Supporting information
Crystallographic Information File (CIF) https://doi.org/10.1107/S1600536804014217/cv6331sup1.cif | |
Structure factor file (CIF format) https://doi.org/10.1107/S1600536804014217/cv6331Isup2.hkl |
CCDC reference: 245145
Key indicators
- Single-crystal X-ray study
- T = 193 K
- Mean (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
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.
(C2H10N2)[Np2F10] | F(000) = 1248 |
Mr = 726.12 | Dx = 4.894 Mg m−3 |
Monoclinic, C2/c | Mo Kα radiation, λ = 0.71073 Å |
Hall symbol: -c_2yc | Cell parameters from 4826 reflections |
a = 16.0190 (11) Å | θ = 3.2–28.3° |
b = 7.0570 (5) Å | µ = 21.10 mm−1 |
c = 8.7203 (6) Å | T = 193 K |
β = 91.536 (1)° | Prism, green |
V = 985.44 (12) Å3 | 0.11 × 0.07 × 0.05 mm |
Z = 4 |
Bruker APEX diffractometer | 1224 independent reflections |
Radiation source: fine-focus sealed tube | 1185 reflections with I > 2σ(I) |
Graphite monochromator | Rint = 0.022 |
0.3 ω exposures scans | θmax = 28.3°, θmin = 3.2° |
Absorption correction: analytical SHELXPREP97 in SHELXTL97 (Sheldrick, 2000) and SADABS (Sheldrick, 1997) | h = −21→21 |
Tmin = 0.126, Tmax = 0.371 | k = −9→9 |
4826 measured reflections | l = −11→11 |
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)] = 0.014 | H 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 reflections | Δρmax = 0.84 e Å−3 |
74 parameters | Δρmin = −0.74 e Å−3 |
0 restraints | Extinction correction: SHELXTL97, Fc*=kFc[1+0.001xFc2λ3/sin(2θ)]-1/4 |
Primary atom site location: structure-invariant direct methods | Extinction coefficient: 0.00049 (5) |
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 | ||
Np1 | 0.219411 (7) | −0.906689 (17) | 0.670144 (13) | 0.00792 (7) | |
F1 | 0.32224 (12) | −0.8217 (3) | 0.5047 (2) | 0.0121 (4) | |
F2 | 0.31883 (12) | −0.7240 (3) | 0.7957 (2) | 0.0128 (4) | |
F3 | 0.08169 (13) | −0.9249 (3) | 0.6639 (2) | 0.0151 (4) | |
F4 | 0.19746 (13) | −0.9529 (3) | 0.9285 (2) | 0.0130 (4) | |
F5 | 0.17109 (13) | −0.6151 (3) | 0.7876 (2) | 0.0125 (4) | |
N1 | 0.54642 (18) | −0.7570 (4) | 0.4833 (3) | 0.0153 (6) | |
H1A | 0.5617 | −0.6696 | 0.5554 | 0.023* | |
H1B | 0.5065 | −0.7069 | 0.4191 | 0.023* | |
H1E | 0.5917 | −0.7901 | 0.4284 | 0.023* | |
C1 | 0.5127 (2) | −0.9275 (5) | 0.5599 (4) | 0.0148 (7) | |
H1C | 0.4637 | −0.8920 | 0.6206 | 0.018* | |
H1D | 0.5557 | −0.9818 | 0.6307 | 0.018* |
U11 | U22 | U33 | U12 | U13 | U23 | |
Np1 | 0.00944 (9) | 0.00774 (9) | 0.00655 (8) | −0.00003 (4) | −0.00027 (5) | 0.00017 (4) |
F1 | 0.0119 (9) | 0.0119 (10) | 0.0126 (9) | 0.0014 (7) | 0.0018 (7) | 0.0007 (7) |
F2 | 0.0122 (10) | 0.0112 (9) | 0.0146 (9) | 0.0015 (7) | −0.0032 (8) | −0.0018 (8) |
F3 | 0.0123 (10) | 0.0138 (10) | 0.0191 (11) | 0.0003 (7) | 0.0003 (8) | 0.0018 (8) |
F4 | 0.0184 (10) | 0.0112 (9) | 0.0096 (9) | 0.0003 (8) | 0.0012 (8) | 0.0014 (8) |
F5 | 0.0143 (10) | 0.0110 (9) | 0.0121 (10) | 0.0000 (7) | −0.0009 (8) | −0.0016 (7) |
