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An organically templated neptunium(IV) fluoride compound, {(C2H10N2)[Np2F10]}n, has been synthesized under mild hydro­thermal conditions. The compound crystallizes in the monoclinic space group C2/c (No. 15). The structure consists of NpF9 tricapped trigonal prisms connected through edge- and corner-sharing to form infinite two-dimensional [Np2F10]2- sheets, that are separated by the ethyl­enedi­ammonium dications. The C2H10N22+ cations form hydrogen-bonding interactions with the [Np2F10]2- layers.

Supporting information

cif

Crystallographic Information File (CIF) https://doi.org/10.1107/S1600536804014217/cv6331sup1.cif
Contains datablocks global, I

hkl

Structure factor file (CIF format) https://doi.org/10.1107/S1600536804014217/cv6331Isup2.hkl
Contains datablock I

CCDC reference: 245145

Key indicators

  • Single-crystal X-ray study
  • T = 193 K
  • Mean [sigma](C-C) = 0.005 Å
  • R factor = 0.014
  • wR factor = 0.033
  • Data-to-parameter ratio = 16.5

checkCIF/PLATON results

No syntax errors found



Alert level C PLAT041_ALERT_1_C Calc. and Rep. SumFormula Strings Differ .... ? PLAT042_ALERT_1_C Calc. and Rep. MoietyFormula Strings Differ .... ? PLAT045_ALERT_1_C Calculated and Reported Z Differ by ............ 2.00 Ratio PLAT764_ALERT_4_C Overcomplete CIF Bond List Detected (Rep/Expd) . 1.18 Ratio
0 ALERT level A = In general: serious problem 0 ALERT level B = Potentially serious problem 4 ALERT level C = Check and explain 0 ALERT level G = General alerts; check 3 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 0 ALERT type 3 Indicator that the structure quality may be low 1 ALERT type 4 Improvement, methodology, query or suggestion

Computing details top

Data collection: SMART (Bruker, 2000); cell refinement: SMART and SAINT (Bruker, 1999); data reduction: SAINT; program(s) used to solve structure: SHELXS97 in SHELXTL97 (Sheldrick, 2000); program(s) used to refine structure: SHELXL97 in SHELXTL97; molecular graphics: SHELXP97 in SHELXTL97; software used to prepare material for publication: SHELXCIF97 in in SHELXTL97.

