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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

cif

Crystallographic Information File (CIF) https://doi.org/10.1107/S1600536806005095/cf6492sup1.cif
Contains datablocks global, I

hkl

Structure factor file (CIF format) https://doi.org/10.1107/S1600536806005095/cf6492Isup2.hkl
Contains datablock I

CCDC reference: 601134

Key indicators

  • Single-crystal X-ray study
  • T = 203 K
  • Mean [sigma](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

Computing details top

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(µ2-4,4'-bipyridine N,N'-dioxide)bis[trinitratothallium(III)]] dichloromethane disolvate] top
Crystal data top
[Tl2(NO3)6(C10H8N2O2)3]·2CH2Cl2Z = 1
Mr = 1515.22F(000) = 726
Triclinic, P1Dx = 2.121 Mg m3
Hall symbol: -P 1Mo Kα radiation, λ = 0.71073 Å
a = 8.0425 (16) ÅCell parameters from 35318 reflections
b = 11.687 (2) Åθ = 1.0–27.5°
c = 13.079 (3) ŵ = 7.11 mm1
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 tube4847 reflections with I > 2σ(I)
Graphite monochromatorRint = 0.038
ω and φ scansθmax = 27.5°, θmin = 3.6°
Absorption correction: multi-scan
(SADABS; Sheldrick, 2001)
h = 1010
Tmin = 0.435, Tmax = 0.560k = 1515
35318 measured reflectionsl = 1616
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)] = 0.036Hydrogen site location: inferred from neighbouring sites
wR(F2) = 0.107H-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 parametersΔρmax = 1.40 e Å3
0 restraintsΔρmin = 0.71 e Å3
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
xyzUiso*/UeqOcc. (<1)
Tl10.28328 (3)0.332297 (19)0.216643 (16)0.02379 (9)
O20.5308 (5)0.3244 (3)0.0935 (3)0.0169 (7)
N30.6610 (5)0.2355 (4)0.0680 (3)0.0125 (8)
C40.7749 (7)0.2003 (5)0.1315 (4)0.0221 (12)
H130.76410.23910.19390.027*
C50.9073 (7)0.1084 (5)0.1067 (4)0.0230 (12)
H110.98540.08400.15280.028*
C60.9284 (6)0.0500 (4)0.0138 (4)0.0122 (9)
C70.8097 (8)0.0918 (5)0.0517 (5)0.0267 (13)
H100.82070.05680.11600.032*
C80.6766 (8)0.1837 (6)0.0237 (4)0.0265 (13)
H90.59660.21040.06830.032*
N100.2004 (5)0.3662 (4)0.0251 (3)0.0129 (8)
C110.2190 (9)0.2653 (5)0.0750 (4)0.0269 (13)
H150.19540.19770.03720.032*
C120.2724 (9)0.2611 (5)0.1811 (4)0.0234 (12)
H160.28570.19060.21530.028*
C130.3066 (6)0.3607 (4)0.2373 (4)0.0117 (9)
C140.2934 (8)0.4608 (5)0.1823 (4)0.0191 (11)
H180.32130.52860.21780.023*
C150.2400 (8)0.4620 (5)0.0764 (4)0.0202 (11)
H190.23140.53050.04010.024*
N170.4218 (5)0.3693 (4)0.4334 (3)0.0113 (8)
C180.4871 (7)0.2734 (5)0.4857 (4)0.0170 (10)
H20.55660.20960.44910.020*
