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In coordination chemistry and crystal engineering, many factors influence the construction of coordination polymers and the final frameworks depend greatly on the organic ligands used. The diverse coordination modes of N-donor ligands have been employed to assemble metal–organic frameworks. Carb­oxy­lic acid ligands can deprotonate completely or partially when bonding to metal ions and can also act as donors or acceptors of hydrogen bonds; they are thus good candidates for the construction of supra­molecular architectures. We synthesized under reflux or hydro­thermal conditions two new alkaline earth(II) complexes, namely poly[(1,10-phenanthroline-κ2N,N′)bis­(μ-3-phenyl­prop-2-enoato-κ3O,O′:O)calcium(II)], [Ca(C10H7O2)2(C10H8N2)]n, (1), and poly[(1,10-phenanthroline-κ2N,N′)(μ3-3-phenyl­prop-2-enoato-κ4O:O,O′:O′)(μ-3-phenyl­prop-2-enoato-κ3O,O′:O)barium(II)], [Ba(C10H7O2)2(C10H8N2)]n, (2), and characterized them by FT–IR and UV–Vis spectroscopies, thermogravimetric analysis (TGA) and single-crystal X-ray diffraction analysis, as well as by powder X-ray diffraction (PXRD) analysis. Complex (1) features a chain topology of type 2,4 C4, where the Ca atoms are connected by O and N atoms, forming a distorted bicapped trigonal prismatic geometry. Complex (2) displays chains of topology type 2,3,5 C4, where the Ba atom is nine-coordinated by seven O atoms of bridging/chelating carboxyl­ate groups from two cinnamate ligands and by two N atoms from one phenanthroline ligand, forming a distorted tricapped prismatic arrangement. Weak C—H...O hydrogen bonds and π–π stacking inter­actions between phenanthroline ligands are responsible to the formation of a supra­molecular three-dimensional network. The thermal decompositions of (1) and (2) in the temperature range 297–1173 K revealed that they both decompose in three steps and transform to the corresponding metal oxide.

Supporting information

cif

Crystallographic Information File (CIF) https://doi.org/10.1107/S2053229618001420/fp3050sup1.cif
Contains datablocks Ca, Ba, global

hkl

Structure factor file (CIF format) https://doi.org/10.1107/S2053229618001420/fp3050Casup3.hkl
Contains datablock Ca

pdf

Portable Document Format (PDF) file https://doi.org/10.1107/S2053229618001420/fp3050sup4.pdf
IR/TG/UV/PXRD plots and schematics of the connected nets

hkl

Structure factor file (CIF format) https://doi.org/10.1107/S2053229618001420/fp3050Basup2.hkl
Contains datablock Ba

CCDC references: 1818540; 1818539

Computing details top

For both structures, data collection: APEX2 (Bruker, 2011); cell refinement: APEX2 (Bruker, 2011); data reduction: APEX2 (Bruker, 2011); program(s) used to solve structure: SIR2002 (Burla et al., 2005). Program(s) used to refine structure: SHELXL97 (Sheldrick, 2008) for Ca; SHELXT (Sheldrick, 2015) for Ba. For both structures, molecular graphics: ORTEP-3 for Windows (Farrugia, 2012) and DIAMOND (Brandenburg & Berndt, 2001); software used to prepare material for publication: WinGX (Farrugia, 2012) and CRYSCAL (T. Roisnel, local program).

Poly[(1,10-phenanthroline-κ2N,N')bis(µ-3-phenylprop-2-enoato-κ3O,O':O)calcium(I)] (Ca) top
Crystal data top
[Ca(C10H7O2)2(C10H8N2)]F(000) = 1072
Mr = 514.58Dx = 1.414 Mg m3
Orthorhombic, PbcnMo Kα radiation, λ = 0.71073 Å
Hall symbol: -P 2n 2abCell parameters from 1362 reflections
a = 27.0933 (11) Åθ = 3.0–23.0°
b = 11.2988 (4) ŵ = 0.30 mm1
c = 7.8989 (3) ÅT = 295 K
V = 2418.03 (16) Å3Prism, colorless
Z = 40.25 × 0.17 × 0.15 mm
Data collection top
Bruker APEXII
diffractometer
1617 reflections with I > 2σ(I)
Graphite monochromatorRint = 0.061
CCD rotation images, thick slices scansθmax = 27°, θmin = 3.2°
Absorption correction: multi-scan
(SADABS; Sheldrick, 2002)
h = 3134
Tmin = 0.672, Tmax = 0.746k = 1014
10605 measured reflectionsl = 1010
2587 independent reflections
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)] = 0.051Hydrogen site location: inferred from neighbouring sites
wR(F2) = 0.146H-atom parameters constrained
S = 1.04 w = 1/[σ2(Fo2) + (0.0695P)2 + 0.1557P]
where P = (Fo2 + 2Fc2)/3
2585 reflections(Δ/σ)max < 0.001
168 parametersΔρmax = 0.28 e Å3
0 restraintsΔρmin = 0.20 e Å3
Special details top

