Buy article online - an online subscription or single-article purchase is required to access this article.
The title compound, poly[[tris(μ2-4,4′-bipyridine N,N′-dioxide)bis[trinitratothallium(III)]] dichloromethane disolvate], [Tl2(NO3)6(C10H8N2O2)3]·2CH2Cl2, forms a ladder polymer with channels which accommodate the CH2Cl2 solvent molecules.
Supporting information
CCDC reference: 601134
Key indicators
- Single-crystal X-ray study
- T = 203 K
- Mean (C-C) = 0.007 Å
- Disorder in main residue
- R factor = 0.036
- wR factor = 0.107
- Data-to-parameter ratio = 16.1
checkCIF/PLATON results
No syntax errors found
Alert level A
PLAT220_ALERT_2_A Large Non-Solvent O Ueq(max)/Ueq(min) ... 10.00 Ratio
| Author Response: Elemental analysis confirms that the assignment of atom types is
correct. Several different crystals were tried, at room temperature as well
as low temperature. The refinement presented here is the best obtainable for
this compound.
|
Alert level B
PLAT201_ALERT_2_B Isotropic non-H Atoms in Main Residue(s) ....... 2
Alert level C
PLAT041_ALERT_1_C Calc. and Rep. SumFormula Strings Differ .... ?
PLAT042_ALERT_1_C Calc. and Rep. MoietyFormula Strings Differ .... ?
PLAT045_ALERT_1_C Calculated and Reported Z Differ by ............ 2.00 Ratio
PLAT213_ALERT_2_C Atom O28 has ADP max/min Ratio ............. 3.60 prolat
PLAT213_ALERT_2_C Atom N17 has ADP max/min Ratio ............. 3.70 prolat
PLAT213_ALERT_2_C Atom C4 has ADP max/min Ratio ............. 3.10 prolat
PLAT213_ALERT_2_C Atom C7 has ADP max/min Ratio ............. 3.20 prolat
PLAT220_ALERT_2_C Large Non-Solvent C Ueq(max)/Ueq(min) ... 2.56 Ratio
| Author Response: Elemental analysis confirms that the assignment of atom types is
correct. Several different crystals were tried, at room temperature as well
as low temperature. The refinement presented here is the best obtainable for
this compound.
|
PLAT220_ALERT_2_C Large Non-Solvent N Ueq(max)/Ueq(min) ... 2.52 Ratio
| Author Response: Elemental analysis confirms that the assignment of atom types is
correct. Several different crystals were tried, at room temperature as well
as low temperature. The refinement presented here is the best obtainable for
this compound.
|
PLAT301_ALERT_3_C Main Residue Disorder ......................... 6.00 Perc.
PLAT431_ALERT_2_C Short Inter HL..A Contact Cl2A .. O33 .. 3.14 Ang.
1 ALERT level A = In general: serious problem
1 ALERT level B = Potentially serious problem
11 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
9 ALERT type 2 Indicator that the structure model may be wrong or deficient
1 ALERT type 3 Indicator that the structure quality may be low
0 ALERT type 4 Improvement, methodology, query or suggestion
Data collection: COLLECT (Nonius, 1998); cell refinement: DENZO (Otwinowski & Minor, 1997); data reduction: DENZO; program(s) used to solve structure: SHELXS97 (Sheldrick, 1997); program(s) used to refine structure: SHELXL97 (Sheldrick, 1997); molecular graphics: X-SEED (Barbour, 2001) and POV-RAY (Persistence of Vision, 1999); software used to prepare material for publication: SHELXL97.