C190.4527 (7)0.2677 (5)0.5939 (4)0.0170 (10)
H30.49830.20000.62990.020*
C200.3508 (6)0.3622 (4)0.6486 (4)0.0108 (9)
C210.2858 (7)0.4606 (5)0.5910 (4)0.0152 (10)
H50.21770.52630.62550.018*
C220.3211 (7)0.4617 (5)0.4843 (4)0.0159 (10)
H70.27470.52750.44640.019*
O230.0125 (5)0.2907 (4)0.2745 (3)0.0256 (9)
O240.1221 (5)0.2574 (4)0.4340 (4)0.0311 (10)
O250.1455 (5)0.2756 (4)0.3931 (3)0.0250 (9)
N260.0001 (6)0.2730 (4)0.3692 (4)0.0167 (9)
O270.3141 (5)0.5367 (3)0.1608 (3)0.0230 (8)
O280.1457 (11)0.6900 (5)0.2320 (7)0.083 (3)
O290.1045 (5)0.5171 (4)0.2843 (3)0.0235 (8)
N300.1871 (7)0.5840 (4)0.2259 (4)0.0286 (11)
O310.3054 (6)0.1376 (4)0.1429 (4)0.0303 (10)
O320.4716 (7)0.0228 (4)0.1857 (5)0.0473 (14)
O330.4545 (6)0.1396 (4)0.2633 (4)0.0278 (9)
N340.4129 (6)0.0805 (4)0.1975 (4)0.0241 (10)
Cl1A1.1264 (3)0.0437 (2)0.35456 (18)0.0591 (6)
C1A0.9417 (10)0.1052 (7)0.3953 (7)0.0451 (19)
H1A0.96060.18310.36660.054*
H2A0.92160.11370.47130.054*
Cl2A0.7590 (3)0.01826 (16)0.35498 (17)0.0464 (4)
O9A0.1385 (15)0.386 (4)0.0758 (9)0.010 (5)*0.40 (12)
O16A0.447 (3)0.390 (3)0.3284 (8)0.005 (4)*0.40 (11)
O9B0.1370 (10)0.360 (3)0.0763 (6)0.011 (3)*0.60 (12)
O16B0.4660 (19)0.364 (2)0.3306 (6)0.008 (3)*0.60 (11)
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
Tl10.02515 (14)0.02800 (14)0.01757 (13)0.00431 (9)0.00189 (8)0.00267 (8)
O20.0138 (17)0.0150 (17)0.0157 (18)0.0023 (14)0.0091 (14)0.0030 (14)
N30.0132 (19)0.0121 (19)0.0096 (19)0.0022 (16)0.0064 (15)0.0043 (15)
C40.017 (3)0.032 (3)0.018 (3)0.001 (2)0.003 (2)0.019 (2)
C50.019 (3)0.033 (3)0.016 (3)0.003 (2)0.005 (2)0.016 (2)
C60.014 (2)0.014 (2)0.009 (2)0.002 (2)0.0011 (18)0.0064 (17)
C70.031 (3)0.029 (3)0.015 (3)0.013 (3)0.008 (2)0.015 (2)
C80.026 (3)0.035 (3)0.013 (3)0.012 (3)0.007 (2)0.010 (2)
N100.0131 (19)0.021 (2)0.0047 (18)0.0031 (17)0.0020 (15)0.0002 (15)
C110.051 (4)0.021 (3)0.011 (3)0.016 (3)0.002 (2)0.002 (2)
C120.049 (4)0.015 (2)0.008 (2)0.008 (2)0.005 (2)0.0004 (19)
C130.012 (2)0.015 (2)0.007 (2)0.0011 (18)0.0013 (17)0.0002 (17)
C140.033 (3)0.017 (2)0.008 (2)0.011 (2)0.001 (2)0.0026 (19)
C150.032 (3)0.017 (2)0.010 (2)0.002 (2)0.001 (2)0.0047 (19)
N170.0117 (19)0.021 (2)0.0026 (17)0.0075 (16)0.0015 (14)0.0043 (15)
C180.018 (2)0.021 (3)0.010 (2)0.000 (2)0.0005 (19)0.0054 (19)
C190.022 (3)0.016 (2)0.009 (2)0.004 (2)0.0012 (19)0.0011 (18)
C200.011 (2)0.016 (2)0.005 (2)0.0037 (18)0.0008 (17)0.0015 (17)
C210.018 (2)0.018 (2)0.007 (2)0.0023 (19)0.0020 (18)0.0031 (18)
C220.021 (3)0.016 (2)0.009 (2)0.001 (2)0.0015 (19)0.0018 (18)
O230.022 (2)0.046 (3)0.0131 (19)0.0152 (19)0.0071 (15)0.0012 (17)
