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metal-organic compounds
S. T. Liddle and W. Clegg
The title compound, catena-poly[[caesium(I)-μ-18-crown-6-caesium(I)-di-μ-2-amidopyridine] toluene], [{[Cs{2-N(H)C5H4N}]2(C12H24O6)·(C6H5CH3)}∞] or [Cs2(C5H5N2)2(C12H24O6)]·C7H8, crystallizes as a toluene solvate. The polymeric structure is constructed from dimeric amido-bridged Cs2N2 four-membered rings with additional supporting coordination by bridging pyridyl N atoms. Each dimeric unit is linked to the next in the polymeric chain by bridging κ6:κ6 18-crown-6 ether molecules, in which each of the six O atoms bonds to both caesium ions; each caesium is ten-coordinate. The polymer has crystallographic mirror (Cs) symmetry, the mirror running through all the caesium ions, so that there is only one unique amidopyridine ligand and each crown ligand is bisected by the mirror. Consequently, the amide ligands are arranged cis with respect to each other, which is unusual.
Supporting information
Crystallographic Information File (CIF) https://doi.org/10.1107/S1600536803023821/bt6368sup1.cif | |
Structure factor file (CIF format) https://doi.org/10.1107/S1600536803023821/bt6368Isup2.hkl |
CCDC reference: 226670
Key indicators
- Single-crystal X-ray study
- T = 160 K
- Mean (C-C) = 0.016 Å
- R factor = 0.028
- wR factor = 0.065
- Data-to-parameter ratio = 19.3
checkCIF/PLATON results
No syntax errors found
Alert level A PLAT063_ALERT_3_A Crystal Probably too Large for Beam Size ....... 1.30 mm PLAT213_ALERT_2_A Atom C8 has ADP max/min Ratio ............. 6.10 prolat
Alert level B CRYSS02_ALERT_3_B The value of _exptl_crystal_size_max is > 1.0 Maximum crystal size given = 1.300 PLAT241_ALERT_2_B Check High U(eq) as Compared to Neighbors .... C10 PLAT242_ALERT_2_B Check Low U(eq) as Compared to Neighbors .... Cs2 PLAT353_ALERT_3_B Long N-H Bond (0.87A) N2 - H2N = 1.10 Ang. PLAT415_ALERT_2_B Short Inter D-H..H-X H2N .. H16A = 2.06 Ang. PLAT415_ALERT_2_B Short Inter D-H..H-X H2N .. H16D = 2.09 Ang.
Alert level C STRVA01_ALERT_4_C Flack test results are ambiguous. From the CIF: _refine_ls_abs_structure_Flack 0.460 From the CIF: _refine_ls_abs_structure_Flack_su 0.040 PLAT033_ALERT_2_C Flack Parameter Value Deviates from Zero ....... 0.46 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 PLAT125_ALERT_4_C No _symmetry_space_group_name_Hall Given ....... ? PLAT213_ALERT_2_C Atom O3 has ADP max/min Ratio ............. 