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The centrosymmetric title compound, [(NpO2)2(C7H4FO2)2(C10H8N2)2], contains the dimeric dioxocation (NpO2+)2 in which two of the four O atoms bridge the Np atoms. Two bidentate chelating-bridging fluoro­benzoate anions link the Np atoms of the dimeric cation. The N atoms of the 2,2′-bipyridine ligand occupy two positions in the equatorial plane of the distorted penta­gonal bipyramid, forming a five-membered metallacycle.

Supporting information

cif

Crystallographic Information File (CIF) https://doi.org/10.1107/S1600536807002164/ng2205sup1.cif
Contains datablocks global, I

hkl

Structure factor file (CIF format) https://doi.org/10.1107/S1600536807002164/ng2205Isup2.hkl
Contains datablock I

CCDC reference: 636765

Key indicators

  • Single-crystal X-ray study
  • T = 100 K
  • Mean [sigma](C-C) = 0.005 Å
  • R factor = 0.023
  • wR factor = 0.043
  • Data-to-parameter ratio = 21.2

checkCIF/PLATON results

No syntax errors found



Alert level C PLAT062_ALERT_4_C Rescale T(min) & T(max) by ..................... 0.75 PLAT764_ALERT_4_C Overcomplete CIF Bond List Detected (Rep/Expd) . 1.14 Ratio
Alert level G ABSTM02_ALERT_3_G When printed, the submitted absorption T values will be replaced by the scaled T values. Since the ratio of scaled T's is identical to the ratio of reported T values, the scaling does not imply a change to the absorption corrections used in the study. Ratio of Tmax expected/reported 0.750 Tmax scaled 0.601 Tmin scaled 0.389
0 ALERT level A = In general: serious problem 0 ALERT level B = Potentially serious problem 2 ALERT level C = Check and explain 1 ALERT level G = General alerts; check 0 ALERT type 1 CIF construction/syntax error, inconsistent or missing data 0 ALERT type 2 Indicator that the structure model may be wrong or deficient 1 ALERT type 3 Indicator that the structure quality may be low 2 ALERT type 4 Improvement, methodology, query or suggestion 0 ALERT type 5 Informative message, check

Computing details top

Data collection: SMART (Bruker, 1998); cell refinement: SAINT-Plus (Bruker, 1998); data reduction: SAINT-Plus; program(s) used to solve structure: SHELXS97 (Sheldrick, 1997a); program(s) used to refine structure: SHELXL97 (Sheldrick, 1997a); molecular graphics: SHELXTL (Sheldrick, 1997b); software used to prepare material for publication: SHELXTL.

