An unusual phase transition
P4/
mnc →
has been detected after cooling the (NH
4)
3TiF
7 compound. Some TiF
6 octahedra, which are disordered in the room-temperature tetragonal structure, become ordered in the low-temperature cubic phase due to the disappearance of the fourfold axis. Other TiF
6 octahedra undergo large rotations resulting in huge displacements of the F atoms by 1.5–1.8 Å that implies a reconstructive phase transition. It was supposed that phases
P4/
mbm and
could be a high-temperature phase and a parent phase, respectively, in (NH
4)
3TiF
7. Therefore, the sequence of phase transitions can be written as
→
P4/
mbm →
P4/
mnc →
. The interrelation between (NH
4)
3TiF
7, (NH
4)
3GeF
7 and (NH
4)
3PbF
7 is found, which allows us to suppose phase transitions in relative compounds.
Supporting information
CCDC references: 1025663; 1025664
Crystal data, data collection and structure refinement details are summarized
in Table 1.
S2. Results and discussion
top
Data collection: APEX2 (Bruker, 2008) for (I). Cell refinement: APEX2 (Bruker, 2008) for (I). Data reduction: SAINT (Bruker, 2008) for (I). Program(s) used to solve structure: SHELXS97 (Sheldrick, 2008) for (I). Program(s) used to refine structure: SHELXL97 (Sheldrick, 2008) for (I). Molecular graphics: DIAMOND (Brandenburg, 2005) for (I). Software used to prepare material for publication: publCIF (Westrip, 2010) for (I).
(I) Ammonium heptafluorotitanate
top
Crystal data top
F6Ti·F·3(H4N) | Dx = 1.870 Mg m−3 |
Mr = 235.03 | Mo Kα radiation, λ = 0.71073 Å |
Tetragonal, P4/mnc | Cell parameters from 1741 reflections |
Hall symbol: -P 4 2n | θ = 3.4–25.0° |
a = 11.9597 (19) Å | µ = 1.10 mm−1 |
c = 11.6747 (19) Å | T = 296 K |
V = 1669.9 (5) Å3 | Bulk, colourless |
Z = 8 | 0.3 × 0.2 × 0.2 mm |
F(000) = 944 | |
Data collection top
Bruker APEX-II CCD diffractometer | 959 independent reflections |
Radiation source: fine-focus sealed tube | 483 reflections with I > 2σ(I) |
Graphite monochromator | Rint = 0.075 |
ϕ and ω scans | θmax = 26.9°, θmin = 2.4° |
Absorption correction: multi-scan SADABS2004/1. Bruker AXS Inc., Madison, Wisconsin, USA, 2004 | h = −15→15 |
Tmin = 0.611, Tmax = 0.746 | k = −15→15 |
13112 measured reflections | l = −14→14 |
Refinement top
Refinement on F2 | Secondary atom site location: difference Fourier map |
Least-squares matrix: full | Hydrogen site location: difference Fourier map |
R[F2 > 2σ(F2)] = 0.048 | Only H-atom coordinates refined |
wR(F2) = 0.152 | w = 1/[σ2(Fo2) + (0.0536P)2 + 3.8962P] where P = (Fo2 + 2Fc2)/3 |
S = 1.07 | (Δ/σ)max = 0.004 |