3.30 prolat PLAT213_ALERT_2_C Atom C7 has ADP max/min Ratio ............. 3.40 prolat PLAT222_ALERT_3_C Large Non-Solvent H Ueq(max)/Ueq(min) ... 3.95 Ratio PLAT241_ALERT_2_C Check High U(eq) as Compared to Neighbors .... C4 PLAT241_ALERT_2_C Check High U(eq) as Compared to Neighbors .... C9 PLAT242_ALERT_2_C Check Low U(eq) as Compared to Neighbors .... Cs1 PLAT244_ALERT_4_C Low Solvent U(eq) as Compared to Neighbors .... C12 PLAT250_ALERT_2_C Large U3/U1 ratio for average U(i,j) tensor .... 2.51 PLAT342_ALERT_3_C Low Bond Precision on C-C bonds (x 1000) Ang ... 16 PLAT369_ALERT_2_C Long C(sp2)-C(sp2) Bond C4 - C5 = 1.56 Ang. PLAT420_ALERT_2_C D-H Without Acceptor N2 - H2N ... ? PLAT731_ALERT_1_C Bond Calc 1.350(17), Rep 1.350(8) ...... 2.12 su-Rat N1 -C5 1.555 1.555 PLAT731_ALERT_1_C Bond Calc 1.48(2), Rep 1.483(9) ...... 2.22 su-Rat C8 -C9 1.555 1.555 PLAT764_ALERT_4_C Overcomplete CIF Bond list Detected (Rep/Expd) . 1.12 Ratio
Alert level G REFLT03_ALERT_4_G Please check that the estimate of the number of Friedel pairs is correct. If it is not, please give the correct count in the _publ_section_exptl_refinement section of the submitted CIF. From the CIF: _diffrn_reflns_theta_max 28.51 From the CIF: _reflns_number_total 3879 Count of symmetry unique reflns 2223 Completeness (_total/calc) 174.49% TEST3: Check Friedels for noncentro structure Estimate of Friedel pairs measured 1656 Fraction of Friedel pairs measured 0.745 Are heavy atom types Z>Si present yes
2 ALERT level A = In general: serious problem 6 ALERT level B = Potentially serious problem 20 ALERT level C = Check and explain 1 ALERT level G = General alerts; check 5 ALERT type 1 CIF construction/syntax error, inconsistent or missing data 14 ALERT type 2 Indicator that the structure model may be wrong or deficient 5 ALERT type 3 Indicator that the structure quality may be low 5 ALERT type 4 Improvement, methodology, query or suggestion
Computing details top
Data collection: SMART (Bruker, 2001); cell refinement: SAINT (Bruker, 2001); data reduction: SAINT; program(s) used to solve structure: SHELXTL (Sheldrick, 2001); program(s) used to refine structure: SHELXTL; molecular graphics: SHELXTL; software used to prepare material for publication: SHELXTL and local programs.
catena-poly[[caesium(I)-µ-18-crown-6-caesium(I)-di-µ-2-amidopyridine]
toluene] top
Crystal data top
[Cs2(C5H5N2)2(C12H24O6)]·C7H8 | F(000) = 804 |
Mr = 808.49 | Dx = 1.592 Mg m−3 |
Monoclinic, Cm | Mo Kα radiation, λ = 0.71073 Å |
