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Commercially available nitronium tetrafluoroborate, NO2+·BF4-, has been recrystallized from CH2Cl2 as a side-product of a reaction in which it has been used as a starting material. Both the NO2+ cations and the BF4-anions are packed in considerably distorted cubic environments. The N=O distances of 1.1153 (8) and 1.1160 (7) Å as well as the O=N=O bond angle of 179.89 (7)° are similar to those found in other NO2+-containing salts described in the literature.
Supporting information
Key indicators
- Single-crystal X-ray study
- T = 100 K
- Mean (O-N) = 0.001 Å
- R factor = 0.019
- wR factor = 0.061
- Data-to-parameter ratio = 10.5
checkCIF/PLATON results
No syntax errors found
Alert level A
PLAT431_ALERT_2_A Short Inter HL..A Contact F1 .. N1 .. 2.50 Ang.
| Author Response: Bonding interaction between cation and anion
PROBLEM: Short Inter HL..A Contact F2 .. N1 .. 2.50 Ang.
RESPONSE: Bonding interaction between cation and anion
Bonding interaction between cation and anion
PROBLEM: Short Inter HL..A Contact F5 .. N1 .. 2.50 Ang.
RESPONSE: Bonding interaction between cation and anion
Bonding interaction between cation and anion
PROBLEM: Short Inter HL..A Contact F6 .. N1 .. 2.50 Ang.
RESPONSE: Bonding interaction between cation and anion
Bonding interaction between cation and anion
|
PLAT431_ALERT_2_A Short Inter HL..A Contact F2 .. N1 .. 2.48 Ang.
| Author Response: Bonding interaction between cation and anion
PROBLEM: Short Inter HL..A Contact F2 .. N1 .. 2.50 Ang.
RESPONSE: Bonding interaction between cation and anion
Bonding interaction between cation and anion
PROBLEM: Short Inter HL..A Contact F5 .. N1 .. 2.50 Ang.
RESPONSE: Bonding interaction between cation and anion
Bonding interaction between cation and anion
PROBLEM: Short Inter HL..A Contact F6 .. N1 .. 2.50 Ang.
RESPONSE: Bonding interaction between cation and anion
Bonding interaction between cation and anion
|
PLAT431_ALERT_2_A Short Inter HL..A Contact F5 .. N1 .. 2.47 Ang.
| Author Response: Bonding interaction between cation and anion
PROBLEM: Short Inter HL..A Contact F2 .. N1 .. 2.50 Ang.
RESPONSE: Bonding interaction between cation and anion
Bonding interaction between cation and anion
PROBLEM: Short Inter HL..A Contact F5 .. N1 .. 2.50 Ang.
RESPONSE: Bonding interaction between cation and anion
Bonding interaction between cation and anion
PROBLEM: Short Inter HL..A Contact F6 .. N1 .. 2.50 Ang.
RESPONSE: Bonding interaction between cation and anion
Bonding interaction between cation and anion
|
PLAT431_ALERT_2_A Short Inter HL..A Contact F6 .. N1 .. 2.48 Ang.
| Author Response: Bonding interaction between cation and anion
PROBLEM: Short Inter HL..A Contact F2 .. N1 .. 2.50 Ang.
RESPONSE: Bonding interaction between cation and anion
Bonding interaction between cation and anion
PROBLEM: Short Inter HL..A Contact F5 .. N1 .. 2.50 Ang.
RESPONSE: Bonding interaction between cation and anion
Bonding interaction between cation and anion
PROBLEM: Short Inter HL..A Contact F6 .. N1 .. 2.50 Ang.
RESPONSE: Bonding interaction between cation and anion
Bonding interaction between cation and anion
|
Alert level B
PLAT110_ALERT_2_B ADDSYM Detects Potential Lattice Centering or Halving . ?
PLAT431_ALERT_2_B Short Inter HL..A Contact F2 .. O2 .. 2.68 Ang.
| Author Response: Bonding interaction between cation and anion
PROBLEM: Short Inter HL..A Contact F2 .. N1 .. 2.50 Ang.
RESPONSE: Bonding interaction between cation and anion
Bonding interaction between cation and anion
PROBLEM: Short Inter HL..A Contact F5 .. N1 .. 2.50 Ang.
RESPONSE: Bonding interaction between cation and anion
Bonding interaction between cation and anion
PROBLEM: Short Inter HL..A Contact F6 .. N1 .. 2.50 Ang.
