A new barium acetate phase, di-μ5-acetato-tri-μ4-acetato-tri-μ3-acetato-tri-μ2-acetato-μ2-acetato-triaquahemiaquahexabarium(II), of analytical formula [Ba6(C2H3O2)12(H2O)3.5], is described. The asymmetric unit contains six independent Ba centres with coordination numbers varying from 7 to 10 arising from bonding to 12 crystallographically independent acetate ligands and four molecules of water, one of which is disordered over two sites both of occupancy 0.5. Bonding to the acetate ligands creates a completely connected three-dimensional structure. All H atoms of the water molecules participate in hydrogen bonding.
Supporting information
CCDC reference: 669169
Crystals of (I) were obtained by the low-temperature recrystallization from aqueous solution of the as-purchased monohydrated salt at 268 K. After leaving the saturated solution unattended in the refrigerator for about 6 months, very large colourless blocks were observed, which proved to correspond to a unique and unknown phase of barium acetate. Thermogravimetric analysis suggested a degree of hydration of about 0.6 H2O per Ba, a figure later confirmed by the structural analysis, which gave a more precise value of 0.583 H2O per Ba.
Methyl H atoms were placed in calculated positions with C—H = 0.96 Å and refined with a riding model, while the torsion angles of the methyl groups were also refined. Water H atoms were located in difference maps and their coordinates refined with restrained O—H = 0.85 (1) Å and H···H = 1.40 (2) Å. In all cases, Uiso(H) = 1.5Ueq(C,O).
Data collection: SMART-NT (Bruker, 2001); cell refinement: SAINT-NT (Bruker, 2001); data reduction: SAINT-NT (Bruker, 2001); program(s) used to solve structure: SHELXS97 (Sheldrick, 1997); program(s) used to refine structure: SHELXL97 (Sheldrick, 1997); molecular graphics: SHELXTL-NT (Bruker, 2001); software used to prepare material for publication: SHELXTL-NT (Bruker, 2001) and PLATON (Spek, 2003).
triaquahemiaquadi-µ
5-acetato-tri-µ
4-acetato-tri-µ
3-acetato-tri-µ
2– acetato-µ
2-acetato-hexabarium(II)
top
Crystal data top
[Ba6(C2H3O2)12(H2O)3.5] | F(000) = 2972 |
Mr = 1595.62 | Dx = 2.328 Mg m−3 |
Monoclinic, P21/n | Mo Kα radiation, λ = 0.71073 Å |
Hall symbol: -P 2yn | Cell parameters from 8703 reflections |
a = 14.040 (3) Å | θ = 2.4–27.9° |
b = 19.903 (4) Å | µ = 5.19 mm−1 |
c = 17.721 (4) Å | T = 294 K |
β = 113.19 (3)° | Block, colourless |
V = 4551.6 (19) Å3 | 0.36 × 0.24 × 0.20 mm |
Z = 4 | |
Data collection top
Bruker SMART? CCD area-detector diffractometer | 10282 independent reflections |
Radiation source: sealed tube | 8906 reflections with I > 2σ(I) |
Graphite monochromator | Rint = 0.042 |
ϕ and ω scans | θmax = 28.0°, θmin = 1.9° |
Absorption correction: multi-scan (SADABS; Sheldrick, 2001) | h = −18→18 |
Tmin = 0.24, Tmax = 0.36 | k = −25→24 |
38138 measured reflections | l = −22→22 |
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)] = 0.040 | Hydrogen site location: geom and difmap |
wR(F2) = 0.087 | H atoms treated by a mixture of independent and constrained refinement |
S = 1.11 | w = 1/[σ2(Fo2) + (0.0378P)2 + 2.7573P] where P = (Fo2 + 2Fc2)/3 |
10282 reflections | (Δ/σ)max = 0.004 |
559 parameters | Δρmax = 1.21 e Å−3 |
13 restraints | Δρmin = −0.79 e Å−3 |
Crystal data top
[Ba6(C2H3O2)12(H2O)3.5] | V = 4551.6 (19) Å3 |
Mr = 1595.62 | Z = 4 |
Monoclinic, P21/n | Mo Kα radiation |
a = 14.040 (3) Å | µ = 5.19 mm−1 |
b = 19.903 (4) Å | T = 294 K |
c = 17.721 (4) Å | 0.36 × 0.24 × 0.20 mm |
β = 113.19 (3)° | |
Data collection top
Bruker SMART? CCD area-detector diffractometer | 10282 independent reflections |
Absorption correction: multi-scan (SADABS; Sheldrick, 2001) | 8906 reflections with I > 2σ(I) |
Tmin = 0.24, Tmax = 0.36 | Rint = 0.042 |
38138 measured reflections | |
Refinement top
R[F2 > 2σ(F2)] = 0.040 | 13 restraints |
wR(F2) = 0.087 | H atoms treated by a mixture of independent and constrained refinement |
S = 1.11 | Δρmax = 1.21 e Å−3 |
10282 reflections | Δρmin = −0.79 e Å−3 |
559 parameters | |
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. |
Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top | x | y | z | Uiso*/Ueq | Occ. (<1) |
Ba1 | 0.41960 (3) | 0.467956 (17) | 0.30949 (2) | 0.03100 (9) | |
Ba2 | 0.29624 (3) | 0.271290 (16) | 0.002437 (19) | 0.02498 (8) | |
Ba3 | 0.33300 (3) | 0.108571 (17) | 0.173896 (19) | 0.02673 (9) | |
Ba4 | 0.54205 (2) | 0.280167 (16) | 0.259917 (19) | 0.02372 (8) | |