bis(µ-2-fluorobenzoato-κ2O:O')di-µ-oxo-bis[(2,2'-bipyridine- κ2N,N')oxoneptunium(V)] top
Crystal data top
[Np2(C7H4FO2)2O4(C10H8N2)2]F(000) = 1048
Mr = 1128.67Dx = 2.283 Mg m3
Monoclinic, P21/nMo Kα radiation, λ = 0.71073 Å
Hall symbol: -P 2ynCell parameters from 5634 reflections
a = 9.3373 (5) Åθ = 2.3–30.0°
b = 10.1342 (6) ŵ = 6.36 mm1
c = 17.507 (1) ÅT = 100 K
β = 97.6551 (11)°Parallelepiped, green
V = 1641.85 (16) Å30.28 × 0.10 × 0.08 mm
Z = 2
Data collection top
Bruker SMART APEX CCD area-detector
diffractometer
4784 independent reflections
Radiation source: fine-focus sealed tube3900 reflections with I > 2σ(I)
Graphite monochromatorRint = 0.046
ω and φ scansθmax = 30.0°, θmin = 2.3°
Absorption correction: multi-scan
(SADABS; Sheldrick, 1996)
h = 1313
Tmin = 0.519, Tmax = 0.802k = 1414
20861 measured reflectionsl = 2424
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)] = 0.023Hydrogen site location: inferred from neighbouring sites
wR(F2) = 0.043H-atom parameters constrained
S = 0.99 w = 1/[σ2(Fo2) + (0.0167P)2]
where P = (Fo2 + 2Fc2)/3
4784 reflections(Δ/σ)max = 0.003
226 parametersΔρmax = 0.96 e Å3
0 restraintsΔρmin = 0.82 e Å3
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*/Ueq
Np0.864592 (12)0.586326 (11)0.535338 (7)0.00967 (3)
F0.8346 (2)0.2179 (2)0.25657 (12)0.0333 (6)
O10.9733 (2)0.60944 (19)0.45449 (12)0.0127 (4)
O20.7665 (2)0.5534 (2)0.61579 (13)0.0160 (5)
O30.7394 (2)0.4153 (2)0.45367 (12)0.0143 (4)
O40.9129 (2)0.3536 (2)0.38384 (12)0.0144 (4)
N10.6438 (3)0.7115 (2)0.45741 (15)0.0153 (5)
N20.8456 (3)0.8426 (3)0.55293 (16)0.0175 (6)
C10.5406 (4)0.6459 (3)0.4136 (2)0.0198 (7)
H10.53330.55360.42170.024*
C20.4428 (4)0.7038 (3)0.3568 (2)0.0230 (8)
H20.36920.65260.32800.028*
C30.4546 (4)0.8365 (4)0.3430 (2)0.0261 (8)
H30.39320.87850.30260.031*
C40.5595 (4)0.9078 (4)0.3901 (2)0.0245 (7)
H40.56841.00010.38270.029*
C50.6507 (3)0.8445 (3)0.44742 (19)0.0167 (7)
C60.7556 (3)0.9162 (3)0.50354 (18)0.0167 (6)
C70.7569 (4)1.0537 (3)0.5077 (2)0.0248 (8)
H70.69261.10390.47240.030*
C80.8514 (4)1.1164 (3)0.5629 (2)0.0299 (9)
H80.85431.21000.56560.036*
C90.9420 (4)1.0415 (3)0.6144 (2)0.0277 (8)
H91.00721.08210.65370.033*
C100.9354 (4)0.9049 (3)0.6072 (2)0.0239 (7)
H100.99780.85320.64260.029*
C110.7835 (3)0.3571 (3)0.39716 (17)0.0130 (6)
C120.6713 (3)0.2870 (3)0.34232 (17)0.0125 (6)
C130.6995 (3)0.2211 (3)0.27640 (18)0.0169 (6)
C140.5956 (4)0.1549 (3)0.22735 (19)0.0205 (7)
H140.62060.11030.18330.025*
C150.4539 (4)0.1548 (3)0.24348 (19)0.0197 (7)
H150.38080.11000.21040.024*
C160.4195 (4)0.2205 (3)0.3083 (2)0.0208 (7)
H160.32250.22160.31920.025*
C170.5269 (3)0.2846 (3)0.35714 (19)0.0167 (7)
H170.50220.32800.40170.020*
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
Np0.00991 (5)0.00864 (5)0.01045 (5)0.00014 (5)0.00138 (4)0.00104 (5)
F0.0206 (11)0.0547 (15)0.0255 (12)0.0050 (10)0.0059 (9)0.0164 (11)