Geometry. All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds 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 > 2sigma(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*/Ueq
C10.07507 (9)0.5961 (2)0.3964 (3)0.0418 (6)
C20.11192 (10)0.6796 (2)0.4654 (4)0.0515 (7)
H20.10310.72240.56130.062*
C30.15583 (10)0.6980 (2)0.4023 (4)0.0484 (7)
H30.16480.65140.31030.058*
C40.19290 (9)0.7848 (2)0.4610 (3)0.0411 (6)
C50.18367 (10)0.8693 (2)0.5833 (3)0.0521 (7)
H50.15330.86970.63820.063*
C60.21802 (13)0.9519 (3)0.6248 (4)0.0641 (9)
H60.21041.00930.7050.077*
C70.26384 (12)0.9521 (3)0.5506 (4)0.0644 (9)
H70.28711.0090.58010.077*
C80.27482 (10)0.8667 (3)0.4316 (4)0.0639 (9)
H80.3060.86410.38210.077*
C90.23904 (10)0.7846 (2)0.3862 (4)0.0534 (7)
H90.24620.72840.30380.064*
C110.02276 (9)0.1500 (2)0.2029 (3)0.0436 (6)
C120.04485 (12)0.0408 (2)0.1608 (4)0.0552 (8)
C130.08922 (13)0.0451 (3)0.0717 (4)0.0711 (10)
H130.10560.02490.04530.085*
C140.10861 (11)0.1497 (3)0.0234 (4)0.0686 (9)
H140.13780.15250.03820.082*
C150.08385 (10)0.2544 (3)0.0679 (4)0.0554 (7)
H150.09720.32630.03310.066*
C160.02101 (12)0.0679 (3)0.2095 (4)0.0712 (11)
H160.03590.13970.18260.085*
Ca100.44729 (6)0.250.0390 (2)
N10.04254 (8)0.25573 (18)0.1570 (3)0.0456 (6)
O10.03319 (6)0.59409 (17)0.4666 (2)0.0552 (5)
O20.08423 (8)0.53279 (18)0.2711 (3)0.0637 (6)
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
C10.0369 (13)0.0426 (14)0.0458 (15)0.0012 (11)0.0001 (12)0.0045 (12)
C20.0469 (16)0.0558 (16)0.0519 (17)0.0055 (13)0.0015 (13)0.0011 (13)
C30.0457 (15)0.0458 (15)0.0538 (16)0.0014 (12)0.0004 (13)0.0009 (13)
C40.0362 (13)0.0403 (13)0.0467 (15)0.0007 (11)0.0037 (11)0.0055 (12)
C50.0473 (15)0.0578 (17)0.0513 (16)0.0050 (13)0.0051 (13)0.0004 (14)
C60.076 (2)0.0515 (17)0.065 (2)0.0042 (16)0.0192 (18)0.0078 (15)
C70.064 (2)0.0546 (18)0.074 (2)0.0212 (16)0.0251 (17)0.0180 (17)
C80.0399 (16)0.079 (2)0.073 (2)0.0069 (15)0.0026 (14)0.0232 (19)
C90.0468 (16)0.0526 (16)0.0609 (18)0.0019 (13)0.0017 (14)0.0041 (13)
C110.0465 (15)0.0457 (15)0.0387 (14)0.0031 (12)0.0144 (12)0.0030 (11)
C120.0640 (19)0.0530 (16)0.0488 (17)0.0115 (15)0.0191 (15)0.0087 (13)
C130.072 (2)0.073 (2)0.068 (2)0.0259 (18)0.0170 (18)0.0219 (18)
C140.0492 (17)0.094 (3)0.062 (2)0.0184 (18)0.0006 (15)0.0211 (19)
C150.0433 (15)0.069 (2)0.0535 (17)0.0035 (14)0.0000 (13)0.0019 (14)
C160.095 (3)0.0459 (16)0.072 (2)0.0126 (14)0.029 (2)0.0073 (15)
Ca10.0344 (4)0.0420 (4)0.0407 (4)00.0027 (3)0
N10.0407 (12)0.0518 (13)0.0444 (13)0.0033 (10)0.0026 (10)0.0017 (10)
O10.0445 (11)0.0700 (12)0.0512 (11)0.0057 (9)0.0077 (9)0.0002 (9)
O20.0552 (12)0.0676 (13)0.0682 (14)0.0123 (10)0.0097 (10)0.0243 (11)
Geometric parameters (Å, º) top
C1—O21.246 (3)C11—C11i1.440 (5)
C1—O11.263 (3)C12—C131.394 (4)
C1—C21.478 (4)C12—C161.439 (4)
C1—Ca12.881 (3)C13—C141.349 (5)
C2—C31.307 (4)C13—H130.93
C2—H20.93C14—C151.405 (4)
C3—C41.478 (3)C14—H140.93
C3—H30.93C15—N11.322 (3)
C4—C51.381 (4)C15—H150.93
C4—C91.383 (4)C16—C16i1.306 (7)
C5—C61.358 (4)C16—H160.93
C5—H50.93Ca1—O1ii2.4575 (19)
C6—C71.373 (5)Ca1—O1iii2.4575 (19)
C6—H60.93Ca1—O12.5468 (19)
C7—C81.380 (5)Ca1—O1i2.5468 (19)
C7—H70.93Ca1—O2i2.484 (2)
C8—C91.389 (4)Ca1—O22.484 (2)