Ba5 | 0.25680 (2) | 0.065510 (16) | −0.088808 (19) | 0.02378 (8) | |
Ba6 | 0.71783 (2) | 0.088388 (17) | 0.27067 (2) | 0.02498 (8) | |
O1A | 0.3258 (3) | 0.6028 (2) | 0.2779 (3) | 0.0428 (11) | |
O2A | 0.4270 (3) | 0.5761 (2) | 0.2141 (3) | 0.0439 (11) | |
C1A | 0.3576 (5) | 0.6108 (3) | 0.2222 (4) | 0.0350 (14) | |
C2A | 0.3080 (7) | 0.6654 (4) | 0.1585 (5) | 0.070 (2) | |
H2AA | 0.2449 | 0.6803 | 0.1622 | 0.105* | |
H2AB | 0.2930 | 0.6478 | 0.1046 | 0.105* | |
H2AC | 0.3549 | 0.7027 | 0.1685 | 0.105* | |
O1B | 0.2160 (4) | −0.0141 (2) | 0.1145 (3) | 0.0531 (13) | |
O2B | 0.3324 (3) | −0.0022 (2) | 0.0620 (2) | 0.0375 (10) | |
C1B | 0.2814 (5) | −0.0379 (3) | 0.0904 (3) | 0.0341 (14) | |
C2B | 0.2993 (6) | −0.1125 (3) | 0.0972 (5) | 0.0540 (19) | |
H2BA | 0.2339 | −0.1353 | 0.0789 | 0.081* | |
H2BB | 0.3398 | −0.1241 | 0.1533 | 0.081* | |
H2BC | 0.3356 | −0.1256 | 0.0636 | 0.081* | |
O1C | 0.4515 (4) | 0.1729 (3) | 0.3126 (3) | 0.0554 (14) | |
O2C | 0.5943 (4) | 0.2083 (3) | 0.4092 (3) | 0.0573 (14) | |
C1C | 0.5166 (5) | 0.1711 (3) | 0.3843 (4) | 0.0369 (14) | |
C2C | 0.4966 (6) | 0.1264 (4) | 0.4452 (4) | 0.064 (2) | |
H2CA | 0.5614 | 0.1120 | 0.4865 | 0.096* | |
H2CB | 0.4575 | 0.0878 | 0.4173 | 0.096* | |
H2CC | 0.4581 | 0.1508 | 0.4705 | 0.096* | |
O1D | 0.0750 (3) | 0.0816 (2) | −0.2460 (2) | 0.0370 (10) | |
O2D | 0.2057 (3) | 0.0392 (2) | −0.2693 (3) | 0.0415 (11) | |
C1D | 0.1121 (5) | 0.0531 (3) | −0.2918 (3) | 0.0304 (13) | |
C2D | 0.0377 (6) | 0.0352 (3) | −0.3779 (4) | 0.0479 (18) | |
H2DA | −0.0279 | 0.0226 | −0.3773 | 0.072* | |
H2DB | 0.0653 | −0.0016 | −0.3979 | 0.072* | |
H2DC | 0.0286 | 0.0734 | −0.4133 | 0.072* | |
O1E | 0.1032 (3) | −0.0375 (2) | −0.1021 (3) | 0.0370 (10) | |
O2E | 0.2237 (3) | −0.0661 (2) | −0.1455 (2) | 0.0363 (10) | |
C1E | 0.1496 (5) | −0.0807 (3) | −0.1267 (3) | 0.0306 (13) | |
C2E | 0.1179 (6) | −0.1538 (3) | −0.1326 (4) | 0.0471 (17) | |
H2EA | 0.0441 | −0.1568 | −0.1496 | 0.071* | |
H2EB | 0.1514 | −0.1748 | −0.0799 | 0.071* | |
H2EC | 0.1380 | −0.1762 | −0.1720 | 0.071* | |
O1F | 0.7352 (3) | 0.2245 (2) | 0.2716 (3) | 0.0447 (12) | |
O2F | 0.7609 (3) | 0.3065 (2) | 0.3594 (2) | 0.0336 (9) | |
C1F | 0.7853 (4) | 0.2743 (3) | 0.3090 (3) | 0.0277 (12) | |
C2F | 0.8785 (5) | 0.2968 (4) | 0.2933 (4) | 0.0491 (18) | |
H2FA | 0.9180 | 0.2582 | 0.2903 | 0.074* | |
H2FB | 0.9209 | 0.3255 | 0.3372 | 0.074* | |
H2FC | 0.8560 | 0.3209 | 0.2423 | 0.074* | |
O1G | 0.2631 (4) | 0.3971 (2) | 0.0529 (3) | 0.0433 (11) | |
O2G | 0.2691 (4) | 0.4012 (2) | −0.0689 (3) | 0.0493 (12) | |
C1G | 0.2633 (5) | 0.4298 (3) | −0.0081 (4) | 0.0391 (15) | |
C2G | 0.2565 (7) | 0.5050 (3) | −0.0078 (5) | 0.066 (2) | |
H2GA | 0.1965 | 0.5182 | 0.0018 | 0.098* | |
H2GB | 0.2513 | 0.5223 | −0.0599 | 0.098* | |
H2GC | 0.3176 | 0.5228 | 0.0350 | 0.098* | |
O1H | 0.3580 (3) | 0.3354 (2) | 0.2557 (3) | 0.0412 (11) | |
O2H | 0.3283 (3) | 0.2543 (2) | 0.1638 (2) | 0.0308 (9) | |
C1H | 0.2989 (4) | 0.2961 (3) | 0.2038 (3) | 0.0285 (12) | |
C2H | 0.1850 (5) | 0.2988 (4) | 0.1854 (5) | 0.058 (2) | |
H2HA | 0.1492 | 0.3196 | 0.1328 | 0.087* | |
H2HB | 0.1739 | 0.3246 | 0.2270 | 0.087* | |
H2HC | 0.1592 | 0.2541 | 0.1845 | 0.087* | |
O1I | 0.4191 (4) | 0.0041 (3) | 0.2828 (4) | 0.0674 (16) | |
O2I | 0.5612 (4) | 0.0072 (3) | 0.2623 (4) | 0.0731 (18) | |
C1I | 0.5040 (5) | −0.0193 (3) | 0.2915 (4) | 0.0394 (15) | |
C2I | 0.5351 (6) | −0.0837 (4) | 0.3357 (6) | 0.072 (3) | |
H2IA | 0.5250 | −0.0815 | 0.3862 | 0.108* | |
H2IB | 0.6069 | −0.0922 | 0.3475 | 0.108* | |
H2IC | 0.4937 | −0.1194 | 0.3023 | 0.108* | |
O1J | 0.5313 (3) | 0.1479 (2) | 0.1672 (2) | 0.0375 (10) | |
O2J | 0.3988 (3) | 0.1464 (2) | 0.0469 (2) | 0.0316 (9) | |
C1J | 0.4943 (4) | 0.1462 (3) | 0.0894 (3) | 0.0284 (12) | |
C2J | 0.5669 (5) | 0.1434 (4) | 0.0460 (4) | 0.0433 (16) | |
H2JA | 0.5354 | 0.1649 | −0.0065 | 0.065* | |
H2JB | 0.5816 | 0.0973 | 0.0384 | 0.065* | |
H2JC | 0.6303 | 0.1660 | 0.0783 | 0.065* | |
O1K | 0.4705 (4) | 0.2987 (3) | −0.0308 (3) | 0.0494 (12) | |
O2K | 0.5107 (3) | 0.2971 (2) | 0.1024 (2) | 0.0377 (10) | |
C1K | 0.5350 (5) | 0.3043 (3) | 0.0414 (4) | 0.0335 (13) | |
C2K | 0.6452 (6) | 0.3200 (4) | 0.0566 (5) | 0.061 (2) | |
H2KA | 0.6902 | 0.3004 | 0.1077 | 0.091* | |
H2KB | 0.6549 | 0.3678 | 0.0589 | 0.091* | |
H2KC | 0.6614 | 0.3019 | 0.0128 | 0.091* | |
O1L | 0.0663 (3) | 0.1279 (2) | −0.1012 (2) | 0.0346 (10) | |