poly[[tris(µ
2-4,4'-bipyridine
N,
N'-dioxide)bis[trinitratothallium(III)]] dichloromethane
disolvate]
top
Crystal data top
[Tl2(NO3)6(C10H8N2O2)3]·2CH2Cl2 | Z = 1 |
Mr = 1515.22 | F(000) = 726 |
Triclinic, P1 | Dx = 2.121 Mg m−3 |
Hall symbol: -P 1 | Mo Kα radiation, λ = 0.71073 Å |
a = 8.0425 (16) Å | Cell parameters from 35318 reflections |
b = 11.687 (2) Å | θ = 1.0–27.5° |
c = 13.079 (3) Å | µ = 7.11 mm−1 |
α = 86.51 (3)° | T = 203 K |
β = 79.83 (3)° | Block, colorless |
γ = 78.75 (3)° | 0.15 × 0.10 × 0.08 mm |
V = 1186.3 (4) Å3 | |
Data collection top
Nonius KappaCCD diffractometer | 5387 independent reflections |
Radiation source: fine-focus sealed tube | 4847 reflections with I > 2σ(I) |
Graphite monochromator | Rint = 0.038 |
ω and φ scans | θmax = 27.5°, θmin = 3.6° |
Absorption correction: multi-scan (SADABS; Sheldrick, 2001) | h = −10→10 |
Tmin = 0.435, Tmax = 0.560 | k = −15→15 |
35318 measured reflections | l = −16→16 |
Refinement top
Refinement on F2 | Primary atom site location: structure-invariant direct methods |
Least-squares matrix: full | Secondary atom site location: difference Fourier map |
R[F2 > 2σ(F2)] = 0.036 | Hydrogen site location: inferred from neighbouring sites |
wR(F2) = 0.107 | H-atom parameters constrained |
S = 1.06 | w = 1/[σ2(Fo2) + (0.0619P)2 + 7.0981P] where P = (Fo2 + 2Fc2)/3 |
5387 reflections | (Δ/σ)max = 0.008 |
334 parameters | Δρmax = 1.40 e Å−3 |
0 restraints | Δρmin = −0.71 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 | Occ. (<1) |
Tl1 | 0.28328 (3) | 0.332297 (19) | 0.216643 (16) | 0.02379 (9) | |
O2 | 0.5308 (5) | 0.3244 (3) | 0.0935 (3) | 0.0169 (7) | |
N3 | 0.6610 (5) | 0.2355 (4) | 0.0680 (3) | 0.0125 (8) | |
C4 | 0.7749 (7) | 0.2003 (5) | 0.1315 (4) | 0.0221 (12) | |
H13 | 0.7641 | 0.2391 | 0.1939 | 0.027* | |
C5 | 0.9073 (7) | 0.1084 (5) | 0.1067 (4) | 0.0230 (12) | |
H11 | 0.9854 | 0.0840 | 0.1528 | 0.028* | |
C6 | 0.9284 (6) | 0.0500 (4) | 0.0138 (4) | 0.0122 (9) | |
C7 | 0.8097 (8) | 0.0918 (5) | −0.0517 (5) | 0.0267 (13) | |
H10 | 0.8207 | 0.0568 | −0.1160 | 0.032* | |
C8 | 0.6766 (8) | 0.1837 (6) | −0.0237 (4) | 0.0265 (13) | |
H9 | 0.5966 | 0.2104 | −0.0683 | 0.032* | |
N10 | 0.2004 (5) | 0.3662 (4) | −0.0251 (3) | 0.0129 (8) | |