959 reflections | Δρmax = 0.52 e Å−3 |
100 parameters | Δρmin = −0.40 e Å−3 |
7 restraints | Extinction correction: SHELXL, Fc*=kFc[1+0.001xFc2λ3/sin(2θ)]-1/4 |
Primary atom site location: structure-invariant direct methods | Extinction coefficient: 0.0028 (7) |
Crystal data top
F6Ti·F·3(H4N) | Z = 8 |
Mr = 235.03 | Mo Kα radiation |
Tetragonal, P4/mnc | µ = 1.10 mm−1 |
a = 11.9597 (19) Å | T = 296 K |
c = 11.6747 (19) Å | 0.3 × 0.2 × 0.2 mm |
V = 1669.9 (5) Å3 | |
Data collection top
Bruker APEX-II CCD diffractometer | 959 independent reflections |
Absorption correction: multi-scan SADABS2004/1. Bruker AXS Inc., Madison, Wisconsin, USA, 2004 | 483 reflections with I > 2σ(I) |
Tmin = 0.611, Tmax = 0.746 | Rint = 0.075 |
13112 measured reflections | |
Refinement top
R[F2 > 2σ(F2)] = 0.048 | 7 restraints |
wR(F2) = 0.152 | Only H-atom coordinates refined |
S = 1.07 | Δρmax = 0.52 e Å−3 |
959 reflections | Δρmin = −0.40 e Å−3 |
100 parameters | |
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 | Occ. (<1) |
Ti1 | 0.0000 | 0.0000 | 0.0000 | 0.0272 (6) | |
Ti2 | 0.5000 | 0.0000 | 0.0000 | 0.0286 (5) | |
Ti3 | 0.0000 | 0.0000 | 0.5000 | 0.0289 (6) | |
N1 | 0.2850 (7) | 0.2606 (6) | 0.0000 | 0.072 (2) | |
N2 | 0.0121 (6) | 0.2468 (5) | 0.2206 (5) | 0.0702 (16) | |
F1 | 0.1326 (3) | 0.0788 (4) | 0.0000 | 0.0669 (14) | |
F2 | 0.6365 (4) | 0.0726 (4) | 0.0000 | 0.0755 (15) | |
F3 | 0.0000 | 0.0000 | 0.1578 (4) | 0.0620 (18) | |
F4 | 0.4467 (3) | 0.0950 (3) | 0.1117 (3) | 0.0796 (12) | |
F5 | −0.031 (5) | 0.116 (3) | 0.407 (3) | 0.068 (10) | 0.25 |
F6 | 0.014 (4) | 0.1430 (17) | 0.433 (2) | 0.051 (5) | 0.25 |
F7 | 0.061 (4) | 0.095 (5) | 0.396 (3) | 0.076 (7) | 0.25 |
F8 | 0.2399 (3) | 0.2601 (3) | 0.2500 | 0.0751 (15) | |
H21 | 0.003 (6) | 0.196 (4) | 0.264 (4) | 0.090* | |
H22 | −0.023 (5) | 0.289 (4) | 0.259 (5) | 0.090* | |
H23 | −0.010 (5) | 0.210 (5) | 0.168 (4) | 0.090* | |
H24 | 0.075 (2) | 0.268 (5) | 0.226 (6) | 0.090* | |
H11 | 0.240 (4) | 0.250 (5) | 0.049 (4) | 0.090* | |
H13 | 0.313 (7) | 0.321 (3) | 0.0000 | 0.090* | |
H14 | 0.324 (6) | 0.206 (5) | 0.0000 | 0.090* | |
Atomic displacement parameters (Å2) top | U11 | U22 | U33 | U12 | U13 | U23 |
Ti1 | 0.0255 (7) | 0.0255 (7) | 0.0305 (11) | 0.000 | 0.000 | 0.000 |
Ti2 | 0.0292 (9) | 0.0278 (9) | 0.0289 (8) | −0.0014 (7) | 0.000 | 0.000 |
Ti3 | 0.0304 (8) | 0.0304 (8) | 0.0259 (11) | 0.000 | 0.000 | 0.000 |
N1 | 0.040 (4) | 0.042 (4) | 0.133 (8) | −0.008 (3) | 0.000 | 0.000 |
N2 | 0.108 (5) | 0.052 (3) | 0.051 (3) | 0.001 (3) | 0.001 (4) | −0.008 (2) |