a = 13.0109 (10) Å | Cell parameters from 5667 reflections |
b = 17.3720 (14) Å | θ = 2.4–28.4° |
c = 7.8427 (6) Å | µ = 2.21 mm−1 |
β = 107.979 (2)° | T = 160 K |
V = 1686.1 (2) Å3 | Needle, yellow |
Z = 2 | 1.30 × 0.22 × 0.12 mm |
Data collection top
Bruker SMART 1K CCD diffractometer | 3879 independent reflections |
Radiation source: sealed tube | 2911 reflections with I > 2σ(I) |
Graphite monochromator | Rint = 0.025 |
Detector resolution: 8.192 pixels mm-1 | θmax = 28.5°, θmin = 2.0° |
thin–slice ω scans | h = −17→16 |
Absorption correction: multi-scan (SADABS; Sheldrick, 2002) | k = −22→23 |
Tmin = 0.478, Tmax = 0.768 | l = −10→10 |
7390 measured 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)] = 0.028 | H atoms treated by a mixture of independent and constrained refinement |
wR(F2) = 0.065 | w = 1/[σ2(Fo2) + (0.03P)2] where P = (Fo2 + 2Fc2)/3 |
S = 0.94 | (Δ/σ)max = 0.038 |
3879 reflections | Δρmax = 0.81 e Å−3 |
201 parameters | Δρmin = −0.53 e Å−3 |
65 restraints | Absolute structure: Flack (1983) |
Primary atom site location: structure-invariant direct methods | Absolute structure parameter: 0.46 (4) |
Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top
x | y | z | Uiso*/Ueq | Occ. (<1) | |
Cs1 | 0.54337 (3) | 0.5000 | 0.55808 (5) | 0.0412 (3) | |
Cs2 | 0.53181 (3) | 0.5000 | 1.04501 (4) | 0.0398 (2) | |
N1 | 0.5867 (9) | 0.6431 (5) | 0.3252 (12) | 0.056 (2) | |
N2 | 0.4028 (4) | 0.6085 (3) | 0.2416 (6) | 0.0515 (12) | |
H2N | 0.322 (4) | 0.635 (3) | 0.191 (6) | 0.037 (13)* | |
C1 | 0.6594 (6) | 0.6920 (4) | 0.3401 (8) | 0.0607 (17) | |
H1 | 0.7316 | 0.6754 | 0.3591 | 0.073* | |
C2 | 0.6372 (10) | 0.7678 (5) | 0.3297 (17) | 0.077 (2) | |
H2 | 0.6950 | 0.8033 | 0.3462 | 0.092* | |
C3 | 0.5353 (13) | 0.7953 (3) | 0.296 (2) | 0.0702 (15) | |
H3 | 0.5223 | 0.8491 | 0.2859 | 0.084* | |
C4 | 0.4519 (10) | 0.7457 (5) | 0.2780 (14) | 0.077 (3) | |
H4 | 0.3803 | 0.7633 | 0.2608 | 0.092* | |
C5 | 0.4802 (9) | 0.6582 (6) | 0.2867 (13) | 0.051 (2) | |
O1 | 0.7602 (10) | 0.5000 | 0.9015 (16) | 0.081 (4) | |
O2 | 0.6388 (8) | 0.6418 (4) | 0.8835 (12) | 0.074 (2) | |
O3 | 0.4197 (7) | 0.6345 (4) | 0.7223 (9) | 0.0673 (19) | |
O4 | 0.3166 (8) | 0.5000 | 0.7064 (15) | 0.076 (3) | |
C6 | 0.8016 (9) | 0.5711 (7) | 0.9845 (16) | 0.091 (3) | |
H6A | 0.8804 | 0.5728 | 1.0038 | 0.109* | |
H6B | 0.7901 | 0.5736 | 1.1034 | 0.109* | |
C7 | 0.7501 (10) | 0.6398 (7) | 0.8767 (16) | 0.097 (3) | |
H7A | 0.7890 | 0.6874 | 0.9286 | 0.117* | |
