The title compound, [Y
2(C
4H
5O
2)
6(H
2O)
4]
2·4.6H
2O, has two independent dimeric units, displaying different bridging patterns between metal ions which lead to dissimilar Y
Y distances. The compound is isostructural with an already reported Gd complex.
Supporting information
CCDC reference: 630443
Key indicators
- Single-crystal X-ray study
- T = 298 K
- Mean (C-C) = 0.006 Å
- H-atom completeness 99%
- Disorder in main residue
- R factor = 0.043
- wR factor = 0.112
- Data-to-parameter ratio = 17.6
checkCIF/PLATON results
No syntax errors found
Alert level B
PLAT420_ALERT_2_B D-H Without Acceptor O1W - H1WB ... ?
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
PLAT068_ALERT_1_C Reported F000 Differs from Calcd (or Missing)... ?
PLAT220_ALERT_2_C Large Non-Solvent C Ueq(max)/Ueq(min) ... 2.81 Ratio
PLAT220_ALERT_2_C Large Non-Solvent C Ueq(max)/Ueq(min) ... 2.69 Ratio
PLAT242_ALERT_2_C Check Low Ueq as Compared to Neighbors for C33
PLAT301_ALERT_3_C Main Residue Disorder ......................... 5.00 Perc.
PLAT302_ALERT_4_C Anion/Solvent Disorder ......................... 10.00 Perc.
PLAT311_ALERT_2_C Isolated Disordered Oxygen Atom (No H's ?) ..... <O7W
PLAT720_ALERT_4_C Number of Unusual/Non-Standard Label(s) ........ 12
Alert level G
FORMU01_ALERT_2_G There is a discrepancy between the atom counts in the
_chemical_formula_sum and the formula from the _atom_site* data.
Atom count from _chemical_formula_sum:C48 H85.2 O36.6 Y4
Atom count from the _atom_site data: C48 H84 O36.6 Y4
CELLZ01_ALERT_1_G Difference between formula and atom_site contents detected.
CELLZ01_ALERT_1_G WARNING: H atoms missing from atom site list. Is this intentional?
From the CIF: _cell_formula_units_Z 1
From the CIF: _chemical_formula_sum C48 H85.2 O36.6 Y4
TEST: Compare cell contents of formula and atom_site data
atom Z*formula cif sites diff
C 48.00 48.00 0.00
H 85.20 84.00 1.20
O 36.60 36.60 0.00
Y 4.00 4.00 0.00
0 ALERT level A = In general: serious problem
1 ALERT level B = Potentially serious problem
11 ALERT level C = Check and explain
3 ALERT level G = General alerts; check
6 ALERT type 1 CIF construction/syntax error, inconsistent or missing data
6 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
2 ALERT type 4 Improvement, methodology, query or suggestion
0 ALERT type 5 Informative message, check
Data collection: SMART-NT (Bruker, 2001); cell refinement: SAINT-NT (Bruker, 2001); data reduction: SAINT-NT; 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 and PLATON (Spek, 2005).
Tetra-µ-but-2-enoato-bis[diaqua(but-2-enoato)yttrium]
di-µ-but-2-enoato-bis[diaquabis(but-2-enoato)yttrium] 4.6-hydrate
top
Crystal data top
[Y2(C4H5O2)6(H2O)4]2·4.6H2O | Z = 1 |
Mr = 1603.60 | F(000) = 822 |
Triclinic, P1 | Dx = 1.556 Mg m−3 |
Hall symbol: -P 1 | Mo Kα radiation, λ = 0.71073 Å |
a = 10.431 (4) Å | Cell parameters from 4562 reflections |
b = 10.519 (4) Å | θ = 3.7–24.5° |
c = 15.802 (6) Å | µ = 3.45 mm−1 |
α = 89.382 (6)° | T = 298 K |
β = 81.627 (6)° | Block, colourless |
γ = 86.338 (6)° | 0.22 × 0.19 × 0.17 mm |
V = 1711.9 (11) Å3 | |
Data collection top
Bruker SMART CCD area-detector diffractometer | 8173 independent reflections |
Radiation source: fine-focus sealed tube | 5632 reflections with I > 2σ(I) |
Graphite monochromator | Rint = 0.035 |
φ and ω scans | θmax = 27.9°, θmin = 1.9° |
Absorption correction: multi-scan (SADABS; Sheldrick, 2001) | h = −13→13 |
Tmin = 0.48, Tmax = 0.56 | k = −13→13 |
14298 measured reflections | l = −20→20 |
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)] = 0.043 | Hydrogen site location: inferred from neighbouring sites |
wR(F2) = 0.112 | H atoms treated by a mixture of independent and constrained refinement |
S = 0.97 | w = 1/[σ2(Fo2) + (0.0649P)2] where P = (Fo2 + 2Fc2)/3 |
8173 reflections | (Δ/σ)max = 0.001 |
465 parameters | Δρmax = 0.65 e Å−3 |
21 restraints | Δρmin = −0.36 e Å−3 |
Special details top
Geometry. All e.s.d.'s (except the e.s.d. in the dihedral angle between two l.s. planes)
are estimated using the full covariance matrix. The cell e.s.d.'s are taken
into account individually in the estimation of e.s.d.'s in distances, angles
and torsion angles; correlations between e.s.d.'s in cell parameters are only
used when they are defined by crystal symmetry. An approximate (isotropic)
treatment of cell e.s.d.'s is used for estimating e.s.d.'s involving l.s.