C8—H80.93Ca1—N12.560 (2)
C9—H90.93Ca1—N1i2.560 (2)
C11—N11.359 (3)Ca1—C1i2.881 (3)
C11—C121.411 (4)O1—Ca1ii2.4575 (19)
O2—C1—O1121.1 (2)O2—Ca1—O1i96.67 (7)
O2—C1—C2121.7 (2)O1—Ca1—O1i98.72 (9)
O1—C1—C2117.2 (2)O1ii—Ca1—N186.31 (7)
O2—C1—Ca159.13 (14)O1iii—Ca1—N175.08 (6)
O1—C1—Ca162.06 (13)O2i—Ca1—N184.03 (7)
C2—C1—Ca1175.95 (18)O2—Ca1—N1139.63 (7)
C3—C2—C1125.2 (3)O1—Ca1—N1154.47 (6)
C3—C2—H2117.4O1i—Ca1—N1101.48 (6)
C1—C2—H2117.4O1ii—Ca1—N1i75.08 (6)
C2—C3—C4127.2 (3)O1iii—Ca1—N1i86.31 (7)
C2—C3—H3116.4O2i—Ca1—N1i139.63 (7)
C4—C3—H3116.4O2—Ca1—N1i84.03 (7)
C5—C4—C9117.6 (2)O1—Ca1—N1i101.48 (6)
C5—C4—C3123.7 (2)O1i—Ca1—N1i154.47 (7)
C9—C4—C3118.6 (2)N1—Ca1—N1i64.54 (10)
C6—C5—C4121.3 (3)O1ii—Ca1—C1i102.61 (7)
C6—C5—H5119.3O1iii—Ca1—C1i90.21 (7)
C4—C5—H5119.3O2i—Ca1—C1i25.50 (6)
C5—C6—C7121.2 (3)O2—Ca1—C1i116.65 (8)
C5—C6—H6119.4O1—Ca1—C1i97.97 (7)
C7—C6—H6119.4O1i—Ca1—C1i25.99 (6)
C6—C7—C8119.0 (3)N1—Ca1—C1i93.46 (7)
C6—C7—H7120.5N1i—Ca1—C1i157.89 (7)
C8—C7—H7120.5O1ii—Ca1—C190.21 (7)
C7—C8—C9119.5 (3)O1iii—Ca1—C1102.61 (7)
C7—C8—H8120.2O2i—Ca1—C1116.65 (8)
C9—C8—H8120.2O2—Ca1—C125.50 (6)
C4—C9—C8121.3 (3)O1—Ca1—C125.99 (6)
C4—C9—H9119.3O1i—Ca1—C197.97 (7)
C8—C9—H9119.3N1—Ca1—C1157.89 (7)
N1—C11—C12122.6 (2)N1i—Ca1—C193.46 (7)
N1—C11—C11i118.39 (14)C1i—Ca1—C1108.60 (10)
C12—C11—C11i119.01 (17)O1ii—Ca1—Ca1ii35.19 (4)
C13—C12—C11117.0 (3)O1iii—Ca1—Ca1ii157.99 (4)
C13—C12—C16123.5 (3)O2i—Ca1—Ca1ii87.24 (5)
C11—C12—C16119.5 (3)O2—Ca1—Ca1ii79.83 (5)
C14—C13—C12120.6 (3)O1—Ca1—Ca1ii33.78 (4)
C14—C13—H13119.7O1i—Ca1—Ca1ii117.07 (5)
C12—C13—H13119.7N1—Ca1—Ca1ii121.25 (5)
C13—C14—C15118.8 (3)N1i—Ca1—Ca1ii88.25 (5)
C13—C14—H14120.6C1i—Ca1—Ca1ii102.46 (6)
C15—C14—H14120.6C1—Ca1—Ca1ii56.45 (5)
N1—C15—C14123.2 (3)O1ii—Ca1—Ca1iv157.99 (4)
N1—C15—H15118.4O1iii—Ca1—Ca1iv35.19 (4)
C14—C15—H15118.4O2i—Ca1—Ca1iv79.83 (5)
C16i—C16—C12121.47 (18)O2—Ca1—Ca1iv87.24 (5)
C16i—C16—H16119.3O1—Ca1—Ca1iv117.07 (5)
C12—C16—H16119.3O1i—Ca1—Ca1iv33.78 (4)
O1ii—Ca1—O1iii158.06 (10)N1—Ca1—Ca1iv88.25 (5)
O1ii—Ca1—O2i78.40 (6)N1i—Ca1—Ca1iv121.25 (5)
O1iii—Ca1—O2i110.43 (7)C1i—Ca1—Ca1iv56.45 (5)
O1ii—Ca1—O2110.43 (7)C1—Ca1—Ca1iv102.46 (6)
O1iii—Ca1—O278.40 (6)Ca1ii—Ca1—Ca1iv146.43 (4)
O2i—Ca1—O2134.22 (10)C15—N1—C11117.8 (2)
O1ii—Ca1—O168.97 (7)C15—N1—Ca1122.92 (19)
O1iii—Ca1—O1127.35 (7)C11—N1—Ca1119.31 (16)
O2i—Ca1—O196.67 (7)C1—O1—Ca1ii137.05 (17)
O2—Ca1—O151.48 (6)C1—O1—Ca191.95 (15)
O1ii—Ca1—O1i127.35 (7)Ca1ii—O1—Ca1111.03 (7)
O1iii—Ca1—O1i68.97 (7)C1—O2—Ca195.37 (16)
O2i—Ca1—O1i51.48 (6)
O2—C1—C2—C32.0 (4)O1i—Ca1—N1—C1523.0 (2)
O1—C1—C2—C3175.8 (3)N1i—Ca1—N1—C15179.6 (2)
C1—C2—C3—C4176.5 (2)C1i—Ca1—N1—C151.9 (2)
C2—C3—C4—C57.4 (4)C1—Ca1—N1—C15174.2 (2)
C2—C3—C4—C9174.9 (3)Ca1ii—Ca1—N1—C15108.77 (19)
C9—C4—C5—C62.1 (4)Ca1iv—Ca1—N1—C1554.29 (19)
C3—C4—C5—C6175.7 (3)O1ii—Ca1—N1—C1174.37 (17)
C4—C5—C6—C72.1 (4)O1iii—Ca1—N1—C1193.90 (17)
C5—C6—C7—C80.1 (5)O2i—Ca1—N1—C11153.08 (18)
C6—C7—C8—C91.7 (5)O2—Ca1—N1—C1143.3 (2)
C5—C4—C9—C80.2 (4)O1—Ca1—N1—C1160.1 (2)
C3—C4—C9—C8177.7 (3)O1i—Ca1—N1—C11158.23 (17)
C7—C8—C9—C41.7 (4)N1i—Ca1—N1—C110.85 (12)
N1—C11—C12—C131.4 (4)C1i—Ca1—N1—C11176.81 (17)
C11i—C11—C12—C13179.1 (3)C1—Ca1—N1—C117.1 (3)