C11 | 0.2190 (9) | 0.2653 (5) | −0.0750 (4) | 0.0269 (13) | |
H15 | 0.1954 | 0.1977 | −0.0372 | 0.032* | |
C12 | 0.2724 (9) | 0.2611 (5) | −0.1811 (4) | 0.0234 (12) | |
H16 | 0.2857 | 0.1906 | −0.2153 | 0.028* | |
C13 | 0.3066 (6) | 0.3607 (4) | −0.2373 (4) | 0.0117 (9) | |
C14 | 0.2934 (8) | 0.4608 (5) | −0.1823 (4) | 0.0191 (11) | |
H18 | 0.3213 | 0.5286 | −0.2178 | 0.023* | |
C15 | 0.2400 (8) | 0.4620 (5) | −0.0764 (4) | 0.0202 (11) | |
H19 | 0.2314 | 0.5305 | −0.0401 | 0.024* | |
N17 | 0.4218 (5) | 0.3693 (4) | 0.4334 (3) | 0.0113 (8) | |
C18 | 0.4871 (7) | 0.2734 (5) | 0.4857 (4) | 0.0170 (10) | |
H2 | 0.5566 | 0.2096 | 0.4491 | 0.020* | |
C19 | 0.4527 (7) | 0.2677 (5) | 0.5939 (4) | 0.0170 (10) | |
H3 | 0.4983 | 0.2000 | 0.6299 | 0.020* | |
C20 | 0.3508 (6) | 0.3622 (4) | 0.6486 (4) | 0.0108 (9) | |
C21 | 0.2858 (7) | 0.4606 (5) | 0.5910 (4) | 0.0152 (10) | |
H5 | 0.2177 | 0.5263 | 0.6255 | 0.018* | |
C22 | 0.3211 (7) | 0.4617 (5) | 0.4843 (4) | 0.0159 (10) | |
H7 | 0.2747 | 0.5275 | 0.4464 | 0.019* | |
O23 | −0.0125 (5) | 0.2907 (4) | 0.2745 (3) | 0.0256 (9) | |
O24 | −0.1221 (5) | 0.2574 (4) | 0.4340 (4) | 0.0311 (10) | |
O25 | 0.1455 (5) | 0.2756 (4) | 0.3931 (3) | 0.0250 (9) | |
N26 | 0.0001 (6) | 0.2730 (4) | 0.3692 (4) | 0.0167 (9) | |
O27 | 0.3141 (5) | 0.5367 (3) | 0.1608 (3) | 0.0230 (8) | |
O28 | 0.1457 (11) | 0.6900 (5) | 0.2320 (7) | 0.083 (3) | |
O29 | 0.1045 (5) | 0.5171 (4) | 0.2843 (3) | 0.0235 (8) | |
N30 | 0.1871 (7) | 0.5840 (4) | 0.2259 (4) | 0.0286 (11) | |
O31 | 0.3054 (6) | 0.1376 (4) | 0.1429 (4) | 0.0303 (10) | |
O32 | 0.4716 (7) | −0.0228 (4) | 0.1857 (5) | 0.0473 (14) | |
O33 | 0.4545 (6) | 0.1396 (4) | 0.2633 (4) | 0.0278 (9) | |
N34 | 0.4129 (6) | 0.0805 (4) | 0.1975 (4) | 0.0241 (10) | |
Cl1A | 1.1264 (3) | −0.0437 (2) | 0.35456 (18) | 0.0591 (6) | |
C1A | 0.9417 (10) | −0.1052 (7) | 0.3953 (7) | 0.0451 (19) | |
H1A | 0.9606 | −0.1831 | 0.3666 | 0.054* | |
H2A | 0.9216 | −0.1137 | 0.4713 | 0.054* | |
Cl2A | 0.7590 (3) | −0.01826 (16) | 0.35498 (17) | 0.0464 (4) | |
O9A | 0.1385 (15) | 0.386 (4) | 0.0758 (9) | 0.010 (5)* | 0.40 (12) |
O16A | 0.447 (3) | 0.390 (3) | 0.3284 (8) | 0.005 (4)* | 0.40 (11) |