H7B | 0.7508 | 0.6348 | 0.7513 | 0.117* | |
C8 | 0.6008 (13) | 0.7062 (5) | 0.7947 (13) | 0.099 (3) | |
H8A | 0.6020 | 0.7046 | 0.6692 | 0.118* | |
H8B | 0.6395 | 0.7525 | 0.8556 | 0.118* | |
C9 | 0.4897 (13) | 0.7008 (6) | 0.8073 (16) | 0.109 (4) | |
H9A | 0.4954 | 0.7009 | 0.9361 | 0.131* | |
H9B | 0.4511 | 0.7486 | 0.7549 | 0.131* | |
C10 | 0.3123 (10) | 0.6290 (9) | 0.716 (2) | 0.122 (4) | |
H10A | 0.2738 | 0.6767 | 0.6635 | 0.146* | |
H10B | 0.3083 | 0.6242 | 0.8400 | 0.146* | |
C11 | 0.2592 (11) | 0.5630 (8) | 0.6108 (18) | 0.114 (4) | |
H11A | 0.1819 | 0.5606 | 0.6037 | 0.137* | |
H11B | 0.2649 | 0.5650 | 0.4879 | 0.137* | |
C12 | 0.5908 (8) | 1.0000 | 0.9116 (16) | 0.072 (3) | |
C13 | 0.5411 (14) | 0.9324 (4) | 0.826 (2) | 0.081 (3) | |
H13 | 0.5612 | 0.8844 | 0.8855 | 0.097* | |
C14 | 0.4648 (7) | 0.9335 (5) | 0.6611 (12) | 0.094 (3) | |
H14 | 0.4398 | 0.8850 | 0.6088 | 0.113* | |
C15 | 0.4190 (12) | 1.0000 | 0.559 (3) | 0.096 (5) | |
H15 | 0.3669 | 1.0000 | 0.4437 | 0.115* | |
C16 | 0.6800 (16) | 1.0000 | 1.069 (2) | 0.155 (9) | |
H16A | 0.7024 | 1.0531 | 1.1033 | 0.232* | 0.25 |
H16B | 0.7400 | 0.9716 | 1.0483 | 0.232* | 0.25 |
H16C | 0.6594 | 0.9752 | 1.1664 | 0.232* | 0.25 |
H16D | 0.6988 | 0.9469 | 1.1087 | 0.232* | 0.25 |
H16E | 0.6612 | 1.0284 | 1.1637 | 0.232* | 0.25 |
H16F | 0.7418 | 1.0248 | 1.0456 | 0.232* | 0.25 |
Atomic displacement parameters (Å2) top
U11 | U22 | U33 | U12 | U13 | U23 | |
Cs1 | 0.0662 (7) | 0.0356 (4) | 0.0282 (6) | 0.000 | 0.0239 (5) | 0.000 |
Cs2 | 0.0638 (7) | 0.0361 (4) | 0.0232 (5) | 0.000 | 0.0190 (5) | 0.000 |
N1 | 0.072 (4) | 0.072 (4) | 0.027 (4) | −0.015 (3) | 0.019 (4) | 0.004 (3) |
N2 | 0.053 (3) | 0.066 (3) | 0.037 (2) | −0.004 (2) | 0.015 (2) | −0.003 (2) |
C1 | 0.059 (4) | 0.082 (5) | 0.042 (3) | −0.014 (3) | 0.019 (3) | 0.003 (3) |
C2 | 0.115 (5) | 0.068 (5) | 0.054 (5) | 0.002 (5) | 0.036 (5) | −0.008 (4) |
C3 | 0.127 (4) | 0.037 (3) | 0.051 (3) | 0.014 (6) | 0.034 (3) | 0.016 (6) |
C4 | 0.107 (6) | 0.085 (6) | 0.037 (5) | −0.013 (5) | 0.020 (5) | −0.005 (5) |
C5 | 0.056 (5) | 0.083 (6) | 0.023 (4) | −0.039 (5) | 0.024 (4) | −0.018 (4) |
O1 | 0.077 (8) | 0.127 (8) | 0.036 (7) | 0.000 | 0.013 (6) | 0.000 |
O2 | 0.137 (6) | 0.038 (3) | 0.062 (5) | 0.000 (4) | 0.050 (4) | −0.001 (3) |
O3 | 0.117 (5) | 0.062 (4) | 0.033 (3) | 0.062 (4) | 0.038 (3) | 0.012 (3) |
O4 | 0.028 (5) | 0.154 (8) | 0.045 (8) | 0.000 | 0.010 (5) | 0.000 |
C6 | 0.037 (4) | 0.180 (9) | 0.050 (6) | −0.045 (5) | 0.004 (4) | −0.020 (6) |
