Crystals of uranium iodine phthalocyanine present an example of a disordered commensurate modulated structure of the intergrowth type. The short-range order of both uranium ions and iodine chains [I
]
n has been analysed by Reverse Monte Carlo (RMC) simulation of X-ray diffuse scattering. The diffraction pattern of uranium iodine phthalocyanine contains diffuse superstructure reflections. In the routine crystal structure analysis diffuse superstructure reflections may be either omitted or measured and classified along with other Bragg reflections. The crystal structure of uranium iodine phthalocyanine is an example of such ambiguity. The crystal structures of two specimens of [U
1-xPc
2]I
2-y with slightly different composition have been published in the literature with different space groups and unit cells. We have shown that the structure of both specimens differs only in the degree of short-range order and is isostructural with [YbPc
2]I
2. We have also shown that while the omission of diffuse reflections results in the average crystal structure, the treatment of these reflections as normal Bragg reflections is incorrect and produces the structure averaged over a limited small range.
Supporting information
CCDC references: 219248; 219249
For both compounds, data collection: CrysAlis 189; cell refinement: CrysAlis 189; data reduction: CrysAlis 189; program(s) used to solve structure: SHELXS97 (Sheldrick, 1990); program(s) used to refine structure: SHELXL97 (Sheldrick, 1997).
Crystal data top
C64H32H0I1.74N16U0.96 | F(000) = 709 |
Mr = 1474.37 | Dx = 1.916 Mg m−3 |
Tetragonal, P4/mcc | Mo Kα radiation, λ = 0.71073 Å |
a = 13.997 (2) Å | µ = 4.16 mm−1 |
c = 6.523 (1) Å | T = 293 K |
V = 1278.0 (3) Å3 | Irregular, black |
Z = 1 | 0.37 × 0.13 × 0.13 mm |
Data collection top
KM4-CCD diffractometer | 867 reflections with I > 2σ(I) |
Radiation source: fine-focus sealed tube | Rint = 0.064 |
Graphite monochromator | θmax = 29.6°, θmin = 2.9° |
Absorption correction: numerical | h = −18→19 |
Tmin = 0.438, Tmax = 0.734 | k = −19→18 |
15699 measured reflections | l = −7→8 |
980 independent reflections | |
Refinement top
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)] = 0.036 | H atoms treated by a mixture of independent and constrained refinement |
wR(F2) = 0.082 | Calculated w = 1/[σ2(Fo2) + (0.0313P)2 + 0.9211P] where P = (Fo2 + 2Fc2)/3 |
S = 1.20 | (Δ/σ)max = 2.708 |
980 reflections | Δρmax = 0.47 e Å−3 |
78 parameters | Δρmin = −0.50 e Å−3 |
0 restraints | Extinction correction: SHELXL, Fc*=kFc[1+0.001xFc2λ3/sin(2θ)]-1/4 |
Primary atom site location: structure-invariant direct methods | Extinction coefficient: 0.0000 (8) |