O240.0150 (19)0.044 (3)0.029 (2)0.0073 (18)0.0078 (17)0.013 (2)
O250.0170 (19)0.047 (3)0.0146 (19)0.0153 (18)0.0057 (15)0.0105 (17)
N260.013 (2)0.015 (2)0.020 (2)0.0020 (16)0.0004 (17)0.0019 (17)
O270.027 (2)0.0200 (19)0.0176 (19)0.0008 (16)0.0036 (16)0.0005 (15)
O280.104 (6)0.016 (3)0.100 (6)0.006 (3)0.043 (5)0.004 (3)
O290.021 (2)0.023 (2)0.022 (2)0.0005 (16)0.0058 (16)0.0046 (16)
N300.033 (3)0.018 (2)0.029 (3)0.005 (2)0.001 (2)0.001 (2)
O310.039 (3)0.017 (2)0.039 (3)0.0033 (18)0.018 (2)0.0049 (18)
O320.050 (3)0.016 (2)0.077 (4)0.009 (2)0.025 (3)0.015 (2)
O330.033 (2)0.020 (2)0.031 (2)0.0040 (17)0.0145 (19)0.0016 (17)
N340.019 (2)0.018 (2)0.035 (3)0.0040 (19)0.002 (2)0.003 (2)
Cl1A0.0447 (11)0.0765 (15)0.0506 (12)0.0073 (10)0.0023 (9)0.0129 (11)
C1A0.047 (4)0.037 (4)0.045 (4)0.003 (3)0.008 (4)0.014 (3)
Cl2A0.0552 (11)0.0329 (9)0.0539 (11)0.0008 (8)0.0242 (9)0.0022 (8)
Geometric parameters (Å, º) top
Tl1—O22.320 (3)C13—C141.387 (7)
Tl1—O9B2.324 (8)C13—C20ii1.472 (6)
Tl1—O9A2.340 (12)C14—C151.376 (7)
Tl1—O16A2.343 (10)C14—H180.940
Tl1—O16B2.361 (8)C15—H190.940
Tl1—O292.467 (4)N17—O16B1.330 (8)
Tl1—O312.487 (4)N17—C181.344 (7)
Tl1—O252.488 (4)N17—C221.349 (7)
Tl1—O232.497 (4)N17—O16A1.366 (14)
Tl1—O272.501 (4)C18—C191.392 (7)
Tl1—O332.502 (4)C18—H20.940
O2—N31.334 (5)C19—C201.393 (7)
N3—C41.334 (7)C19—H30.940
N3—C81.351 (7)C20—C211.401 (7)
C4—C51.367 (8)C20—C13iii1.472 (6)
C4—H130.940C21—C221.373 (7)
C5—C61.397 (7)C21—H50.940
C5—H110.940C22—H70.940
C6—C71.394 (8)O23—N261.263 (6)
C6—C6i1.484 (9)O24—N261.214 (6)
C7—C81.376 (8)O25—N261.269 (6)
C7—H100.940O27—N301.266 (7)
C8—H90.940O28—N301.222 (8)
N10—C151.333 (7)O29—N301.260 (7)
N10—O9B1.337 (9)O31—N341.279 (7)
N10—O9A1.342 (14)O32—N341.216 (7)
N10—C111.353 (7)O33—N341.262 (7)
C11—C121.379 (8)Cl1A—C1A1.760 (9)
C11—H150.940C1A—Cl2A1.759 (8)
C12—C131.386 (7)C1A—H1A0.980
C12—H160.940C1A—H2A0.980
O2—Tl1—O9B85.8 (2)C6—C7—H10119.5
O2—Tl1—O9A84.8 (3)N3—C8—C7119.9 (5)
O9B—Tl1—O9A7.6 (5)N3—C8—H9120.0
O2—Tl1—O16A84.6 (3)C7—C8—H9120.0
O9B—Tl1—O16A153.4 (11)C15—N10—O9B125.1 (14)
O9A—Tl1—O16A146.0 (14)C15—N10—O9A112 (2)
O2—Tl1—O16B83.0 (2)C15—N10—C11120.9 (4)
O9B—Tl1—O16B159.5 (9)O9B—N10—C11114.0 (14)
O9A—Tl1—O16B152.5 (12)O9A—N10—C11127 (2)
O16A—Tl1—O16B7.8 (4)N10—C11—C12120.4 (5)
O2—Tl1—O29123.04 (13)N10—C11—H15119.8
O9B—Tl1—O2987.7 (6)C12—C11—H15119.8
O9A—Tl1—O2981.9 (9)C11—C12—C13120.0 (5)
O16A—Tl1—O2977.1 (9)C11—C12—H16120.0
O16B—Tl1—O2984.2 (7)C13—C12—H16120.0
O2—Tl1—O3179.31 (15)C12—C13—C14117.6 (5)
O9B—Tl1—O3172.4 (8)C12—C13—C20ii121.7 (4)