F1 | 0.048 (3) | 0.063 (3) | 0.090 (3) | −0.025 (2) | 0.000 | 0.000 |
F2 | 0.050 (3) | 0.090 (4) | 0.086 (3) | −0.031 (2) | 0.000 | 0.000 |
F3 | 0.076 (3) | 0.076 (3) | 0.033 (3) | 0.000 | 0.000 | 0.000 |
F4 | 0.094 (3) | 0.075 (2) | 0.069 (2) | 0.0024 (19) | 0.0164 (19) | −0.032 (2) |
F5 | 0.08 (3) | 0.06 (2) | 0.060 (17) | −0.001 (16) | 0.018 (15) | 0.038 (16) |
F6 | 0.049 (15) | 0.021 (7) | 0.083 (13) | −0.002 (11) | 0.001 (12) | 0.015 (7) |
F7 | 0.069 (18) | 0.09 (2) | 0.069 (14) | −0.039 (13) | −0.022 (13) | 0.052 (14) |
F8 | 0.076 (2) | 0.076 (2) | 0.074 (3) | 0.006 (2) | 0.0041 (18) | 0.0041 (18) |
Geometric parameters (Å, º) top
Ti1—F3i | 1.842 (5) | Ti3—F5ix | 1.80 (2) |
Ti1—F3 | 1.842 (5) | Ti3—F5x | 1.80 (2) |
Ti1—F1i | 1.845 (4) | Ti3—F5xi | 1.80 (2) |
Ti1—F1ii | 1.845 (4) | Ti3—F5xii | 1.80 (2) |
Ti1—F1iii | 1.845 (4) | Ti3—F7viii | 1.819 (16) |
Ti1—F1 | 1.845 (4) | Ti3—F7ix | 1.819 (16) |
Ti2—F4iv | 1.843 (3) | Ti3—F7vii | 1.819 (16) |
Ti2—F4v | 1.843 (3) | Ti3—F7iii | 1.819 (16) |
Ti2—F4vi | 1.843 (3) | F5—F6 | 0.70 (5) |
Ti2—F4 | 1.843 (3) | F5—F7iii | 1.02 (2) |
Ti2—F2iv | 1.850 (4) | F5—F7 | 1.13 (4) |
Ti2—F2 | 1.850 (4) | F6—F7 | 0.91 (8) |
Ti3—F5 | 1.80 (2) | F6—F6viii | 1.57 (6) |
Ti3—F5vii | 1.80 (2) | F6—F7iii | 1.69 (4) |
Ti3—F5iii | 1.80 (2) | F7—F5xi | 1.02 (2) |
Ti3—F5viii | 1.80 (2) | F7—F6xi | 1.69 (4) |
| | | |
F3i—Ti1—F3 | 180.0 | F5iii—Ti3—F7viii | 147.2 (8) |
F3i—Ti1—F1i | 90.0 | F5viii—Ti3—F7viii | 36.4 (12) |
F3—Ti1—F1i | 90.0 | F5ix—Ti3—F7viii | 143.6 (12) |
F3i—Ti1—F1ii | 90.0 | F5x—Ti3—F7viii | 91.7 (11) |
F3—Ti1—F1ii | 90.0 | F5xi—Ti3—F7viii | 88.3 (11) |
F1i—Ti1—F1ii | 90.0 | F5xii—Ti3—F7viii | 89.7 (10) |
F3i—Ti1—F1iii | 90.0 | F5—Ti3—F7ix | 89.7 (10) |
F3—Ti1—F1iii | 90.0 | F5vii—Ti3—F7ix | 147.2 (8) |
F1i—Ti1—F1iii | 90.0 | F5iii—Ti3—F7ix | 32.8 (8) |
F1ii—Ti1—F1iii | 180.0 (2) | F5viii—Ti3—F7ix | 143.6 (12) |
F3i—Ti1—F1 | 90.0 | F5ix—Ti3—F7ix | 36.4 (12) |
F3—Ti1—F1 | 90.0 | F5x—Ti3—F7ix | 88.3 (11) |
F1i—Ti1—F1 | 180.0 | F5xi—Ti3—F7ix | 91.7 (11) |
F1ii—Ti1—F1 | 90.0 | F5xii—Ti3—F7ix | 90.3 (10) |
F1iii—Ti1—F1 | 90.0 | F7viii—Ti3—F7ix | 180.000 (2) |
F4iv—Ti2—F4v | 90.0 (2) | F5—Ti3—F7vii | 147.2 (8) |
F4iv—Ti2—F4vi | 90.0 (2) | F5vii—Ti3—F7vii | 36.4 (12) |
F4v—Ti2—F4vi | 180.0 (3) | F5iii—Ti3—F7vii | 143.6 (12) |
F4iv—Ti2—F4 | 180.0 | F5viii—Ti3—F7vii | 91.7 (11) |
F4v—Ti2—F4 | 90.0 (2) | F5ix—Ti3—F7vii | 88.3 (11) |
F4vi—Ti2—F4 | 90.0 (2) | F5x—Ti3—F7vii | 89.7 (10) |
F4iv—Ti2—F2iv | 90.91 (15) | F5xi—Ti3—F7vii | 90.3 (10) |
F4v—Ti2—F2iv | 89.09 (15) | F5xii—Ti3—F7vii | 32.8 (8) |
