2002 ▶); Kumar et al. (2004 ▶). For torsion angles about the penta­fluoro­benzoate anion, see: Reddy et al. (2004 ▶); Bach et al. (2001 ▶); For Mo–Mo quadruple bond lengths, see: Cotton et al. (2005 ▶).

Experimental

Crystal data

[Mo2(C7F5O2)4(C10n class="Species">H8N2)] M = 1192.34 Triclinic, a = 8.8858 (8) Å b = 9.9311 (9) Å c = 11.1978 (10) Å α = 101.158 (1)° β = 94.697 (1)° γ = 99.092 (1)° V = 950.83 (15) Å3 Z = 1 Mo Kα radiation μ = 0.82 mm−1 T = 293 K 0.20 × 0.18 × 0.15 mm

Data collection

Bruker APEXII CCD diffractometer Absorption correction: multi-scan (SADABS; Sheldrick, 2004 ▶) T min = 0.849, T max = 0.884 4937 measured reflections 3294 independent reflections 3072 reflections with I > 2σ(I) R int = 0.013

Refinement

R[F 2 > 2σ(F 2)] = 0.024 wR(F 2) = 0.061 S = 1.01 3294 reflections 316 parameters H-atom parameters constrained Δρmax = 0.32 e Å−3 Δρmin = −0.47 e Å−3 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 in SHELXTL (Sheldrick, 2008 ▶); software used to prepare material for publication: SHELXL97. Crystal structure: contains datablock(s) global, I. DOI: 10.1107/S1600536811031734/jj2094sup1.cif Structure factors: contains datablock(s) I. DOI: 10.1107/S1600536811031734/jj2094Isup2.hkl Additional supplementary materials: crystallographic information; 3D view; checkCIF report
[Mo2(C7F5O2)4(C10H8N2)]Z = 1
Mr = 1192.34F(000) = 578
Triclinic, P1Dx = 2.082 Mg m−3
Hall symbol: -P 1Mo Kα radiation, λ = 0.71073 Å
a = 8.8858 (8) ÅCell parameters from 4122 reflections
b = 9.9311 (9) Åθ = 2.5–27.6°
c = 11.1978 (10) ŵ = 0.82 mm−1
α = 101.158 (1)°T = 293 K
β = 94.697 (1)°Block, yellow
γ = 99.092 (1)°0.20 × 0.18 × 0.15 mm
V = 950.83 (15) Å3
Bruker APEXII CCD diffractometer3294 independent reflections
Radiation source: fine-focus sealed tube3072 reflections with I > 2σ(I)
graphiteRint = 0.013
ω scansθmax = 25.0°, θmin = 2.1°
Absorption correction: multi-scan (SADABS; Sheldrick, 2004)h = −8→10
Tmin = 0.849, Tmax = 0.884k = −11→11
4937 measured reflectionsl = −13→12
Refinement on F2Primary atom site location: structure-invariant direct methods
Least-squares matrix: fullSecondary atom site location: difference Fourier map
R[F2 > 2σ(F2)] = 0.024Hydrogen site location: inferred from neighbouring sites
wR(F2) = 0.061H-atom parameters constrained