N1—C11—C12—C16178.2 (2)Ca1ii—Ca1—N1—C1169.98 (18)
C11i—C11—C12—C161.3 (4)Ca1iv—Ca1—N1—C11126.96 (17)
C11—C12—C13—C142.4 (4)O2—C1—O1—Ca1ii122.0 (3)
C16—C12—C13—C14177.1 (3)C2—C1—O1—Ca1ii60.2 (3)
C12—C13—C14—C151.4 (5)Ca1—C1—O1—Ca1ii124.3 (2)
C13—C14—C15—N10.8 (4)O2—C1—O1—Ca12.3 (3)
C13—C12—C16—C16i178.8 (4)C2—C1—O1—Ca1175.5 (2)
C11—C12—C16—C16i0.7 (6)O1ii—Ca1—O1—C1142.91 (18)
O2—C1—Ca1—O1ii143.41 (17)O1iii—Ca1—O1—C120.18 (17)
O1—C1—Ca1—O1ii34.26 (17)O2i—Ca1—O1—C1142.27 (15)
O2—C1—Ca1—O1iii18.65 (18)O2—Ca1—O1—C11.28 (14)
O1—C1—Ca1—O1iii163.68 (13)O1i—Ca1—O1—C190.32 (15)
O2—C1—Ca1—O2i139.48 (15)N1—Ca1—O1—C1127.64 (18)
O1—C1—Ca1—O2i42.85 (17)N1i—Ca1—O1—C173.98 (15)
O1—C1—Ca1—O2177.7 (3)C1i—Ca1—O1—C1116.59 (15)
O2—C1—Ca1—O1177.7 (3)Ca1ii—Ca1—O1—C1142.91 (18)
O2—C1—Ca1—O1i88.78 (17)Ca1iv—Ca1—O1—C160.31 (15)
O1—C1—Ca1—O1i93.56 (16)O1ii—Ca1—O1—Ca1ii0
O2—C1—Ca1—N162.7 (3)O1iii—Ca1—O1—Ca1ii163.08 (7)
O1—C1—Ca1—N1115.0 (2)O2i—Ca1—O1—Ca1ii74.82 (8)
O2—C1—Ca1—N1i68.34 (17)O2—Ca1—O1—Ca1ii141.62 (12)
O1—C1—Ca1—N1i109.33 (15)O1i—Ca1—O1—Ca1ii126.77 (9)
O2—C1—Ca1—C1i113.20 (18)N1—Ca1—O1—Ca1ii15.27 (18)
O1—C1—Ca1—C1i69.13 (14)N1i—Ca1—O1—Ca1ii68.93 (8)
O2—C1—Ca1—Ca1ii153.94 (18)C1i—Ca1—O1—Ca1ii100.51 (8)
O1—C1—Ca1—Ca1ii23.73 (12)C1—Ca1—O1—Ca1ii142.91 (18)
O2—C1—Ca1—Ca1iv54.73 (17)Ca1iv—Ca1—O1—Ca1ii156.78 (5)
O1—C1—Ca1—Ca1iv127.61 (14)O1—C1—O2—Ca12.4 (3)
C14—C15—N1—C111.9 (4)C2—C1—O2—Ca1175.4 (2)
C14—C15—N1—Ca1176.9 (2)O1ii—Ca1—O2—C139.50 (18)
C12—C11—N1—C150.7 (3)O1iii—Ca1—O2—C1161.42 (18)
C11i—C11—N1—C15178.8 (3)O2i—Ca1—O2—C154.12 (15)
C12—C11—N1—Ca1178.07 (18)O1—Ca1—O2—C11.31 (15)
C11i—C11—N1—Ca12.4 (3)O1i—Ca1—O2—C194.55 (17)
O1ii—Ca1—N1—C15104.4 (2)N1—Ca1—O2—C1148.90 (15)
O1iii—Ca1—N1—C1587.4 (2)N1i—Ca1—O2—C1111.13 (17)
O2i—Ca1—N1—C1525.7 (2)C1i—Ca1—O2—C177.1 (2)
O2—Ca1—N1—C15137.96 (19)Ca1ii—Ca1—O2—C121.84 (16)
O1—Ca1—N1—C15118.6 (2)Ca1iv—Ca1—O2—C1127.05 (16)
Symmetry codes: (i) x, y, z+1/2; (ii) x, y+1, z+1; (iii) x, y+1, z1/2; (iv) x, y+1, z.
Hydrogen-bond geometry (Å, º) top
D—H···AD—HH···AD···AD—H···A
C3—H3···O20.932.582.886 (3)100
Poly[(1,10-phenanthroline-κ2N,N')(µ-3-phenylprop-2-enoato-κ3O,O':O)(µ-3-phenylprop-2-enoato-κ4O:O,O':O')barium(I)] (Ba) top
Crystal data top
[Ba(C10H7O2)2(C10H8N2)]Dx = 1.535 Mg m3
Mr = 611.84Mo Kα radiation, λ = 0.71073 Å
Trigonal, R3Cell parameters from 9950 reflections
Hall symbol: -R 3θ = 2.6–26.4°
a = 36.4542 (7) ŵ = 1.54 mm1
c = 10.3535 (2) ÅT = 295 K
V = 11915.5 (6) Å3Prism, colorless
Z = 180.16 × 0.14 × 0.13 mm
F(000) = 5472
Data collection top
Bruker APEXII
diffractometer
7729 independent reflections
Radiation source: Enraf Nonius FR5905619 reflections with I > 2σ(I)
Graphite monochromatorRint = 0.060
CCD rotation images, thick slices scansθmax = 30.1°, θmin = 3.1°
Absorption correction: multi-scan
(SADABS; Sheldrick, 2002)
h = 5151
Tmin = 0.668, Tmax = 0.764k = 4551
66922 measured reflectionsl = 1414
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) = 0.087H-atom parameters constrained
S = 1.02 w = 1/[σ2(Fo2) + (0.0391P)2 + 16.9728P]
where P = (Fo2 + 2Fc2)/3
7729 reflections(Δ/σ)max = 0.006
334 parametersΔρmax = 1.98 e Å3
0 restraintsΔρmin = 0.55 e Å3
Special details top