RESPONSE: Bonding interaction between cation and anion
Bonding interaction between cation and anion
|
PLAT431_ALERT_2_B Short Inter HL..A Contact F5 .. O1 .. 2.68 Ang.
| Author Response: Bonding interaction between cation and anion
PROBLEM: Short Inter HL..A Contact F2 .. N1 .. 2.50 Ang.
RESPONSE: Bonding interaction between cation and anion
Bonding interaction between cation and anion
PROBLEM: Short Inter HL..A Contact F5 .. N1 .. 2.50 Ang.
RESPONSE: Bonding interaction between cation and anion
Bonding interaction between cation and anion
PROBLEM: Short Inter HL..A Contact F6 .. N1 .. 2.50 Ang.
RESPONSE: Bonding interaction between cation and anion
Bonding interaction between cation and anion
|
PLAT431_ALERT_2_B Short Inter HL..A Contact F6 .. O2 .. 2.67 Ang.
| Author Response: Bonding interaction between cation and anion
PROBLEM: Short Inter HL..A Contact F2 .. N1 .. 2.50 Ang.
RESPONSE: Bonding interaction between cation and anion
Bonding interaction between cation and anion
PROBLEM: Short Inter HL..A Contact F5 .. N1 .. 2.50 Ang.
RESPONSE: Bonding interaction between cation and anion
Bonding interaction between cation and anion
PROBLEM: Short Inter HL..A Contact F6 .. N1 .. 2.50 Ang.
RESPONSE: Bonding interaction between cation and anion
Bonding interaction between cation and anion
|
Alert level C
PLAT042_ALERT_1_C Calc. and Rep. MoietyFormula Strings Differ .... ?
PLAT068_ALERT_1_C Reported F000 Differs from Calcd (or Missing)... ?
PLAT431_ALERT_2_C Short Inter HL..A Contact F1 .. O1 .. 2.72 Ang.
| Author Response: Bonding interaction between cation and anion
PROBLEM: Short Inter HL..A Contact F2 .. N1 .. 2.50 Ang.
RESPONSE: Bonding interaction between cation and anion
Bonding interaction between cation and anion
PROBLEM: Short Inter HL..A Contact F5 .. N1 .. 2.50 Ang.
RESPONSE: Bonding interaction between cation and anion
Bonding interaction between cation and anion
PROBLEM: Short Inter HL..A Contact F6 .. N1 .. 2.50 Ang.
RESPONSE: Bonding interaction between cation and anion
Bonding interaction between cation and anion
|
PLAT431_ALERT_2_C Short Inter HL..A Contact F1 .. O2 .. 2.76 Ang.
| Author Response: Bonding interaction between cation and anion
PROBLEM: Short Inter HL..A Contact F2 .. N1 .. 2.50 Ang.
RESPONSE: Bonding interaction between cation and anion
Bonding interaction between cation and anion
PROBLEM: Short Inter HL..A Contact F5 .. N1 .. 2.50 Ang.
RESPONSE: Bonding interaction between cation and anion
Bonding interaction between cation and anion
PROBLEM: Short Inter HL..A Contact F6 .. N1 .. 2.50 Ang.
RESPONSE: Bonding interaction between cation and anion
Bonding interaction between cation and anion
|
PLAT431_ALERT_2_C Short Inter HL..A Contact F1 .. O2 .. 2.79 Ang.
| Author Response: Bonding interaction between cation and anion
PROBLEM: Short Inter HL..A Contact F2 .. N1 .. 2.50 Ang.
RESPONSE: Bonding interaction between cation and anion
Bonding interaction between cation and anion
PROBLEM: Short Inter HL..A Contact F5 .. N1 .. 2.50 Ang.
RESPONSE: Bonding interaction between cation and anion
Bonding interaction between cation and anion
PROBLEM: Short Inter HL..A Contact F6 .. N1 .. 2.50 Ang.
RESPONSE: Bonding interaction between cation and anion
Bonding interaction between cation and anion
|
PLAT431_ALERT_2_C Short Inter HL..A Contact F2 .. O1 .. 2.76 Ang.
| Author Response: Bonding interaction between cation and anion
PROBLEM: Short Inter HL..A Contact F2 .. N1 .. 2.50 Ang.
RESPONSE: Bonding interaction between cation and anion
Bonding interaction between cation and anion
PROBLEM: Short Inter HL..A Contact F5 .. N1 .. 2.50 Ang.
RESPONSE: Bonding interaction between cation and anion
Bonding interaction between cation and anion
PROBLEM: Short Inter HL..A Contact F6 .. N1 .. 2.50 Ang.