C7 | 0.125 (6) | 0.127 (7) | 0.033 (5) | −0.105 (5) | 0.013 (5) | −0.006 (5) |
C8 | 0.248 (8) | 0.025 (5) | 0.042 (6) | −0.040 (5) | 0.073 (7) | 0.001 (4) |
C9 | 0.207 (8) | 0.051 (7) | 0.070 (8) | 0.041 (5) | 0.045 (8) | 0.034 (6) |
C10 | 0.121 (8) | 0.173 (10) | 0.065 (8) | 0.074 (7) | 0.020 (7) | −0.023 (8) |
C11 | 0.080 (7) | 0.201 (11) | 0.062 (8) | 0.053 (6) | 0.023 (6) | −0.007 (7) |
C12 | 0.065 (6) | 0.067 (7) | 0.094 (7) | 0.000 | 0.037 (5) | 0.000 |
C13 | 0.102 (5) | 0.047 (3) | 0.114 (8) | −0.010 (6) | 0.063 (5) | −0.003 (5) |
C14 | 0.087 (6) | 0.097 (7) | 0.100 (6) | −0.005 (5) | 0.029 (4) | −0.014 (5) |
C15 | 0.058 (8) | 0.058 (8) | 0.179 (16) | 0.000 | 0.048 (8) | 0.000 |
C16 | 0.119 (14) | 0.26 (3) | 0.084 (10) | 0.000 | 0.031 (8) | 0.000 |
Geometric parameters (Å, º) top
Cs1—N1 | 3.235 (9) | O2—C7 | 1.465 (10) |
Cs1—N1i | 3.235 (9) | O2—C8 | 1.330 (9) |
Cs1—N2 | 3.202 (5) | O3—C9 | 1.492 (11) |
Cs1—N2i | 3.202 (5) | O3—C10 | 1.387 (11) |
Cs1—O1 | 3.243 (12) | O4—C11 | 1.404 (10) |
Cs1—O2 | 3.488 (8) | O4—C11i | 1.404 (10) |
Cs1—O2i | 3.488 (8) | C6—H6A | 0.990 |
Cs1—O3 | 3.315 (6) | C6—H6B | 0.990 |
Cs1—O3i | 3.315 (6) | C6—C7 | 1.496 (10) |
Cs1—O4 | 3.490 (10) | C7—H7A | 0.990 |
Cs2—N1ii | 3.247 (9) | C7—H7B | 0.990 |
Cs2—N1iii | 3.247 (9) | C8—H8A | 0.990 |
Cs2—N2iii | 3.216 (5) | C8—H8B | 0.990 |
Cs2—N2ii | 3.216 (5) | C8—C9 | 1.483 (9) |
Cs2—O1 | 3.487 (13) | C9—H9A | 0.990 |
Cs2—O2 | 3.272 (8) | C9—H9B | 0.990 |
Cs2—O2i | 3.272 (8) | C10—H10A | 0.990 |
Cs2—O3 | 3.423 (6) | C10—H10B | 0.990 |
Cs2—O3i | 3.423 (6) | C10—C11 | 1.458 (12) |
Cs2—O4 | 3.210 (10) | C11—H11A | 0.990 |
N1—Cs2iv | 3.247 (9) | C11—H11B | 0.990 |
N1—C1 | 1.250 (11) | C12—C13 | 1.406 (10) |
N1—C5 | 1.350 (8) | C12—C13v | 1.406 (10) |
N2—Cs2iv | 3.216 (5) | C12—C16 | 1.41 (2) |
N2—H2N | 1.11 (5) | C13—H13 | 0.950 |
N2—C5 | 1.289 (10) | C13—C14 | 1.368 (16) |
C1—H1 | 0.950 | C14—H14 | 0.950 |
C1—C2 | 1.344 (10) | C14—C15 | 1.426 (14) |
C2—H2 | 0.950 | C15—C14v | 1.426 (14) |
C2—C3 | 1.358 (11) | C15—H15 | 0.950 |
C3—H3 | 0.950 | C16—H16A | 0.980 |
C3—C4 | 1.357 (10) | C16—H16B | 0.980 |
C4—H4 | 0.950 | C16—H16C | 0.980 |
C4—C5 | 1.562 (11) | C16—H16D | 0.980 |
O1—C6 | 1.422 (9) | C16—H16E | 0.980 |
O1—C6i | 1.422 (9) | C16—H16F | 0.980 |
N1—Cs1—N1i | 100.4 (3) | N1—C1—C2 | 121.2 (10) |
N1—Cs1—N2 | 42.9 (2) | H1—C1—C2 | 119.4 |
N1i—Cs1—N2i | 42.9 (2) | C1—C2—H2 | 118.8 |
N1i—Cs1—N2 | 99.90 (18) | C1—C2—C3 | 122.3 (9) |