Geometry. All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds 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 > 2sigma(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*/Ueq
C1A0.37461 (9)0.05822 (9)1.3496 (3)0.0332 (6)
C1B0.42708 (9)0.10078 (9)0.8721 (3)0.0361 (6)
C2A0.42061 (11)0.09183 (10)1.3431 (3)0.0473 (8)
H2A0.4330.10161.26260.057*
C2B0.46905 (10)0.12678 (10)0.9366 (3)0.0409 (7)
H2B0.4750.11571.00930.049*
C3A0.44365 (11)0.10765 (10)1.4460 (3)0.0472 (8)
H3A0.42930.09931.52430.057*
C3B0.49809 (10)0.16460 (10)0.8960 (3)0.0441 (7)
H3B0.49060.17570.82650.053*
C4A0.48975 (11)0.13723 (11)1.4543 (4)0.0558 (9)
C4B0.54107 (10)0.19127 (10)0.9487 (3)0.0440 (7)
C5A0.51003 (13)0.13953 (14)1.5686 (5)0.0729 (12)
H5A0.4940.12311.63790.088*
C5B0.56149 (12)0.17450 (12)1.0195 (4)0.0584 (10)
H5B0.54760.14561.03660.07*
C6A0.55259 (16)0.16488 (18)1.5842 (6)0.0986 (18)
H6A0.56550.16531.66220.118*
C6B0.60215 (13)0.20007 (14)1.0650 (4)0.0716 (12)
H6B0.61560.18821.11060.086*
C7A0.57595 (17)0.1896 (2)1.4837 (8)0.125 (3)
H7A0.60520.20651.49230.15*
C7B0.62277 (13)0.24273 (14)1.0435 (5)0.0732 (12)
H7B0.64990.261.07620.088*
C8A0.55688 (19)0.1899 (2)1.3701 (7)0.127 (3)
H8A0.57290.20791.30360.152*
C9B0.60304 (13)0.26010 (12)0.9725 (5)0.0709 (12)
H9B0.6170.28910.95720.085*
C10A0.51308 (15)0.16288 (16)1.3537 (5)0.0978 (18)
H10A0.50010.16241.27590.117*
C10B0.56295 (12)0.23465 (11)0.9247 (4)0.0554 (9)
H10B0.55020.24660.87560.066*
C110.46767 (10)0.03124 (11)0.8532 (3)0.0439 (7)
H110.44580.02070.7930.053*
C120.50933 (11)0.05264 (12)0.8076 (3)0.0506 (8)
H120.51480.05610.71930.061*
C130.54152 (11)0.06817 (11)0.8933 (4)0.0506 (8)
H130.56940.08220.86450.061*
C140.53275 (10)0.06311 (10)1.0260 (3)0.0409 (7)
C150.56511 (11)0.07948 (12)1.1230 (4)0.0526 (9)
H150.59340.09371.0980.063*
C160.55558 (11)0.07484 (12)1.2474 (4)0.0554 (9)
H160.57730.08671.3080.066*
C170.51261 (10)0.05196 (10)1.2904 (3)0.0428 (7)
C180.50107 (12)0.04412 (13)1.4216 (3)0.0557 (9)
H180.52190.05521.48520.067*
C190.45939 (13)0.02022 (13)1.4559 (3)0.0559 (9)
H190.45160.01461.54230.067*
C200.42900 (11)0.00459 (11)1.3587 (3)0.0446 (8)
H200.40070.01161.38280.054*
C210.47915 (9)0.03451 (9)1.1999 (3)0.0344 (6)
C220.48975 (9)0.04100 (9)1.0638 (3)0.0339 (6)
N10.45755 (7)0.02511 (8)0.9766 (2)0.0351 (5)
N20.43772 (8)0.01131 (8)1.2350 (2)0.0372 (6)
O1A0.35922 (7)0.03538 (7)1.2511 (2)0.0443 (5)
O1B0.39982 (6)0.06800 (6)0.9313 (2)0.0399 (5)
O2A0.35425 (7)0.05311 (7)1.4510 (2)0.0438 (5)
O2B0.42084 (7)0.11185 (7)0.7640 (2)0.0496 (6)
Ba10.368903 (5)0.007544 (5)1.049353 (15)0.02866 (6)
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
C1A0.0411 (16)0.0282 (14)0.0334 (15)0.0196 (13)0.0030 (12)0.0032 (12)
C1B0.0387 (16)0.0299 (15)0.0389 (17)0.0166 (13)0.0008 (13)0.0000 (12)
C2A0.0506 (19)0.0420 (18)0.0426 (19)0.0180 (16)0.0094 (15)0.0072 (15)
C2B0.0428 (17)0.0385 (16)0.0365 (17)0.0165 (14)0.0047 (13)0.0022 (13)
C3A0.0469 (19)0.0421 (18)0.050 (2)0.0204 (16)0.0070 (15)0.0040 (15)
C3B0.0414 (17)0.0397 (17)0.0487 (19)0.0184 (15)0.0035 (14)0.0036 (14)
C4A0.0436 (19)0.0442 (19)0.069 (3)0.0140 (16)0.0059 (18)0.0175 (18)
C4B0.0401 (17)0.0392 (17)0.0458 (19)0.0147 (14)0.0011 (14)0.0039 (14)
C5A0.051 (2)0.073 (3)0.078 (3)0.019 (2)0.005 (2)0.019 (2)
C5B0.052 (2)0.0428 (19)0.071 (3)0.0168 (17)0.0123 (19)0.0008 (18)
C6A0.055 (3)0.114 (4)0.099 (4)0.021 (3)0.009 (3)0.035 (3)
C6B0.050 (2)0.076 (3)0.079 (3)0.024 (2)0.014 (2)0.005 (2)
C7A0.048 (3)0.142 (6)0.133 (6)0.009 (3)0.002 (3)0.071 (5)
C7B0.043 (2)0.065 (3)0.085 (3)0.007 (2)0.009 (2)0.013 (2)
C8A0.077 (4)0.126 (5)0.099 (5)0.008 (3)0.036 (3)0.024 (4)
C9B0.048 (2)0.040 (2)0.102 (3)0.0049 (18)0.008 (2)0.010 (2)
C10A0.063 (3)0.095 (4)0.077 (3)0.003 (3)0.009 (2)0.022 (3)
C10B0.050 (2)0.0376 (18)0.074 (3)0.0184 (16)0.0056 (18)0.0018 (17)
