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The single-crystal X-ray study of hydrazinium tetra­fluoro­borate, N2H5+·BF4, confirms the previous structure determinations in the space group C2/c [Conant, Corrigan & Sparks (1964). Acta Cryst. 17, 1085; Conant & Roof (1970). Acta Cryst. B26, 1928–1932]. The present study includes the determination of the H-atom parameters, which reveal an extensively hydrogen-bonded structure, as expected. Several inter­ionic hydrogen bonds are found, involving short N...F distances [2.929 (3)–2.989 (3) Å] and a short N...N distance [2.916 (3) Å].

Supporting information

cif

Crystallographic Information File (CIF) https://doi.org/10.1107/S1600536806045922/sg2079sup1.cif
Contains datablocks I, global

hkl

Structure factor file (CIF format) https://doi.org/10.1107/S1600536806045922/sg2079Isup2.hkl
Contains datablock I

Key indicators

  • Single-crystal X-ray study
  • T = 200 K
  • Mean [sigma](F-B) = 0.003 Å
  • R factor = 0.050
  • wR factor = 0.121
  • Data-to-parameter ratio = 11.3

checkCIF/PLATON results

No syntax errors found



Alert level B CHEMS01_ALERT_1_B The sum formula contains elements in the wrong order. H precedes B Sequence must be C, H, then alphabetical. PLAT242_ALERT_2_B Check Low Ueq as Compared to Neighbors for B
Alert level C PLAT041_ALERT_1_C Calc. and Rep. SumFormula Strings Differ .... ? PLAT042_ALERT_1_C Calc. and Rep. MoietyFormula Strings Differ .... ? PLAT125_ALERT_4_C No _symmetry_space_group_name_Hall Given ....... ? PLAT480_ALERT_4_C Long H...A H-Bond Reported H2 .. F1 .. 2.56 Ang. PLAT480_ALERT_4_C Long H...A H-Bond Reported H4 .. F4 .. 2.63 Ang. PLAT790_ALERT_4_C Centre of Gravity not Within Unit Cell: Resd. # 1 H5 N2
0 ALERT level A = In general: serious problem 2 ALERT level B = Potentially serious problem 6 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 1 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 4 ALERT type 4 Improvement, methodology, query or suggestion 0 ALERT type 5 Informative message, check

Computing details top

Data collection: COLLECT (Nonius, 1999); cell refinement: SCALEPACK (Otwinowski & Minor, 1997); data reduction: SCALEPACK and DENZO (Otwinowski & Minor, 1997); program(s) used to solve structure: SHELXS97 (Sheldrick, 1997); program(s) used to refine structure: SHELXL97 (Sheldrick, 1997); molecular graphics: ORTEP-3 (Farrugia, 1997); software used to prepare material for publication: SHELXL97.

hydrazinium tetrafluoroborate top
Crystal data top
N2H5+·BF4F(000) = 480
Mr = 119.87Dx = 1.914 Mg m3
Monoclinic, C2/cMo Kα radiation, λ = 0.71073 Å
a = 13.8644 (5) ÅCell parameters from 2082 reflections
b = 5.3233 (2) Åθ = 3.1–27.5°
c = 12.2334 (4) ŵ = 0.25 mm1
β = 112.8848 (16)°T = 200 K
V = 831.81 (5) Å3Square prism, colourless
Z = 80.24 × 0.08 × 0.04 mm
Data collection top
Nonius KappaCCD area-detector
diffractometer
752 reflections with I > 2σ(I)
Radiation source: fine-focus sealed tubeRint = 0.019
Graphite monochromatorθmax = 27.5°, θmin = 3.2°
Detector resolution: 9 pixels mm-1h = 1817
φ and ω scansk = 66
1779 measured reflectionsl = 1515
953 independent reflections
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)] = 0.050Hydrogen site location: inferred from neighbouring sites
wR(F2) = 0.121All H-atom parameters refined
S = 1.07 w = 1/[σ2(Fo2) + (0.0411P)2 + 1.8993P]
where P = (Fo2 + 2Fc2)/3
953 reflections(Δ/σ)max < 0.001
84 parametersΔρmax = 0.45 e Å3
0 restraintsΔρmin = 0.39 e Å3
Special details top

Experimental. The following faces (with distances from a common point in mm) were indexed: 1 0 0, 0.03; 1 0 0, 0.02; 0 1 0, 0.04; 0 1 0, 0.04; 0 0 1, 0.12; 0 0 1, 0.10.