planes. |
Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top | x | y | z | Uiso*/Ueq | Occ. (<1) |
Y1 | 0.51497 (3) | 0.99836 (3) | 0.376227 (19) | 0.02639 (10) | |
Y2 | 0.00392 (3) | 0.03105 (3) | 0.127815 (19) | 0.02734 (10) | |
O11 | 0.6103 (3) | 0.8927 (3) | 0.24494 (15) | 0.0436 (7) | |
O12 | 0.4230 (2) | 0.8287 (2) | 0.30361 (16) | 0.0405 (6) | |
C11 | 0.5249 (4) | 0.8123 (4) | 0.2503 (2) | 0.0364 (8) | |
C12 | 0.5467 (4) | 0.6980 (4) | 0.1966 (3) | 0.0478 (10) | |
H12 | 0.6187 | 0.6945 | 0.1542 | 0.057* | |
C13 | 0.4748 (4) | 0.6017 (4) | 0.2028 (3) | 0.0567 (11) | |
H13 | 0.4010 | 0.6081 | 0.2437 | 0.068* | |
C14 | 0.4964 (5) | 0.4821 (5) | 0.1523 (4) | 0.0809 (16) | |
H14A | 0.4351 | 0.4817 | 0.1125 | 0.121* | |
H14B | 0.4851 | 0.4104 | 0.1902 | 0.121* | |
H14C | 0.5830 | 0.4767 | 0.1215 | 0.121* | |
O21 | 0.6299 (2) | 1.0426 (2) | 0.50521 (14) | 0.0317 (5) | |
O22 | 0.7430 (2) | 1.0403 (2) | 0.37842 (14) | 0.0358 (6) | |
C21 | 0.7353 (3) | 1.0594 (3) | 0.4575 (2) | 0.0288 (7) | |
C22 | 0.8420 (3) | 1.1083 (4) | 0.4968 (2) | 0.0364 (8) | |
H22 | 0.8378 | 1.1032 | 0.5559 | 0.044* | |
C23 | 0.9428 (4) | 1.1589 (4) | 0.4523 (3) | 0.0442 (9) | |
H23 | 0.9486 | 1.1586 | 0.3930 | 0.053* | |
C24 | 1.0485 (4) | 1.2167 (5) | 0.4901 (3) | 0.0643 (13) | |
H24A | 1.0327 | 1.2086 | 0.5513 | 0.096* | |
H24B | 1.0504 | 1.3052 | 0.4749 | 0.096* | |
H24C | 1.1304 | 1.1735 | 0.4686 | 0.096* | |
O31 | 0.5960 (2) | 0.8074 (2) | 0.42767 (15) | 0.0374 (6) | |
O32 | 0.5474 (2) | 0.7979 (2) | 0.56988 (15) | 0.0381 (6) | |
C31 | 0.5908 (4) | 0.7498 (3) | 0.4973 (2) | 0.0353 (8) | |
C32 | 0.6409 (5) | 0.6145 (4) | 0.4950 (3) | 0.0561 (12) | |
H32A | 0.6672 | 0.5783 | 0.4391 | 0.067* | 0.75 |
H32B | 0.6634 | 0.5856 | 0.5490 | 0.067* | 0.25 |
C33 | 0.6516 (6) | 0.5413 (5) | 0.5569 (4) | 0.0495 (14) | 0.75 |
H33A | 0.6241 | 0.5761 | 0.6130 | 0.059* | 0.75 |
C34 | 0.7038 (7) | 0.4064 (6) | 0.5525 (5) | 0.078 (2) | 0.75 |
H34A | 0.7021 | 0.3726 | 0.6093 | 0.117* | 0.75 |
H34B | 0.6515 | 0.3576 | 0.5215 | 0.117* | 0.75 |
H34C | 0.7916 | 0.4019 | 0.5237 | 0.117* | 0.75 |
C33A | 0.657 (2) | 0.5326 (16) | 0.4437 (12) | 0.080 (7) | 0.25 |
H33B | 0.6386 | 0.5567 | 0.3877 | 0.096* | 0.25 |
C34A | 0.708 (2) | 0.3980 (16) | 0.4547 (15) | 0.079 (7) | 0.25 |
H34D | 0.7135 | 0.3544 | 0.4011 | 0.119* | 0.25 |
H34E | 0.7926 | 0.3959 | 0.4722 | 0.119* | 0.25 |
H34F | 0.6495 | 0.3569 | 0.4973 | 0.119* | 0.25 |
O41 | −0.1750 (2) | 0.1774 (2) | 0.19385 (15) | 0.0386 (6) | |
O42 | 0.0213 (2) | 0.2414 (3) | 0.18192 (17) | 0.0445 (7) | |