C110.0433 (18)0.062 (2)0.0325 (16)0.0306 (17)0.0021 (13)0.0016 (14)
C120.051 (2)0.066 (2)0.0402 (19)0.0328 (18)0.0099 (16)0.0019 (16)
C130.0384 (18)0.056 (2)0.060 (2)0.0258 (16)0.0090 (16)0.0018 (17)
C140.0363 (16)0.0445 (17)0.0489 (19)0.0255 (14)0.0023 (14)0.0005 (14)
C150.0314 (17)0.060 (2)0.065 (2)0.0213 (16)0.0060 (16)0.0061 (18)
C160.0380 (18)0.067 (2)0.060 (2)0.0254 (17)0.0181 (16)0.0142 (19)
C170.0440 (18)0.0485 (18)0.0441 (18)0.0293 (15)0.0136 (14)0.0103 (14)
C180.062 (2)0.073 (3)0.041 (2)0.040 (2)0.0215 (17)0.0121 (18)
C190.069 (3)0.075 (3)0.0335 (18)0.044 (2)0.0061 (17)0.0010 (17)
C200.0479 (19)0.056 (2)0.0361 (17)0.0304 (16)0.0003 (14)0.0029 (15)
C210.0365 (15)0.0364 (15)0.0366 (16)0.0230 (13)0.0084 (12)0.0050 (12)
C220.0352 (15)0.0351 (15)0.0382 (16)0.0226 (13)0.0049 (12)0.0033 (12)
N10.0337 (13)0.0442 (14)0.0322 (13)0.0229 (11)0.0012 (10)0.0003 (11)
N20.0368 (14)0.0460 (15)0.0323 (13)0.0234 (12)0.0050 (10)0.0015 (11)
O1A0.0504 (13)0.0427 (12)0.0346 (12)0.0194 (11)0.0036 (10)0.0057 (9)
O1B0.0371 (11)0.0330 (11)0.0437 (12)0.0132 (9)0.0011 (9)0.0068 (9)
O2A0.0509 (13)0.0445 (12)0.0306 (11)0.0199 (11)0.0088 (10)0.0012 (9)
O2B0.0450 (13)0.0493 (13)0.0406 (13)0.0132 (11)0.0053 (10)0.0118 (10)
Ba10.03078 (9)0.03180 (10)0.02337 (9)0.01563 (7)0.00041 (6)0.00206 (6)
Geometric parameters (Å, º) top
C1A—O2A1.244 (3)C11—H110.93
C1A—O1A1.258 (3)C12—C131.350 (5)
C1A—C2A1.505 (4)C12—H120.93
C1A—Ba1i3.279 (3)C13—C141.402 (5)
C1B—O2B1.249 (4)C13—H130.93
C1B—O1B1.266 (3)C14—C221.413 (4)
C1B—C2B1.495 (4)C14—C151.433 (5)
C1B—Ba1ii3.209 (3)C15—C161.322 (5)
C2A—C3A1.300 (5)C15—H150.93
C2A—H2A0.93C16—C171.429 (5)
C2B—C3B1.318 (4)C16—H160.93
C2B—H2B0.93C17—C181.408 (5)
C3A—C4A1.477 (5)C17—C211.413 (4)
C3A—H3A0.93C18—C191.367 (5)
C3B—C4B1.475 (4)C18—H180.93
C3B—H3B0.93C19—C201.391 (5)
C4A—C10A1.374 (6)C19—H190.93
C4A—C5A1.375 (6)C20—N21.313 (4)
C4B—C5B1.386 (5)C20—H200.93
C4B—C10B1.392 (5)C21—N21.361 (4)
C5A—C6A1.361 (6)C21—C221.449 (4)
C5A—H5A0.93C22—N11.359 (4)
C5B—C6B1.381 (5)Ba1—N12.929 (2)
C5B—H5B0.93Ba1—N22.956 (2)
C6A—C7A1.361 (9)O1A—Ba12.736 (2)
C6A—H6A0.93O1A—Ba1i2.893 (2)
C6B—C7B1.365 (6)O1B—Ba12.692 (2)
C6B—H6B0.93O1B—Ba1ii2.908 (2)
C7A—C8A1.369 (9)O2A—Ba1iii2.779 (2)
C7A—H7A0.93O2A—Ba1i2.976 (2)
C7B—C9B1.383 (6)O2B—Ba1ii2.778 (2)
C7B—H7B0.93Ba1—O1Aii2.893 (2)
C8A—C10A1.405 (7)Ba1—O1Bi2.908 (2)
C8A—H8A0.93Ba1—O2Aiv2.779 (2)
C9B—C10B1.373 (5)Ba1—O2Aii2.975 (2)
C9B—H9B0.93Ba1—O2Bi2.778 (2)
C10A—H10A0.93Ba1—C1Aii3.279 (3)
C10B—H10B0.93Ba1—C1Bi3.209 (3)
C11—N11.318 (4)Ba1—Ba1ii4.2721 (2)
C11—C121.398 (5)
O2A—C1A—O1A123.4 (3)C19—C20—H20118
O2A—C1A—C2A119.9 (3)N2—C21—C17122.9 (3)
O1A—C1A—C2A116.7 (3)N2—C21—C22118.9 (2)
O2A—C1A—Ba1i65.01 (16)C17—C21—C22118.2 (3)
O1A—C1A—Ba1i61.26 (15)N1—C22—C14122.3 (3)
C2A—C1A—Ba1i159.5 (2)N1—C22—C21118.2 (3)
O2B—C1B—O1B123.7 (3)C14—C22—C21119.4 (3)
O2B—C1B—C2B119.3 (3)C11—N1—C22117.6 (3)
O1B—C1B—C2B117.0 (3)C11—N1—Ba1118.45 (19)
O2B—C1B—Ba1ii58.89 (15)C22—N1—Ba1123.01 (18)
O1B—C1B—Ba1ii64.90 (15)C20—N2—C21117.8 (3)
C2B—C1B—Ba1ii175.3 (2)C20—N2—Ba1119.5 (2)
C3A—C2A—C1A122.3 (3)C21—N2—Ba1121.33 (18)
C3A—C2A—H2A118.9C1A—O1A—Ba1148.8 (2)
C1A—C2A—H2A118.9C1A—O1A—Ba1i96.34 (17)
C3B—C2B—C1B123.6 (3)Ba1—O1A—Ba1i98.70 (6)
C3B—C2B—H2B118.2C1B—O1B—Ba1156.17 (19)
C1B—C2B—H2B118.2C1B—O1B—Ba1ii91.89 (17)
C2A—C3A—C4A128.2 (3)Ba1—O1B—Ba1ii99.37 (6)
C2A—C3A—H3A115.9C1A—O2A—Ba1iii154.8 (2)
C4A—C3A—H3A115.9C1A—O2A—Ba1i92.71 (17)
C2B—C3B—C4B127.2 (3)Ba1iii—O2A—Ba1i95.81 (6)
C2B—C3B—H3B116.4C1B—O2B—Ba1ii98.47 (18)
C4B—C3B—H3B116.4O1B—Ba1—O1A82.49 (6)
C10A—C4A—C5A118.7 (4)O1B—Ba1—O2Bi157.13 (6)
C10A—C4A—C3A123.0 (4)O1A—Ba1—O2Bi118.04 (6)
C5A—C4A—C3A118.4 (4)O1B—Ba1—O2Aiv71.95 (7)
C5B—C4B—C10B117.8 (3)O1A—Ba1—O2Aiv147.88 (7)
C5B—C4B—C3B122.2 (3)O2Bi—Ba1—O2Aiv91.27 (7)
C10B—C4B—C3B120.0 (3)O1B—Ba1—O1Aii73.92 (6)
C6A—C5A—C4A122.6 (5)O1A—Ba1—O1Aii90.240 (18)