S = 1.01w = 1/[σ2(Fo2) + (0.0323P)2 + 0.6373P] where P = (Fo2 + 2Fc2)/3
3294 reflections(Δ/σ)max = 0.001
316 parametersΔρmax = 0.32 e Å−3
0 restraintsΔρmin = −0.47 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.
xyzUiso*/Ueq
Mo10.94356 (2)0.58128 (2)0.480838 (17)0.02757 (8)
F110.46291 (19)0.34697 (17)0.29542 (17)0.0569 (4)
F120.2509 (2)0.1493 (2)0.1523 (2)0.0712 (5)
F130.3174 (2)−0.10294 (19)0.05942 (18)0.0682 (5)
F140.6015 (2)−0.15799 (17)0.11139 (18)0.0662 (5)
F150.81465 (19)0.03236 (17)0.25713 (17)0.0568 (4)
F311.0522 (2)0.7439 (2)0.89717 (17)0.0701 (5)
F320.9848 (3)0.8073 (2)1.13037 (18)0.0825 (6)
F330.7539 (2)0.6435 (2)1.20533 (14)0.0708 (6)
F340.5986 (3)0.4110 (2)1.05142 (19)0.0823 (6)
F350.6643 (2)0.3488 (2)0.81764 (17)0.0770 (6)
O10.75702 (18)0.43333 (16)0.38004 (15)0.0332 (4)
O20.87528 (19)0.26377 (17)0.42436 (15)0.0345 (4)
O50.85431 (19)0.59500 (18)0.65400 (15)0.0355 (4)
O61.03083 (19)0.58024 (17)0.31053 (15)0.0352 (4)
C10.7665 (3)0.3051 (3)0.3681 (2)0.0330 (5)
C30.8955 (3)0.5167 (3)0.7219 (2)0.0325 (5)
C110.6483 (3)0.1984 (3)0.2857 (2)0.0341 (5)
C120.5018 (3)0.2234 (3)0.2528 (2)0.0391 (6)
C130.3913 (3)0.1235 (3)0.1796 (3)0.0456 (7)
C140.4231 (3)−0.0065 (3)0.1325 (3)0.0467 (7)
C150.5677 (3)−0.0340 (3)0.1609 (2)0.0437 (6)
C160.6762 (3)0.0656 (3)0.2357 (2)0.0382 (6)
C310.8594 (3)0.5460 (3)0.8527 (2)0.0346 (5)
C320.9392 (3)0.6610 (3)0.9340 (2)0.0428 (6)
C330.9070 (4)0.6945 (3)1.0538 (2)0.0497 (7)
C340.7909 (3)0.6100 (3)1.0917 (2)0.0480 (7)
C350.7115 (3)0.4929 (3)1.0133 (3)0.0502 (7)
C360.7458 (3)0.4611 (3)0.8941 (2)0.0437 (6)
N10.2434 (3)0.2426 (2)0.5169 (2)0.0434 (5)
C510.3883 (4)0.2800 (3)0.5640 (2)0.0498 (7)
H51A0.42260.37270.60270.060*
C520.1981 (3)0.1097 (3)0.4617 (3)0.0555 (8)
H52A0.09660.08100.42700.067*
C530.2934 (3)0.0113 (3)0.4527 (3)0.0540 (8)
H53A0.2554−0.08050.41300.065*
C540.4463 (3)0.0507 (3)0.5034 (2)0.0377 (6)
C550.4927 (3)0.1900 (3)0.5594 (2)0.0467 (7)
H55A0.59380.22300.59380.056*
U11U22U33U12U13U23
Mo10.03074 (12)0.03149 (12)0.02725 (12)0.01909 (8)0.00822 (8)0.00964 (8)
F110.0419 (9)0.0543 (10)0.0761 (12)0.0260 (8)0.0033 (8)0.0049 (9)
F120.0397 (9)0.0805 (13)0.0925 (14)0.0211 (9)−0.0114 (9)0.0154 (11)
F130.0585 (11)0.0614 (11)0.0735 (12)−0.0033 (9)−0.0153 (10)0.0079 (9)
F140.0698 (12)0.0416 (9)0.0795 (13)0.0163 (9)−0.0058 (10)−0.0049 (9)
F150.0458 (9)0.0479 (9)0.0739 (12)0.0251 (8)−0.0035 (8)−0.0034 (8)