C41 | −0.0991 (4) | 0.2637 (4) | 0.2036 (2) | 0.0362 (8) | |
C42 | −0.1526 (4) | 0.3881 (4) | 0.2374 (3) | 0.0492 (10) | |
H42 | −0.2404 | 0.3964 | 0.2594 | 0.059* | |
C43 | −0.0852 (4) | 0.4880 (4) | 0.2386 (3) | 0.0576 (12) | |
H43 | 0.0032 | 0.4756 | 0.2192 | 0.069* | |
C44 | −0.1317 (5) | 0.6193 (4) | 0.2670 (4) | 0.0780 (16) | |
H44A | −0.2240 | 0.6230 | 0.2839 | 0.117* | |
H44B | −0.1106 | 0.6779 | 0.2208 | 0.117* | |
H44C | −0.0903 | 0.6419 | 0.3147 | 0.117* | |
O51 | 0.2149 (2) | 0.0300 (2) | 0.18038 (15) | 0.0387 (6) | |
O52 | 0.2024 (2) | 0.0874 (2) | 0.04852 (14) | 0.0358 (6) | |
C51 | 0.2675 (3) | 0.0743 (3) | 0.1098 (2) | 0.0329 (8) | |
C52 | 0.4016 (3) | 0.1106 (4) | 0.1008 (2) | 0.0418 (9) | |
H52 | 0.4469 | 0.0988 | 0.1471 | 0.050* | |
C53 | 0.4603 (3) | 0.1588 (4) | 0.0303 (3) | 0.0412 (9) | |
H53 | 0.4132 | 0.1679 | −0.0153 | 0.049* | |
C54 | 0.5948 (4) | 0.2006 (4) | 0.0158 (3) | 0.0602 (13) | |
H54A | 0.6360 | 0.1806 | 0.0652 | 0.090* | |
H54B | 0.5928 | 0.2909 | 0.0060 | 0.090* | |
H54C | 0.6427 | 0.1574 | −0.0332 | 0.090* | |
O61 | 0.0509 (2) | −0.1247 (2) | −0.00374 (15) | 0.0327 (5) | |
O62 | 0.0925 (2) | −0.1863 (2) | 0.12206 (15) | 0.0372 (6) | |
C61 | 0.0863 (3) | −0.2131 (3) | 0.0454 (2) | 0.0290 (7) | |
C62 | 0.1170 (4) | −0.3424 (4) | 0.0122 (2) | 0.0387 (9) | |
H62 | 0.1018 | −0.3587 | −0.0431 | 0.046* | |
C63 | 0.1644 (4) | −0.4363 (4) | 0.0551 (3) | 0.0422 (9) | |
H63 | 0.1777 | −0.4193 | 0.1107 | 0.051* | |
C64 | 0.1993 (5) | −0.5694 (4) | 0.0226 (3) | 0.0596 (12) | |
H64A | 0.1735 | −0.5774 | −0.0329 | 0.089* | |
H64B | 0.1553 | −0.6287 | 0.0614 | 0.089* | |
H64C | 0.2914 | −0.5871 | 0.0186 | 0.089* | |
O1W | 0.5753 (3) | 1.1642 (3) | 0.27107 (17) | 0.0436 (6) | |
H1WA | 0.6514 (18) | 1.162 (3) | 0.243 (2) | 0.052* | |
H1WB | 0.565 (3) | 1.233 (2) | 0.298 (2) | 0.052* | |
O2W | 0.3186 (3) | 1.0733 (3) | 0.32572 (16) | 0.0407 (6) | |
H2WA | 0.294 (4) | 1.046 (3) | 0.2805 (15) | 0.049* | |
H2WB | 0.306 (4) | 1.1533 (10) | 0.324 (2) | 0.049* | |
O3W | −0.1826 (2) | −0.0777 (3) | 0.11993 (15) | 0.0384 (6) | |
H3WA | −0.248 (2) | −0.080 (4) | 0.1576 (14) | 0.046* | |
H3WB | −0.209 (3) | −0.088 (4) | 0.0722 (10) | 0.046* | |
O4W | −0.0398 (3) | −0.0351 (3) | 0.26913 (15) | 0.0416 (6) | |
H4WA | −0.109 (2) | −0.027 (3) | 0.3044 (18) | 0.050* | |
H4WB | 0.008 (3) | −0.092 (3) | 0.2882 (19) | 0.050* | |
O5W | 0.1597 (3) | 0.7735 (3) | 0.28720 (18) | 0.0537 (8) | |
H5WA | 0.174 (3) | 0.765 (3) | 0.2330 (7) | 0.064* | |
H5WB | 0.2337 (19) | 0.784 (4) | 0.302 (2) | 0.064* | |