O10.0151 (10)0.0099 (10)0.0132 (10)0.0009 (8)0.0022 (8)0.0020 (8)
O20.0173 (11)0.0155 (11)0.0157 (11)0.0005 (9)0.0045 (9)0.0014 (9)
O30.0167 (10)0.0125 (10)0.0133 (10)0.0012 (9)0.0011 (8)0.0041 (9)
O40.0141 (11)0.0132 (10)0.0155 (11)0.0007 (9)0.0003 (9)0.0021 (9)
N10.0148 (13)0.0138 (12)0.0175 (14)0.0002 (11)0.0032 (10)0.0001 (11)
N20.0155 (14)0.0134 (13)0.0243 (16)0.0013 (11)0.0053 (11)0.0030 (11)
C10.0178 (17)0.0149 (15)0.0269 (19)0.0022 (13)0.0031 (14)0.0006 (14)
C20.0146 (16)0.0256 (18)0.0275 (19)0.0007 (14)0.0017 (14)0.0006 (15)
C30.0217 (19)0.0232 (18)0.032 (2)0.0036 (15)0.0027 (15)0.0059 (16)
C40.0241 (17)0.0182 (16)0.0316 (19)0.0042 (15)0.0053 (14)0.0062 (16)
C50.0151 (16)0.0152 (15)0.0209 (17)0.0021 (12)0.0070 (13)0.0002 (13)
C60.0179 (15)0.0139 (14)0.0198 (15)0.0006 (14)0.0086 (12)0.0022 (14)
C70.034 (2)0.0135 (16)0.0269 (19)0.0003 (14)0.0057 (16)0.0028 (14)
C80.041 (2)0.0140 (17)0.038 (2)0.0082 (15)0.0174 (18)0.0048 (15)
C90.0252 (19)0.0207 (17)0.038 (2)0.0069 (15)0.0060 (16)0.0170 (16)
C100.0198 (16)0.0190 (16)0.0320 (19)0.0010 (15)0.0001 (14)0.0097 (16)
C110.0151 (15)0.0104 (13)0.0128 (15)0.0012 (12)0.0004 (12)0.0028 (11)
C120.0140 (14)0.0100 (13)0.0130 (14)0.0018 (11)0.0001 (11)0.0007 (11)
C130.0150 (15)0.0192 (16)0.0158 (15)0.0008 (13)0.0008 (12)0.0031 (13)
C140.0218 (18)0.0219 (17)0.0158 (16)0.0034 (14)0.0054 (13)0.0051 (14)
C150.0184 (17)0.0169 (16)0.0211 (17)0.0004 (13)0.0078 (13)0.0064 (13)
C160.0135 (15)0.0191 (16)0.0288 (19)0.0008 (13)0.0014 (13)0.0048 (14)
C170.0163 (16)0.0147 (15)0.0185 (16)0.0009 (12)0.0005 (12)0.0017 (12)
Geometric parameters (Å, º) top
Np—O11.863 (2)C4—C51.384 (5)
Np—O21.810 (2)C4—H40.9500
Np—O32.443 (2)C5—C61.482 (4)
Np—O1i2.488 (2)C6—C71.395 (4)
Np—O4i2.431 (2)C7—C81.375 (5)
Np—N12.640 (3)C7—H70.9500
Np—N22.624 (3)C8—C91.378 (6)
Np—Npi3.4381 (3)C8—H80.9500
F—C131.353 (4)C9—C101.391 (5)
O1—Npi2.488 (2)C9—H90.9500
O3—C111.267 (4)C10—H100.9500
O4—C111.261 (4)C11—C121.502 (4)
O4—Npi2.431 (2)C12—C131.388 (4)
N1—C11.328 (4)C12—C171.407 (4)
N1—C51.361 (4)C13—C141.380 (4)
N2—C101.339 (4)C14—C151.390 (5)
N2—C61.347 (4)C14—H140.9500
C1—C21.388 (5)C15—C161.390 (5)
C1—H10.9500C15—H150.9500
C2—C31.374 (5)C16—C171.389 (4)
C2—H20.9500C16—H160.9500
C3—C41.394 (5)C17—H170.9500
C3—H30.9500
O1—Np—O2175.93 (9)C2—C3—C4118.0 (3)
O1—Np—O384.90 (8)C2—C3—H3121.0
O1—Np—O1i76.51 (8)C4—C3—H3121.0
O1—Np—O4i84.31 (8)C5—C4—C3120.3 (3)
O1—Np—N190.78 (8)C5—C4—H4119.9
O1—Np—N290.97 (8)C3—C4—H4119.9
O2—Np—O394.15 (8)N1—C5—C4121.1 (3)
O2—Np—O1i99.42 (8)N1—C5—C6116.0 (3)
O2—Np—O4i94.31 (9)C4—C5—C6122.8 (3)
O2—Np—N192.83 (9)N2—C6—C7121.3 (3)
O2—Np—N292.40 (9)N2—C6—C5117.1 (3)
O3—Np—O1i73.47 (7)C7—C6—C5121.6 (3)
O4i—Np—O1i72.12 (7)C8—C7—C6119.9 (3)
O3—Np—N176.04 (7)C8—C7—H7120.1
O4i—Np—N275.50 (8)C6—C7—H7120.1
N1—Np—N261.62 (8)C7—C8—C9119.0 (3)
O4i—Np—O3145.46 (7)C7—C8—H8120.5