O2L | 0.1865 (3) | 0.1528 (2) | 0.0186 (2) | 0.0406 (11) | |
C1L | 0.0932 (4) | 0.1494 (3) | −0.0295 (4) | 0.0306 (13) | |
C2L | 0.0114 (6) | 0.1716 (5) | 0.0005 (5) | 0.068 (3) | |
H2LA | −0.0528 | 0.1789 | −0.0456 | 0.102* | |
H2LB | 0.0330 | 0.2125 | 0.0312 | 0.102* | |
H2LC | 0.0020 | 0.1373 | 0.0351 | 0.102* | |
O1W | 0.9217 (3) | 0.1232 (3) | 0.3323 (3) | 0.0422 (11) | |
H1WA | 0.970 (3) | 0.112 (4) | 0.317 (3) | 0.063* | |
H1WB | 0.945 (4) | 0.135 (4) | 0.3822 (15) | 0.063* | |
O2W | 0.4395 (4) | 0.0299 (3) | −0.1132 (3) | 0.0523 (13) | |
H2WA | 0.5026 (17) | 0.027 (4) | −0.081 (3) | 0.078* | |
H2WB | 0.431 (5) | 0.028 (4) | −0.1631 (11) | 0.078* | |
O3W | 0.2406 (4) | 0.4713 (3) | 0.1754 (3) | 0.0574 (14) | |
H3WA | 0.241 (5) | 0.446 (4) | 0.137 (4) | 0.086* | |
H3WB | 0.180 (3) | 0.475 (4) | 0.175 (5) | 0.086* | |
O4W | 0.4909 (15) | 0.4867 (11) | 0.4863 (10) | 0.055 (4) | 0.50 |
H4WB | 0.556 (3) | 0.483 (10) | 0.515 (9) | 0.082* | 0.50 |
H4WA | 0.457 (11) | 0.474 (10) | 0.514 (8) | 0.082* | 0.50 |
Atomic displacement parameters (Å2) top | U11 | U22 | U33 | U12 | U13 | U23 |
Ba1 | 0.02427 (18) | 0.02735 (19) | 0.0437 (2) | 0.00338 (13) | 0.01593 (16) | 0.00432 (15) |
Ba2 | 0.02668 (18) | 0.02526 (18) | 0.01978 (16) | 0.00244 (13) | 0.00569 (13) | −0.00036 (13) |
Ba3 | 0.02825 (18) | 0.02906 (19) | 0.02241 (16) | −0.00784 (14) | 0.00948 (14) | −0.00105 (13) |
Ba4 | 0.02144 (16) | 0.02400 (17) | 0.02287 (16) | −0.00041 (12) | 0.00565 (13) | 0.00096 (13) |
Ba5 | 0.02419 (17) | 0.02304 (17) | 0.02283 (16) | 0.00192 (12) | 0.00787 (13) | −0.00023 (13) |
Ba6 | 0.02409 (17) | 0.02563 (18) | 0.02670 (17) | 0.00063 (13) | 0.01159 (14) | −0.00140 (13) |
O1A | 0.048 (3) | 0.044 (3) | 0.049 (3) | 0.000 (2) | 0.032 (2) | 0.002 (2) |
O2A | 0.040 (3) | 0.047 (3) | 0.058 (3) | 0.007 (2) | 0.033 (2) | 0.015 (2) |
C1A | 0.038 (4) | 0.034 (3) | 0.036 (3) | −0.007 (3) | 0.018 (3) | −0.001 (3) |
C2A | 0.088 (6) | 0.064 (6) | 0.067 (5) | 0.032 (5) | 0.040 (5) | 0.029 (4) |
O1B | 0.069 (3) | 0.048 (3) | 0.065 (3) | −0.012 (3) | 0.050 (3) | −0.010 (2) |
O2B | 0.042 (2) | 0.041 (3) | 0.032 (2) | −0.007 (2) | 0.016 (2) | 0.0065 (19) |
C1B | 0.038 (3) | 0.036 (3) | 0.024 (3) | −0.007 (3) | 0.007 (3) | −0.002 (3) |
C2B | 0.070 (5) | 0.037 (4) | 0.063 (5) | 0.000 (4) | 0.035 (4) | 0.008 (3) |
O1C | 0.062 (3) | 0.061 (3) | 0.027 (2) | −0.027 (3) | 0.000 (2) | 0.008 (2) |
O2C | 0.039 (3) | 0.060 (3) | 0.049 (3) | −0.018 (2) | −0.008 (2) | 0.024 (2) |
C1C | 0.034 (3) | 0.038 (4) | 0.031 (3) | −0.006 (3) | 0.004 (3) | 0.003 (3) |
C2C | 0.057 (5) | 0.085 (6) | 0.039 (4) | −0.032 (4) | 0.007 (4) | 0.018 (4) |
O1D | 0.049 (3) | 0.034 (2) | 0.032 (2) | 0.006 (2) | 0.020 (2) | −0.0019 (18) |
O2D | 0.038 (3) | 0.040 (3) | 0.044 (3) | 0.008 (2) | 0.014 (2) | −0.003 (2) |
C1D | 0.041 (4) | 0.022 (3) | 0.024 (3) | 0.002 (2) | 0.009 (3) | 0.007 (2) |
C2D | 0.062 (5) | 0.041 (4) | 0.032 (3) | 0.001 (3) | 0.010 (3) | −0.002 (3) |
O1E | 0.045 (3) | 0.032 (2) | 0.037 (2) | 0.0051 (19) | 0.019 (2) | −0.0018 (19) |
O2E | 0.040 (2) | 0.035 (2) | 0.041 (2) | −0.0003 (19) | 0.025 (2) | −0.0041 (19) |
C1E | 0.037 (3) | 0.034 (3) | 0.016 (3) | 0.003 (3) | 0.006 (2) | −0.004 (2) |
C2E | 0.062 (5) | 0.033 (4) | 0.050 (4) | −0.008 (3) | 0.027 (4) | −0.008 (3) |
O1F | 0.033 (2) | 0.029 (2) | 0.069 (3) | −0.0045 (18) | 0.016 (2) | −0.017 (2) |
O2F | 0.036 (2) | 0.033 (2) | 0.029 (2) | −0.0014 (18) | 0.0098 (19) | −0.0016 (18) |
C1F | 0.022 (3) | 0.031 (3) | 0.026 (3) | 0.004 (2) | 0.006 (2) | 0.006 (2) |
C2F | 0.052 (4) | 0.046 (4) | 0.059 (5) | −0.013 (3) | 0.032 (4) | −0.008 (3) |
O1G | 0.064 (3) | 0.034 (2) | 0.037 (2) | 0.009 (2) | 0.026 (2) | 0.003 (2) |
O2G | 0.082 (4) | 0.041 (3) | 0.035 (2) | 0.009 (2) | 0.033 (3) | 0.002 (2) |
C1G | 0.043 (4) | 0.032 (4) | 0.037 (3) | 0.009 (3) | 0.011 (3) | 0.004 (3) |
C2G | 0.101 (7) | 0.030 (4) | 0.061 (5) | 0.013 (4) | 0.026 (5) | 0.009 (3) |
O1H | 0.033 (2) | 0.042 (3) | 0.044 (3) | 0.000 (2) | 0.010 (2) | −0.017 (2) |
O2H | 0.032 (2) | 0.034 (2) | 0.025 (2) | 0.0045 (17) | 0.0095 (18) | −0.0030 (17) |
C1H | 0.029 (3) | 0.031 (3) | 0.025 (3) | −0.003 (2) | 0.011 (2) | −0.001 (2) |
C2H | 0.035 (4) | 0.073 (5) | 0.061 (5) | 0.003 (4) | 0.014 (4) | −0.012 (4) |
O1I | 0.052 (3) | 0.066 (4) | 0.087 (4) | 0.016 (3) | 0.031 (3) | 0.029 (3) |
O2I | 0.083 (4) | 0.078 (4) | 0.087 (4) | −0.043 (3) | 0.064 (4) | −0.024 (3) |
C1I | 0.035 (4) | 0.047 (4) | 0.038 (3) | −0.012 (3) | 0.016 (3) | −0.001 (3) |