O6W | 0.2233 (4) | 0.3183 (5) | 0.2731 (3) | 0.0998 (14) | |
H6WA | 0.163 (4) | 0.292 (6) | 0.248 (3) | 0.120* | |
H6WB | 0.186 (5) | 0.339 (7) | 0.3229 (17) | 0.120* | |
O7W | 0.1333 (19) | 0.5368 (14) | 0.3689 (11) | 0.137 (6) | 0.30 |
Atomic displacement parameters (Å2) top | U11 | U22 | U33 | U12 | U13 | U23 |
Y1 | 0.02379 (17) | 0.03423 (19) | 0.02093 (17) | −0.00224 (13) | −0.00239 (12) | 0.00078 (13) |
Y2 | 0.02334 (18) | 0.0368 (2) | 0.02202 (18) | −0.00410 (14) | −0.00296 (13) | 0.00210 (13) |
O11 | 0.0468 (16) | 0.0510 (16) | 0.0313 (14) | −0.0113 (13) | 0.0038 (12) | −0.0073 (12) |
O12 | 0.0314 (14) | 0.0481 (16) | 0.0413 (15) | −0.0048 (12) | −0.0016 (12) | −0.0098 (12) |
C11 | 0.043 (2) | 0.044 (2) | 0.0240 (18) | −0.0055 (18) | −0.0102 (16) | 0.0003 (15) |
C12 | 0.050 (2) | 0.054 (3) | 0.038 (2) | −0.001 (2) | −0.0010 (19) | −0.0112 (19) |
C13 | 0.054 (3) | 0.053 (3) | 0.063 (3) | −0.003 (2) | −0.009 (2) | −0.016 (2) |
C14 | 0.087 (4) | 0.065 (3) | 0.092 (4) | −0.009 (3) | −0.014 (3) | −0.027 (3) |
O21 | 0.0267 (12) | 0.0405 (14) | 0.0268 (12) | −0.0048 (10) | 0.0007 (10) | 0.0007 (10) |
O22 | 0.0287 (13) | 0.0584 (17) | 0.0204 (12) | −0.0077 (12) | −0.0014 (10) | 0.0016 (11) |
C21 | 0.0253 (17) | 0.0306 (18) | 0.0301 (18) | 0.0022 (14) | −0.0043 (14) | 0.0041 (14) |
C22 | 0.0306 (19) | 0.049 (2) | 0.0302 (19) | −0.0033 (17) | −0.0061 (15) | −0.0033 (16) |
C23 | 0.035 (2) | 0.051 (2) | 0.048 (2) | −0.0085 (18) | −0.0046 (18) | −0.0056 (19) |
C24 | 0.040 (2) | 0.075 (3) | 0.079 (3) | −0.023 (2) | −0.004 (2) | −0.013 (3) |
O31 | 0.0457 (15) | 0.0344 (14) | 0.0307 (13) | 0.0062 (11) | −0.0044 (11) | −0.0007 (11) |
O32 | 0.0485 (16) | 0.0356 (14) | 0.0297 (13) | 0.0029 (12) | −0.0062 (12) | 0.0009 (11) |
C31 | 0.037 (2) | 0.033 (2) | 0.037 (2) | −0.0007 (16) | −0.0102 (16) | −0.0003 (16) |
C32 | 0.072 (3) | 0.044 (3) | 0.050 (3) | 0.009 (2) | −0.006 (2) | −0.006 (2) |
C33 | 0.063 (4) | 0.035 (3) | 0.049 (3) | 0.003 (3) | −0.009 (3) | 0.005 (2) |
C34 | 0.103 (6) | 0.041 (4) | 0.085 (5) | 0.020 (4) | −0.011 (4) | 0.017 (3) |
C33A | 0.093 (17) | 0.085 (16) | 0.054 (13) | 0.015 (13) | 0.011 (11) | −0.016 (11) |
C34A | 0.084 (16) | 0.046 (11) | 0.103 (18) | 0.013 (11) | −0.004 (13) | −0.010 (11) |
O41 | 0.0348 (14) | 0.0412 (15) | 0.0390 (14) | −0.0039 (12) | −0.0016 (11) | −0.0015 (11) |
O42 | 0.0340 (15) | 0.0484 (16) | 0.0501 (16) | −0.0064 (12) | −0.0009 (12) | −0.0093 (13) |
C41 | 0.041 (2) | 0.042 (2) | 0.0261 (18) | −0.0068 (17) | −0.0028 (16) | 0.0036 (15) |