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) |
I1 | 0.0000 | 0.0000 | 0.2141 (3) | 0.0503 (6) | 0.436 (3) |
U | 0.5000 | 0.5000 | 0.2500 | 0.02419 (19) | 0.479 (3) |
N1 | 0.5827 (2) | 0.2731 (2) | 0.0000 | 0.0353 (8) | |
N2 | 0.4402 (2) | 0.3730 (2) | 0.0000 | 0.0487 (10) | |
C1 | 0.4891 (3) | 0.2874 (3) | 0.0000 | 0.0364 (9) | |
C2 | 0.4189 (3) | 0.2095 (3) | 0.0000 | 0.0368 (9) | |
C3 | 0.4299 (4) | 0.1109 (3) | 0.0000 | 0.0561 (12) | |
C4 | 0.3478 (4) | 0.0559 (3) | 0.0000 | 0.0734 (17) | |
C5 | 0.2571 (4) | 0.0975 (3) | 0.0000 | 0.0671 (15) | |
C6 | 0.2460 (3) | 0.1959 (3) | 0.0000 | 0.0489 (10) | |
C7 | 0.3280 (3) | 0.2510 (3) | 0.0000 | 0.0367 (8) | |
C8 | 0.3444 (3) | 0.3541 (3) | 0.0000 | 0.0355 (8) | |
H3 | 0.492 (3) | 0.083 (3) | 0.0000 | 0.043* | |
H4 | 0.354 (3) | −0.014 (3) | 0.0000 | 0.043* | |
H5 | 0.200 (3) | 0.064 (3) | 0.0000 | 0.043* | |
H6 | 0.186 (3) | 0.232 (3) | 0.0000 | 0.043* | |
Atomic displacement parameters (Å2) top | U11 | U22 | U33 | U12 | U13 | U23 |
I1 | 0.0456 (3) | 0.0456 (3) | 0.0598 (16) | 0.000 | 0.000 | 0.000 |
U | 0.0244 (2) | 0.0244 (2) | 0.0237 (3) | 0.000 | 0.000 | 0.000 |
N1 | 0.0336 (16) | 0.0335 (16) | 0.0389 (17) | 0.0033 (12) | 0.000 | 0.000 |
N2 | 0.0317 (17) | 0.0322 (17) | 0.082 (3) | 0.0007 (13) | 0.000 | 0.000 |
C1 | 0.046 (2) | 0.0321 (17) | 0.0310 (16) | −0.0005 (15) | 0.000 | 0.000 |
C2 | 0.0369 (19) | 0.038 (2) | 0.0360 (19) | −0.0030 (15) | 0.000 | 0.000 |
C3 | 0.049 (2) | 0.037 (2) | 0.082 (4) | −0.0014 (18) | 0.000 | 0.000 |
C4 | 0.066 (3) | 0.033 (2) | 0.122 (5) | −0.008 (2) | 0.000 | 0.000 |
C5 | 0.053 (3) | 0.045 (3) | 0.103 (4) | −0.017 (2) | 0.000 | 0.000 |
C6 | 0.041 (2) | 0.047 (2) | 0.059 (3) | −0.0050 (18) | 0.000 | 0.000 |
C7 | 0.042 (2) | 0.0343 (18) | 0.0333 (19) | −0.0046 (15) | 0.000 | 0.000 |
C8 | 0.0323 (18) | 0.039 (2) | 0.0353 (17) | −0.0034 (14) | 0.000 | 0.000 |
Geometric parameters (Å, º) top
I1—I1i | 0.468 (4) | U—Uxiii | 3.2615 (5) |
I1—I1ii | 2.794 (4) | U—Uxvi | 3.2615 (5) |
I1—H5ii | 3.26 (4) | N1—C1 | 1.326 (4) |
I1—H5iii | 3.26 (4) | N1—C8xv | 1.334 (5) |
I1—H5 | 3.26 (4) | N2—C8 | 1.367 (5) |
I1—H5iv | 3.26 (4) | N2—C1 | 1.380 (5) |
I1—I1v | 3.2615 (5) | N2—Uxiii | 2.553 (2) |
I1—I1vi | 3.2615 (5) | C1—C2 | 1.469 (5) |
I1—H5vii | 3.48 (4) | C2—C3 | 1.389 (6) |
I1—H5v | 3.48 (4) | C2—C7 | 1.398 (5) |
I1—H5i | 3.48 (4) | C3—H3 | 0.96 (4) |
I1—H5viii | 3.48 (4) | C3—C4 | 1.382 (7) |
I1—I1ix | 3.729 (4) | C4—H4 | 0.98 (4) |
I1—C5ii | 4.094 (5) | C4—C5 | 1.397 (7) |
I1—C5iii | 4.094 (5) | C5—H5 | 0.93 (4) |
I1—C5 | 4.094 (5) | C5—C6 | 1.387 (6) |
U—N2x | 2.553 (2) | C5—I1ii | 4.094 (5) |
U—N2 | 2.553 (2) | C6—H6 | 0.98 (4) |