O9B | 0.1370 (10) | 0.360 (3) | 0.0763 (6) | 0.011 (3)* | 0.60 (12) |
O16B | 0.4660 (19) | 0.364 (2) | 0.3306 (6) | 0.008 (3)* | 0.60 (11) |
Atomic displacement parameters (Å2) top | U11 | U22 | U33 | U12 | U13 | U23 |
Tl1 | 0.02515 (14) | 0.02800 (14) | 0.01757 (13) | −0.00431 (9) | −0.00189 (8) | −0.00267 (8) |
O2 | 0.0138 (17) | 0.0150 (17) | 0.0157 (18) | 0.0023 (14) | 0.0091 (14) | −0.0030 (14) |
N3 | 0.0132 (19) | 0.0121 (19) | 0.0096 (19) | −0.0022 (16) | 0.0064 (15) | −0.0043 (15) |
C4 | 0.017 (3) | 0.032 (3) | 0.018 (3) | 0.001 (2) | −0.003 (2) | −0.019 (2) |
C5 | 0.019 (3) | 0.033 (3) | 0.016 (3) | 0.003 (2) | −0.005 (2) | −0.016 (2) |
C6 | 0.014 (2) | 0.014 (2) | 0.009 (2) | −0.002 (2) | 0.0011 (18) | −0.0064 (17) |
C7 | 0.031 (3) | 0.029 (3) | 0.015 (3) | 0.013 (3) | −0.008 (2) | −0.015 (2) |
C8 | 0.026 (3) | 0.035 (3) | 0.013 (3) | 0.012 (3) | −0.007 (2) | −0.010 (2) |
N10 | 0.0131 (19) | 0.021 (2) | 0.0047 (18) | −0.0031 (17) | −0.0020 (15) | −0.0002 (15) |
C11 | 0.051 (4) | 0.021 (3) | 0.011 (3) | −0.016 (3) | −0.002 (2) | 0.002 (2) |
C12 | 0.049 (4) | 0.015 (2) | 0.008 (2) | −0.008 (2) | −0.005 (2) | 0.0004 (19) |
C13 | 0.012 (2) | 0.015 (2) | 0.007 (2) | −0.0011 (18) | −0.0013 (17) | −0.0002 (17) |
C14 | 0.033 (3) | 0.017 (2) | 0.008 (2) | −0.011 (2) | 0.001 (2) | −0.0026 (19) |
C15 | 0.032 (3) | 0.017 (2) | 0.010 (2) | −0.002 (2) | −0.001 (2) | −0.0047 (19) |
N17 | 0.0117 (19) | 0.021 (2) | 0.0026 (17) | −0.0075 (16) | 0.0015 (14) | −0.0043 (15) |
C18 | 0.018 (2) | 0.021 (3) | 0.010 (2) | 0.000 (2) | −0.0005 (19) | −0.0054 (19) |
C19 | 0.022 (3) | 0.016 (2) | 0.009 (2) | 0.004 (2) | −0.0012 (19) | −0.0011 (18) |
C20 | 0.011 (2) | 0.016 (2) | 0.005 (2) | −0.0037 (18) | −0.0008 (17) | −0.0015 (17) |
C21 | 0.018 (2) | 0.018 (2) | 0.007 (2) | 0.0023 (19) | 0.0020 (18) | −0.0031 (18) |
C22 | 0.021 (3) | 0.016 (2) | 0.009 (2) | −0.001 (2) | −0.0015 (19) | 0.0018 (18) |
O23 | 0.022 (2) | 0.046 (3) | 0.0131 (19) | −0.0152 (19) | −0.0071 (15) | 0.0012 (17) |
O24 | 0.0150 (19) | 0.044 (3) | 0.029 (2) | −0.0073 (18) | 0.0078 (17) | 0.013 (2) |
O25 | 0.0170 (19) | 0.047 (3) | 0.0146 (19) | −0.0153 (18) | −0.0057 (15) | 0.0105 (17) |
N26 | 0.013 (2) | 0.015 (2) | 0.020 (2) | −0.0020 (16) | 0.0004 (17) | 0.0019 (17) |