F4vi—Ti2—F2iv | 90.91 (15) | F7viii—Ti3—F7vii | 63.3 (16) |
F4—Ti2—F2iv | 89.10 (15) | F7ix—Ti3—F7vii | 116.7 (16) |
F4iv—Ti2—F2 | 89.09 (15) | F5—Ti3—F7iii | 32.8 (8) |
F4v—Ti2—F2 | 90.91 (15) | F5vii—Ti3—F7iii | 143.6 (12) |
F4vi—Ti2—F2 | 89.09 (15) | F5iii—Ti3—F7iii | 36.4 (12) |
F4—Ti2—F2 | 90.90 (15) | F5viii—Ti3—F7iii | 88.3 (11) |
F2iv—Ti2—F2 | 180.0 | F5ix—Ti3—F7iii | 91.7 (11) |
F5—Ti3—F5vii | 111.5 (14) | F5x—Ti3—F7iii | 90.3 (10) |
F5—Ti3—F5iii | 68.5 (14) | F5xi—Ti3—F7iii | 89.7 (10) |
F5vii—Ti3—F5iii | 180.000 (3) | F5xii—Ti3—F7iii | 147.2 (8) |
F5—Ti3—F5viii | 74 (3) | F7viii—Ti3—F7iii | 116.7 (16) |
F5vii—Ti3—F5viii | 68.5 (14) | F7ix—Ti3—F7iii | 63.3 (16) |
F5iii—Ti3—F5viii | 111.5 (14) | F7vii—Ti3—F7iii | 180.0 (18) |
F5—Ti3—F5ix | 106 (3) | F6—F5—F7iii | 159 (6) |
F5vii—Ti3—F5ix | 111.5 (14) | F6—F5—F7 | 54 (6) |
F5iii—Ti3—F5ix | 68.5 (14) | F7iii—F5—F7 | 125 (6) |
F5viii—Ti3—F5ix | 180.000 (3) | F6—F5—Ti3 | 86 (4) |
F5—Ti3—F5x | 111.5 (14) | F7iii—F5—Ti3 | 74.4 (17) |
F5vii—Ti3—F5x | 106 (3) | F7—F5—Ti3 | 72.5 (15) |
F5iii—Ti3—F5x | 74 (3) | F5—F6—F7 | 89 (5) |
F5viii—Ti3—F5x | 68.5 (14) | F5—F6—F6viii | 116 (4) |
F5ix—Ti3—F5x | 111.5 (14) | F7—F6—F6viii | 118 (2) |
F5—Ti3—F5xi | 68.5 (14) | F7—F6—F7iii | 89 (3) |
F5vii—Ti3—F5xi | 74 (3) | F6viii—F6—F7iii | 105 (2) |
F5iii—Ti3—F5xi | 106 (3) | F5—F6—Ti3 | 72 (3) |
F5viii—Ti3—F5xi | 111.5 (14) | F7—F6—Ti3 | 71.4 (19) |
F5ix—Ti3—F5xi | 68.5 (14) | F6viii—F6—Ti3 | 65.4 (8) |
F5x—Ti3—F5xi | 180.000 (2) | F7iii—F6—Ti3 | 60.7 (11) |
F5—Ti3—F5xii | 180.000 (5) | F6—F7—F5xi | 144 (5) |
F5vii—Ti3—F5xii | 68.5 (14) | F5xi—F7—F5 | 141 (3) |
F5iii—Ti3—F5xii | 111.5 (14) | F6—F7—F6xi | 136 (4) |
F5viii—Ti3—F5xii | 106 (3) | F5—F7—F6xi | 135.0 (18) |
F5ix—Ti3—F5xii | 74 (3) | F6—F7—Ti3 | 80 (2) |
F5x—Ti3—F5xii | 68.5 (14) | F5xi—F7—Ti3 | 72.8 (16) |
F5xi—Ti3—F5xii | 111.5 (14) | F5—F7—Ti3 | 71.1 (16) |
F5—Ti3—F7viii | 90.3 (10) | F6xi—F7—Ti3 | 65.1 (13) |
F5vii—Ti3—F7viii | 32.8 (8) | | |
Symmetry codes: (i) −x, −y, −z; (ii) y, −x, −z; (iii) −y, x, z; (iv) −x+1, −y, −z; (v) x, y, −z; (vi) −x+1, −y, z; (vii) y, −x, −z+1; (viii) x, y, −z+1; (ix) −x, −y, z; (x) −y, x, −z+1; (xi) y, −x, z; (xii) −x, −y, −z+1. |
Hydrogen-bond geometry (Å, º) top
D—H···A | D—H | H···A | D···A | D—H···A |
N1—H11···F1 | 0.80 (5) | 2.48 (6) | 2.837 (9) | 108 (5) |
N1—H11···F8 | 0.80 (5) | 2.35 (5) | 2.968 (2) | 135 (4) |
N1—H11···F2xiii | 0.80 (5) | 2.49 (5) | 2.823 (9) | 107 (4) |
N1—H11···F2xiv | 0.80 (5) | 2.49 (5) | 2.823 (9) | 107 (4) |
N1—H14···F4 | 0.80 (5) | 2.37 (6) | 3.060 (8) | 145 (2) |