C6A—C5A—H5A118.7O2Bi—Ba1—O1Aii113.42 (7)
C4A—C5A—H5A118.7O2Aiv—Ba1—O1Aii64.53 (6)
C6B—C5B—C4B121.0 (4)O1B—Ba1—O1Bi155.46 (7)
C6B—C5B—H5B119.5O1A—Ba1—O1Bi73.03 (6)
C4B—C5B—H5B119.5O2Bi—Ba1—O1Bi45.83 (6)
C7A—C6A—C5A118.8 (6)O2Aiv—Ba1—O1Bi131.45 (6)
C7A—C6A—H6A120.6O1Aii—Ba1—O1Bi107.26 (6)
C5A—C6A—H6A120.6O1B—Ba1—N169.82 (6)
C7B—C6B—C5B120.5 (4)O1A—Ba1—N1113.29 (7)
C7B—C6B—H6B119.8O2Bi—Ba1—N191.50 (7)
C5B—C6B—H6B119.8O2Aiv—Ba1—N176.15 (6)
C6A—C7A—C8A120.7 (5)O1Aii—Ba1—N1132.85 (6)
C6A—C7A—H7A119.7O1Bi—Ba1—N1118.29 (6)
C8A—C7A—H7A119.7O1B—Ba1—N2100.66 (7)
C6B—C7B—C9B119.5 (4)O1A—Ba1—N273.01 (7)
C6B—C7B—H7B120.3O2Bi—Ba1—N277.90 (7)
C9B—C7B—H7B120.3O2Aiv—Ba1—N2129.86 (7)
C7A—C8A—C10A120.1 (6)O1Aii—Ba1—N2163.05 (7)
C7A—C8A—H8A119.9O1Bi—Ba1—N270.89 (7)
C10A—C8A—H8A119.9N1—Ba1—N255.74 (7)
C10B—C9B—C7B120.2 (4)O1B—Ba1—O2Aii104.64 (6)
C10B—C9B—H9B119.9O1A—Ba1—O2Aii63.90 (6)
C7B—C9B—H9B119.9O2Bi—Ba1—O2Aii94.17 (7)
C4A—C10A—C8A119.0 (5)O2Aiv—Ba1—O2Aii103.62 (5)
C4A—C10A—H10A120.5O1Aii—Ba1—O2Aii44.06 (6)
C8A—C10A—H10A120.5O1Bi—Ba1—O2Aii66.22 (6)
C9B—C10B—C4B121.0 (4)N1—Ba1—O2Aii174.33 (6)
C9B—C10B—H10B119.5N2—Ba1—O2Aii125.69 (6)
C4B—C10B—H10B119.5O1B—Ba1—C1Bi174.52 (7)
N1—C11—C12123.8 (3)O1A—Ba1—C1Bi95.98 (7)
N1—C11—H11118.1O2Bi—Ba1—C1Bi22.64 (7)
C12—C11—H11118.1O2Aiv—Ba1—C1Bi111.18 (7)
C13—C12—C11119.1 (3)O1Aii—Ba1—C1Bi111.41 (7)
C13—C12—H12120.5O1Bi—Ba1—C1Bi23.22 (6)
C11—C12—H12120.5N1—Ba1—C1Bi106.20 (7)
C12—C13—C14119.7 (3)N2—Ba1—C1Bi73.86 (7)
C12—C13—H13120.1O2Aii—Ba1—C1Bi79.23 (7)
C14—C13—H13120.1O1B—Ba1—C1Aii86.61 (7)
C13—C14—C22117.5 (3)O1A—Ba1—C1Aii73.36 (7)
C13—C14—C15123.1 (3)O2Bi—Ba1—C1Aii108.06 (7)
C22—C14—C15119.4 (3)O2Aiv—Ba1—C1Aii85.76 (7)
C16—C15—C14121.3 (3)O1Aii—Ba1—C1Aii22.41 (6)
C16—C15—H15119.3O1Bi—Ba1—C1Aii88.00 (6)
C14—C15—H15119.3N1—Ba1—C1Aii153.69 (7)
C15—C16—C17121.3 (3)N2—Ba1—C1Aii144.25 (7)
C15—C16—H16119.3O2Aii—Ba1—C1Aii22.28 (6)
C17—C16—H16119.3C1Bi—Ba1—C1Aii98.03 (7)
C18—C17—C21116.5 (3)O1B—Ba1—Ba1ii42.19 (4)
C18—C17—C16123.3 (3)O1A—Ba1—Ba1ii104.02 (5)
C21—C17—C16120.2 (3)O2Bi—Ba1—Ba1ii131.02 (5)
C19—C18—C17120.2 (3)O2Aiv—Ba1—Ba1ii43.86 (5)
C19—C18—H18119.9O1Aii—Ba1—Ba1ii39.28 (4)
C17—C18—H18119.9O1Bi—Ba1—Ba1ii146.35 (4)
C18—C19—C20118.5 (3)N1—Ba1—Ba1ii94.03 (5)
C18—C19—H19120.7N2—Ba1—Ba1ii141.58 (5)
C20—C19—H19120.7O2Aii—Ba1—Ba1ii82.19 (4)
N2—C20—C19124.1 (3)C1Bi—Ba1—Ba1ii143.09 (5)
N2—C20—H20118C1Aii—Ba1—Ba1ii59.91 (5)
O2A—C1A—C2A—C3A20.4 (5)Ba1ii—O1B—Ba1—O1A120.62 (7)
O1A—C1A—C2A—C3A156.8 (3)C1B—O1B—Ba1—O2Bi32.9 (6)
Ba1i—C1A—C2A—C3A77.9 (7)Ba1ii—O1B—Ba1—O2Bi84.22 (18)
O2B—C1B—C2B—C3B11.0 (5)C1B—O1B—Ba1—O2Aiv77.5 (5)
O1B—C1B—C2B—C3B169.9 (3)Ba1ii—O1B—Ba1—O2Aiv39.68 (6)
C1A—C2A—C3A—C4A173.1 (3)C1B—O1B—Ba1—O1Aii145.3 (5)
C1B—C2B—C3B—C4B176.1 (3)Ba1ii—O1B—Ba1—O1Aii28.19 (6)
C2A—C3A—C4A—C10A21.6 (6)C1B—O1B—Ba1—O1Bi118.2 (4)
C2A—C3A—C4A—C5A159.3 (4)Ba1ii—O1B—Ba1—O1Bi124.62 (13)
C2B—C3B—C4B—C5B22.1 (6)C1B—O1B—Ba1—N14.0 (5)
C2B—C3B—C4B—C10B159.7 (4)Ba1ii—O1B—Ba1—N1121.13 (8)
C10A—C4A—C5A—C6A2.8 (7)C1B—O1B—Ba1—N251.2 (5)
C3A—C4A—C5A—C6A178.0 (4)Ba1ii—O1B—Ba1—N2168.33 (6)
C10B—C4B—C5B—C6B0.2 (6)C1B—O1B—Ba1—O2Aii177.3 (5)
C3B—C4B—C5B—C6B178.4 (4)Ba1ii—O1B—Ba1—O2Aii60.16 (7)
C4A—C5A—C6A—C7A1.3 (8)C1B—O1B—Ba1—C1Aii164.1 (5)
C4B—C5B—C6B—C7B1.5 (7)Ba1ii—O1B—Ba1—C1Aii46.97 (7)
C5A—C6A—C7A—C8A1.8 (10)C1B—O1B—Ba1—Ba1ii117.1 (5)
C5B—C6B—C7B—C9B1.7 (7)C1A—O1A—Ba1—O1B88.1 (4)
C6A—C7A—C8A—C10A3.3 (11)Ba1i—O1A—Ba1—O1B153.97 (8)
C6B—C7B—C9B—C10B0.3 (7)C1A—O1A—Ba1—O2Bi81.2 (4)
C5A—C4A—C10A—C8A1.3 (8)Ba1i—O1A—Ba1—O2Bi36.69 (10)
C3A—C4A—C10A—C8A179.6 (5)C1A—O1A—Ba1—O2Aiv125.2 (3)
C7A—C8A—C10A—C4A1.7 (10)Ba1i—O1A—Ba1—O2Aiv116.88 (11)
C7B—C9B—C10B—C4B1.4 (6)C1A—O1A—Ba1—O1Aii161.9 (4)
C5B—C4B—C10B—C9B1.6 (6)Ba1i—O1A—Ba1—O1Aii80.22 (5)
C3B—C4B—C10B—C9B179.9 (3)C1A—O1A—Ba1—O1Bi90.2 (4)
N1—C11—C12—C130.0 (5)Ba1i—O1A—Ba1—O1Bi27.77 (6)