O27 | 0.027 (2) | 0.0200 (19) | 0.0176 (19) | −0.0008 (16) | 0.0036 (16) | 0.0005 (15) |
O28 | 0.104 (6) | 0.016 (3) | 0.100 (6) | 0.006 (3) | 0.043 (5) | −0.004 (3) |
O29 | 0.021 (2) | 0.023 (2) | 0.022 (2) | 0.0005 (16) | 0.0058 (16) | −0.0046 (16) |
N30 | 0.033 (3) | 0.018 (2) | 0.029 (3) | 0.005 (2) | −0.001 (2) | −0.001 (2) |
O31 | 0.039 (3) | 0.017 (2) | 0.039 (3) | −0.0033 (18) | −0.018 (2) | −0.0049 (18) |
O32 | 0.050 (3) | 0.016 (2) | 0.077 (4) | 0.009 (2) | −0.025 (3) | −0.015 (2) |
O33 | 0.033 (2) | 0.020 (2) | 0.031 (2) | 0.0040 (17) | −0.0145 (19) | −0.0016 (17) |
N34 | 0.019 (2) | 0.018 (2) | 0.035 (3) | −0.0040 (19) | −0.002 (2) | −0.003 (2) |
Cl1A | 0.0447 (11) | 0.0765 (15) | 0.0506 (12) | −0.0073 (10) | −0.0023 (9) | 0.0129 (11) |
C1A | 0.047 (4) | 0.037 (4) | 0.045 (4) | 0.003 (3) | −0.008 (4) | 0.014 (3) |
Cl2A | 0.0552 (11) | 0.0329 (9) | 0.0539 (11) | −0.0008 (8) | −0.0242 (9) | −0.0022 (8) |
Geometric parameters (Å, º) top
Tl1—O2 | 2.320 (3) | C13—C14 | 1.387 (7) |
Tl1—O9B | 2.324 (8) | C13—C20ii | 1.472 (6) |
Tl1—O9A | 2.340 (12) | C14—C15 | 1.376 (7) |
Tl1—O16A | 2.343 (10) | C14—H18 | 0.940 |
Tl1—O16B | 2.361 (8) | C15—H19 | 0.940 |
Tl1—O29 | 2.467 (4) | N17—O16B | 1.330 (8) |
Tl1—O31 | 2.487 (4) | N17—C18 | 1.344 (7) |
Tl1—O25 | 2.488 (4) | N17—C22 | 1.349 (7) |
Tl1—O23 | 2.497 (4) | N17—O16A | 1.366 (14) |
Tl1—O27 | 2.501 (4) | C18—C19 | 1.392 (7) |
Tl1—O33 | 2.502 (4) | C18—H2 | 0.940 |
O2—N3 | 1.334 (5) | C19—C20 | 1.393 (7) |
N3—C4 | 1.334 (7) | C19—H3 | 0.940 |
N3—C8 | 1.351 (7) | C20—C21 | 1.401 (7) |
C4—C5 | 1.367 (8) | C20—C13iii | 1.472 (6) |
C4—H13 | 0.940 | C21—C22 | 1.373 (7) |
C5—C6 | 1.397 (7) | C21—H5 | 0.940 |
C5—H11 | 0.940 | C22—H7 | 0.940 |
C6—C7 | 1.394 (8) | O23—N26 | 1.263 (6) |
C6—C6i | 1.484 (9) | O24—N26 | 1.214 (6) |
C7—C8 | 1.376 (8) | O25—N26 | 1.269 (6) |
C7—H10 | 0.940 | O27—N30 | 1.266 (7) |
C8—H9 | 0.940 | O28—N30 | 1.222 (8) |
N10—C15 | 1.333 (7) | O29—N30 | 1.260 (7) |
N10—O9B | 1.337 (9) | O31—N34 | 1.279 (7) |
N10—O9A | 1.342 (14) | O32—N34 | 1.216 (7) |
N10—C11 | 1.353 (7) | O33—N34 | 1.262 (7) |
C11—C12 | 1.379 (8) | Cl1A—C1A | 1.760 (9) |
C11—H15 | 0.940 | C1A—Cl2A | 1.759 (8) |