(I) top
Crystal data top
(C2H10N2)[Np2F10]F(000) = 1248
Mr = 726.12Dx = 4.894 Mg m3
Monoclinic, C2/cMo Kα radiation, λ = 0.71073 Å
Hall symbol: -c_2ycCell parameters from 4826 reflections
a = 16.0190 (11) Åθ = 3.2–28.3°
b = 7.0570 (5) ŵ = 21.10 mm1
c = 8.7203 (6) ÅT = 193 K
β = 91.536 (1)°Prism, green
V = 985.44 (12) Å30.11 × 0.07 × 0.05 mm
Z = 4
Data collection top
Bruker APEX
diffractometer
1224 independent reflections
Radiation source: fine-focus sealed tube1185 reflections with I > 2σ(I)
Graphite monochromatorRint = 0.022
0.3 ω exposures scansθmax = 28.3°, θmin = 3.2°
Absorption correction: analytical
SHELXPREP97 in SHELXTL97 (Sheldrick, 2000) and SADABS (Sheldrick, 1997)
h = 2121
Tmin = 0.126, Tmax = 0.371k = 99
4826 measured reflectionsl = 1111
Refinement top
Refinement on F2Secondary atom site location: difference Fourier map
Least-squares matrix: fullHydrogen site location: inferred from neighbouring sites
R[F2 > 2σ(F2)] = 0.014H atoms treated by a mixture of independent and constrained refinement
wR(F2) = 0.033 w = 1/[σ2(Fo2) + (0.0131P)2 + 2.3052P]
where P = (Fo2 + 2Fc2)/3
S = 1.15(Δ/σ)max = 0.002
1224 reflectionsΔρmax = 0.84 e Å3
74 parametersΔρmin = 0.74 e Å3
0 restraintsExtinction correction: SHELXTL97, Fc*=kFc[1+0.001xFc2λ3/sin(2θ)]-1/4
Primary atom site location: structure-invariant direct methodsExtinction coefficient: 0.00049 (5)
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
Np10.219411 (7)0.906689 (17)0.670144 (13)0.00792 (7)
F10.32224 (12)0.8217 (3)0.5047 (2)0.0121 (4)
F20.31883 (12)0.7240 (3)0.7957 (2)0.0128 (4)
F30.08169 (13)0.9249 (3)0.6639 (2)0.0151 (4)
F40.19746 (13)0.9529 (3)0.9285 (2)0.0130 (4)
F50.17109 (13)0.6151 (3)0.7876 (2)0.0125 (4)
N10.54642 (18)0.7570 (4)0.4833 (3)0.0153 (6)
H1A0.56170.66960.55540.023*
H1B0.50650.70690.41910.023*
H1E0.59170.79010.42840.023*
C10.5127 (2)0.9275 (5)0.5599 (4)0.0148 (7)
H1C0.46370.89200.62060.018*
H1D0.55570.98180.63070.018*
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
Np10.00944 (9)0.00774 (9)0.00655 (8)0.00003 (4)0.00027 (5)0.00017 (4)
F10.0119 (9)0.0119 (10)0.0126 (9)0.0014 (7)0.0018 (7)0.0007 (7)
F20.0122 (10)0.0112 (9)0.0146 (9)0.0015 (7)0.0032 (8)0.0018 (8)
F30.0123 (10)0.0138 (10)0.0191 (11)0.0003 (7)0.0003 (8)0.0018 (8)
F40.0184 (10)0.0112 (9)0.0096 (9)0.0003 (8)0.0012 (8)0.0014 (8)
F50.0143 (10)0.0110 (9)0.0121 (10)0.0000 (7)0.0009 (8)0.0016 (7)
N10.0138 (14)0.0162 (16)0.0157 (14)0.0010 (11)0.0024 (11)0.0015 (12)
C10.0129 (17)0.0177 (18)0.0137 (17)0.0014 (13)0.0009 (13)0.0010 (13)
Geometric parameters (Å, º) top
Np1—F32.209 (2)Np1—Np1i3.8487 (3)
Np1—F12.2981 (19)Np1—Np1iv3.9086 (3)
Np1—F22.3029 (19)N1—C11.485 (4)
Np1—F1i2.3053 (19)N1—H1A0.9100
Np1—F5ii2.311 (2)N1—H1B0.9100
Np1—F42.3124 (19)N1—H1E0.9100
Np1—F2ii2.343 (2)C1—C1v1.511 (7)
Np1—F4iii2.3467 (19)C1—H1C0.9900
Np1—F52.4341 (19)C1—H1D0.9900
F3—Np1—F1137.04 (7)F4—Np1—Np1i151.72 (5)
F3—Np1—F2136.20 (7)F2ii—Np1—Np1i136.07 (5)
F1—Np1—F269.77 (7)F4iii—Np1—Np1i65.51 (5)
F3—Np1—F1i75.72 (7)F5—Np1—Np1i85.94 (5)
F1—Np1—F1i66.54 (8)F3—Np1—Np1iv107.58 (5)
F2—Np1—F1i96.16 (7)F1—Np1—Np1iv79.11 (5)
F3—Np1—F5ii136.06 (7)F2—Np1—Np1iv33.03 (5)
F1—Np1—F5ii73.28 (7)F1i—Np1—Np1iv70.72 (5)
F2—Np1—F5ii76.61 (7)F5ii—Np1—Np1iv109.62 (5)
F1i—Np1—F5ii139.06 (7)F4—Np1—Np1iv79.83 (5)
F3—Np1—F480.67 (8)F2ii—Np1—Np1iv151.83 (5)
F1—Np1—F4141.13 (7)F4iii—Np1—Np1iv137.00 (5)
F2—Np1—F474.76 (7)F5—Np1—Np1iv33.53 (5)
F1i—Np1—F4133.96 (7)Np1i—Np1—Np1iv71.905 (6)
F5ii—Np1—F483.66 (7)F3—Np1—Np1ii101.35 (5)
F3—Np1—F2ii71.52 (7)F1—Np1—Np1ii106.39 (5)
F1—Np1—F2ii121.57 (7)F2—Np1—Np1ii99.93 (5)
F2—Np1—F2ii130.88 (5)F1i—Np1—Np1ii158.79 (5)
F1i—Np1—F2ii132.88 (7)F5ii—Np1—Np1ii35.58 (5)
F5ii—Np1—F2ii64.61 (7)F4—Np1—Np1ii64.46 (5)
F4—Np1—F2ii72.20 (7)F2ii—Np1—Np1ii32.40 (5)
F3—Np1—F4iii80.08 (7)F4iii—Np1—Np1ii88.22 (5)
F1—Np1—F4iii68.85 (7)F5—Np1—Np1ii133.84 (5)
F2—Np1—F4iii138.45 (7)Np1i—Np1—Np1ii136.624 (7)
F1i—Np1—F4iii70.58 (7)Np1iv—Np1—Np1ii129.045 (8)
F5ii—Np1—F4iii88.23 (7)Np1—F1—Np1i113.46 (8)
F4—Np1—F4iii142.40 (5)Np1—F2—Np1iv114.56 (8)
F2ii—Np1—F4iii71.16 (7)Np1—F4—Np1vi155.69 (10)
F3—Np1—F574.40 (7)Np1iv—F5—Np1110.89 (8)
F1—Np1—F5106.56 (7)C1—N1—H1A109.5
F2—Np1—F563.28 (7)C1—N1—H1B109.5
F1i—Np1—F566.28 (7)H1A—N1—H1B109.5
F5ii—Np1—F5136.01 (3)C1—N1—H1E109.5
F4—Np1—F569.56 (7)H1A—N1—H1E109.5
F2ii—Np1—F5131.86 (7)H1B—N1—H1E109.5
F4iii—Np1—F5133.89 (7)N1—C1—C1v109.4 (4)
F3—Np1—Np1i106.81 (5)N1—C1—H1C109.8
F1—Np1—Np1i33.33 (5)C1v—C1—H1C109.8
F2—Np1—Np1i81.82 (5)N1—C1—H1D109.8
F1i—Np1—Np1i33.21 (5)C1v—C1—H1D109.8
F5ii—Np1—Np1i106.30 (5)H1C—C1—H1D108.2
Symmetry codes: (i) x+1/2, y3/2, z+1; (ii) x+1/2, y1/2, z+3/2; (iii) x, y2, z1/2; (iv) x+1/2, y+1/2, z+3/2; (v) x+1, y2, z+1; (vi) x, y2, z+1/2.
 

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