F310.0668 (12)0.0753 (13)0.0585 (11)−0.0139 (10)0.0155 (9)0.0085 (9)
F320.1018 (17)0.0801 (14)0.0504 (11)0.0059 (12)0.0050 (11)−0.0135 (10)
F330.0872 (14)0.1141 (16)0.0306 (8)0.0598 (12)0.0245 (9)0.0213 (9)
F340.0797 (14)0.1097 (17)0.0669 (12)0.0041 (12)0.0374 (11)0.0393 (12)
F350.0870 (15)0.0773 (13)0.0534 (11)−0.0205 (11)0.0149 (10)0.0069 (10)
O10.0319 (9)0.0335 (9)0.0390 (9)0.0169 (7)0.0043 (7)0.0098 (7)
O20.0357 (9)0.0349 (9)0.0375 (9)0.0162 (7)0.0044 (7)0.0108 (7)
O50.0391 (9)0.0449 (10)0.0318 (9)0.0260 (8)0.0126 (7)0.0124 (7)
O60.0403 (10)0.0412 (9)0.0334 (9)0.0225 (8)0.0121 (7)0.0153 (7)
C10.0331 (13)0.0395 (13)0.0328 (12)0.0160 (11)0.0105 (10)0.0123 (10)
C30.0317 (12)0.0401 (13)0.0312 (12)0.0150 (11)0.0092 (10)0.0116 (10)
C110.0344 (13)0.0394 (13)0.0339 (12)0.0131 (11)0.0097 (10)0.0131 (10)
C120.0380 (14)0.0440 (14)0.0426 (14)0.0178 (12)0.0109 (11)0.0162 (12)
C130.0342 (14)0.0573 (17)0.0504 (16)0.0141 (13)0.0022 (12)0.0196 (14)
C140.0457 (16)0.0500 (16)0.0420 (15)0.0011 (13)−0.0020 (13)0.0126 (13)
C150.0505 (16)0.0375 (14)0.0441 (15)0.0117 (12)0.0056 (13)0.0079 (12)
C160.0351 (13)0.0423 (14)0.0419 (14)0.0151 (11)0.0053 (11)0.0132 (11)
C310.0365 (13)0.0452 (14)0.0298 (12)0.0206 (11)0.0109 (10)0.0128 (11)
C320.0408 (15)0.0538 (16)0.0387 (14)0.0140 (13)0.0112 (12)0.0141 (12)
C330.0576 (18)0.0579 (17)0.0334 (14)0.0234 (15)0.0003 (13)0.0008 (13)
C340.0540 (17)0.076 (2)0.0283 (13)0.0404 (16)0.0159 (12)0.0177 (14)
C350.0463 (16)0.073 (2)0.0427 (16)0.0201 (15)0.0188 (13)0.0262 (15)
C360.0443 (15)0.0543 (16)0.0357 (14)0.0124 (13)0.0101 (12)0.0117 (12)
N10.0503 (14)0.0533 (14)0.0405 (12)0.0343 (11)0.0176 (11)0.0187 (10)
C510.0609 (19)0.0551 (17)0.0396 (15)0.0382 (15)0.0052 (13)0.0025 (13)
C520.0399 (16)0.0552 (18)0.084 (2)0.0259 (14)0.0165 (15)0.0281 (17)
C530.0416 (16)0.0402 (15)0.090 (2)0.0202 (13)0.0163 (15)0.0234 (15)
C540.0446 (15)0.0458 (14)0.0363 (13)0.0264 (12)0.0179 (11)0.0211 (11)
C550.0491 (16)0.0586 (17)0.0360 (14)0.0320 (14)0.0019 (12)0.0018 (12)
Mo1—O2i2.0955 (17)C11—C121.397 (3)
Mo1—O12.1124 (17)C11—C161.398 (3)
Mo1—O62.1155 (16)C12—C131.366 (4)
Mo1—Mo1i2.1227 (4)C13—C141.379 (4)
Mo1—O52.1427 (16)C14—C151.379 (4)
Mo1—N1ii2.594 (2)C15—C161.362 (4)
F11—C121.337 (3)C31—C321.368 (4)
F12—C131.335 (3)C31—C361.379 (4)
F13—C141.325 (3)C32—C331.383 (4)