C12—C13 | 1.386 (7) | C1A—H1A | 0.980 |
C12—H16 | 0.940 | C1A—H2A | 0.980 |
| | | |
O2—Tl1—O9B | 85.8 (2) | C6—C7—H10 | 119.5 |
O2—Tl1—O9A | 84.8 (3) | N3—C8—C7 | 119.9 (5) |
O9B—Tl1—O9A | 7.6 (5) | N3—C8—H9 | 120.0 |
O2—Tl1—O16A | 84.6 (3) | C7—C8—H9 | 120.0 |
O9B—Tl1—O16A | 153.4 (11) | C15—N10—O9B | 125.1 (14) |
O9A—Tl1—O16A | 146.0 (14) | C15—N10—O9A | 112 (2) |
O2—Tl1—O16B | 83.0 (2) | C15—N10—C11 | 120.9 (4) |
O9B—Tl1—O16B | 159.5 (9) | O9B—N10—C11 | 114.0 (14) |
O9A—Tl1—O16B | 152.5 (12) | O9A—N10—C11 | 127 (2) |
O16A—Tl1—O16B | 7.8 (4) | N10—C11—C12 | 120.4 (5) |
O2—Tl1—O29 | 123.04 (13) | N10—C11—H15 | 119.8 |
O9B—Tl1—O29 | 87.7 (6) | C12—C11—H15 | 119.8 |
O9A—Tl1—O29 | 81.9 (9) | C11—C12—C13 | 120.0 (5) |
O16A—Tl1—O29 | 77.1 (9) | C11—C12—H16 | 120.0 |
O16B—Tl1—O29 | 84.2 (7) | C13—C12—H16 | 120.0 |
O2—Tl1—O31 | 79.31 (15) | C12—C13—C14 | 117.6 (5) |
O9B—Tl1—O31 | 72.4 (8) | C12—C13—C20ii | 121.7 (4) |
O9A—Tl1—O31 | 79.7 (11) | C14—C13—C20ii | 120.7 (4) |
O16A—Tl1—O31 | 129.5 (10) | C15—C14—C13 | 120.9 (5) |
O16B—Tl1—O31 | 121.7 (7) | C15—C14—H18 | 119.6 |
O29—Tl1—O31 | 149.49 (15) | C13—C14—H18 | 119.6 |
O2—Tl1—O25 | 148.48 (14) | N10—C15—C14 | 120.1 (5) |
O9B—Tl1—O25 | 122.0 (4) | N10—C15—H19 | 120.0 |
O9A—Tl1—O25 | 124.7 (5) | C14—C15—H19 | 120.0 |
O16A—Tl1—O25 | 75.8 (3) | O16B—N17—C18 | 114.5 (13) |
O16B—Tl1—O25 | 74.2 (2) | O16B—N17—C22 | 124.7 (13) |
O29—Tl1—O25 | 76.51 (15) | C18—N17—C22 | 120.8 (4) |
O31—Tl1—O25 | 94.31 (17) | C18—N17—O16A | 127.9 (17) |
O2—Tl1—O23 | 151.05 (14) | C22—N17—O16A | 111.3 (17) |
O9B—Tl1—O23 | 70.9 (4) | N17—C18—C19 | 120.5 (5) |
O9A—Tl1—O23 | 74.2 (6) | N17—C18—H2 | 119.7 |
O16A—Tl1—O23 | 123.8 (3) | C19—C18—H2 | 119.7 |
O16B—Tl1—O23 | 124.2 (2) | C18—C19—C20 | 120.0 (5) |
O29—Tl1—O23 | 74.14 (15) | C18—C19—H3 | 120.0 |
O31—Tl1—O23 | 77.51 (16) | C20—C19—H3 | 120.0 |
O25—Tl1—O23 | 51.15 (13) | C19—C20—C21 | 117.6 (4) |
O2—Tl1—O27 | 71.78 (13) | C19—C20—C13iii | 122.6 (4) |
O9B—Tl1—O27 | 79.4 (8) | C21—C20—C13iii | 119.7 (4) |
O9A—Tl1—O27 | 71.9 (11) | C22—C21—C20 | 120.4 (5) |
O16A—Tl1—O27 | 74.1 (9) | C22—C21—H5 | 119.8 |
O16B—Tl1—O27 | 80.9 (6) | C20—C21—H5 | 119.8 |
O29—Tl1—O27 | 51.43 (13) | N17—C22—C21 | 120.7 (5) |