U—N2xi | 2.553 (2) | C6—C7 | 1.383 (6) |
U—N2xii | 2.553 (2) | C7—C8 | 1.461 (5) |
U—N2xiii | 2.553 (2) | C8—N1xi | 1.334 (5) |
U—N2xiv | 2.553 (2) | H5—I1ii | 3.26 (4) |
U—N2vii | 2.553 (2) | H5—I1vi | 3.48 (4) |
U—N2xv | 2.553 (2) | H5—I1i | 3.48 (4) |
| | | |
I1i—I1—I1ii | 180.0 | H5ii—I1—C5 | 134.5 (3) |
I1i—I1—H5ii | 115.4 (3) | H5iii—I1—C5 | 79.0 (7) |
I1ii—I1—H5ii | 64.6 (3) | H5—I1—C5 | 6.1 (4) |
I1i—I1—H5iii | 115.4 (3) | H5iv—I1—C5 | 84.2 (7) |
I1ii—I1—H5iii | 64.6 (3) | I1v—I1—C5 | 109.95 (3) |
H5ii—I1—H5iii | 79.4 (3) | I1vi—I1—C5 | 70.05 (3) |
I1i—I1—H5 | 115.4 (3) | H5vii—I1—C5 | 71.8 (6) |
I1ii—I1—H5 | 64.6 (3) | H5v—I1—C5 | 143.5 (7) |
H5ii—I1—H5 | 129.2 (6) | H5i—I1—C5 | 64.0 (5) |
H5iii—I1—H5 | 79.4 (3) | H5viii—I1—C5 | 132.6 (7) |
I1i—I1—H5iv | 115.4 (3) | I1ix—I1—C5 | 109.95 (3) |
I1ii—I1—H5iv | 64.6 (3) | C5ii—I1—C5 | 140.11 (7) |
H5ii—I1—H5iv | 79.4 (3) | C5iii—I1—C5 | 83.32 (2) |
H5iii—I1—H5iv | 129.2 (6) | N2x—U—N2 | 149.82 (13) |
H5—I1—H5iv | 79.4 (3) | N2x—U—N2xi | 141.72 (13) |
I1i—I1—I1v | 0.0 | N2—U—N2xi | 65.92 (5) |
I1ii—I1—I1v | 180.0 | N2x—U—N2xii | 65.92 (5) |
H5ii—I1—I1v | 115.4 (3) | N2—U—N2xii | 141.72 (13) |
H5iii—I1—I1v | 115.4 (3) | N2xi—U—N2xii | 87.23 (10) |
H5—I1—I1v | 115.4 (3) | N2x—U—N2xiii | 87.23 (10) |
H5iv—I1—I1v | 115.4 (3) | N2—U—N2xiii | 100.60 (9) |
I1i—I1—I1vi | 180.0 | N2xi—U—N2xiii | 65.92 (5) |
I1ii—I1—I1vi | 0.0 | N2xii—U—N2xiii | 91.78 (11) |
H5ii—I1—I1vi | 64.6 (3) | N2x—U—N2xiv | 65.92 (5) |
H5iii—I1—I1vi | 64.6 (3) | N2—U—N2xiv | 91.78 (11) |
H5—I1—I1vi | 64.6 (3) | N2xi—U—N2xiv | 149.82 (13) |
H5iv—I1—I1vi | 64.6 (3) | N2xii—U—N2xiv | 100.60 (9) |
I1v—I1—I1vi | 180.0 | N2xiii—U—N2xiv | 141.72 (13) |
I1i—I1—H5vii | 57.6 (4) | N2x—U—N2vii | 100.60 (9) |
I1ii—I1—H5vii | 122.4 (4) | N2—U—N2vii | 87.23 (10) |
H5ii—I1—H5vii | 132.3 (14) | N2xi—U—N2vii | 91.78 (11) |
H5iii—I1—H5vii | 67.0 (10) | N2xii—U—N2vii | 65.92 (5) |
H5—I1—H5vii | 77.7 (11) | N2xiii—U—N2vii | 149.82 (13) |
H5iv—I1—H5vii | 148.3 (14) | N2xiv—U—N2vii | 65.92 (5) |
I1v—I1—H5vii | 57.6 (4) | N2x—U—N2xv | 91.78 (11) |
I1vi—I1—H5vii | 122.4 (4) | N2—U—N2xv | 65.92 (5) |
I1i—I1—H5v | 57.6 (4) | N2xi—U—N2xv | 100.60 (9) |
I1ii—I1—H5v | 122.4 (4) | N2xii—U—N2xv | 149.82 (13) |
H5ii—I1—H5v | 67.0 (10) | N2xiii—U—N2xv | 65.92 (5) |
H5iii—I1—H5v | 77.7 (11) | N2xiv—U—N2xv | 87.23 (10) |
H5—I1—H5v | 148.3 (14) | N2vii—U—N2xv | 141.72 (13) |
H5iv—I1—H5v | 132.3 (14) | N2x—U—Uxiii | 129.70 (4) |
I1v—I1—H5v | 57.6 (4) | N2—U—Uxiii | 50.30 (4) |
I1vi—I1—H5v | 122.4 (4) | N2xi—U—Uxiii | 50.30 (4) |
H5vii—I1—H5v | 73.3 (4) | N2xii—U—Uxiii | 129.70 (4) |
I1i—I1—H5i | 57.6 (4) | N2xiii—U—Uxiii | 50.30 (4) |