C42 | 0.038 (2) | 0.044 (2) | 0.063 (3) | 0.0005 (19) | 0.002 (2) | −0.008 (2) |
C43 | 0.047 (3) | 0.053 (3) | 0.070 (3) | 0.001 (2) | 0.000 (2) | −0.004 (2) |
C44 | 0.078 (4) | 0.048 (3) | 0.104 (4) | −0.005 (3) | 0.003 (3) | −0.020 (3) |
O51 | 0.0328 (14) | 0.0555 (16) | 0.0296 (13) | −0.0097 (12) | −0.0075 (11) | 0.0051 (12) |
O52 | 0.0252 (12) | 0.0597 (17) | 0.0235 (12) | −0.0079 (11) | −0.0042 (10) | 0.0024 (11) |
C51 | 0.0291 (18) | 0.039 (2) | 0.0309 (19) | −0.0039 (15) | −0.0043 (15) | −0.0049 (15) |
C52 | 0.030 (2) | 0.058 (3) | 0.039 (2) | −0.0070 (18) | −0.0089 (16) | −0.0012 (18) |
C53 | 0.032 (2) | 0.045 (2) | 0.047 (2) | −0.0034 (17) | −0.0025 (17) | −0.0068 (18) |
C54 | 0.036 (2) | 0.065 (3) | 0.076 (3) | −0.011 (2) | 0.007 (2) | −0.011 (2) |
O61 | 0.0298 (13) | 0.0370 (14) | 0.0314 (13) | −0.0016 (10) | −0.0056 (10) | 0.0064 (10) |
O62 | 0.0418 (15) | 0.0423 (15) | 0.0282 (13) | 0.0012 (12) | −0.0094 (11) | −0.0003 (11) |
C61 | 0.0224 (17) | 0.0372 (19) | 0.0278 (18) | −0.0032 (14) | −0.0048 (14) | 0.0033 (14) |
C62 | 0.040 (2) | 0.043 (2) | 0.035 (2) | −0.0064 (17) | −0.0070 (17) | −0.0007 (16) |
C63 | 0.043 (2) | 0.041 (2) | 0.043 (2) | −0.0050 (18) | −0.0054 (18) | 0.0037 (17) |
C64 | 0.060 (3) | 0.042 (2) | 0.074 (3) | 0.004 (2) | −0.003 (2) | 0.002 (2) |
O1W | 0.0355 (15) | 0.0525 (17) | 0.0407 (16) | −0.0046 (13) | 0.0016 (12) | 0.0109 (13) |
O2W | 0.0376 (15) | 0.0489 (16) | 0.0380 (15) | 0.0011 (13) | −0.0147 (12) | −0.0001 (12) |
O3W | 0.0302 (13) | 0.0615 (17) | 0.0235 (12) | −0.0153 (12) | 0.0015 (10) | −0.0005 (12) |
O4W | 0.0388 (15) | 0.0588 (18) | 0.0243 (13) | 0.0052 (13) | 0.0012 (11) | 0.0048 (12) |
O5W | 0.0468 (17) | 0.075 (2) | 0.0408 (16) | −0.0042 (16) | −0.0129 (13) | 0.0085 (15) |
O6W | 0.103 (3) | 0.093 (3) | 0.115 (4) | −0.006 (3) | −0.057 (3) | −0.012 (3) |
O7W | 0.191 (19) | 0.081 (11) | 0.134 (14) | 0.000 (11) | −0.015 (13) | 0.016 (10) |
Geometric parameters (Å, º) top
Y1—O21i | 2.285 (2) | C34—H34B | 0.9601 |
Y1—O31 | 2.314 (2) | C34—H34C | 0.9600 |
Y1—O32i | 2.332 (3) | C33A—C34A | 1.498 (17) |
Y1—O2W | 2.390 (3) | C33A—H33B | 0.9600 |
Y1—O11 | 2.415 (2) | C34A—H34D | 0.9601 |
Y1—O1W | 2.444 (3) | C34A—H34E | 0.9600 |
Y1—O12 | 2.451 (3) | C34A—H34F | 0.9600 |
Y1—O22 | 2.452 (2) | O41—C41 | 1.267 (4) |
Y1—O21 | 2.571 (2) | O42—C41 | 1.261 (4) |
Y2—O61ii | 2.314 (2) | C41—C42 | 1.465 (5) |
Y2—O4W | 2.322 (2) | C42—C43 | 1.303 (6) |
Y2—O3W | 2.339 (2) | C42—H42 | 0.9300 |
Y2—O52 | 2.365 (2) | C43—C44 | 1.486 (6) |
Y2—O42 | 2.407 (3) | C43—H43 | 0.9300 |
Y2—O62 | 2.408 (3) | C44—H44A | 0.9600 |