O9A—Tl1—O3179.7 (11)C14—C13—C20ii120.7 (4)
O16A—Tl1—O31129.5 (10)C15—C14—C13120.9 (5)
O16B—Tl1—O31121.7 (7)C15—C14—H18119.6
O29—Tl1—O31149.49 (15)C13—C14—H18119.6
O2—Tl1—O25148.48 (14)N10—C15—C14120.1 (5)
O9B—Tl1—O25122.0 (4)N10—C15—H19120.0
O9A—Tl1—O25124.7 (5)C14—C15—H19120.0
O16A—Tl1—O2575.8 (3)O16B—N17—C18114.5 (13)
O16B—Tl1—O2574.2 (2)O16B—N17—C22124.7 (13)
O29—Tl1—O2576.51 (15)C18—N17—C22120.8 (4)
O31—Tl1—O2594.31 (17)C18—N17—O16A127.9 (17)
O2—Tl1—O23151.05 (14)C22—N17—O16A111.3 (17)
O9B—Tl1—O2370.9 (4)N17—C18—C19120.5 (5)
O9A—Tl1—O2374.2 (6)N17—C18—H2119.7
O16A—Tl1—O23123.8 (3)C19—C18—H2119.7
O16B—Tl1—O23124.2 (2)C18—C19—C20120.0 (5)
O29—Tl1—O2374.14 (15)C18—C19—H3120.0
O31—Tl1—O2377.51 (16)C20—C19—H3120.0
O25—Tl1—O2351.15 (13)C19—C20—C21117.6 (4)
O2—Tl1—O2771.78 (13)C19—C20—C13iii122.6 (4)
O9B—Tl1—O2779.4 (8)C21—C20—C13iii119.7 (4)
O9A—Tl1—O2771.9 (11)C22—C21—C20120.4 (5)
O16A—Tl1—O2774.1 (9)C22—C21—H5119.8
O16B—Tl1—O2780.9 (6)C20—C21—H5119.8
O29—Tl1—O2751.43 (13)N17—C22—C21120.7 (5)
O31—Tl1—O27140.75 (15)N17—C22—H7119.6
O25—Tl1—O27124.04 (15)C21—C22—H7119.6
O23—Tl1—O27118.31 (15)N26—O23—Tl196.0 (3)
O2—Tl1—O3378.98 (15)N26—O25—Tl196.3 (3)
O9B—Tl1—O33123.0 (7)O24—N26—O23121.5 (5)
O9A—Tl1—O33129.9 (10)O24—N26—O25122.1 (5)
O16A—Tl1—O3379.2 (10)O23—N26—O25116.4 (4)
O16B—Tl1—O3371.4 (7)N30—O27—Tl194.8 (3)
O29—Tl1—O33145.28 (14)N30—O29—Tl196.6 (3)
O31—Tl1—O3350.90 (14)O28—N30—O29121.2 (6)
O25—Tl1—O3373.34 (15)O28—N30—O27121.7 (6)
O23—Tl1—O3399.21 (16)O29—N30—O27117.2 (5)
O27—Tl1—O33141.73 (15)N34—O31—Tl197.1 (3)
N3—O2—Tl1129.9 (3)N34—O33—Tl196.9 (3)
C4—N3—O2120.2 (4)O32—N34—O33122.8 (5)
C4—N3—C8121.0 (5)O32—N34—O31122.1 (5)
O2—N3—C8118.9 (4)O33—N34—O31115.1 (5)
N3—C4—C5120.5 (5)Cl2A—C1A—Cl1A111.6 (4)
N3—C4—H13119.7Cl2A—C1A—H1A109.3
C5—C4—H13119.7Cl1A—C1A—H1A109.3
C4—C5—C6121.1 (5)Cl2A—C1A—H2A109.3
C4—C5—H11119.4Cl1A—C1A—H2A109.3
C6—C5—H11119.4H1A—C1A—H2A108.0
C7—C6—C5116.5 (5)N10—O9A—Tl1127.3 (11)
C7—C6—C6i122.0 (5)N17—O16A—Tl1123.8 (8)
C5—C6—C6i121.6 (6)N10—O9B—Tl1128.8 (6)
C8—C7—C6120.9 (5)N17—O16B—Tl1124.7 (5)
C8—C7—H10119.5
Symmetry codes: (i) x+2, y, z; (ii) x, y, z1; (iii) x, y, z+1.
Hydrogen-bond geometry (Å, º) top
D—H···AD—HH···AD···AD—H···A
C1A—H1A···O28iv0.982.463.292 (11)143
C1A—H2A···O24v0.982.523.148 (9)122
C1A—H2A···O25v0.982.583.362 (9)137
C4—H13···O23vi0.942.423.100 (7)129
C12—H16···O32vii0.942.553.119 (8)120
C14—H18···O16Aviii0.942.453.260 (17)144
Symmetry codes: (iv) x+1, y1, z; (v) x+1, y, z+1; (vi) x+1, y, z; (vii) x+1, y, z; (viii) x+1, y+1, z.
 

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