I1ii—I1—H5i | 122.4 (4) | N2xiv—U—Uxiii | 129.70 (4) |
H5ii—I1—H5i | 148.3 (14) | N2vii—U—Uxiii | 129.70 (4) |
H5iii—I1—H5i | 132.3 (14) | N2xv—U—Uxiii | 50.30 (4) |
H5—I1—H5i | 67.0 (10) | N2x—U—Uxvi | 50.30 (4) |
H5iv—I1—H5i | 77.7 (11) | N2—U—Uxvi | 129.70 (4) |
I1v—I1—H5i | 57.6 (4) | N2xi—U—Uxvi | 129.70 (4) |
I1vi—I1—H5i | 122.4 (4) | N2xii—U—Uxvi | 50.30 (4) |
H5vii—I1—H5i | 73.3 (4) | N2xiii—U—Uxvi | 129.70 (4) |
H5v—I1—H5i | 115.2 (7) | N2xiv—U—Uxvi | 50.30 (4) |
I1i—I1—H5viii | 57.6 (4) | N2vii—U—Uxvi | 50.30 (4) |
I1ii—I1—H5viii | 122.4 (4) | N2xv—U—Uxvi | 129.70 (4) |
H5ii—I1—H5viii | 77.7 (11) | Uxiii—U—Uxvi | 180.0 |
H5iii—I1—H5viii | 148.3 (14) | C1—N1—C8xv | 122.8 (3) |
H5—I1—H5viii | 132.3 (14) | C8—N2—C1 | 108.5 (3) |
H5iv—I1—H5viii | 67.0 (10) | C8—N2—U | 117.19 (17) |
I1v—I1—H5viii | 57.6 (4) | C1—N2—U | 116.23 (17) |
I1vi—I1—H5viii | 122.4 (4) | C8—N2—Uxiii | 117.19 (17) |
H5vii—I1—H5viii | 115.2 (7) | C1—N2—Uxiii | 116.23 (17) |
H5v—I1—H5viii | 73.3 (4) | U—N2—Uxiii | 79.40 (9) |
H5i—I1—H5viii | 73.3 (4) | N1—C1—N2 | 128.4 (3) |
I1i—I1—I1ix | 0.0 | N1—C1—C2 | 123.3 (3) |
I1ii—I1—I1ix | 180.0 | N2—C1—C2 | 108.3 (3) |
H5ii—I1—I1ix | 115.4 (3) | C3—C2—C7 | 120.9 (4) |
H5iii—I1—I1ix | 115.4 (3) | C3—C2—C1 | 131.6 (4) |
H5—I1—I1ix | 115.4 (3) | C7—C2—C1 | 107.5 (3) |
H5iv—I1—I1ix | 115.4 (3) | H3—C3—C4 | 122 (3) |
I1v—I1—I1ix | 0.0 | H3—C3—C2 | 120 (3) |
I1vi—I1—I1ix | 180.0 | C4—C3—C2 | 117.4 (4) |
H5vii—I1—I1ix | 57.6 (4) | H4—C4—C3 | 118 (2) |
H5v—I1—I1ix | 57.6 (4) | H4—C4—C5 | 120 (2) |
H5i—I1—I1ix | 57.6 (4) | C3—C4—C5 | 121.6 (4) |
H5viii—I1—I1ix | 57.6 (4) | H5—C5—C6 | 114 (3) |
I1i—I1—C5ii | 109.95 (3) | H5—C5—C4 | 125 (3) |
I1ii—I1—C5ii | 70.05 (3) | C6—C5—C4 | 121.1 (4) |
H5ii—I1—C5ii | 6.1 (4) | H5—C5—I1ii | 22.1 (11) |
H5iii—I1—C5ii | 84.2 (7) | C6—C5—I1ii | 103.4 (3) |
H5—I1—C5ii | 134.5 (3) | C4—C5—I1ii | 131.3 (3) |
H5iv—I1—C5ii | 79.0 (7) | H5—C5—I1 | 22.1 (11) |
I1v—I1—C5ii | 109.95 (3) | C6—C5—I1 | 103.4 (3) |
I1vi—I1—C5ii | 70.05 (3) | C4—C5—I1 | 131.3 (3) |
H5vii—I1—C5ii | 132.6 (7) | I1ii—C5—I1 | 39.89 (7) |
H5v—I1—C5ii | 64.0 (5) | H6—C6—C7 | 115 (3) |
H5i—I1—C5ii | 143.5 (7) | H6—C6—C5 | 128 (3) |
H5viii—I1—C5ii | 71.8 (6) | C7—C6—C5 | 117.4 (4) |
I1ix—I1—C5ii | 109.95 (3) | C6—C7—C2 | 121.6 (3) |
I1i—I1—C5iii | 109.95 (3) | C6—C7—C8 | 132.9 (4) |
I1ii—I1—C5iii | 70.05 (3) | C2—C7—C8 | 105.5 (3) |
H5ii—I1—C5iii | 79.0 (7) | N1xi—C8—N2 | 127.3 (3) |
H5iii—I1—C5iii | 6.1 (4) | N1xi—C8—C7 | 122.5 (3) |
H5—I1—C5iii | 84.2 (7) | N2—C8—C7 | 110.2 (3) |
H5iv—I1—C5iii | 134.5 (3) | C5—H5—I1ii | 151.8 (14) |
I1v—I1—C5iii | 109.95 (3) | C5—H5—I1 | 151.8 (14) |
I1vi—I1—C5iii | 70.05 (3) | I1ii—H5—I1 | 50.8 (6) |