C2I | 0.058 (5) | 0.052 (5) | 0.093 (7) | 0.006 (4) | 0.015 (5) | 0.016 (5) |
O1J | 0.028 (2) | 0.043 (3) | 0.033 (2) | 0.0014 (19) | 0.0025 (18) | 0.0051 (19) |
O2J | 0.027 (2) | 0.034 (2) | 0.031 (2) | 0.0004 (17) | 0.0079 (18) | 0.0069 (17) |
C1J | 0.023 (3) | 0.024 (3) | 0.033 (3) | 0.001 (2) | 0.006 (3) | 0.007 (2) |
C2J | 0.032 (3) | 0.056 (4) | 0.046 (4) | 0.009 (3) | 0.020 (3) | 0.005 (3) |
O1K | 0.050 (3) | 0.065 (3) | 0.031 (2) | −0.003 (2) | 0.013 (2) | 0.011 (2) |
O2K | 0.046 (3) | 0.038 (2) | 0.033 (2) | −0.006 (2) | 0.021 (2) | 0.0028 (19) |
C1K | 0.039 (3) | 0.029 (3) | 0.037 (3) | 0.001 (3) | 0.019 (3) | 0.004 (3) |
C2K | 0.053 (5) | 0.072 (6) | 0.064 (5) | −0.007 (4) | 0.030 (4) | −0.004 (4) |
O1L | 0.034 (2) | 0.041 (2) | 0.022 (2) | −0.0002 (19) | 0.0042 (18) | −0.0077 (18) |
O2L | 0.029 (2) | 0.051 (3) | 0.033 (2) | −0.007 (2) | 0.0028 (19) | 0.001 (2) |
C1L | 0.025 (3) | 0.033 (3) | 0.037 (3) | −0.003 (2) | 0.015 (3) | −0.002 (3) |
C2L | 0.043 (4) | 0.100 (7) | 0.075 (6) | −0.012 (4) | 0.039 (4) | −0.040 (5) |
O1W | 0.028 (2) | 0.056 (3) | 0.040 (3) | 0.000 (2) | 0.011 (2) | −0.014 (2) |
O2W | 0.039 (3) | 0.068 (4) | 0.053 (3) | 0.004 (3) | 0.021 (2) | −0.001 (3) |
O3W | 0.043 (3) | 0.075 (4) | 0.048 (3) | 0.008 (3) | 0.011 (2) | −0.019 (3) |
O4W | 0.034 (7) | 0.093 (16) | 0.037 (10) | −0.013 (8) | 0.015 (8) | −0.009 (6) |
Geometric parameters (Å, º) top
Ba1—O3W | 2.695 (4) | O2C—C1C | 1.245 (7) |
Ba1—O1Bi | 2.754 (4) | C1C—C2C | 1.509 (9) |
Ba1—O2A | 2.763 (4) | C2C—H2CA | 0.9600 |
Ba1—O1Lii | 2.796 (4) | C2C—H2CB | 0.9600 |
Ba1—O1Eii | 2.799 (4) | C2C—H2CC | 0.9600 |
Ba1—O1H | 2.823 (4) | O1D—C1D | 1.259 (7) |
Ba1—O1Dii | 2.897 (4) | O2D—C1D | 1.246 (7) |
Ba1—O1A | 2.944 (4) | C1D—C2D | 1.513 (8) |
Ba1—O4W | 2.914 (14) | C2D—H2DA | 0.9600 |
Ba2—O2Ciii | 2.692 (4) | C2D—H2DB | 0.9600 |
Ba2—O2H | 2.736 (4) | C2D—H2DC | 0.9600 |
Ba2—O1G | 2.760 (4) | O1E—C1E | 1.256 (7) |
Ba2—O1K | 2.787 (5) | O2E—C1E | 1.245 (7) |
Ba2—O2J | 2.826 (4) | C1E—C2E | 1.513 (8) |
Ba2—O2G | 2.838 (4) | C2E—H2EA | 0.9600 |
Ba2—O2Fiii | 2.842 (4) | C2E—H2EB | 0.9600 |
Ba2—O2K | 2.875 (4) | C2E—H2EC | 0.9600 |
Ba2—O2L | 2.891 (4) | O1F—C1F | 1.244 (7) |
Ba3—O1Aiv | 2.686 (4) | O2F—C1F | 1.252 (7) |
Ba3—O1C | 2.689 (4) | C1F—C2F | 1.510 (8) |
Ba3—O1I | 2.770 (5) | C2F—H2FA | 0.9600 |
Ba3—O2L | 2.850 (4) | C2F—H2FB | 0.9600 |
Ba3—O2J | 2.850 (4) | C2F—H2FC | 0.9600 |
Ba3—O1B | 2.899 (5) | O1G—C1G | 1.262 (7) |
Ba3—O2H | 2.904 (4) | O2G—C1G | 1.249 (7) |
Ba3—O1J | 2.940 (4) | C1G—C2G | 1.501 (9) |
Ba3—O2B | 2.962 (4) | C2G—H2GA | 0.9600 |
Ba4—O2K | 2.671 (4) | C2G—H2GB | 0.9600 |
Ba4—O1H | 2.782 (4) | C2G—H2GC | 0.9600 |
Ba4—O1Dii | 2.799 (4) | O1H—C1H | 1.243 (7) |
Ba4—O1C | 2.824 (4) | O2H—C1H | 1.263 (7) |
Ba4—O2C | 2.838 (4) | C1H—C2H | 1.501 (8) |
Ba4—O2H | 2.855 (4) | C2H—H2HA | 0.9600 |
Ba4—O1F | 2.860 (4) | C2H—H2HB | 0.9600 |
Ba4—O2F | 2.925 (4) | C2H—H2HC | 0.9600 |
Ba4—O1Lii | 2.978 (4) | O1I—C1I | 1.231 (8) |
Ba4—O1J | 3.075 (4) | O2I—C1I | 1.232 (7) |
Ba5—O2Fiii | 2.715 (4) | C1I—C2I | 1.477 (10) |
Ba5—O2E | 2.778 (4) | C2I—H2IA | 0.9600 |
Ba5—O2B | 2.802 (4) | C2I—H2IB | 0.9600 |
Ba5—O2W | 2.854 (5) | C2I—H2IC | 0.9600 |
Ba5—O1L | 2.878 (4) | O1J—C1J | 1.267 (6) |
Ba5—O1E | 2.917 (4) | O2J—C1J | 1.253 (6) |
Ba5—O2J | 2.928 (4) | C1J—C2J | 1.500 (8) |
Ba5—O1D | 2.962 (4) | C2J—H2JA | 0.9600 |
Ba5—O2L | 3.016 (5) | C2J—H2JB | 0.9600 |
Ba5—O2D | 3.035 (4) | C2J—H2JC | 0.9600 |
Ba6—O2Gii | 2.651 (4) | O1K—C1K | 1.248 (7) |
Ba6—O2I | 2.686 (5) | O2K—C1K | 1.262 (7) |
Ba6—O2Ev | 2.688 (4) | C1K—C2K | 1.497 (9) |
Ba6—O1F | 2.719 (4) | C2K—H2KA | 0.9600 |
Ba6—O1W | 2.721 (4) | C2K—H2KB | 0.9600 |
Ba6—O2Dv | 2.760 (4) | C2K—H2KC | 0.9600 |
Ba6—O1J | 2.800 (4) | O1L—C1L | 1.249 (7) |
O1A—C1A | 1.244 (7) | O2L—C1L | 1.252 (7) |
O2A—C1A | 1.248 (7) | C1L—C2L | 1.510 (8) |
C1A—C2A | 1.523 (9) | C2L—H2LA | 0.9600 |
C2A—H2AA | 0.9600 | C2L—H2LB | 0.9600 |
C2A—H2AB | 0.9600 | C2L—H2LC | 0.9600 |
C2A—H2AC | 0.9600 | O1W—H1WA | 0.85 (4) |
O1B—C1B | 1.248 (7) | O1W—H1WB | 0.85 (4) |
O2B—C1B | 1.248 (7) | O2W—H2WA | 0.85 (4) |
C1B—C2B | 1.502 (9) | O2W—H2WB | 0.85 (4) |
C2B—H2BA | 0.9600 | O3W—H3WA | 0.85 (4) |
C2B—H2BB | 0.9600 | O3W—H3WB | 0.85 (4) |
C2B—H2BC | 0.9600 | O4W—H4WB | 0.85 (4) |
O1C—C1C | 1.239 (7) | O4W—H4WA | 0.85 (4) |
| | | |
O3W—Ba1—O1Bi | 80.98 (16) | O1F—Ba6—O2Dv | 151.91 (13) |