N1 | 0.0138 (14) | 0.0162 (16) | 0.0157 (14) | −0.0010 (11) | −0.0024 (11) | 0.0015 (12) |
C1 | 0.0129 (17) | 0.0177 (18) | 0.0137 (17) | −0.0014 (13) | 0.0009 (13) | 0.0010 (13) |
Np1—F3 | 2.209 (2) | Np1—Np1i | 3.8487 (3) |
Np1—F1 | 2.2981 (19) | Np1—Np1iv | 3.9086 (3) |
Np1—F2 | 2.3029 (19) | N1—C1 | 1.485 (4) |
Np1—F1i | 2.3053 (19) | N1—H1A | 0.9100 |
Np1—F5ii | 2.311 (2) | N1—H1B | 0.9100 |
Np1—F4 | 2.3124 (19) | N1—H1E | 0.9100 |
Np1—F2ii | 2.343 (2) | C1—C1v | 1.511 (7) |
Np1—F4iii | 2.3467 (19) | C1—H1C | 0.9900 |
Np1—F5 | 2.4341 (19) | C1—H1D | 0.9900 |
F3—Np1—F1 | 137.04 (7) | F4—Np1—Np1i | 151.72 (5) |
F3—Np1—F2 | 136.20 (7) | F2ii—Np1—Np1i | 136.07 (5) |
F1—Np1—F2 | 69.77 (7) | F4iii—Np1—Np1i | 65.51 (5) |
F3—Np1—F1i | 75.72 (7) | F5—Np1—Np1i | 85.94 (5) |
F1—Np1—F1i | 66.54 (8) | F3—Np1—Np1iv | 107.58 (5) |
F2—Np1—F1i | 96.16 (7) | F1—Np1—Np1iv | 79.11 (5) |
F3—Np1—F5ii | 136.06 (7) | F2—Np1—Np1iv | 33.03 (5) |
F1—Np1—F5ii | 73.28 (7) | F1i—Np1—Np1iv | 70.72 (5) |
F2—Np1—F5ii | 76.61 (7) | F5ii—Np1—Np1iv | 109.62 (5) |
F1i—Np1—F5ii | 139.06 (7) | F4—Np1—Np1iv | 79.83 (5) |
F3—Np1—F4 | 80.67 (8) | F2ii—Np1—Np1iv | 151.83 (5) |
F1—Np1—F4 | 141.13 (7) | F4iii—Np1—Np1iv | 137.00 (5) |
F2—Np1—F4 | 74.76 (7) | F5—Np1—Np1iv | 33.53 (5) |
F1i—Np1—F4 | 133.96 (7) | Np1i—Np1—Np1iv | 71.905 (6) |
F5ii—Np1—F4 | 83.66 (7) | F3—Np1—Np1ii | 101.35 (5) |
F3—Np1—F2ii | 71.52 (7) | F1—Np1—Np1ii | 106.39 (5) |
F1—Np1—F2ii | 121.57 (7) | F2—Np1—Np1ii | 99.93 (5) |
F2—Np1—F2ii | 130.88 (5) | F1i—Np1—Np1ii | 158.79 (5) |
F1i—Np1—F2ii | 132.88 (7) | F5ii—Np1—Np1ii | 35.58 (5) |
F5ii—Np1—F2ii | 64.61 (7) | F4—Np1—Np1ii | 64.46 (5) |
F4—Np1—F2ii | 72.20 (7) | F2ii—Np1—Np1ii | 32.40 (5) |
F3—Np1—F4iii | 80.08 (7) | F4iii—Np1—Np1ii | 88.22 (5) |
F1—Np1—F4iii | 68.85 (7) | F5—Np1—Np1ii | 133.84 (5) |
F2—Np1—F4iii | 138.45 (7) | Np1i—Np1—Np1ii | 136.624 (7) |
F1i—Np1—F4iii | 70.58 (7) | Np1iv—Np1—Np1ii | 129.045 (8) |
F5ii—Np1—F4iii | 88.23 (7) | Np1—F1—Np1i | 113.46 (8) |
F4—Np1—F4iii | 142.40 (5) | Np1—F2—Np1iv | 114.56 (8) |
F2ii—Np1—F4iii | 71.16 (7) | Np1—F4—Np1vi | 155.69 (10) |
F3—Np1—F5 | 74.40 (7) | Np1iv—F5—Np1 | 110.89 (8) |
F1—Np1—F5 | 106.56 (7) | C1—N1—H1A | 109.5 |
F2—Np1—F5 | 63.28 (7) | C1—N1—H1B | 109.5 |
F1i—Np1—F5 | 66.28 (7) | H1A—N1—H1B | 109.5 |
F5ii—Np1—F5 | 136.01 (3) | C1—N1—H1E | 109.5 |
F4—Np1—F5 | 69.56 (7) | H1A—N1—H1E | 109.5 |
F2ii—Np1—F5 | 131.86 (7) | H1B—N1—H1E | 109.5 |
F4iii—Np1—F5 | 133.89 (7) | N1—C1—C1v | 109.4 (4) |
F3—Np1—Np1i | 106.81 (5) | N1—C1—H1C | 109.8 |
F1—Np1—Np1i | 33.33 (5) | C1v—C1—H1C | 109.8 |
F2—Np1—Np1i | 81.82 (5) | N1—C1—H1D | 109.8 |
F1i—Np1—Np1i | 33.21 (5) | C1v—C1—H1D | 109.8 |
F5ii—Np1—Np1i | 106.30 (5) | H1C—C1—H1D | 108.2 |
Symmetry codes: (i) −x+1/2, −y−3/2, −z+1; (ii) −x+1/2, y−1/2, −z+3/2; (iii) x, −y−2, z−1/2; (iv) −x+1/2, y+1/2, −z+3/2; (v) −x+1, −y−2, −z+1; (vi) x, −y−2, z+1/2. |