N1—Cs1—N2i | 99.90 (18) | H2—C2—C3 | 118.8 |
N1—Cs1—O1 | 102.1 (2) | C2—C3—H3 | 120.0 |
N1i—Cs1—O1 | 102.1 (2) | C2—C3—C4 | 119.9 (6) |
N1—Cs1—O2 | 77.6 (2) | H3—C3—C4 | 120.0 |
N1i—Cs1—O2 | 150.6 (2) | C3—C4—H4 | 121.8 |
N1i—Cs1—O2i | 77.6 (2) | C3—C4—C5 | 116.3 (8) |
N1—Cs1—O2i | 150.6 (2) | H4—C4—C5 | 121.8 |
N1—Cs1—O3 | 82.4 (2) | N1—C5—N2 | 126.3 (11) |
N1i—Cs1—O3i | 82.4 (2) | N1—C5—C4 | 114.3 (9) |
N1—Cs1—O3i | 162.0 (2) | N2—C5—C4 | 119.1 (10) |
N1i—Cs1—O3 | 162.0 (2) | Cs1—O1—Cs2 | 70.0 (2) |
N1—Cs1—O4 | 120.1 (2) | Cs1—O1—C6 | 119.3 (6) |
N1i—Cs1—O4 | 120.1 (2) | Cs1—O1—C6i | 119.3 (6) |
N2—Cs1—N2i | 72.11 (17) | Cs2—O1—C6 | 95.3 (7) |
N2—Cs1—O1 | 141.79 (11) | Cs2—O1—C6i | 95.3 (7) |
N2i—Cs1—O1 | 141.79 (11) | C6—O1—C6i | 120.5 (13) |
N2—Cs1—O2 | 98.08 (15) | Cs1—O2—Cs2 | 69.72 (16) |
N2i—Cs1—O2 | 166.39 (17) | Cs1—O2—C7 | 95.1 (6) |
N2i—Cs1—O2i | 98.08 (16) | Cs1—O2—C8 | 102.7 (7) |
N2—Cs1—O2i | 166.39 (17) | Cs2—O2—C7 | 122.6 (6) |
N2—Cs1—O3 | 69.92 (14) | Cs2—O2—C8 | 134.6 (9) |
N2i—Cs1—O3i | 69.92 (15) | C7—O2—C8 | 102.3 (11) |
N2—Cs1—O3i | 119.11 (19) | Cs1—O3—Cs2 | 70.05 (12) |
N2i—Cs1—O3 | 119.11 (19) | Cs1—O3—C9 | 114.6 (8) |
N2—Cs1—O4 | 85.36 (17) | Cs1—O3—C10 | 122.9 (8) |
N2i—Cs1—O4 | 85.36 (17) | Cs2—O3—C9 | 97.8 (6) |
O1—Cs1—O2 | 50.99 (17) | Cs2—O3—C10 | 99.9 (8) |
O1—Cs1—O2i | 50.99 (17) | C9—O3—C10 | 122.5 (10) |
O1—Cs1—O3 | 94.6 (2) | Cs1—O4—Cs2 | 70.38 (19) |
O1—Cs1—O3i | 94.6 (2) | Cs1—O4—C11 | 100.8 (7) |
O1—Cs1—O4 | 109.3 (3) | Cs1—O4—C11i | 100.8 (7) |
O2—Cs1—O2i | 89.9 (3) | Cs2—O4—C11 | 128.8 (7) |
O2—Cs1—O3 | 47.45 (14) | Cs2—O4—C11i | 128.8 (7) |
O2—Cs1—O3i | 108.6 (2) | C11—O4—C11i | 102.4 (14) |
O2i—Cs1—O3i | 47.45 (14) | O1—C6—H6A | 109.0 |
O2i—Cs1—O3 | 108.6 (2) | O1—C6—H6B | 108.9 |
O2—Cs1—O4 | 84.4 (2) | O1—C6—C7 | 113.2 (8) |
O2i—Cs1—O4 | 84.4 (2) | H6A—C6—H6B | 107.8 |
O3—Cs1—O3i | 89.7 (3) | H6A—C6—C7 | 108.9 |
O3—Cs1—O4 | 46.27 (17) | H6B—C6—C7 | 109.0 |
O3i—Cs1—O4 | 46.27 (17) | O2—C7—C6 | 105.9 (8) |
N1ii—Cs2—N1iii | 99.9 (3) | O2—C7—H7A | 110.6 |
N1ii—Cs2—N2iii | 99.34 (19) | O2—C7—H7B | 110.6 |
N1ii—Cs2—N2ii | 42.7 (2) | C6—C7—H7A | 110.6 |
N1iii—Cs2—N2iii | 42.7 (2) | C6—C7—H7B | 110.5 |
N1iii—Cs2—N2ii | 99.34 (19) | H7A—C7—H7B | 108.7 |
N1ii—Cs2—O1 | 100.8 (2) | O2—C8—H8A | 112.3 |
N1iii—Cs2—O1 | 100.8 (2) | O2—C8—H8B | 112.3 |
N1ii—Cs2—O2 | 69.8 (2) | O2—C8—C9 | 97.2 (10) |
N1iii—Cs2—O2 | 143.8 (2) | H8A—C8—H8B | 109.9 |
N1ii—Cs2—O2i | 143.8 (2) | H8A—C8—C9 | 112.3 |