Y2—O41 | 2.458 (2) | C44—H44B | 0.9600 |
Y2—O51 | 2.462 (3) | C44—H44C | 0.9600 |
Y2—O61 | 2.631 (2) | O51—C51 | 1.267 (4) |
O11—C11 | 1.260 (4) | O52—C51 | 1.264 (4) |
O12—C11 | 1.259 (4) | C51—C52 | 1.459 (5) |
C11—C12 | 1.466 (5) | C52—C53 | 1.306 (5) |
C12—C13 | 1.293 (6) | C52—H52 | 0.9300 |
C12—H12 | 0.9300 | C53—C54 | 1.481 (5) |
C13—C14 | 1.484 (6) | C53—H53 | 0.9300 |
C13—H13 | 0.9300 | C54—H54A | 0.9600 |
C14—H14A | 0.9600 | C54—H54B | 0.9600 |
C14—H14B | 0.9600 | C54—H54C | 0.9600 |
C14—H14C | 0.9600 | O61—C61 | 1.276 (4) |
O21—C21 | 1.261 (4) | O61—Y2ii | 2.314 (2) |
O21—Y1i | 2.285 (2) | O62—C61 | 1.259 (4) |
O22—C21 | 1.258 (4) | C61—C62 | 1.462 (5) |
C21—C22 | 1.473 (5) | C62—C63 | 1.304 (5) |
C22—C23 | 1.316 (5) | C62—H62 | 0.9300 |
C22—H22 | 0.9300 | C63—C64 | 1.500 (6) |
C23—C24 | 1.493 (6) | C63—H63 | 0.9300 |
C23—H23 | 0.9300 | C64—H64A | 0.9600 |
C24—H24A | 0.9600 | C64—H64B | 0.9600 |
C24—H24B | 0.9600 | C64—H64C | 0.9600 |
C24—H24C | 0.9600 | O1W—H1WA | 0.85 (3) |
O31—C31 | 1.246 (4) | O1W—H1WB | 0.85 (3) |
O32—C31 | 1.269 (4) | O2W—H2WA | 0.85 (2) |
O32—Y1i | 2.332 (3) | O2W—H2WB | 0.85 (2) |
C31—C32 | 1.483 (6) | O3W—H3WA | 0.85 (3) |
C32—C33A | 1.176 (14) | O3W—H3WB | 0.85 (3) |
C32—C33 | 1.252 (6) | O4W—H4WA | 0.85 (3) |
C32—H32A | 0.9601 | O4W—H4WB | 0.85 (3) |
C32—H32B | 0.9599 | O5W—H5WA | 0.85 (2) |
C33—C34 | 1.485 (7) | O5W—H5WB | 0.85 (2) |
C33—H33A | 0.9599 | O6W—H6WA | 0.85 (3) |
C34—H34A | 0.9600 | O6W—H6WB | 0.85 (3) |
| | | |
O21i—Y1—O31 | 75.90 (8) | C31—O32—Y1i | 136.3 (2) |
O21i—Y1—O32i | 77.63 (8) | O31—C31—O32 | 125.2 (3) |
O31—Y1—O32i | 136.78 (9) | O31—C31—C32 | 117.2 (3) |
O21i—Y1—O2W | 80.75 (9) | O32—C31—C32 | 117.5 (3) |
O31—Y1—O2W | 135.94 (10) | C33A—C32—C31 | 135.8 (11) |
O32i—Y1—O2W | 70.73 (9) | C33—C32—C31 | 127.9 (5) |
O21i—Y1—O11 | 138.23 (9) | C33—C32—H32A | 116.0 |
O31—Y1—O11 | 78.70 (9) | C31—C32—H32A | 116.0 |
O32i—Y1—O11 | 140.55 (9) | C33A—C32—H32B | 111.8 |
O2W—Y1—O11 | 95.63 (9) | C31—C32—H32B | 112.4 |
O21i—Y1—O1W | 142.35 (9) | H32A—C32—H32B | 129.1 |
O31—Y1—O1W | 140.85 (9) | C32—C33—C34 | 126.7 (6) |
O32i—Y1—O1W | 67.96 (9) | C34—C33—H32B | 142.8 |
O2W—Y1—O1W | 74.02 (9) | C32—C33—H33A | 116.7 |
O11—Y1—O1W | 72.74 (10) | C34—C33—H33A | 116.6 |
O21i—Y1—O12 | 87.68 (9) | C33—C34—H34A | 109.7 |
O31—Y1—O12 | 73.38 (9) | C33—C34—H34B | 109.3 |
O32i—Y1—O12 | 138.61 (9) | H34A—C34—H34B | 109.5 |
O2W—Y1—O12 | 68.80 (9) | C33—C34—H34C | 109.4 |
O11—Y1—O12 | 53.24 (8) | H34A—C34—H34C | 109.5 |
O1W—Y1—O12 | 108.01 (10) | H34B—C34—H34C | 109.5 |