H5vii—I1—C5iii | 64.0 (5) | C5—H5—I1vi | 145.5 (11) |
H5v—I1—C5iii | 71.8 (6) | I1ii—H5—I1vi | 6.97 (8) |
H5i—I1—C5iii | 132.6 (7) | I1—H5—I1vi | 57.8 (7) |
H5viii—I1—C5iii | 143.5 (7) | C5—H5—I1i | 145.5 (11) |
I1ix—I1—C5iii | 109.95 (3) | I1ii—H5—I1i | 57.8 (7) |
C5ii—I1—C5iii | 83.32 (2) | I1—H5—I1i | 6.97 (8) |
I1i—I1—C5 | 109.95 (3) | I1vi—H5—I1i | 64.8 (7) |
I1ii—I1—C5 | 70.05 (3) | | |
Symmetry codes: (i) x, −y, −z+1/2; (ii) −x, −y, −z; (iii) −y, x, z; (iv) y, −x, −z; (v) −x, y, z+1/2; (vi) −x, y, z−1/2; (vii) y, x, z+1/2; (viii) −y, −x, −z+1/2; (ix) −x, −y, −z+1; (x) −y+1, −x+1, −z+1/2; (xi) y, −x+1, −z; (xii) x, −y+1, −z+1/2; (xiii) −x+1, −y+1, −z; (xiv) −x+1, y, z+1/2; (xv) −y+1, x, z; (xvi) −x+1, −y+1, −z+1. |
Crystal data top
C64H32H0I1.86N16U0.97 | F(000) = 716 |
Mr = 1491.98 | Dx = 1.942 Mg m−3 |
Tetragonal, P4/mcc | Mo Kα radiation, λ = 0.71073 Å |
a = 13.995 (2) Å | µ = 4.28 mm−1 |
c = 6.513 (1) Å | T = 293 K |
V = 1275.5 (3) Å3 | Irreglar, black |
Z = 1 | 0.33 × 0.10 × 0.09 mm |
Data collection top
KM4-CCD diffractometer | 894 reflections with I > 2σ(I) |
Radiation source: fine-focus sealed tube | Rint = 0.064 |
Graphite monochromator | θmax = 29.6°, θmin = 2.9° |
Absorption correction: numerical | h = −19→18 |
Tmin = 0.417, Tmax = 0.601 | k = −18→19 |
16555 measured reflections | l = −9→6 |
979 independent reflections | |
Refinement top
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)] = 0.039 | H atoms treated by a mixture of independent and constrained refinement |
wR(F2) = 0.094 | Calculated w = 1/[σ2(Fo2) + (0.0424P)2 + 1.1429P] where P = (Fo2 + 2Fc2)/3 |
S = 1.17 | (Δ/σ)max = 2.498 |
979 reflections | Δρmax = 0.49 e Å−3 |
78 parameters | Δρmin = −0.41 e Å−3 |
0 restraints | Extinction correction: SHELXL, Fc*=kFc[1+0.001xFc2λ3/sin(2θ)]-1/4 |
Primary atom site location: structure-invariant direct methods | Extinction coefficient: 0.0000 (9) |
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) |
I1 | 0.0000 | 0.0000 | 0.2147 (2) | 0.0479 (5) | 0.466 (4) |
U | 0.5000 | 0.5000 | 0.2500 | 0.0226 (2) | 0.484 (4) |
N1 | 0.5827 (2) | 0.2730 (2) | 0.0000 | 0.0332 (8) | |
N2 | 0.4401 (2) | 0.3731 (2) | 0.0000 | 0.0468 (10) | |
C1 | 0.4890 (3) | 0.2873 (3) | 0.0000 | 0.0338 (9) | |
C2 | 0.4190 (3) | 0.2095 (3) | 0.0000 | 0.0340 (9) | |
C3 | 0.4301 (4) | 0.1112 (3) | 0.0000 | 0.0538 (13) | |
C4 | 0.3478 (4) | 0.0558 (4) | 0.0000 | 0.0709 (18) | |
C5 | 0.2569 (4) | 0.0972 (4) | 0.0000 | 0.0638 (16) | |
C6 | 0.2457 (3) | 0.1955 (3) | 0.0000 | 0.0467 (11) | |
C7 | 0.3279 (3) | 0.2511 (3) | 0.0000 | 0.0346 (9) | |
C8 | 0.3445 (3) | 0.3537 (3) | 0.0000 | 0.0326 (8) | |
H3 | 0.491 (3) | 0.083 (4) | 0.0000 | 0.039* | |