N1iii—Cs2—O2i | 69.8 (2) | H8B—C8—C9 | 112.3 |
N1ii—Cs2—O3i | 167.8 (2) | Cs2—C9—O3 | 60.1 (5) |
N1iii—Cs2—O3i | 86.1 (2) | Cs2—C9—C8 | 95.2 (7) |
N1ii—Cs2—O3 | 86.1 (2) | Cs2—C9—H9A | 63.8 |
N1iii—Cs2—O3 | 167.8 (2) | Cs2—C9—H9B | 157.3 |
N1ii—Cs2—O4 | 120.9 (2) | O3—C9—C8 | 119.5 (11) |
N1iii—Cs2—O4 | 120.9 (2) | O3—C9—H9A | 107.5 |
N2iii—Cs2—N2ii | 71.75 (18) | O3—C9—H9B | 107.5 |
N2iii—Cs2—O1 | 141.03 (11) | C8—C9—H9A | 107.5 |
N2ii—Cs2—O1 | 141.03 (12) | C8—C9—H9B | 107.5 |
N2iii—Cs2—O2 | 167.02 (16) | H9A—C9—H9B | 107.0 |
N2ii—Cs2—O2 | 95.27 (18) | O3—C10—H10A | 109.3 |
N2iii—Cs2—O2i | 95.27 (18) | O3—C10—H10B | 109.3 |
N2ii—Cs2—O2i | 167.02 (16) | O3—C10—C11 | 111.7 (11) |
N2iii—Cs2—O3i | 77.76 (14) | H10A—C10—H10B | 108.0 |
N2ii—Cs2—O3i | 126.04 (19) | H10A—C10—C11 | 109.3 |
N2iii—Cs2—O3 | 126.04 (19) | H10B—C10—C11 | 109.3 |
N2ii—Cs2—O3 | 77.76 (14) | O4—C11—C10 | 103.3 (10) |
N2iii—Cs2—O4 | 86.87 (18) | O4—C11—H11A | 111.1 |
N2ii—Cs2—O4 | 86.87 (17) | O4—C11—H11B | 111.1 |
O1—Cs2—O2 | 50.80 (16) | C10—C11—H11A | 111.1 |
O1—Cs2—O2i | 50.80 (16) | C10—C11—H11B | 111.1 |
O1—Cs2—O3 | 88.4 (2) | H11A—C11—H11B | 109.1 |
O1—Cs2—O3i | 88.4 (2) | C13—C12—C13v | 113.3 (14) |
O1—Cs2—O4 | 110.2 (3) | C13—C12—C16 | 123.3 (7) |
O2—Cs2—O2i | 97.7 (3) | C13v—C12—C16 | 123.3 (7) |
O2—Cs2—O3 | 48.29 (15) | C12—C13—H13 | 119.0 |
O2—Cs2—O3i | 111.3 (2) | C12—C13—C14 | 122.1 (10) |
O2i—Cs2—O3i | 48.29 (15) | H13—C13—C14 | 119.0 |
O2i—Cs2—O3 | 111.3 (2) | C13—C14—H14 | 116.7 |
O2—Cs2—O4 | 92.7 (2) | C13—C14—C15 | 126.7 (11) |
O2i—Cs2—O4 | 92.7 (2) | H14—C14—C15 | 116.7 |
O3—Cs2—O3i | 86.1 (3) | C14—C15—C14v | 108.2 (16) |
O3—Cs2—O4 | 47.51 (17) | C14—C15—H15 | 125.9 |
O3i—Cs2—O4 | 47.51 (17) | C14v—C15—H15 | 125.9 |
Cs1—N1—Cs2iv | 75.75 (19) | C12—C16—H16A | 109.5 |
Cs1—N1—C1 | 136.8 (7) | C12—C16—H16B | 109.5 |
Cs1—N1—C5 | 86.0 (6) | C12—C16—H16C | 109.5 |
Cs2iv—N1—C1 | 125.9 (7) | C12—C16—H16D | 109.5 |
Cs2iv—N1—C5 | 90.1 (6) | C12—C16—H16E | 109.5 |
C1—N1—C5 | 125.7 (11) | C12—C16—H16F | 109.5 |
Cs1—N2—Cs2iv | 76.64 (11) | H16A—C16—H16B | 109.5 |
Cs1—N2—H2N | 141 (3) | H16A—C16—H16C | 109.5 |
Cs1—N2—C5 | 88.3 (6) | H16B—C16—H16C | 109.5 |
Cs2iv—N2—H2N | 131 (2) | H16D—C16—H16E | 109.5 |
Cs2iv—N2—C5 | 92.6 (6) | H16D—C16—H16F | 109.5 |
H2N—N2—C5 | 114 (3) | H16E—C16—H16F | 109.5 |
N1—C1—H1 | 119.4 |
Symmetry codes: (i) x, −y+1, z; (ii) x, y, z+1; (iii) x, −y+1, z+1; (iv) x, y, z−1; (v) x, −y+2, z. |
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