F14—C151.340 (3)C33—C341.373 (4)
F15—C161.338 (3)C34—C351.365 (4)
F31—C321.338 (3)C35—C361.381 (4)
F32—C331.325 (3)N1—C511.318 (4)
F33—C341.333 (3)N1—C521.327 (4)
F34—C351.341 (3)C51—C551.383 (4)
F35—C361.333 (3)C51—H51A0.9300
O1—C11.272 (3)C52—C531.385 (4)
O2—C11.274 (3)C52—H52A0.9300
O2—Mo1i2.0955 (17)C53—C541.393 (4)
O5—C31.261 (3)C53—H53A0.9300
O6—C3i1.261 (3)C54—C551.385 (4)
C1—C111.480 (3)C54—C54iii1.489 (5)
C3—O6i1.261 (3)C55—H55A0.9300
C3—C311.508 (3)
O2i—Mo1—O1176.82 (6)F15—C16—C11120.6 (2)
O2i—Mo1—O692.90 (7)C15—C16—C11122.5 (2)
O1—Mo1—O685.79 (7)C32—C31—C36118.0 (2)
O2i—Mo1—Mo1i92.41 (4)C32—C31—C3119.8 (2)
O1—Mo1—Mo1i90.57 (4)C36—C31—C3122.2 (2)
O6—Mo1—Mo1i93.70 (4)F31—C32—C31119.4 (2)
O2i—Mo1—O585.43 (7)F31—C32—C33118.7 (3)
O1—Mo1—O595.73 (7)C31—C32—C33121.9 (3)
O6—Mo1—O5176.63 (6)F32—C33—C34120.4 (3)
Mo1i—Mo1—O589.29 (4)F32—C33—C32120.8 (3)
C1—O1—Mo1117.52 (15)C34—C33—C32118.9 (3)
C1—O2—Mo1i116.51 (15)F33—C34—C35119.8 (3)
C3—O5—Mo1117.24 (14)F33—C34—C33119.8 (3)
C3i—O6—Mo1114.32 (14)C35—C34—C33120.5 (2)
O1—C1—O2122.5 (2)F34—C35—C34119.9 (3)
O1—C1—C11119.5 (2)F34—C35—C36120.3 (3)
O2—C1—C11118.0 (2)C34—C35—C36119.8 (3)
O5—C3—O6i124.7 (2)F35—C36—C31119.9 (2)
O5—C3—C31117.2 (2)F35—C36—C35119.0 (3)
O6i—C3—C31118.1 (2)C31—C36—C35121.0 (3)
C12—C11—C16115.6 (2)C51—N1—C52116.5 (2)
C12—C11—C1122.4 (2)N1—C51—C55124.1 (3)
C16—C11—C1122.0 (2)N1—C51—H51A117.9
F11—C12—C13117.1 (2)C55—C51—H51A117.9
F11—C12—C11120.6 (2)N1—C52—C53123.8 (3)
C13—C12—C11122.3 (2)N1—C52—H52A118.1
F12—C13—C12121.0 (3)C53—C52—H52A118.1
F12—C13—C14118.7 (3)C52—C53—C54119.7 (3)
C12—C13—C14120.3 (2)C52—C53—H53A120.2
F13—C14—C15120.5 (3)C54—C53—H53A120.2
F13—C14—C13120.6 (3)C55—C54—C53116.0 (2)
C15—C14—C13119.0 (3)C55—C54—C54iii122.0 (3)
F14—C15—C16120.4 (2)C53—C54—C54iii122.0 (3)
F14—C15—C14119.3 (3)C51—C55—C54119.9 (3)
C16—C15—C14120.3 (2)C51—C55—H55A120.1
F15—C16—C15116.8 (2)C54—C55—H55A120.1
O6—Mo1—O1—C191.22 (16)C1—C11—C16—F15−2.7 (4)
Mo1i—Mo1—O1—C1−2.45 (16)C12—C11—C16—C15−0.8 (4)
O5—Mo1—O1—C1−91.80 (16)C1—C11—C16—C15179.2 (2)
O2i—Mo1—O5—C3−89.66 (18)O5—C3—C31—C32−72.1 (3)
O1—Mo1—O5—C393.32 (18)O6i—C3—C31—C32105.4 (3)
Mo1i—Mo1—O5—C32.82 (18)O5—C3—C31—C36107.0 (3)
O2i—Mo1—O6—C3i98.99 (17)O6i—C3—C31—C36−75.6 (3)
O1—Mo1—O6—C3i−83.91 (17)C36—C31—C32—F31178.7 (2)
Mo1i—Mo1—O6—C3i6.38 (17)C3—C31—C32—F31−2.2 (4)