H4 | 0.352 (3) | −0.014 (3) | 0.0000 | 0.039* | |
H5 | 0.201 (3) | 0.065 (3) | 0.0000 | 0.039* | |
H6 | 0.186 (3) | 0.231 (3) | 0.0000 | 0.039* | |
Atomic displacement parameters (Å2) top | U11 | U22 | U33 | U12 | U13 | U23 |
I1 | 0.0441 (3) | 0.0441 (3) | 0.0554 (14) | 0.000 | 0.000 | 0.000 |
U | 0.0225 (2) | 0.0225 (2) | 0.0228 (3) | 0.000 | 0.000 | 0.000 |
N1 | 0.0309 (17) | 0.0314 (17) | 0.0373 (17) | 0.0038 (12) | 0.000 | 0.000 |
N2 | 0.0275 (17) | 0.0330 (19) | 0.080 (3) | 0.0005 (14) | 0.000 | 0.000 |
C1 | 0.042 (2) | 0.0297 (18) | 0.0301 (16) | −0.0017 (15) | 0.000 | 0.000 |
C2 | 0.034 (2) | 0.033 (2) | 0.0353 (19) | −0.0030 (14) | 0.000 | 0.000 |
C3 | 0.046 (3) | 0.033 (2) | 0.082 (4) | −0.0009 (18) | 0.000 | 0.000 |
C4 | 0.062 (3) | 0.031 (2) | 0.120 (5) | −0.006 (2) | 0.000 | 0.000 |
C5 | 0.051 (3) | 0.043 (3) | 0.097 (4) | −0.017 (2) | 0.000 | 0.000 |
C6 | 0.039 (2) | 0.045 (2) | 0.056 (3) | −0.0060 (19) | 0.000 | 0.000 |
C7 | 0.039 (2) | 0.0336 (19) | 0.0315 (18) | −0.0053 (15) | 0.000 | 0.000 |
C8 | 0.0315 (19) | 0.033 (2) | 0.0334 (17) | −0.0035 (14) | 0.000 | 0.000 |
Geometric parameters (Å, º) top
I1—I1i | 0.460 (3) | U—Uxii | 3.2565 (5) |
I1—I1ii | 2.797 (3) | U—Uxvi | 3.2565 (5) |
I1—I1iii | 3.2565 (5) | N1—C1 | 1.326 (5) |
I1—I1iv | 3.2565 (5) | N1—C8xiv | 1.340 (5) |
I1—H5v | 3.28 (4) | N2—C8 | 1.365 (5) |
I1—H5vi | 3.28 (4) | N2—C1 | 1.383 (5) |
I1—H5ii | 3.28 (4) | N2—Uxii | 2.551 (3) |
I1—H5 | 3.28 (4) | C1—C2 | 1.464 (5) |
I1—H5vii | 3.50 (4) | C2—C3 | 1.384 (6) |
I1—H5viii | 3.50 (4) | C2—C7 | 1.403 (6) |
I1—H5i | 3.50 (4) | C3—H3 | 0.94 (4) |
I1—H5iii | 3.50 (4) | C3—C4 | 1.388 (7) |
I1—I1ix | 3.716 (3) | C4—H4 | 0.97 (4) |
I1—C5v | 4.091 (5) | C4—C5 | 1.398 (8) |
I1—C5vi | 4.091 (5) | C5—H5 | 0.90 (4) |
I1—C5ii | 4.091 (5) | C5—C6 | 1.384 (7) |
U—N2 | 2.551 (3) | C5—I1ii | 4.091 (5) |
U—N2x | 2.551 (3) | C6—H6 | 0.98 (5) |
U—N2xi | 2.551 (3) | C6—C7 | 1.389 (6) |
U—N2xii | 2.551 (3) | C7—C8 | 1.455 (5) |
U—N2xiii | 2.551 (3) | C8—N1xv | 1.340 (5) |
U—N2xiv | 2.551 (3) | H5—I1ii | 3.28 (4) |
U—N2xv | 2.551 (3) | H5—I1iv | 3.50 (4) |
U—N2vii | 2.551 (3) | H5—I1i | 3.50 (4) |
| | | |
I1i—I1—I1ii | 180.0 | I1iii—I1—C5ii | 109.99 (3) |
I1i—I1—I1iii | 0.0 | I1iv—I1—C5ii | 70.01 (3) |
I1ii—I1—I1iii | 180.0 | H5v—I1—C5ii | 79.2 (8) |
I1i—I1—I1iv | 180.0 | H5vi—I1—C5ii | 84.0 (8) |
I1ii—I1—I1iv | 0.0 | H5ii—I1—C5ii | 5.9 (5) |
I1iii—I1—I1iv | 180.0 | H5—I1—C5ii | 134.7 (4) |
I1i—I1—H5v | 115.3 (3) | H5vii—I1—C5ii | 132.8 (7) |
I1ii—I1—H5v | 64.7 (3) | H5viii—I1—C5ii | 71.6 (6) |
I1iii—I1—H5v | 115.3 (3) | H5i—I1—C5ii | 143.4 (7) |
I1iv—I1—H5v | 64.7 (3) | H5iii—I1—C5ii | 63.9 (6) |