N1—H14···F4v | 0.80 (5) | 2.37 (6) | 3.060 (8) | 145 (2) |
N2—H22···F4xv | 0.80 (6) | 2.08 (5) | 2.833 (7) | 158 (6) |
N2—H23···F1iii | 0.80 (5) | 2.32 (5) | 3.111 (6) | 170 (6) |
N2—H24···F8 | 0.80 (3) | 1.99 (3) | 2.751 (8) | 159 (6) |
Symmetry codes: (iii) −y, x, z; (v) x, y, −z; (xiii) y, −x+1, z; (xiv) y, −x+1, −z; (xv) x−1/2, −y+1/2, −z+1/2. |
Crystal data top
F6Ti·F·3(H4N) | Z = 8 |
Mr = 235.00 | Dx = 1.908 Mg m−3 |
Cubic, Pa3 | Cu Kα12 radiation, λ = 1.5406, 1.5443 Å |
Hall symbol: -P 2ac 2ab 3 | T = 143 K |
a = 11.78316 (15) Å | colourless |
V = 1636.01 (6) Å3 | ?, ? × ? × ? mm |
Data collection top
D8 ADVANCE Bruker diffractometer | Data collection mode: reflection |
None monochromator | Scan method: step |
Specimen mounting: flat, densely packed | 2θmin = 11.013°, 2θmax = 139.987°, 2θstep = 0.016° |
Refinement top
Rp = 3.926 | Profile function: PearsonVII |
Rwp = 4.850 | 61 parameters |
Rexp = 2.213 | 9 restraints |
RBragg = 1.79 | (Δ/σ)max = 0.010 |
χ2 = 4.800 | Preferred orientation correction: no preferred orientation |
8060.88125 data points | |
Crystal data top
F6Ti·F·3(H4N) | Z = 8 |
Mr = 235.00 | Cu Kα12 radiation, λ = 1.5406, 1.5443 Å |
Cubic, Pa3 | T = 143 K |
a = 11.78316 (15) Å | ?, ? × ? × ? mm |
V = 1636.01 (6) Å3 | |
Data collection top
D8 ADVANCE Bruker diffractometer | Scan method: step |
Specimen mounting: flat, densely packed | 2θmin = 11.013°, 2θmax = 139.987°, 2θstep = 0.016° |
Data collection mode: reflection | |
Refinement top
Rp = 3.926 | χ2 = 4.800 |
Rwp = 4.850 | 8060.88125 data points |
Rexp = 2.213 | 61 parameters |
RBragg = 1.79 | 9 restraints |
Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top | x | y | z | Biso*/Beq | |
Ti1 | 0 | 0 | 0 | 0 | |
Ti2 | 0.5 | 0 | 0 | 0 | |
F1 | 0.15394 (17) | −0.0155 (2) | 0.0142 (3) | 0 | |
F2 | 0.3899 (2) | 0.0958 (3) | 0.05309 (17) | 0 | |
F3 | 0.2569 (3) | 0.2569 (3) | 0.2569 (3) | 0 | |
N | 0.2406 (4) | 0.2352 (3) | 0.4821 (3) | 0 | |
H1 | 0.263145 | 0.164540 | 0.500386 | 4* | |
H2 | 0.236375 | 0.241701 | 0.406118 | 4* | |
H3 | 0.171917 | 0.248703 | 0.512671 | 4* | |
H4 | 0.290951 | 0.285805 | 0.509237 | 4* | |
Atomic displacement parameters (Å2) top | U11 | U22 | U33 | U12 | U13 | U23 |
Ti1 | 0.0210 (17) | 0.0210 (17) | 0.0210 (17) | −0.0010 (11) | −0.0010 (11) | −0.0010 (11) |
Ti2 | 0.0143 (17) | 0.0143 (17) | 0.0143 (17) | −0.0042 (10) | −0.0042 (10) | −0.0042 (10) |
F1 | 0.035 (2) | 0.034 (4) | 0.053 (4) | 0.0183 (19) | −0.009 (2) | −0.0085 (19) |
F2 | 0.031 (3) | 0.013 (3) | 0.027 (2) | 0.0031 (14) | −0.0034 (18) | 0.0033 (18) |