O3W—Ba1—O2A | 71.83 (16) | O1W—Ba6—O2Dv | 83.50 (14) |
O1Bi—Ba1—O2A | 113.43 (13) | O2Gii—Ba6—O1J | 117.30 (14) |
O3W—Ba1—O1Lii | 137.68 (15) | O2I—Ba6—O1J | 71.59 (17) |
O1Bi—Ba1—O1Lii | 107.97 (13) | O2Ev—Ba6—O1J | 92.30 (13) |
O2A—Ba1—O1Lii | 132.92 (12) | O1F—Ba6—O1J | 68.96 (12) |
O3W—Ba1—O1Eii | 144.56 (16) | O1W—Ba6—O1J | 136.00 (14) |
O1Bi—Ba1—O1Eii | 108.89 (14) | O2Dv—Ba6—O1J | 130.54 (12) |
O2A—Ba1—O1Eii | 73.08 (13) | C1A—O1A—Ba3i | 148.1 (4) |
O1Lii—Ba1—O1Eii | 73.14 (12) | C1A—O1A—Ba1 | 89.7 (4) |
O3W—Ba1—O1H | 70.74 (15) | Ba3i—O1A—Ba1 | 110.11 (14) |
O1Bi—Ba1—O1H | 96.18 (14) | C1A—O2A—Ba1 | 98.2 (4) |
O2A—Ba1—O1H | 126.98 (14) | O1A—C1A—O2A | 124.0 (6) |
O1Lii—Ba1—O1H | 67.23 (12) | O1A—C1A—C2A | 118.6 (6) |
O1Eii—Ba1—O1H | 138.02 (12) | O2A—C1A—C2A | 117.4 (6) |
O3W—Ba1—O1Dii | 105.97 (14) | C1A—C2A—H2AA | 109.5 |
O1Bi—Ba1—O1Dii | 165.55 (13) | C1A—C2A—H2AB | 109.5 |
O2A—Ba1—O1Dii | 80.96 (12) | H2AA—C2A—H2AB | 109.5 |
O1Lii—Ba1—O1Dii | 58.31 (11) | C1A—C2A—H2AC | 109.5 |
O1Eii—Ba1—O1Dii | 73.00 (12) | H2AA—C2A—H2AC | 109.5 |
O1H—Ba1—O1Dii | 74.85 (12) | H2AB—C2A—H2AC | 109.5 |
O3W—Ba1—O1A | 67.52 (15) | C1B—O1B—Ba1iv | 149.4 (4) |
O1Bi—Ba1—O1A | 68.35 (13) | C1B—O1B—Ba3 | 93.2 (4) |
O2A—Ba1—O1A | 45.23 (12) | Ba1iv—O1B—Ba3 | 109.51 (15) |
O1Lii—Ba1—O1A | 154.69 (12) | C1B—O2B—Ba5 | 126.6 (4) |
O1Eii—Ba1—O1A | 84.26 (12) | C1B—O2B—Ba3 | 90.3 (4) |
O1H—Ba1—O1A | 137.15 (13) | Ba5—O2B—Ba3 | 100.41 (13) |
O1Dii—Ba1—O1A | 125.89 (11) | O2B—C1B—O1B | 122.5 (6) |
O3W—Ba1—O4W | 138.7 (4) | O2B—C1B—C2B | 119.4 (6) |
O1Bi—Ba1—O4W | 57.9 (4) | O1B—C1B—C2B | 118.1 (6) |
O2A—Ba1—O4W | 118.6 (4) | C1B—C2B—H2BA | 109.5 |
O1Lii—Ba1—O4W | 67.3 (5) | C1B—C2B—H2BB | 109.5 |
O1Eii—Ba1—O4W | 59.0 (4) | H2BA—C2B—H2BB | 109.5 |
O1H—Ba1—O4W | 114.4 (4) | C1B—C2B—H2BC | 109.5 |
O1Dii—Ba1—O4W | 115.0 (4) | H2BA—C2B—H2BC | 109.5 |
O1A—Ba1—O4W | 91.5 (5) | H2BB—C2B—H2BC | 109.5 |
O2Ciii—Ba2—O2H | 111.09 (15) | C1C—O1C—Ba3 | 149.8 (5) |
O2Ciii—Ba2—O1G | 77.92 (14) | C1C—O1C—Ba4 | 96.6 (4) |
O2H—Ba2—O1G | 75.71 (12) | Ba3—O1C—Ba4 | 104.77 (14) |
O2Ciii—Ba2—O1K | 129.88 (15) | C1C—O2C—Ba2ii | 150.5 (4) |
O2H—Ba2—O1K | 116.66 (12) | C1C—O2C—Ba4 | 95.7 (4) |
O1G—Ba2—O1K | 99.46 (15) | Ba2ii—O2C—Ba4 | 108.60 (16) |
O2Ciii—Ba2—O2J | 127.01 (13) | O1C—C1C—O2C | 122.4 (6) |
O2H—Ba2—O2J | 75.15 (11) | O1C—C1C—C2C | 118.7 (6) |
O1G—Ba2—O2J | 147.22 (12) | O2C—C1C—C2C | 118.7 (6) |
O1K—Ba2—O2J | 80.67 (13) | C1C—C2C—H2CA | 109.5 |
O2Ciii—Ba2—O2G | 70.44 (16) | C1C—C2C—H2CB | 109.5 |
O2H—Ba2—O2G | 121.12 (12) | H2CA—C2C—H2CB | 109.5 |
O1G—Ba2—O2G | 46.14 (12) | C1C—C2C—H2CC | 109.5 |
O1K—Ba2—O2G | 72.66 (14) | H2CA—C2C—H2CC | 109.5 |
O2J—Ba2—O2G | 152.92 (12) | H2CB—C2C—H2CC | 109.5 |
O2Ciii—Ba2—O2Fiii | 76.30 (13) | C1D—O1D—Ba4iii | 125.7 (4) |
O2H—Ba2—O2Fiii | 139.81 (12) | C1D—O1D—Ba1iii | 128.6 (4) |
O1G—Ba2—O2Fiii | 142.26 (12) | Ba4iii—O1D—Ba1iii | 99.45 (12) |
O1K—Ba2—O2Fiii | 77.17 (13) | C1D—O1D—Ba5 | 97.8 (3) |
O2J—Ba2—O2Fiii | 70.12 (11) | Ba4iii—O1D—Ba5 | 99.51 (12) |
O2G—Ba2—O2Fiii | 98.83 (12) | Ba1iii—O1D—Ba5 | 97.43 (12) |
O2Ciii—Ba2—O2K | 161.04 (14) | C1D—O2D—Ba6v | 124.5 (4) |
O2H—Ba2—O2K | 71.17 (12) | C1D—O2D—Ba5 | 94.6 (3) |
O1G—Ba2—O2K | 84.71 (13) | Ba6v—O2D—Ba5 | 103.69 (14) |
O1K—Ba2—O2K | 45.68 (12) | O2D—C1D—O1D | 123.1 (5) |
O2J—Ba2—O2K | 71.94 (12) | O2D—C1D—C2D | 119.5 (6) |
O2G—Ba2—O2K | 92.06 (13) | O1D—C1D—C2D | 117.4 (6) |
O2Fiii—Ba2—O2K | 114.78 (12) | C1D—C2D—H2DA | 109.5 |
O2Ciii—Ba2—O2L | 73.16 (15) | C1D—C2D—H2DB | 109.5 |
O2H—Ba2—O2L | 70.74 (12) | H2DA—C2D—H2DB | 109.5 |
O1G—Ba2—O2L | 122.94 (13) | C1D—C2D—H2DC | 109.5 |
O1K—Ba2—O2L | 136.64 (14) | H2DA—C2D—H2DC | 109.5 |
O2J—Ba2—O2L | 59.19 (12) | H2DB—C2D—H2DC | 109.5 |
O2G—Ba2—O2L | 143.52 (13) | C1E—O1E—Ba1iii | 129.3 (4) |
O2Fiii—Ba2—O2L | 74.41 (12) | C1E—O1E—Ba5 | 92.4 (4) |
O2K—Ba2—O2L | 123.65 (11) | Ba1iii—O1E—Ba5 | 100.72 (13) |
O1Aiv—Ba3—O1C | 91.28 (15) | C1E—O2E—Ba6v | 137.8 (4) |
O1Aiv—Ba3—O1I | 86.27 (15) | C1E—O2E—Ba5 | 99.3 (3) |
O1C—Ba3—O1I | 77.15 (17) | Ba6v—O2E—Ba5 | 113.08 (14) |
O1Aiv—Ba3—O2L | 86.95 (13) | O2E—C1E—O1E | 122.3 (6) |
O1C—Ba3—O2L | 133.38 (14) | O2E—C1E—C2E | 117.4 (5) |
O1I—Ba3—O2L | 148.86 (15) | O1E—C1E—C2E | 120.2 (6) |
O1Aiv—Ba3—O2J | 146.14 (12) | C1E—C2E—H2EA | 109.5 |
O1C—Ba3—O2J | 108.64 (13) | C1E—C2E—H2EB | 109.5 |
O1I—Ba3—O2J | 124.07 (14) | H2EA—C2E—H2EB | 109.5 |
O2L—Ba3—O2J | 59.39 (11) | C1E—C2E—H2EC | 109.5 |
O1Aiv—Ba3—O1B | 69.90 (13) | H2EA—C2E—H2EC | 109.5 |