O31—Tl1—O27 | 140.75 (15) | N17—C22—H7 | 119.6 |
O25—Tl1—O27 | 124.04 (15) | C21—C22—H7 | 119.6 |
O23—Tl1—O27 | 118.31 (15) | N26—O23—Tl1 | 96.0 (3) |
O2—Tl1—O33 | 78.98 (15) | N26—O25—Tl1 | 96.3 (3) |
O9B—Tl1—O33 | 123.0 (7) | O24—N26—O23 | 121.5 (5) |
O9A—Tl1—O33 | 129.9 (10) | O24—N26—O25 | 122.1 (5) |
O16A—Tl1—O33 | 79.2 (10) | O23—N26—O25 | 116.4 (4) |
O16B—Tl1—O33 | 71.4 (7) | N30—O27—Tl1 | 94.8 (3) |
O29—Tl1—O33 | 145.28 (14) | N30—O29—Tl1 | 96.6 (3) |
O31—Tl1—O33 | 50.90 (14) | O28—N30—O29 | 121.2 (6) |
O25—Tl1—O33 | 73.34 (15) | O28—N30—O27 | 121.7 (6) |
O23—Tl1—O33 | 99.21 (16) | O29—N30—O27 | 117.2 (5) |
O27—Tl1—O33 | 141.73 (15) | N34—O31—Tl1 | 97.1 (3) |
N3—O2—Tl1 | 129.9 (3) | N34—O33—Tl1 | 96.9 (3) |
C4—N3—O2 | 120.2 (4) | O32—N34—O33 | 122.8 (5) |
C4—N3—C8 | 121.0 (5) | O32—N34—O31 | 122.1 (5) |
O2—N3—C8 | 118.9 (4) | O33—N34—O31 | 115.1 (5) |
N3—C4—C5 | 120.5 (5) | Cl2A—C1A—Cl1A | 111.6 (4) |
N3—C4—H13 | 119.7 | Cl2A—C1A—H1A | 109.3 |
C5—C4—H13 | 119.7 | Cl1A—C1A—H1A | 109.3 |
C4—C5—C6 | 121.1 (5) | Cl2A—C1A—H2A | 109.3 |
C4—C5—H11 | 119.4 | Cl1A—C1A—H2A | 109.3 |
C6—C5—H11 | 119.4 | H1A—C1A—H2A | 108.0 |
C7—C6—C5 | 116.5 (5) | N10—O9A—Tl1 | 127.3 (11) |
C7—C6—C6i | 122.0 (5) | N17—O16A—Tl1 | 123.8 (8) |
C5—C6—C6i | 121.6 (6) | N10—O9B—Tl1 | 128.8 (6) |
C8—C7—C6 | 120.9 (5) | N17—O16B—Tl1 | 124.7 (5) |
C8—C7—H10 | 119.5 | | |
Symmetry codes: (i) −x+2, −y, −z; (ii) x, y, z−1; (iii) x, y, z+1. |
Hydrogen-bond geometry (Å, º) top
D—H···A | D—H | H···A | D···A | D—H···A |
C1A—H1A···O28iv | 0.98 | 2.46 | 3.292 (11) | 143 |
C1A—H2A···O24v | 0.98 | 2.52 | 3.148 (9) | 122 |
C1A—H2A···O25v | 0.98 | 2.58 | 3.362 (9) | 137 |
C4—H13···O23vi | 0.94 | 2.42 | 3.100 (7) | 129 |
C12—H16···O32vii | 0.94 | 2.55 | 3.119 (8) | 120 |
C14—H18···O16Aviii | 0.94 | 2.45 | 3.260 (17) | 144 |
Symmetry codes: (iv) x+1, y−1, z; (v) −x+1, −y, −z+1; (vi) x+1, y, z; (vii) −x+1, −y, −z; (viii) −x+1, −y+1, −z. |
Subscribe to Acta Crystallographica Section E: Crystallographic Communications
The full text of this article is available to subscribers to the journal.
If you have already registered and are using a computer listed in your registration details, please email
support@iucr.org for assistance.