Mo1—O1—C1—O27.3 (3)C36—C31—C32—C33−1.2 (4)
Mo1—O1—C1—C11−172.39 (15)C3—C31—C32—C33177.9 (2)
Mo1i—O2—C1—O1−8.4 (3)F31—C32—C33—F320.9 (4)
Mo1i—O2—C1—C11171.27 (15)C31—C32—C33—F32−179.3 (3)
Mo1—O5—C3—O6i−9.2 (3)F31—C32—C33—C34179.8 (2)
Mo1—O5—C3—C31168.03 (16)C31—C32—C33—C34−0.3 (4)
O1—C1—C11—C12−22.4 (3)F32—C33—C34—F331.7 (4)
O2—C1—C11—C12157.9 (2)C32—C33—C34—F33−177.3 (2)
O1—C1—C11—C16157.6 (2)F32—C33—C34—C35−179.4 (3)
O2—C1—C11—C16−22.1 (3)C32—C33—C34—C351.7 (4)
C16—C11—C12—F11−179.9 (2)F33—C34—C35—F34−1.1 (4)
C1—C11—C12—F110.0 (4)C33—C34—C35—F34179.9 (3)
C16—C11—C12—C132.0 (4)F33—C34—C35—C36177.4 (3)
C1—C11—C12—C13−178.1 (2)C33—C34—C35—C36−1.5 (4)
F11—C12—C13—F120.0 (4)C32—C31—C36—F35179.4 (2)
C11—C12—C13—F12178.2 (2)C3—C31—C36—F350.3 (4)
F11—C12—C13—C14−179.9 (2)C32—C31—C36—C351.3 (4)
C11—C12—C13—C14−1.8 (4)C3—C31—C36—C35−177.8 (2)
F12—C13—C14—F131.4 (4)F34—C35—C36—F350.5 (4)
C12—C13—C14—F13−178.6 (2)C34—C35—C36—F35−178.0 (3)
F12—C13—C14—C15−179.6 (3)F34—C35—C36—C31178.6 (3)
C12—C13—C14—C150.3 (4)C34—C35—C36—C310.0 (4)
F13—C14—C15—F141.7 (4)C52—N1—C51—C55−0.3 (4)
C13—C14—C15—F14−177.2 (3)C51—N1—C52—C530.6 (4)
F13—C14—C15—C16179.7 (2)N1—C52—C53—C54−0.1 (5)
C13—C14—C15—C160.8 (4)C52—C53—C54—C55−0.7 (4)
F14—C15—C16—F15−0.7 (4)C52—C53—C54—C54iii179.9 (3)
C14—C15—C16—F15−178.7 (2)N1—C51—C55—C54−0.5 (4)
F14—C15—C16—C11177.5 (2)C53—C54—C55—C511.0 (4)
C14—C15—C16—C11−0.5 (4)C54iii—C54—C55—C51−179.6 (3)
C12—C11—C16—F15177.3 (2)
D—H···AD—HH···AD···AD—H···A
C55—H55A···F350.932.553.152 (2)122.
C51—H51A···F33iv0.932.782.987 (3)94.
Table 1

Selected bond lengths (Å)

Mo1—O12.1124 (17)
Mo1—O62.1155 (16)
Mo1—O52.1427 (16)
Table 2

Hydrogen-bond geometry (Å, °)

D—H⋯AD—HH⋯AD⋯AD—H⋯A
C55—H55A⋯F350.932.553.152 (2)122
C51—H51A⋯F33ii0.932.782.987 (3)94

Symmetry code: (ii) .

  2 in total

1.  Expanding and shrinking porous modulation based on pillared-layer coordination polymers showing selective guest adsorption.

Authors:  Tapas Kumar Maji; Kazuhiro Uemura; Ho-Chol Chang; Ryotaro Matsuda; Susumu Kitagawa
Journal:  Angew Chem Int Ed Engl       Date:  2004-06-21       Impact factor: 15.336

2.  A short history of SHELX.

Authors:  George M Sheldrick
Journal:  Acta Crystallogr A       Date:  2007-12-21       Impact factor: 2.290
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