O1C—Ba3—O1B | 142.30 (14) | H2EB—C2E—H2EC | 109.5 |
O1I—Ba3—O1B | 69.51 (17) | C1F—O1F—Ba6 | 145.8 (4) |
O2L—Ba3—O1B | 79.61 (14) | C1F—O1F—Ba4 | 92.9 (3) |
O2J—Ba3—O1B | 104.44 (12) | Ba6—O1F—Ba4 | 107.79 (14) |
O1Aiv—Ba3—O2H | 93.48 (12) | C1F—O2F—Ba5ii | 140.4 (4) |
O1C—Ba3—O2H | 64.62 (13) | C1F—O2F—Ba2ii | 110.9 (3) |
O1I—Ba3—O2H | 141.76 (15) | Ba5ii—O2F—Ba2ii | 103.24 (13) |
O2L—Ba3—O2H | 69.00 (11) | C1F—O2F—Ba4 | 89.7 (3) |
O2J—Ba3—O2H | 72.23 (11) | Ba5ii—O2F—Ba4 | 102.41 (13) |
O1B—Ba3—O2H | 145.34 (13) | Ba2ii—O2F—Ba4 | 102.29 (13) |
O1Aiv—Ba3—O1J | 160.48 (13) | O1F—C1F—O2F | 122.1 (5) |
O1C—Ba3—O1J | 69.82 (14) | O1F—C1F—C2F | 119.2 (5) |
O1I—Ba3—O1J | 93.90 (14) | O2F—C1F—C2F | 118.7 (5) |
O2L—Ba3—O1J | 102.31 (12) | C1F—C2F—H2FA | 109.5 |
O2J—Ba3—O1J | 44.83 (11) | C1F—C2F—H2FB | 109.5 |
O1B—Ba3—O1J | 128.32 (13) | H2FA—C2F—H2FB | 109.5 |
O2H—Ba3—O1J | 74.37 (11) | C1F—C2F—H2FC | 109.5 |
O1Aiv—Ba3—O2B | 113.39 (12) | H2FA—C2F—H2FC | 109.5 |
O1C—Ba3—O2B | 143.49 (15) | H2FB—C2F—H2FC | 109.5 |
O1I—Ba3—O2B | 78.07 (15) | C1G—O1G—Ba2 | 97.6 (4) |
O2L—Ba3—O2B | 76.89 (12) | C1G—O2G—Ba6iii | 143.8 (4) |
O2J—Ba3—O2B | 65.43 (11) | C1G—O2G—Ba2 | 94.2 (4) |
O1B—Ba3—O2B | 43.85 (12) | Ba6iii—O2G—Ba2 | 118.74 (16) |
O2H—Ba3—O2B | 135.06 (11) | O2G—C1G—O1G | 121.9 (6) |
O1J—Ba3—O2B | 85.64 (12) | O2G—C1G—C2G | 118.9 (6) |
O2K—Ba4—O1H | 98.82 (13) | O1G—C1G—C2G | 119.2 (6) |
O2K—Ba4—O1Dii | 78.39 (12) | C1G—C2G—H2GA | 109.5 |
O1H—Ba4—O1Dii | 77.08 (13) | C1G—C2G—H2GB | 109.5 |
O2K—Ba4—O1C | 122.03 (13) | H2GA—C2G—H2GB | 109.5 |
O1H—Ba4—O1C | 76.89 (15) | C1G—C2G—H2GC | 109.5 |
O1Dii—Ba4—O1C | 149.07 (14) | H2GA—C2G—H2GC | 109.5 |
O2K—Ba4—O2C | 156.01 (15) | H2GB—C2G—H2GC | 109.5 |
O1H—Ba4—O2C | 96.91 (15) | C1H—O1H—Ba4 | 96.6 (3) |
O1Dii—Ba4—O2C | 122.98 (13) | C1H—O1H—Ba1 | 149.8 (4) |
O1C—Ba4—O2C | 45.23 (12) | Ba4—O1H—Ba1 | 101.67 (13) |
O2K—Ba4—O2H | 72.40 (12) | C1H—O2H—Ba2 | 123.3 (4) |
O1H—Ba4—O2H | 46.20 (11) | C1H—O2H—Ba4 | 92.6 (3) |
O1Dii—Ba4—O2H | 107.81 (12) | Ba2—O2H—Ba4 | 107.61 (13) |
O1C—Ba4—O2H | 63.66 (12) | C1H—O2H—Ba3 | 128.9 (4) |
O2C—Ba4—O2H | 106.85 (12) | Ba2—O2H—Ba3 | 100.27 (12) |
O2K—Ba4—O1F | 83.44 (14) | Ba4—O2H—Ba3 | 98.65 (11) |
O1H—Ba4—O1F | 177.56 (13) | O1H—C1H—O2H | 124.0 (5) |
O1Dii—Ba4—O1F | 102.57 (12) | O1H—C1H—C2H | 118.8 (6) |
O1C—Ba4—O1F | 102.73 (15) | O2H—C1H—C2H | 117.2 (5) |
O2C—Ba4—O1F | 81.24 (15) | C1H—C2H—H2HA | 109.5 |
O2H—Ba4—O1F | 135.83 (11) | C1H—C2H—H2HB | 109.5 |
O2K—Ba4—O2F | 107.99 (12) | H2HA—C2H—H2HB | 109.5 |
O1H—Ba4—O2F | 133.59 (12) | C1H—C2H—H2HC | 109.5 |
O1Dii—Ba4—O2F | 72.32 (12) | H2HA—C2H—H2HC | 109.5 |
O1C—Ba4—O2F | 116.04 (12) | H2HB—C2H—H2HC | 109.5 |
O2C—Ba4—O2F | 72.79 (12) | C1I—O1I—Ba3 | 120.3 (4) |
O2H—Ba4—O2F | 179.61 (11) | C1I—O2I—Ba6 | 152.8 (5) |
O1F—Ba4—O2F | 44.36 (11) | O1I—C1I—O2I | 123.0 (7) |
O2K—Ba4—O1Lii | 134.83 (12) | O1I—C1I—C2I | 117.6 (6) |
O1H—Ba4—O1Lii | 65.28 (12) | O2I—C1I—C2I | 119.3 (7) |
O1Dii—Ba4—O1Lii | 57.31 (11) | C1I—C2I—H2IA | 109.5 |
O1C—Ba4—O1Lii | 96.37 (13) | C1I—C2I—H2IB | 109.5 |
O2C—Ba4—O1Lii | 68.63 (14) | H2IA—C2I—H2IB | 109.5 |
O2H—Ba4—O1Lii | 110.80 (11) | C1I—C2I—H2IC | 109.5 |
O1F—Ba4—O1Lii | 112.45 (12) | H2IA—C2I—H2IC | 109.5 |
O2F—Ba4—O1Lii | 68.94 (11) | H2IB—C2I—H2IC | 109.5 |
O2K—Ba4—O1J | 66.16 (12) | C1J—O1J—Ba6 | 125.3 (4) |
O1H—Ba4—O1J | 118.31 (11) | C1J—O1J—Ba3 | 92.7 (3) |
O1Dii—Ba4—O1J | 142.69 (11) | Ba6—O1J—Ba3 | 121.13 (15) |
O1C—Ba4—O1J | 66.19 (13) | C1J—O1J—Ba4 | 121.2 (3) |
O2C—Ba4—O1J | 90.42 (14) | Ba6—O1J—Ba4 | 100.12 (12) |
O2H—Ba4—O1J | 73.02 (11) | Ba3—O1J—Ba4 | 93.10 (12) |
O1F—Ba4—O1J | 63.42 (11) | C1J—O2J—Ba2 | 118.5 (3) |
O2F—Ba4—O1J | 107.11 (11) | C1J—O2J—Ba3 | 97.3 (3) |
O1Lii—Ba4—O1J | 159.00 (11) | Ba2—O2J—Ba3 | 99.45 (12) |
O2Fiii—Ba5—O2E | 141.70 (12) | C1J—O2J—Ba5 | 135.5 (4) |
O2Fiii—Ba5—O2B | 136.29 (12) | Ba2—O2J—Ba5 | 98.46 (11) |
O2E—Ba5—O2B | 80.70 (12) | Ba3—O2J—Ba5 | 100.13 (12) |
O2Fiii—Ba5—O2W | 92.40 (14) | O2J—C1J—O1J | 122.5 (5) |
O2E—Ba5—O2W | 75.13 (14) | O2J—C1J—C2J | 118.3 (5) |
O2B—Ba5—O2W | 89.97 (14) | O1J—C1J—C2J | 119.2 (5) |
O2Fiii—Ba5—O1L | 73.29 (12) | C1J—C2J—H2JA | 109.5 |
O2E—Ba5—O1L | 111.15 (12) | C1J—C2J—H2JB | 109.5 |
O2B—Ba5—O1L | 105.76 (12) | H2JA—C2J—H2JB | 109.5 |
O2W—Ba5—O1L | 163.68 (14) | C1J—C2J—H2JC | 109.5 |
O2Fiii—Ba5—O1E | 138.19 (12) | H2JA—C2J—H2JC | 109.5 |
O2E—Ba5—O1E | 45.16 (11) | H2JB—C2J—H2JC | 109.5 |
