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The title complex, [Tb(C11H12N2O)6]I3, has essentially the same structure at 160 K as at room temperature, and is clearly centrosymmetric without any disorder, contrary to some proposals regarding the possible mechanism of tribolumin­escence. Terbium has an octahedral coordination and lies in a position of \overline 3 symmetry, with all six antipyrine ligands crystallographically equivalent. One iodide anion lies in a special position of site symmetry \overline 3, and another is on a threefold rotation axis, to give three iodide anions per terbium-centred complex cation.

Supporting information

cif

Crystallographic Information File (CIF) https://doi.org/10.1107/S1600536802005093/na6149sup1.cif
Contains datablocks I, global

hkl

Structure factor file (CIF format) https://doi.org/10.1107/S1600536802005093/na6149Isup2.hkl
Contains datablock I

CCDC reference: 183769

Key indicators

  • Single-crystal X-ray study
  • T = 160 K
  • Mean [sigma](C-C) = 0.004 Å
  • R factor = 0.019
  • wR factor = 0.047
  • Data-to-parameter ratio = 21.5

checkCIF results

No syntax errors found

ADDSYM reports no extra symmetry


Amber Alert Alert Level B:
SYMMS_02 Alert B The unit-cell lengths a and c should be equal for a rhombohedral cell Cell 13.7474 13.7474 31.9658 Angles 90.0000 90.0000 120.0000 SYMMS_02 Alert B Cell angles alpha and gamma should be equal for a rhombohedral cell Cell 13.7474 13.7474 31.9658 Angles 90.0000 90.0000 120.0000 SYMMS_02 Alert B All angles should not be 90 for a rhombohedral cell Cell 13.7474 13.7474 31.9658 Angles 90.0000 90.0000 120.0000
Yellow Alert Alert Level C:
PLAT_030 Alert C Refined Extinction parameter within range .... 3.00 Sigma General Notes
ABSTM_02 When printed, the submitted absorption T values will be replaced by the scaled T values. Since the ratio of scaled T's is identical to the ratio of reported T values, the scaling does not imply a change to the absorption corrections used in the study. Ratio of Tmax expected/reported 0.878 Tmax scaled 0.432 Tmin scaled 0.340
0 Alert Level A = Potentially serious problem
3 Alert Level B = Potential problem
1 Alert Level C = Please check

Computing details top

Data collection: SMART (Bruker, 1997); cell refinement: SAINT (Bruker, 1997); data reduction: SAINT; program(s) used to solve structure: SHELXTL (Sheldrick, 1997b); program(s) used to refine structure: SHELXTL; molecular graphics: SHELXTL; software used to prepare material for publication: SHELXTL and local programs.