C11—C12—C13—C140.8 (5)C1A—O1A—Ba1—N123.9 (4)
C12—C13—C14—C220.9 (5)Ba1i—O1A—Ba1—N1141.85 (6)
C12—C13—C14—C15178.6 (3)C1A—O1A—Ba1—N215.5 (4)
C13—C14—C15—C16178.6 (4)Ba1i—O1A—Ba1—N2102.42 (8)
C22—C14—C15—C161.0 (5)C1A—O1A—Ba1—O2Aii161.5 (4)
C14—C15—C16—C172.3 (6)Ba1i—O1A—Ba1—O2Aii43.57 (6)
C15—C16—C17—C18176.2 (4)C1A—O1A—Ba1—C1Bi86.6 (4)
C15—C16—C17—C211.4 (5)Ba1i—O1A—Ba1—C1Bi31.33 (8)
C21—C17—C18—C190.9 (5)C1A—O1A—Ba1—C1Aii176.8 (4)
C16—C17—C18—C19176.8 (4)Ba1i—O1A—Ba1—C1Aii65.28 (7)
C17—C18—C19—C201.0 (6)C1A—O1A—Ba1—Ba1ii124.7 (4)
C18—C19—C20—N20.0 (6)Ba1i—O1A—Ba1—Ba1ii117.40 (5)
C18—C17—C21—N20.1 (4)C11—N1—Ba1—O1B61.9 (2)
C16—C17—C21—N2177.9 (3)C22—N1—Ba1—O1B106.4 (2)
C18—C17—C21—C22178.6 (3)C11—N1—Ba1—O1A133.9 (2)
C16—C17—C21—C220.8 (4)C22—N1—Ba1—O1A34.5 (2)
C13—C14—C22—N10.3 (4)C11—N1—Ba1—O2Bi104.6 (2)
C15—C14—C22—N1179.3 (3)C22—N1—Ba1—O2Bi87.1 (2)
C13—C14—C22—C21179.2 (3)C11—N1—Ba1—O2Aiv13.6 (2)
C15—C14—C22—C211.2 (4)C22—N1—Ba1—O2Aiv178.0 (2)
N2—C21—C22—N12.9 (4)C11—N1—Ba1—O1Aii20.0 (3)
C17—C21—C22—N1178.4 (3)C22—N1—Ba1—O1Aii148.41 (19)
N2—C21—C22—C14176.7 (3)C11—N1—Ba1—O1Bi143.5 (2)
C17—C21—C22—C142.0 (4)C22—N1—Ba1—O1Bi48.1 (2)
C12—C11—N1—C220.6 (5)C11—N1—Ba1—N2178.8 (3)
C12—C11—N1—Ba1169.7 (3)C22—N1—Ba1—N212.8 (2)
C14—C22—N1—C110.5 (4)C11—N1—Ba1—C1Bi122.0 (2)
C21—C22—N1—C11180.0 (3)C22—N1—Ba1—C1Bi69.6 (2)
C14—C22—N1—Ba1169.0 (2)C11—N1—Ba1—C1Aii34.3 (3)
C21—C22—N1—Ba111.5 (3)C22—N1—Ba1—C1Aii134.1 (2)
C19—C20—N2—C211.0 (5)C11—N1—Ba1—Ba1ii26.8 (2)
C19—C20—N2—Ba1166.1 (3)C22—N1—Ba1—Ba1ii141.6 (2)
C17—C21—N2—C201.0 (4)C20—N2—Ba1—O1B124.2 (2)
C22—C21—N2—C20177.6 (3)C21—N2—Ba1—O1B42.3 (2)
C17—C21—N2—Ba1165.8 (2)C20—N2—Ba1—O1A45.6 (2)
C22—C21—N2—Ba115.6 (3)C21—N2—Ba1—O1A121.0 (2)
O2A—C1A—O1A—Ba1138.8 (3)C20—N2—Ba1—O2Bi79.0 (2)
C2A—C1A—O1A—Ba138.4 (5)C21—N2—Ba1—O2Bi114.4 (2)
Ba1i—C1A—O1A—Ba1118.5 (4)C20—N2—Ba1—O2Aiv160.4 (2)
O2A—C1A—O1A—Ba1i20.3 (3)C21—N2—Ba1—O2Aiv33.0 (2)
C2A—C1A—O1A—Ba1i156.9 (2)C20—N2—Ba1—O1Aii54.7 (4)
O2B—C1B—O1B—Ba1122.3 (4)C21—N2—Ba1—O1Aii111.9 (3)
C2B—C1B—O1B—Ba156.7 (6)C20—N2—Ba1—O1Bi31.9 (2)
Ba1ii—C1B—O1B—Ba1118.5 (5)C21—N2—Ba1—O1Bi161.5 (2)
O2B—C1B—O1B—Ba1ii3.8 (3)C20—N2—Ba1—N1179.3 (3)
C2B—C1B—O1B—Ba1ii175.3 (2)C21—N2—Ba1—N114.09 (19)
O1A—C1A—O2A—Ba1iii129.4 (4)C20—N2—Ba1—O2Aii7.4 (3)
C2A—C1A—O2A—Ba1iii47.7 (6)C21—N2—Ba1—O2Aii159.21 (19)
Ba1i—C1A—O2A—Ba1iii109.8 (4)C20—N2—Ba1—C1Bi56.1 (2)
O1A—C1A—O2A—Ba1i19.6 (3)C21—N2—Ba1—C1Bi137.4 (2)
C2A—C1A—O2A—Ba1i157.5 (2)C20—N2—Ba1—C1Aii25.1 (3)
O1B—C1B—O2B—Ba1ii4.0 (3)C21—N2—Ba1—C1Aii141.46 (19)
C2B—C1B—O2B—Ba1ii175.0 (2)C20—N2—Ba1—Ba1ii136.9 (2)
C1B—O1B—Ba1—O1A122.2 (5)C21—N2—Ba1—Ba1ii29.7 (2)
Symmetry codes: (i) x+y+2/3, x+1/3, z+1/3; (ii) y+1/3, xy1/3, z1/3; (iii) y+1/3, xy1/3, z+2/3; (iv) x+y+2/3, x+1/3, z2/3.
Hydrogen-bond geometry (Å, º) top
D—H···AD—HH···AD···AD—H···A
C3A—H3A···O2A0.932.512.846 (5)102
C3A—H3A···O2Bv0.932.573.418 (4)152
C3B—H3B···O2B0.932.532.843 (5)100
C11—H11···O2Aiv0.932.543.303 (5)140
C13—H13···O2Bvi0.932.603.379 (6)142
C20—H20···O1Bi0.932.543.248 (5)133
Symmetry codes: (i) x+y+2/3, x+1/3, z+1/3; (iv) x+y+2/3, x+1/3, z2/3; (v) x, y, z+1; (vi) xy+1/3, x1/3, z+5/3.
IR wavenumbers (in cm-1) and tentative assignment of the most important bands for ligands Nacin and 1,10-phen, and complexes (1) and (2). top
Abbreviations: vs is very strong, s is strong, m is medium, w is weak, op is out-of-plane, asym is asymmetric, sym is symmetric, aliph is aliphatic and arom is aromatic.
Nacin1,10-phen(1)(2)Assignment
--486(w)486(w)ν(M—O)
--572(w)572(w)ν(M—N)
825(w)856(s)842(m)842(m)δop(CH)
-1598(m)1612(vs)1613(vs)1612(vs)
1418(vs)-1439(vs)1423(vs)νsym(COO-)
1553(s)-1540(w)1524(w)νasym(COO-)
2922(s)2986(w)2919(w)2917(w)ν(CH)aliph
3032(m)3064(w)3022(w)3020(w)ν(CH)arom
 

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