O2B—Ba5—O1E | 74.31 (12) | C1K—O1K—Ba2 | 98.2 (4) |
O2W—Ba5—O1E | 119.54 (14) | C1K—O2K—Ba4 | 156.9 (4) |
O1L—Ba5—O1E | 70.22 (12) | C1K—O2K—Ba2 | 93.6 (4) |
O2Fiii—Ba5—O2J | 70.36 (11) | Ba4—O2K—Ba2 | 108.82 (14) |
O2E—Ba5—O2J | 141.09 (12) | O1K—C1K—O2K | 122.4 (6) |
O2B—Ba5—O2J | 66.48 (11) | O1K—C1K—C2K | 118.9 (6) |
O2W—Ba5—O2J | 84.19 (13) | O2K—C1K—C2K | 118.6 (6) |
O1L—Ba5—O2J | 97.90 (11) | C1K—C2K—H2KA | 109.5 |
O1E—Ba5—O2J | 134.06 (11) | C1K—C2K—H2KB | 109.5 |
O2Fiii—Ba5—O1D | 72.89 (11) | H2KA—C2K—H2KB | 109.5 |
O2E—Ba5—O1D | 78.60 (12) | C1K—C2K—H2KC | 109.5 |
O2B—Ba5—O1D | 144.24 (12) | H2KA—C2K—H2KC | 109.5 |
O2W—Ba5—O1D | 112.18 (13) | H2KB—C2K—H2KC | 109.5 |
O1L—Ba5—O1D | 56.71 (11) | C1L—O1L—Ba1iii | 132.1 (4) |
O1E—Ba5—O1D | 70.39 (12) | C1L—O1L—Ba5 | 99.8 (3) |
O2J—Ba5—O1D | 140.24 (11) | Ba1iii—O1L—Ba5 | 101.77 (13) |
O2Fiii—Ba5—O2L | 74.24 (12) | C1L—O1L—Ba4iii | 121.3 (4) |
O2E—Ba5—O2L | 136.21 (12) | Ba1iii—O1L—Ba4iii | 97.60 (11) |
O2B—Ba5—O2L | 76.72 (12) | Ba5—O1L—Ba4iii | 97.35 (12) |
O2W—Ba5—O2L | 140.87 (13) | C1L—O2L—Ba3 | 143.6 (4) |
O1L—Ba5—O2L | 43.46 (11) | C1L—O2L—Ba2 | 115.6 (4) |
O1E—Ba5—O2L | 92.35 (11) | Ba3—O2L—Ba2 | 97.92 (12) |
O2J—Ba5—O2L | 56.71 (11) | C1L—O2L—Ba5 | 93.1 (3) |
O1D—Ba5—O2L | 98.99 (11) | Ba3—O2L—Ba5 | 98.07 (13) |
O2Fiii—Ba5—O2D | 80.41 (12) | Ba2—O2L—Ba5 | 95.05 (12) |
O2E—Ba5—O2D | 61.30 (12) | O1L—C1L—O2L | 121.9 (5) |
O2B—Ba5—O2D | 139.97 (12) | O1L—C1L—C2L | 119.4 (5) |
O2W—Ba5—O2D | 69.56 (13) | O2L—C1L—C2L | 118.7 (6) |
O1L—Ba5—O2D | 99.65 (11) | C1L—C2L—H2LA | 109.5 |
O1E—Ba5—O2D | 86.17 (12) | C1L—C2L—H2LB | 109.5 |
O2J—Ba5—O2D | 139.66 (11) | H2LA—C2L—H2LB | 109.5 |
O1D—Ba5—O2D | 43.06 (11) | C1L—C2L—H2LC | 109.5 |
O2L—Ba5—O2D | 139.85 (11) | H2LA—C2L—H2LC | 109.5 |
O2Gii—Ba6—O2I | 88.67 (16) | H2LB—C2L—H2LC | 109.5 |
O2Gii—Ba6—O2Ev | 148.78 (14) | Ba6—O1W—H1WA | 131 (4) |
O2I—Ba6—O2Ev | 111.41 (15) | Ba6—O1W—H1WB | 114 (4) |
O2Gii—Ba6—O1F | 85.98 (14) | H1WA—O1W—H1WB | 111 (4) |
O2I—Ba6—O1F | 131.98 (16) | Ba5—O2W—H2WA | 133 (4) |
O2Ev—Ba6—O1F | 96.54 (13) | Ba5—O2W—H2WB | 114 (4) |
O2Gii—Ba6—O1W | 75.60 (15) | H2WA—O2W—H2WB | 112 (4) |
O2I—Ba6—O1W | 152.22 (18) | Ba1—O3W—H3WA | 114 (5) |
O2Ev—Ba6—O1W | 75.99 (13) | Ba1—O3W—H3WB | 126 (5) |
O1F—Ba6—O1W | 70.49 (14) | H3WA—O3W—H3WB | 112 (4) |
O2Gii—Ba6—O2Dv | 97.96 (14) | Ba1—O4W—H4WB | 117 (10) |
O2I—Ba6—O2Dv | 76.06 (16) | Ba1—O4W—H4WA | 124 (10) |
O2Ev—Ba6—O2Dv | 66.10 (13) | H4WB—O4W—H4WA | 111 (4) |
Symmetry codes: (i) −x+1/2, y+1/2, −z+1/2; (ii) x+1/2, −y+1/2, z+1/2; (iii) x−1/2, −y+1/2, z−1/2; (iv) −x+1/2, y−1/2, −z+1/2; (v) −x+1, −y, −z. |
Hydrogen-bond geometry (Å, º) top
D—H···A | D—H | H···A | D···A | D—H···A |
O1W—H1WA···O2Avi | 0.85 (4) | 1.88 (4) | 2.728 (6) | 173 (8) |
O1W—H1WB···O1Kii | 0.85 (4) | 1.95 (4) | 2.731 (6) | 153 (7) |
O2W—H2WA···O2Bv | 0.85 (4) | 2.26 (4) | 3.015 (6) | 149 (6) |
O2W—H2WB···O2Iv | 0.85 (4) | 1.93 (4) | 2.740 (7) | 158 (8) |
O3W—H3WA···O1G | 0.85 (4) | 1.91 (4) | 2.746 (6) | 170 (7) |
O3W—H3WB···O1Ii | 0.85 (4) | 1.91 (4) | 2.702 (7) | 155 (6) |
O4W—H4WA···O1Ei | 0.85 (4) | 2.05 (5) | 2.885 (19) | 166 (15) |
O4W—H4WB···O1Bii | 0.85 (4) | 2.33 (7) | 3.130 (17) | 157 (18) |
Symmetry codes: (i) −x+1/2, y+1/2, −z+1/2; (ii) x+1/2, −y+1/2, z+1/2; (v) −x+1, −y, −z; (vi) −x+3/2, y−1/2, −z+1/2. |
Experimental details
Crystal data |
Chemical formula | [Ba6(C2H3O2)12(H2O)3.5] |
Mr | 1595.62 |
Crystal system, space group | Monoclinic, P21/n |
Temperature (K) | 294 |
a, b, c (Å) | 14.040 (3), 19.903 (4), 17.721 (4) |
β (°) | 113.19 (3) |
V (Å3) | 4551.6 (19) |
Z | 4 |
Radiation type | Mo Kα |
µ (mm−1) | 5.19 |
Crystal size (mm) | 0.36 × 0.24 × 0.20 |
|
Data collection |
Diffractometer | Bruker SMART? CCD area-detector diffractometer |
Absorption correction | Multi-scan (SADABS; Sheldrick, 2001) |
Tmin, Tmax | 0.24, 0.36 |
No. of measured, independent and observed [I > 2σ(I)] reflections | 38138, 10282, 8906 |
Rint | 0.042 |
(sin θ/λ)max (Å−1) | 0.661 |
|
Refinement |
R[F2 > 2σ(F2)], wR(F2), S | 0.040, 0.087, 1.11 |
No. of reflections | 10282 |
No. of parameters | 559 |
No. of restraints | 13 |
H-atom treatment | H atoms treated by a mixture of independent and constrained refinement |
Δρmax, Δρmin (e Å−3) | 1.21, −0.79 |
Hydrogen-bond geometry (Å, º) top
D—H···A | D—H | H···A | D···A | D—H···A |
O1W—H1WA···O2Ai | 0.85 (4) | 1.88 (4) | 2.728 (6) | 173 (8) |
O1W—H1WB···O1Kii | 0.85 (4) | 1.95 (4) | 2.731 (6) | 153 (7) |