O21i—Y1—O22 | 124.55 (8) | C33—C34—H34E | 105.2 |
O31—Y1—O22 | 78.19 (9) | H34A—C34—H34E | 136.1 |
O32i—Y1—O22 | 89.69 (9) | C33—C34—H34F | 104.9 |
O2W—Y1—O22 | 144.68 (9) | H34A—C34—H34F | 122.8 |
O11—Y1—O22 | 80.89 (8) | H34C—C34—H34F | 99.7 |
O1W—Y1—O22 | 71.39 (8) | C32—C33A—C34A | 127.7 (19) |
O12—Y1—O22 | 129.41 (8) | C32—C33A—H33B | 115.5 |
O21i—Y1—O21 | 74.11 (9) | C34A—C33A—H33B | 116.8 |
O31—Y1—O21 | 70.77 (8) | C33A—C34A—H34B | 107.9 |
O32i—Y1—O21 | 69.46 (8) | C33A—C34A—H34C | 105.8 |
O2W—Y1—O21 | 136.40 (8) | C33A—C34A—H34D | 108.6 |
O11—Y1—O21 | 126.70 (9) | H34B—C34A—H34D | 122.9 |
O1W—Y1—O21 | 106.09 (9) | H34C—C34A—H34D | 135.5 |
O12—Y1—O21 | 142.72 (8) | C33A—C34A—H34E | 110.6 |
O22—Y1—O21 | 51.17 (7) | H34B—C34A—H34E | 96.6 |
O61ii—Y2—O4W | 153.89 (9) | H34D—C34A—H34E | 109.5 |
O61ii—Y2—O3W | 82.17 (8) | C33A—C34A—H34F | 109.1 |
O4W—Y2—O3W | 80.73 (9) | H34C—C34A—H34F | 84.4 |
O61ii—Y2—O52 | 74.60 (8) | H34D—C34A—H34F | 109.5 |
O4W—Y2—O52 | 129.40 (9) | H34E—C34A—H34F | 109.5 |
O3W—Y2—O52 | 143.45 (8) | C41—O41—Y2 | 92.6 (2) |
O61ii—Y2—O42 | 88.26 (9) | C41—O42—Y2 | 95.1 (2) |
O4W—Y2—O42 | 87.31 (10) | O42—C41—O41 | 119.0 (3) |
O3W—Y2—O42 | 128.95 (9) | O42—C41—C42 | 121.3 (3) |
O52—Y2—O42 | 78.70 (9) | O41—C41—C42 | 119.7 (3) |
O61ii—Y2—O62 | 118.63 (8) | C43—C42—C41 | 124.3 (4) |
O4W—Y2—O62 | 77.13 (9) | C43—C42—H42 | 117.9 |
O3W—Y2—O62 | 79.16 (9) | C41—C42—H42 | 117.9 |
O52—Y2—O62 | 87.59 (9) | C42—C43—C44 | 128.3 (4) |
O42—Y2—O62 | 145.44 (9) | C42—C43—H43 | 115.9 |
O61ii—Y2—O41 | 82.04 (8) | C44—C43—H43 | 115.9 |
O4W—Y2—O41 | 74.75 (9) | C43—C44—H44A | 109.5 |
O3W—Y2—O41 | 75.83 (9) | C43—C44—H44B | 109.5 |
O52—Y2—O41 | 126.84 (9) | H44A—C44—H44B | 109.5 |
O42—Y2—O41 | 53.16 (8) | C43—C44—H44C | 109.5 |
O62—Y2—O41 | 144.81 (8) | H44A—C44—H44C | 109.5 |
O61ii—Y2—O51 | 127.23 (8) | H44B—C44—H44C | 109.5 |
O4W—Y2—O51 | 75.67 (9) | C51—O51—Y2 | 91.0 (2) |
O3W—Y2—O51 | 146.80 (9) | C51—O52—Y2 | 95.7 (2) |
O52—Y2—O51 | 53.73 (8) | O52—C51—O51 | 119.2 (3) |
O42—Y2—O51 | 73.21 (9) | O52—C51—C52 | 121.1 (3) |
O62—Y2—O51 | 73.10 (8) | O51—C51—C52 | 119.7 (3) |
O41—Y2—O51 | 118.81 (9) | C53—C52—C51 | 122.5 (4) |
O61ii—Y2—O61 | 67.62 (9) | C53—C52—H52 | 118.7 |
O4W—Y2—O61 | 124.11 (9) | C51—C52—H52 | 118.7 |
O3W—Y2—O61 | 71.46 (8) | C52—C53—C54 | 126.3 (4) |
O52—Y2—O61 | 73.73 (8) | C52—C53—H53 | 116.8 |
O42—Y2—O61 | 147.17 (8) | C54—C53—H53 | 116.8 |
O62—Y2—O61 | 51.01 (8) | C53—C54—H54A | 109.5 |
O41—Y2—O61 | 137.62 (8) | C53—C54—H54B | 109.5 |