I1i—I1—H5vi | 115.3 (3) | I1ix—I1—C5ii | 109.99 (3) |
I1ii—I1—H5vi | 64.7 (3) | C5v—I1—C5ii | 83.30 (2) |
I1iii—I1—H5vi | 115.3 (3) | C5vi—I1—C5ii | 83.29 (2) |
I1iv—I1—H5vi | 64.7 (3) | N2—U—N2x | 91.78 (12) |
H5v—I1—H5vi | 129.5 (7) | N2—U—N2xi | 141.62 (14) |
I1i—I1—H5ii | 115.3 (3) | N2x—U—N2xi | 100.66 (10) |
I1ii—I1—H5ii | 64.7 (3) | N2—U—N2xii | 100.66 (10) |
I1iii—I1—H5ii | 115.3 (3) | N2x—U—N2xii | 141.62 (14) |
I1iv—I1—H5ii | 64.7 (3) | N2xi—U—N2xii | 91.78 (12) |
H5v—I1—H5ii | 79.5 (3) | N2—U—N2xiii | 149.88 (14) |
H5vi—I1—H5ii | 79.5 (3) | N2x—U—N2xiii | 65.95 (5) |
I1i—I1—H5 | 115.3 (3) | N2xi—U—N2xiii | 65.96 (5) |
I1ii—I1—H5 | 64.7 (3) | N2xii—U—N2xiii | 87.13 (11) |
I1iii—I1—H5 | 115.3 (3) | N2—U—N2xiv | 65.96 (5) |
I1iv—I1—H5 | 64.7 (3) | N2x—U—N2xiv | 87.13 (11) |
H5v—I1—H5 | 79.5 (3) | N2xi—U—N2xiv | 149.88 (14) |
H5vi—I1—H5 | 79.5 (3) | N2xii—U—N2xiv | 65.95 (5) |
H5ii—I1—H5 | 129.5 (7) | N2xiii—U—N2xiv | 91.77 (12) |
I1i—I1—H5vii | 57.9 (4) | N2—U—N2xv | 65.95 (5) |
I1ii—I1—H5vii | 122.1 (4) | N2x—U—N2xv | 149.88 (14) |
I1iii—I1—H5vii | 57.9 (4) | N2xi—U—N2xv | 87.13 (11) |
I1iv—I1—H5vii | 122.1 (4) | N2xii—U—N2xv | 65.96 (5) |
H5v—I1—H5vii | 147.9 (15) | N2xiii—U—N2xv | 141.63 (14) |
H5vi—I1—H5vii | 66.8 (11) | N2xiv—U—N2xv | 100.66 (10) |
H5ii—I1—H5vii | 132.6 (15) | N2—U—N2vii | 87.13 (11) |
H5—I1—H5vii | 77.1 (12) | N2x—U—N2vii | 65.96 (5) |
I1i—I1—H5viii | 57.9 (4) | N2xi—U—N2vii | 65.95 (5) |
I1ii—I1—H5viii | 122.1 (4) | N2xii—U—N2vii | 149.88 (14) |
I1iii—I1—H5viii | 57.9 (4) | N2xiii—U—N2vii | 100.66 (10) |
I1iv—I1—H5viii | 122.1 (4) | N2xiv—U—N2vii | 141.63 (14) |
H5v—I1—H5viii | 66.8 (11) | N2xv—U—N2vii | 91.77 (12) |
H5vi—I1—H5viii | 147.9 (15) | N2—U—Uxii | 50.33 (5) |
H5ii—I1—H5viii | 77.1 (12) | N2x—U—Uxii | 129.67 (5) |
H5—I1—H5viii | 132.6 (15) | N2xi—U—Uxii | 129.67 (5) |
H5vii—I1—H5viii | 115.8 (8) | N2xii—U—Uxii | 50.33 (5) |
I1i—I1—H5i | 57.9 (4) | N2xiii—U—Uxii | 129.67 (5) |
I1ii—I1—H5i | 122.1 (4) | N2xiv—U—Uxii | 50.33 (5) |
I1iii—I1—H5i | 57.9 (4) | N2xv—U—Uxii | 50.33 (5) |
I1iv—I1—H5i | 122.1 (4) | N2vii—U—Uxii | 129.67 (5) |
H5v—I1—H5i | 77.1 (12) | N2—U—Uxvi | 129.67 (5) |
H5vi—I1—H5i | 132.6 (15) | N2x—U—Uxvi | 50.33 (5) |
H5ii—I1—H5i | 147.9 (15) | N2xi—U—Uxvi | 50.33 (5) |
H5—I1—H5i | 66.8 (11) | N2xii—U—Uxvi | 129.67 (5) |
H5vii—I1—H5i | 73.6 (4) | N2xiii—U—Uxvi | 50.33 (5) |
H5viii—I1—H5i | 73.6 (4) | N2xiv—U—Uxvi | 129.67 (5) |
I1i—I1—H5iii | 57.9 (4) | N2xv—U—Uxvi | 129.67 (5) |
I1ii—I1—H5iii | 122.1 (4) | N2vii—U—Uxvi | 50.33 (5) |
I1iii—I1—H5iii | 57.9 (4) | Uxii—U—Uxvi | 180.0 |
I1iv—I1—H5iii | 122.1 (4) | C1—N1—C8xiv | 122.9 (3) |
H5v—I1—H5iii | 132.6 (15) | C8—N2—C1 | 108.2 (3) |