(I) top
Crystal data top
[Tb(C11H12N2O)6]I3F(000) = 2472
Mr = 1668.98Dx = 1.589 Mg m3
Rhombohedral, R3Mo Kα radiation, λ = 0.71073 Å
a = 13.7474 (3) ÅCell parameters from 12573 reflections
c = 31.9658 (14) Åθ = 3.0–28.9°
α = 90°µ = 2.40 mm1
γ = 120°T = 160 K
V = 5231.9 (3) Å3Block, colourless
Z = 30.50 × 0.40 × 0.35 mm
Data collection top
Bruker SMART 1K CCD
diffractometer
2945 independent reflections
Radiation source: sealed tube2692 reflections with I > 2σ(I)
Graphite monochromatorRint = 0.020
Detector resolution: 8.192 pixels mm-1θmax = 28.9°, θmin = 1.8°
ω rotation with narrow frames scansh = 1717
Absorption correction: multi-scan
(SADABS; Sheldrick, 1997a)
k = 1818
Tmin = 0.387, Tmax = 0.492l = 4343
15672 measured reflections
Refinement top
Refinement on F2Secondary atom site location: difference Fourier map
Least-squares matrix: fullHydrogen site location: inferred from neighbouring sites
R[F2 > 2σ(F2)] = 0.019H-atom parameters constrained
wR(F2) = 0.047 w = 1/[σ2(Fo2) + (0.0204P)2 + 8.1659P]
where P = (Fo2 + 2Fc2)/3
S = 1.10(Δ/σ)max < 0.001
2945 reflectionsΔρmax = 0.35 e Å3
137 parametersΔρmin = 0.77 e Å3
0 restraintsExtinction correction: SHELXTL, Fc*=kFc[1+0.001xFc2λ3/sin(2θ)]-1/4
Primary atom site location: structure-invariant direct methodsExtinction coefficient: 0.00009 (3)
Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top
xyzUiso*/Ueq
Tb0.00000.00000.00000.01863 (6)
O10.11349 (10)0.02865 (10)0.04196 (4)0.0281 (3)
N10.33249 (14)0.04546 (16)0.08622 (5)0.0415 (4)
N20.27309 (12)0.04007 (13)0.05215 (5)0.0298 (3)
C10.18594 (14)0.02658 (14)0.06669 (5)0.0253 (3)
C20.19706 (17)0.01697 (17)0.11044 (6)0.0363 (4)
H20.15000.00580.12930.044*
C30.28844 (19)0.0268 (2)0.12084 (6)0.0447 (5)
C40.3408 (3)0.0167 (3)0.16288 (8)0.0754 (9)
H4A0.35370.08000.16710.113*
H4B0.29030.01760.18470.113*
H4C0.41250.05390.16440.113*
C50.44747 (18)0.0240 (2)0.08044 (9)0.0561 (6)
H5A0.50100.05230.08980.084*
H5B0.46020.03200.05080.084*
H5C0.45800.07820.09690.084*
C60.27165 (14)0.09003 (15)0.01298 (6)0.0286 (3)
C70.26096 (18)0.19576 (18)0.01085 (9)0.0513 (6)
H70.26080.23460.03540.062*
C80.2505 (2)0.2430 (2)0.02876 (13)0.0748 (10)
H80.24360.31510.03100.090*
C90.2498 (2)0.1883 (3)0.06428 (11)0.0733 (10)
H90.24290.22200.09090.088*
C100.25923 (18)0.0851 (2)0.06136 (7)0.0544 (6)
H100.25760.04740.08600.065*
C110.27111 (15)0.03450 (17)0.02277 (6)0.0337 (4)
H110.27880.03800.02100.040*
I10.33330.33330.124103 (7)0.04370 (8)
I20.33330.33330.16670.05569 (11)
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
Tb0.01812 (7)0.01812 (7)0.01965 (9)0.00906 (3)0.0000.000
O10.0272 (6)0.0347 (6)0.0280 (6)0.0197 (5)0.0042 (5)0.0027 (5)