F3 | 0.0390 (18) | 0.0390 (18) | 0.0390 (18) | 0.012 (3) | 0.012 (3) | 0.012 (3) |
N | 0.028 (9) | 0.029 (10) | 0.054 (4) | −0.006 (3) | −0.020 (4) | −0.010 (4) |
Bond lengths (Å) top
Ti1—F1 | 1.831 (3) | N—H2 | 0.9000 |
Ti2—F2 | 1.830 (3) | N—H3 | 0.9000 |
N—H1 | 0.9000 | N—H4 | 0.9000 |
Experimental details
| (I) | (II) |
Crystal data |
Chemical formula | F6Ti·F·3(H4N) | F6Ti·F·3(H4N) |
Mr | 235.03 | 235.00 |
Crystal system, space group | Tetragonal, P4/mnc | Cubic, Pa3 |
Temperature (K) | 296 | 143 |
a, b, c (Å) | 11.9597 (19), 11.9597 (19), 11.6747 (19) | 11.78316 (15), 11.78316 (15), 11.78316 (15) |
α, β, γ (°) | 90, 90, 90 | 90, 90, 90 |
V (Å3) | 1669.9 (5) | 1636.01 (6) |
Z | 8 | 8 |
Radiation type | Mo Kα | Cu Kα12, λ = 1.5406, 1.5443 Å |
µ (mm−1) | 1.10 | – |
Specimen shape, size (mm) | 0.3 × 0.2 × 0.2 | ?, ? × ? × ? |
|
Data collection |
Diffractometer | Bruker APEX-II CCD diffractometer | D8 ADVANCE Bruker diffractometer |
Specimen mounting | – | Flat, densely packed |
Data collection mode | – | Reflection |
Data collection method | ϕ and ω scans | Step |
Absorption correction | Multi-scan SADABS2004/1. Bruker AXS Inc., Madison, Wisconsin, USA, 2004 | – |
Tmin, Tmax | 0.611, 0.746 | – |
No. of measured, independent and observed [I > 2σ(I)] reflections | 13112, 959, 483 | – |
Rint | 0.075 | – |
θ values (°) | θmax = 26.9, θmin = 2.4 | 2θmin = 11.013 2θmax = 139.987 2θstep = 0.016 |
(sin θ/λ)max (Å−1) | 0.637 | – |
|
Refinement |
R factors and goodness of fit | R[F2 > 2σ(F2)] = 0.048, wR(F2) = 0.152, S = 1.07 | Rp = 3.926, Rwp = 4.850, Rexp = 2.213, RBragg = 1.79, χ2 = 4.800 |
No. of reflections/data points | 959 | 8060.88125 |
No. of parameters | 100 | 61 |
No. of restraints | 7 | 9 |
H-atom treatment | Only H-atom coordinates refined | ? |
Δρmax, Δρmin (e Å−3) | 0.52, −0.40 | – |
Hydrogen-bond geometry (Å, º) for (I) top
D—H···A | D—H | H···A | D···A | D—H···A |
N1—H11···F1 | 0.80 (5) | 2.48 (6) | 2.837 (9) | 108 (5) |
N1—H11···F8 | 0.80 (5) | 2.35 (5) | 2.968 (2) | 135 (4) |
N1—H11···F2i | 0.80 (5) | 2.49 (5) | 2.823 (9) | 107 (4) |
N1—H11···F2ii | 0.80 (5) | 2.49 (5) | 2.823 (9) | 107 (4) |
N1—H14···F4 | 0.80 (5) | 2.37 (6) | 3.060 (8) | 145 (2) |
N1—H14···F4iii | 0.80 (5) | 2.37 (6) | 3.060 (8) | 145 (2) |
N2—H22···F4iv | 0.80 (6) | 2.08 (5) | 2.833 (7) | 158 (6) |
N2—H23···F1v | 0.80 (5) | 2.32 (5) | 3.111 (6) | 170 (6) |
N2—H24···F8 | 0.80 (3) | 1.99 (3) | 2.751 (8) | 159 (6) |
Symmetry codes: (i) y, −x+1, z; (ii) y, −x+1, −z; (iii) x, y, −z; (iv) x−1/2, −y+1/2, −z+1/2; (v) −y, x, z. |