H5vi—I1—H5iii | 77.1 (12) | C8—N2—U | 117.43 (18) |
H5ii—I1—H5iii | 66.8 (11) | C1—N2—U | 116.22 (17) |
H5—I1—H5iii | 147.9 (15) | C8—N2—Uxii | 117.43 (18) |
H5vii—I1—H5iii | 73.6 (4) | C1—N2—Uxii | 116.22 (17) |
H5viii—I1—H5iii | 73.6 (4) | U—N2—Uxii | 79.34 (10) |
H5i—I1—H5iii | 115.8 (8) | N1—C1—N2 | 128.4 (4) |
I1i—I1—I1ix | 0.0 | N1—C1—C2 | 123.3 (3) |
I1ii—I1—I1ix | 180.0 | N2—C1—C2 | 108.3 (3) |
I1iii—I1—I1ix | 0.0 | C3—C2—C7 | 120.9 (4) |
I1iv—I1—I1ix | 180.0 | C3—C2—C1 | 131.6 (4) |
H5v—I1—I1ix | 115.3 (3) | C7—C2—C1 | 107.5 (3) |
H5vi—I1—I1ix | 115.3 (3) | H3—C3—C2 | 121 (3) |
H5ii—I1—I1ix | 115.3 (3) | H3—C3—C4 | 121 (3) |
H5—I1—I1ix | 115.3 (3) | C2—C3—C4 | 117.5 (4) |
H5vii—I1—I1ix | 57.9 (4) | H4—C4—C3 | 120 (3) |
H5viii—I1—I1ix | 57.9 (4) | H4—C4—C5 | 118 (3) |
H5i—I1—I1ix | 57.9 (4) | C3—C4—C5 | 121.6 (4) |
H5iii—I1—I1ix | 57.9 (4) | H5—C5—C6 | 113 (3) |
I1i—I1—C5v | 109.99 (3) | H5—C5—C4 | 126 (3) |
I1ii—I1—C5v | 70.01 (3) | C6—C5—C4 | 121.0 (5) |
I1iii—I1—C5v | 109.99 (3) | H5—C5—I1ii | 21.9 (12) |
I1iv—I1—C5v | 70.01 (3) | C6—C5—I1ii | 103.3 (3) |
H5v—I1—C5v | 5.9 (5) | C4—C5—I1ii | 131.5 (3) |
H5vi—I1—C5v | 134.7 (4) | H5—C5—I1 | 21.9 (12) |
H5ii—I1—C5v | 84.0 (8) | C6—C5—I1 | 103.3 (3) |
H5—I1—C5v | 79.2 (8) | C4—C5—I1 | 131.5 (3) |
H5vii—I1—C5v | 143.4 (7) | I1ii—C5—I1 | 39.97 (6) |
H5viii—I1—C5v | 63.9 (6) | H6—C6—C5 | 128 (3) |
H5i—I1—C5v | 71.6 (6) | H6—C6—C7 | 115 (3) |
H5iii—I1—C5v | 132.8 (7) | C5—C6—C7 | 117.5 (4) |
I1ix—I1—C5v | 109.99 (3) | C6—C7—C2 | 121.4 (4) |
I1i—I1—C5vi | 109.99 (3) | C6—C7—C8 | 133.3 (4) |
I1ii—I1—C5vi | 70.01 (3) | C2—C7—C8 | 105.3 (3) |
I1iii—I1—C5vi | 109.99 (3) | N1xv—C8—N2 | 126.9 (4) |
I1iv—I1—C5vi | 70.01 (3) | N1xv—C8—C7 | 122.4 (3) |
H5v—I1—C5vi | 134.7 (4) | N2—C8—C7 | 110.7 (3) |
H5vi—I1—C5vi | 5.9 (5) | C5—H5—I1ii | 152.3 (15) |
H5ii—I1—C5vi | 79.2 (8) | C5—H5—I1 | 152.3 (15) |
H5—I1—C5vi | 84.0 (8) | I1ii—H5—I1 | 50.5 (7) |
H5vii—I1—C5vi | 63.9 (6) | C5—H5—I1iv | 146.0 (12) |
H5viii—I1—C5vi | 143.4 (7) | I1ii—H5—I1iv | 6.83 (7) |
H5i—I1—C5vi | 132.8 (7) | I1—H5—I1iv | 57.4 (7) |
H5iii—I1—C5vi | 71.6 (6) | C5—H5—I1i | 146.0 (12) |
I1ix—I1—C5vi | 109.99 (3) | I1ii—H5—I1i | 57.4 (7) |
C5v—I1—C5vi | 140.02 (6) | I1—H5—I1i | 6.83 (7) |
I1i—I1—C5ii | 109.99 (3) | I1iv—H5—I1i | 64.2 (8) |
I1ii—I1—C5ii | 70.01 (3) | | |
Symmetry codes: (i) x, −y, −z+1/2; (ii) −x, −y, −z; (iii) −x, y, z+1/2; (iv) −x, y, z−1/2; (v) y, −x, −z; (vi) −y, x, z; (vii) y, x, z+1/2; (viii) −y, −x, −z+1/2; (ix) −x, −y, −z+1; (x) −x+1, y, z+1/2; (xi) x, −y+1, −z+1/2; (xii) −x+1, −y+1, −z; (xiii) −y+1, −x+1, −z+1/2; (xiv) −y+1, x, z; (xv) y, −x+1, −z; (xvi) −x+1, −y+1, −z+1. |