N10.0325 (8)0.0607 (11)0.0376 (9)0.0280 (8)0.0087 (7)0.0089 (8)
N20.0265 (7)0.0415 (8)0.0271 (7)0.0214 (7)0.0020 (6)0.0050 (6)
C10.0235 (8)0.0262 (8)0.0260 (8)0.0123 (6)0.0005 (6)0.0011 (6)
C20.0382 (10)0.0435 (11)0.0251 (9)0.0187 (9)0.0009 (7)0.0009 (8)
C30.0459 (12)0.0555 (13)0.0308 (10)0.0239 (10)0.0105 (9)0.0046 (9)
C40.084 (2)0.110 (3)0.0389 (13)0.053 (2)0.0273 (13)0.0004 (14)
C50.0311 (11)0.0680 (16)0.0738 (17)0.0282 (11)0.0072 (10)0.0171 (13)
C60.0212 (7)0.0289 (8)0.0379 (9)0.0142 (7)0.0026 (7)0.0009 (7)
C70.0363 (11)0.0365 (11)0.0894 (18)0.0243 (9)0.0062 (11)0.0031 (11)
C80.0402 (13)0.0511 (15)0.140 (3)0.0280 (12)0.0030 (16)0.0432 (18)
C90.0369 (12)0.097 (2)0.084 (2)0.0323 (14)0.0048 (13)0.0540 (19)
C100.0342 (11)0.0852 (18)0.0357 (11)0.0237 (12)0.0052 (9)0.0129 (11)
C110.0277 (9)0.0391 (10)0.0323 (9)0.0152 (8)0.0052 (7)0.0014 (8)
I10.04874 (10)0.04874 (10)0.03362 (12)0.02437 (5)0.0000.000
I20.06590 (16)0.06590 (16)0.03527 (18)0.03295 (8)0.0000.000
Geometric parameters (Å, º) top
Tb—O12.2367 (11)C4—H4B0.980
Tb—O1i2.2367 (11)C4—H4C0.980
Tb—O1ii2.2367 (11)C5—H5A0.980
Tb—O1iii2.2367 (11)C5—H5B0.980
Tb—O1iv2.2367 (11)C5—H5C0.980
Tb—O1v2.2367 (11)C6—C71.388 (3)
O1—C11.261 (2)C6—C111.376 (3)
N1—N21.385 (2)C7—H70.950
N1—C31.347 (3)C7—C81.397 (4)
N1—C51.468 (3)C8—H80.950
N2—C11.381 (2)C8—C91.364 (5)
N2—C61.423 (2)C9—H90.950
C1—C21.406 (2)C9—C101.363 (4)
C2—H20.950C10—H100.950
C2—C31.370 (3)C10—C111.385 (3)
C3—C41.498 (3)C11—H110.950
C4—H4A0.980
O1i—Tb—O1ii180.0C3—C4—H4A109.5
O1i—Tb—O1iii87.75 (4)C3—C4—H4B109.5
O1ii—Tb—O1iii92.25 (4)C3—C4—H4C109.5
O1—Tb—O1i92.25 (4)H4A—C4—H4B109.5
O1—Tb—O1ii87.75 (4)H4A—C4—H4C109.5
O1—Tb—O1iii92.25 (4)H4B—C4—H4C109.5
O1i—Tb—O1iv92.25 (4)N1—C5—H5A109.5
O1ii—Tb—O1iv87.75 (4)N1—C5—H5B109.5
O1iii—Tb—O1iv180.0N1—C5—H5C109.5
O1—Tb—O1iv87.75 (4)H5A—C5—H5B109.5
O1i—Tb—O1v87.75 (4)H5A—C5—H5C109.5
O1ii—Tb—O1v92.25 (4)H5B—C5—H5C109.5
O1iii—Tb—O1v87.75 (4)N2—C6—C7121.15 (19)
O1—Tb—O1v180.0N2—C6—C11117.73 (16)
O1iv—Tb—O1v92.25 (4)C7—C6—C11120.9 (2)
Tb—O1—C1170.00 (12)C6—C7—H7121.2
N2—N1—C3107.60 (15)C6—C7—C8117.6 (3)
N2—N1—C5119.66 (17)H7—C7—C8121.2
C3—N1—C5127.39 (19)C7—C8—H8119.1
N1—N2—C1108.47 (14)C7—C8—C9121.8 (2)
N1—N2—C6122.15 (15)H8—C8—C9119.1
C1—N2—C6123.85 (14)C8—C9—H9120.2
O1—C1—N2120.96 (15)C8—C9—C10119.6 (2)
O1—C1—C2132.34 (17)H9—C9—C10120.2
N2—C1—C2106.65 (15)C9—C10—H10119.7
C1—C2—H2126.4C9—C10—C11120.6 (3)
C1—C2—C3107.11 (18)H10—C10—C11119.7
H2—C2—C3126.4C6—C11—C10119.5 (2)
N1—C3—C2109.97 (17)C6—C11—H11120.2
N1—C3—C4120.9 (2)C10—C11—H11120.2
C2—C3—C4129.1 (2)
Symmetry codes: (i) xy, x, z; (ii) x+y, x, z; (iii) y, x+y, z; (iv) y, xy, z; (v) x, y, z.
 

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