RESPONSE: Bonding interaction between cation and anion
Bonding interaction between cation and anion
|
PLAT431_ALERT_2_C Short Inter HL..A Contact F2 .. O1 .. 2.78 Ang.
| Author Response: Bonding interaction between cation and anion
PROBLEM: Short Inter HL..A Contact F2 .. N1 .. 2.50 Ang.
RESPONSE: Bonding interaction between cation and anion
Bonding interaction between cation and anion
PROBLEM: Short Inter HL..A Contact F5 .. N1 .. 2.50 Ang.
RESPONSE: Bonding interaction between cation and anion
Bonding interaction between cation and anion
PROBLEM: Short Inter HL..A Contact F6 .. N1 .. 2.50 Ang.
RESPONSE: Bonding interaction between cation and anion
Bonding interaction between cation and anion
|
PLAT431_ALERT_2_C Short Inter HL..A Contact F2 .. O1 .. 2.90 Ang.
| Author Response: Bonding interaction between cation and anion
PROBLEM: Short Inter HL..A Contact F2 .. N1 .. 2.50 Ang.
RESPONSE: Bonding interaction between cation and anion
Bonding interaction between cation and anion
PROBLEM: Short Inter HL..A Contact F5 .. N1 .. 2.50 Ang.
RESPONSE: Bonding interaction between cation and anion
Bonding interaction between cation and anion
PROBLEM: Short Inter HL..A Contact F6 .. N1 .. 2.50 Ang.
RESPONSE: Bonding interaction between cation and anion
Bonding interaction between cation and anion
|
PLAT431_ALERT_2_C Short Inter HL..A Contact F5 .. O2 .. 2.75 Ang.
| Author Response: Bonding interaction between cation and anion
PROBLEM: Short Inter HL..A Contact F2 .. N1 .. 2.50 Ang.
RESPONSE: Bonding interaction between cation and anion
Bonding interaction between cation and anion
PROBLEM: Short Inter HL..A Contact F5 .. N1 .. 2.50 Ang.
RESPONSE: Bonding interaction between cation and anion
Bonding interaction between cation and anion
PROBLEM: Short Inter HL..A Contact F6 .. N1 .. 2.50 Ang.
RESPONSE: Bonding interaction between cation and anion
Bonding interaction between cation and anion
|
PLAT431_ALERT_2_C Short Inter HL..A Contact F5 .. O2 .. 2.96 Ang.
| Author Response: Bonding interaction between cation and anion
PROBLEM: Short Inter HL..A Contact F2 .. N1 .. 2.50 Ang.
RESPONSE: Bonding interaction between cation and anion
Bonding interaction between cation and anion
PROBLEM: Short Inter HL..A Contact F5 .. N1 .. 2.50 Ang.
RESPONSE: Bonding interaction between cation and anion
Bonding interaction between cation and anion
PROBLEM: Short Inter HL..A Contact F6 .. N1 .. 2.50 Ang.
RESPONSE: Bonding interaction between cation and anion
Bonding interaction between cation and anion
|
PLAT431_ALERT_2_C Short Inter HL..A Contact F6 .. O1 .. 2.76 Ang.
| Author Response: Bonding interaction between cation and anion
PROBLEM: Short Inter HL..A Contact F2 .. N1 .. 2.50 Ang.
RESPONSE: Bonding interaction between cation and anion
Bonding interaction between cation and anion
PROBLEM: Short Inter HL..A Contact F5 .. N1 .. 2.50 Ang.
RESPONSE: Bonding interaction between cation and anion
Bonding interaction between cation and anion
PROBLEM: Short Inter HL..A Contact F6 .. N1 .. 2.50 Ang.
RESPONSE: Bonding interaction between cation and anion
Bonding interaction between cation and anion
|
PLAT790_ALERT_4_C Centre of Gravity not Within Unit Cell: Resd. # 2
N O2
4 ALERT level A = In general: serious problem
4 ALERT level B = Potentially serious problem
12 ALERT level C = Check and explain
0 ALERT level G = General alerts; check
2 ALERT type 1 CIF construction/syntax error, inconsistent or missing data
17 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
0 ALERT type 5 Informative message, check
Data collection: XPOSE (STOE, 2003); cell refinement: CELL (STOE, 2003); data reduction: X-RED32 (STOE, 2003); program(s) used to solve structure: SHELXS97 (Sheldrick, 1997); program(s) used to refine structure: SHELXL97 (Sheldrick, 1997); molecular graphics: DIAMOND (Crystal Impact, 2006); software used to prepare material for publication: SHELXL97.