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
B0.10960 (18)0.0706 (4)0.9215 (2)0.0257 (5)
F10.06696 (13)0.3029 (3)0.92718 (15)0.0548 (5)
F20.19255 (14)0.0268 (4)1.02518 (16)0.0796 (8)
F30.14208 (13)0.0761 (3)0.82854 (14)0.0495 (5)
F40.03750 (13)0.1189 (3)0.90527 (14)0.0551 (5)
N10.15635 (14)0.5875 (3)1.22935 (16)0.0273 (4)
H10.100 (2)0.685 (6)1.190 (3)0.049 (8)*
H20.138 (2)0.511 (5)1.285 (3)0.042 (7)*
N20.15703 (15)0.3931 (4)1.14727 (16)0.0286 (4)
H30.213 (2)0.284 (6)1.185 (3)0.051 (8)*
H40.097 (2)0.311 (6)1.119 (2)0.042 (7)*
H50.174 (3)0.470 (7)1.085 (3)0.068 (10)*
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
B0.0234 (10)0.0263 (11)0.0257 (11)0.0028 (9)0.0075 (8)0.0004 (9)
F10.0585 (10)0.0439 (9)0.0718 (11)0.0126 (7)0.0361 (9)0.0070 (8)
F20.0589 (11)0.0756 (13)0.0601 (11)0.0258 (10)0.0249 (9)0.0393 (10)
F30.0706 (10)0.0393 (8)0.0605 (10)0.0057 (7)0.0494 (9)0.0074 (7)
F40.0551 (10)0.0628 (11)0.0464 (9)0.0366 (8)0.0185 (7)0.0093 (8)
N10.0278 (9)0.0242 (9)0.0278 (9)0.0032 (7)0.0086 (7)0.0006 (7)
N20.0267 (9)0.0289 (9)0.0263 (9)0.0001 (8)0.0060 (7)0.0031 (7)
Geometric parameters (Å, º) top
B—F21.361 (3)N1—H10.91 (3)
B—F31.377 (3)N1—H20.91 (3)
B—F41.379 (3)N2—H30.93 (3)
B—F11.384 (3)N2—H40.89 (3)
N1—N21.445 (2)N2—H50.97 (4)
F2—B—F3110.1 (2)H1—N1—H2103 (2)
F2—B—F4108.12 (19)N1—N2—H3109.4 (19)
F3—B—F4110.38 (19)N1—N2—H4111.3 (18)
F2—B—F1109.2 (2)H3—N2—H4111 (3)
F3—B—F1107.84 (18)N1—N2—H5108 (2)
F4—B—F1111.16 (19)H3—N2—H5104 (3)
N2—N1—H1106.0 (19)H4—N2—H5112 (3)
N2—N1—H2106.3 (18)
Hydrogen-bond geometry (Å, º) top
D—H···AD—HH···AD···AD—H···A
N1—H1···F4i0.91 (3)2.08 (3)2.989 (2)175 (3)
N1—H2···F3ii0.91 (3)2.37 (3)3.019 (2)128 (2)
N1—H2···F1ii0.91 (3)2.56 (3)3.467 (3)174 (2)
N2—H3···N1iii0.93 (3)2.00 (3)2.929 (3)173 (3)
N2—H4···F1iv0.89 (3)2.12 (3)2.916 (3)150 (3)
N2—H4···F40.89 (3)2.63 (3)3.135 (2)118 (2)
N2—H5···F1v0.97 (4)2.27 (4)2.969 (3)128 (3)
Symmetry codes: (i) x, y1, z+2; (ii) x, y, z+1/2; (iii) x+1/2, y+1/2, z+5/2; (iv) x, y, z+2; (v) x, y1, z.
 

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