O2—Np—N292.40 (9)C9—C8—H8120.5
O1—Np—N290.97 (8)C8—C9—C10118.2 (3)
O3—Np—N2137.41 (8)C8—C9—H9120.9
O1i—Np—N2146.19 (8)C10—C9—H9120.9
O4i—Np—N1136.76 (8)N2—C10—C9123.3 (3)
O1i—Np—N1147.79 (7)N2—C10—H10118.3
O2—Np—Npi131.22 (7)C9—C10—H10118.3
O1—Np—Npi44.71 (6)O4—C11—O3125.2 (3)
O4i—Np—Npi73.99 (5)O4—C11—C12118.2 (3)
O3—Np—Npi75.28 (5)O3—C11—C12116.6 (3)
O1i—Np—Npi31.80 (5)C13—C12—C17115.9 (3)
N2—Np—Npi127.61 (6)C13—C12—C11124.5 (3)
N1—Np—Npi128.29 (6)C17—C12—C11119.6 (3)
Np—O1—Npi103.49 (8)F—C13—C14115.5 (3)
C11—O3—Np127.40 (19)F—C13—C12120.7 (3)
C11—O4—Npi130.6 (2)C14—C13—C12123.7 (3)
C1—N1—C5117.7 (3)C13—C14—C15118.9 (3)
C1—N1—Np121.0 (2)C13—C14—H14120.5
C5—N1—Np119.7 (2)C15—C14—H14120.5
C10—N2—C6118.2 (3)C14—C15—C16119.7 (3)
C10—N2—Np120.3 (2)C14—C15—H15120.2
C6—N2—Np121.2 (2)C16—C15—H15120.2
N1—C1—C2124.1 (3)C17—C16—C15120.0 (3)
N1—C1—H1118.0C17—C16—H16120.0
C2—C1—H1118.0C15—C16—H16120.0
C3—C2—C1118.6 (3)C16—C17—C12121.7 (3)
C3—C2—H2120.7C16—C17—H17119.2
C1—C2—H2120.7C12—C17—H17119.2
O4i—Np—O1—Npi72.94 (8)C1—C2—C3—C43.6 (6)
O3—Np—O1—Npi74.19 (8)C2—C3—C4—C51.7 (6)
O1i—Np—O1—Npi0.0C1—N1—C5—C44.3 (5)
N2—Np—O1—Npi148.27 (9)Np—N1—C5—C4161.1 (2)
N1—Np—O1—Npi150.10 (8)C1—N1—C5—C6172.9 (3)
O2—Np—O3—C11156.9 (2)Np—N1—C5—C621.6 (4)
O1—Np—O3—C1119.2 (2)C3—C4—C5—N12.4 (5)
O4i—Np—O3—C1153.1 (3)C3—C4—C5—C6174.6 (3)
O1i—Np—O3—C1158.2 (2)C10—N2—C6—C71.0 (5)
N2—Np—O3—C11105.0 (2)Np—N2—C6—C7172.8 (2)
N1—Np—O3—C11111.3 (2)C10—N2—C6—C5176.0 (3)
Npi—Np—O3—C1125.2 (2)Np—N2—C6—C510.2 (4)
O2—Np—N1—C185.2 (3)N1—C5—C6—N27.6 (4)
O1—Np—N1—C192.9 (3)C4—C5—C6—N2175.2 (3)
O4i—Np—N1—C1175.5 (2)N1—C5—C6—C7169.4 (3)
O3—Np—N1—C18.4 (2)C4—C5—C6—C77.8 (5)
O1i—Np—N1—C127.5 (3)N2—C6—C7—C80.1 (5)
N2—Np—N1—C1176.4 (3)C5—C6—C7—C8176.9 (3)
Npi—Np—N1—C166.4 (3)C6—C7—C8—C91.1 (6)
O2—Np—N1—C5109.9 (2)C7—C8—C9—C101.1 (6)
O1—Np—N1—C572.0 (2)C6—N2—C10—C91.0 (5)
O4i—Np—N1—C510.5 (3)Np—N2—C10—C9172.8 (3)
O3—Np—N1—C5156.6 (2)C8—C9—C10—N20.0 (6)
O1i—Np—N1—C5137.4 (2)Npi—O4—C11—O312.7 (4)
N2—Np—N1—C518.7 (2)Npi—O4—C11—C12167.25 (18)
Npi—Np—N1—C598.5 (2)Np—O3—C11—O417.9 (4)
O2—Np—N2—C1079.8 (3)Np—O3—C11—C12162.17 (18)
O1—Np—N2—C1097.9 (3)O4—C11—C12—C131.8 (4)
O4i—Np—N2—C1014.0 (2)O3—C11—C12—C13178.3 (3)
O3—Np—N2—C10178.6 (2)O4—C11—C12—C17177.6 (3)
O1i—Np—N2—C1031.1 (3)O3—C11—C12—C172.4 (4)
N1—Np—N2—C10171.7 (3)C17—C12—C13—F179.6 (3)
Npi—Np—N2—C1070.1 (3)C11—C12—C13—F1.0 (5)
O2—Np—N2—C6106.5 (2)C17—C12—C13—C140.6 (5)
O1—Np—N2—C675.8 (2)C11—C12—C13—C14178.7 (3)
O4i—Np—N2—C6159.7 (2)F—C13—C14—C15179.4 (3)
O3—Np—N2—C67.7 (3)C12—C13—C14—C150.9 (5)
O1i—Np—N2—C6142.6 (2)C13—C14—C15—C160.1 (5)
N1—Np—N2—C614.6 (2)C14—C15—C16—C170.8 (5)
Npi—Np—N2—C6103.7 (2)C15—C16—C17—C121.0 (5)
C5—N1—C1—C22.2 (5)C13—C12—C17—C160.3 (5)
Np—N1—C1—C2163.0 (3)C11—C12—C17—C16179.7 (3)
N1—C1—C2—C31.8 (6)
Symmetry code: (i) x+2, y+1, z+1.
 

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