O2W—H2WA···O2Biii | 0.85 (4) | 2.26 (4) | 3.015 (6) | 149 (6) |
O2W—H2WB···O2Iiii | 0.85 (4) | 1.93 (4) | 2.740 (7) | 158 (8) |
O3W—H3WA···O1G | 0.85 (4) | 1.91 (4) | 2.746 (6) | 170 (7) |
O3W—H3WB···O1Iiv | 0.85 (4) | 1.91 (4) | 2.702 (7) | 155 (6) |
O4W—H4WA···O1Eiv | 0.85 (4) | 2.05 (5) | 2.885 (19) | 166 (15) |
O4W—H4WB···O1Bii | 0.85 (4) | 2.33 (7) | 3.130 (17) | 157 (18) |
Symmetry codes: (i) −x+3/2, y−1/2, −z+1/2; (ii) x+1/2, −y+1/2, z+1/2; (iii) −x+1, −y, −z; (iv) −x+1/2, y+1/2, −z+1/2. |
Selected structural parameters of the Ba coordination environments in (I) topCompound | Cation (coordination number) | Bond valencea | Average Ba—O (Å) | Range of Ba—O (Å) |
(I)b | Ba1(8/9) | 1.98/2.16 | 2.81 (8)/2.82 (8) | 2.695 (4)–2.944 (4) |
| Ba2(9) | 2.24 | 2.81 (7) | 2.692 (4)–2.891 (4) |
| Ba3(9) | 2.09 | 2.84 (10) | 2.686 (4)–2.962 (4) |
| Ba4(10) | 2.20 | 2.85 (11) | 2.671 (4)–3.075 (4) |
| Ba5(10) | 2.03 | 2.90 (10) | 2.715 (4)–3.035 (4) |
| Ba6(7) | 2.19 | 2.72 (5) | 2.651 (4)–2.800 (4) |
(II)c | Ba1(8) | 2.01 | 2.81 (7) | 2.691–2.927 |
(III)d | Ba1(8) | 2.22 | 2.81 (7) | 2.641–3.083 |
| Ba2(9) | 2.10 | 2.72 (5) | 2.711–2.927 |
References: (a) Brown & Altermatt (1985); (b) this work; (c) Groombridge et al. (1985); (d) Gautier-Luneau & Mosset (1988). |
The title compound, (I), is the serendipitous product of unsuccessful attempts to replicate the reportedly simple and reproducible preparation of barium acetate trihydrate, Ba(C2H3O2)2·3H2O (Maneva & Nikolova, 1988), which has been characterized by an IR vibrational study. The structure of (I) can be compared with those of the monohydrate, Ba(C2H3O2)2·H2O, (II) (Groombridge et al. 1985), and the anhydrous barium acetate, Ba(C2H3O2)2, (III) (Gautier-Luneau & Mosset, 1988).
The complex asymmetric unit of (I) is shown in Fig. 1; the 12 independent acetate ligands are distiguished from one another by suffixes A–L. Table 1 displays relevant data concerning the different Ba coordination polyhedra for crystallographically independent atoms Ba1–Ba6 in (I), along with similar data for (II) and (III). For a complete survey in the case of (I), see the Supplementary material. The bond distances given in Table 1 show no significant differences (on average) between the three known structures. The structures differ, however, in the number of independent Ba atoms and, especially for (I), in the diversity of coordination numbers observed. In (I), the coordination number for Ba1 (8 or 9, average 8.5) arises because of the disorder of a coordinating water molecule (O4W) over two sites related by a crystallographic centre of symmetry at (1/2, 1/2, 1/2) and therefore bonded to one or other (but not both simultaneously) of a pair of similarly symmetry-related Ba1 atoms.
In (I),the summation of the coordination numbers given in Table 1 shows the presence of 53.5 Ba—O bonds. Of these, three and a half involve coordinating water molecules and the remainder are bonds to acetate ligands. All of the acetate ligands, with the sole exception of ligand I, chelate Ba centres as bidentate ligands with bite angles in the range 43.06 (11)–46.14 (12)° [mean 44.8(1.0)°] and at rather long Ba—O distances [mean 2.83 (10) Å]. The bite angles contribute, to some extent, to the somewhat irregular coordination of the Ba cations. This leaves 27 Ba—Oacetate bonds to create connectivity between different Ba centres. As a consequence, the connectivity of each acetate ligand ranges from a maximum of five different Ba cations (for acetate J) to a minimum of two (for acetates A, G and K). This results in complete three-dimensional connectivity between the Ba centres, which are then separated by Ba···Ba distances in the range 4.330 (2)–4.724 (2) Å. Fundamental to the three-dimensional connectivity are ribbons of BaOn polyhedra propagateing in the [101] direction and whose width is in the [010] direction (Fig. 2). As shown in Fig. 3, these ribbons are interconnected in the [101] direction but, in terms of the number of Ba—O bonds, with weaker connectivity than is present in the ribbons themselves. Clearly seen in Fig. 3 are the channels containing hydrophobic methyl groups running through the structure created by the packing of the ribbons.
As shown in Table 2, all of the H atoms of the water molecules participate in hydrogen-bond formation. This also contributes to the three-dimensional connectivity of the structure of (I).