Nitronium Tetrafluoroborate
top
Crystal data top
[NO2][BF4] | F(000) = 64 |
Mr = 132.82 | Dx = 2.232 Mg m−3 |
Monoclinic, P21/c | Mo Kα radiation, λ = 0.71073 Å |
Hall symbol: -P 2ybc | Cell parameters from 2652 reflections |
a = 6.5567 (13) Å | θ = 1.5–26.0° |
b = 6.8243 (14) Å | µ = 0.30 mm−1 |
c = 9.1244 (18) Å | T = 100 K |
β = 104.40 (3)° | Block, colourless |
V = 395.44 (14) Å3 | 0.4 × 0.2 × 0.2 mm |
Z = 4 | |
Data collection top
STOE IPDS-II diffractometer | 662 reflections with I > 2σ(I) |
Radiation source: fine-focus sealed tube | Rint = 0.027 |
Graphite monochromator | θmax = 26.0°, θmin = 3.2° |
φ scans | h = −8→8 |
2652 measured reflections | k = −8→8 |
768 independent reflections | l = −11→11 |
Refinement top
Refinement on F2 | 0 restraints |
Least-squares matrix: full | Primary atom site location: structure-invariant direct methods |
R[F2 > 2σ(F2)] = 0.019 | Secondary atom site location: difference Fourier map |
wR(F2) = 0.061 | w = 1/[σ2(Fo2) + (0.0289P)2 + 0.0515P] where P = (Fo2 + 2Fc2)/3 |
S = 1.16 | (Δ/σ)max = 0.019 |
768 reflections | Δρmax = 0.13 e Å−3 |
73 parameters | Δρmin = −0.12 e Å−3 |
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 | x | y | z | Uiso*/Ueq | |
F1 | 0.91795 (6) | 0.18853 (6) | 0.03448 (4) | 0.02119 (10) | |
F2 | 0.56288 (6) | 0.20088 (6) | −0.05137 (4) | 0.02109 (10) | |
F5 | 0.73340 (6) | 0.42075 (6) | 0.12365 (5) | 0.02709 (11) | |
F6 | 0.76422 (6) | 0.43746 (6) | −0.11913 (5) | 0.02784 (11) | |
B1 | 0.74477 (10) | 0.31239 (11) | −0.00318 (7) | 0.01633 (17) | |
O2 | 0.14914 (7) | 0.19493 (7) | −0.18388 (5) | 0.02076 (12) | |
O1 | 0.33678 (7) | 0.32845 (7) | −0.33137 (5) | 0.02034 (12) | |
N1 | 0.24313 (8) | 0.26166 (8) | −0.25757 (5) | 0.01675 (14) | |
Atomic displacement parameters (Å2) top | U11 | U22 | U33 | U12 | U13 | U23 |
F1 | 0.01870 (18) | 0.0205 (2) | 0.02336 (19) | 0.00454 (14) | 0.00321 (16) | −0.00039 (16) |
F2 | 0.01816 (18) | 0.0210 (2) | 0.02302 (19) | −0.00364 (15) | 0.00311 (16) | −0.00071 (15) |
F5 | 0.0292 (2) | 0.0249 (2) | 0.0259 (2) | 0.00382 (17) | 0.00454 (18) | −0.00991 (17) |
F6 | 0.0297 (2) | 0.0236 (2) | 0.0296 (2) | −0.00244 (16) | 0.00612 (18) | 0.01012 (17) |
B1 | 0.0160 (3) | 0.0152 (4) | 0.0174 (4) | 0.0001 (3) | 0.0034 (3) | −0.0003 (3) |
O2 | 0.0197 (2) | 0.0253 (3) | 0.0183 (2) | −0.00407 (19) | 0.00657 (18) | −0.00158 (19) |
O1 | 0.0203 (2) | 0.0231 (2) | 0.0186 (2) | −0.00378 (18) | 0.00684 (18) | −0.00141 (19) |
N1 | 0.0163 (3) | 0.0168 (3) | 0.0157 (3) | 0.0001 (2) | 0.0013 (2) | −0.0048 (2) |
Geometric parameters (Å, º) top
F1—B1 | 1.3885 (8) | F6—B1 | 1.3896 (9) |
F2—B1 | 1.3907 (8) | O2—N1 | 1.1160 (7) |
F5—B1 | 1.3908 (9) | O1—N1 | 1.1153 (8) |
| | | |
F1—B1—F6 | 109.76 (6) | F6—B1—F5 | 109.93 (6) |
F1—B1—F2 | 109.23 (6) | F2—B1—F5 | 109.56 (6) |
F6—B1—F2 | 109.22 (5) | O1—N1—O2 | 179.89 (7) |
F1—B1—F5 | 109.12 (5) | | |
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