O51—Y2—O61 | 103.23 (8) | H54A—C54—H54B | 109.5 |
C11—O11—Y1 | 93.5 (2) | C53—C54—H54C | 109.5 |
C11—O12—Y1 | 91.9 (2) | H54A—C54—H54C | 109.5 |
O12—C11—O11 | 119.9 (3) | H54B—C54—H54C | 109.5 |
O12—C11—C12 | 120.3 (3) | C61—O61—Y2ii | 157.8 (2) |
O11—C11—C12 | 119.8 (3) | C61—O61—Y2 | 89.56 (19) |
C13—C12—C11 | 125.9 (4) | Y2ii—O61—Y2 | 112.38 (9) |
C13—C12—H12 | 117.1 | C61—O62—Y2 | 100.6 (2) |
C11—C12—H12 | 117.1 | O62—C61—O61 | 118.6 (3) |
C12—C13—C14 | 127.6 (4) | O62—C61—C62 | 121.7 (3) |
C12—C13—H13 | 116.2 | O61—C61—C62 | 119.8 (3) |
C14—C13—H13 | 116.2 | C63—C62—C61 | 124.2 (4) |
C13—C14—H14A | 109.5 | C63—C62—H62 | 117.9 |
C13—C14—H14B | 109.5 | C61—C62—H62 | 117.9 |
H14A—C14—H14B | 109.5 | C62—C63—C64 | 125.7 (4) |
C13—C14—H14C | 109.5 | C62—C63—H63 | 117.1 |
H14A—C14—H14C | 109.5 | C64—C63—H63 | 117.1 |
H14B—C14—H14C | 109.5 | C63—C64—H64A | 109.5 |
C21—O21—Y1i | 161.1 (2) | C63—C64—H64B | 109.5 |
C21—O21—Y1 | 91.84 (19) | H64A—C64—H64B | 109.5 |
Y1i—O21—Y1 | 105.89 (9) | C63—C64—H64C | 109.5 |
C21—O22—Y1 | 97.58 (19) | H64A—C64—H64C | 109.5 |
O22—C21—O21 | 119.1 (3) | H64B—C64—H64C | 109.5 |
O22—C21—C22 | 122.8 (3) | Y1—O1W—H1WA | 120 (3) |
O21—C21—C22 | 117.9 (3) | Y1—O1W—H1WB | 106 (3) |
C23—C22—C21 | 123.2 (3) | Y1—O2W—H2WA | 124 (2) |
C23—C22—H22 | 118.4 | Y1—O2W—H2WB | 115 (2) |
C21—C22—H22 | 118.4 | Y2—O3W—H3WA | 127 (2) |
C22—C23—C24 | 124.7 (4) | Y2—O3W—H3WB | 121 (2) |
C22—C23—H23 | 117.6 | Y2—O4W—H4WA | 131 (2) |
C24—C23—H23 | 117.6 | Y2—O4W—H4WB | 120 (2) |
C23—C24—H24A | 109.5 | H1WA—O1W—H1WB | 107 (4) |
C23—C24—H24B | 109.5 | H2WA—O2W—H2WB | 105 (4) |
H24A—C24—H24B | 109.5 | H3WA—O3W—H3WB | 107 (4) |
C23—C24—H24C | 109.5 | H4WA—O4W—H4WB | 107 (4) |
H24A—C24—H24C | 109.5 | H5WA—O5W—H5WB | 104 (4) |
H24B—C24—H24C | 109.5 | H6WA—O6W—H6WB | 105 (4) |
C31—O31—Y1 | 137.9 (2) | | |
Symmetry codes: (i) −x+1, −y+2, −z+1; (ii) −x, −y, −z. |
Hydrogen-bond geometry (Å, º) top
D—H···A | D—H | H···A | D···A | D—H···A |
O1W—H1WA···O41iii | 0.85 (3) | 1.88 (3) | 2.722 (4) | 171 (3) |
O2W—H2WA···O51iv | 0.85 (2) | 1.90 (3) | 2.731 (4) | 164 (3) |
O2W—H2WB···O6Wiv | 0.85 (2) | 2.09 (3) | 2.861 (6) | 151 (3) |
O3W—H3WA···O11v | 0.85 (3) | 1.90 (3) | 2.738 (3) | 173 (4) |
O3W—H3WB···O52ii | 0.85 (3) | 1.90 (3) | 2.703 (3) | 158 (3) |
O4W—H4WA···O22v | 0.85 (3) | 1.90 (3) | 2.721 (3) | 164 (3) |
O4W—H4WB···O5Wvi | 0.85 (3) | 2.05 (3) | 2.844 (4) | 158 (3) |
O5W—H5WA···O62iv | 0.85 (2) | 2.10 (3) | 2.820 (4) | 141 (2) |
O5W—H5WB···O12 | 0.85 (2) | 2.06 (3) | 2.891 (4) | 165 (4) |
O6W—H6WA···O42 | 0.85 (3) | 2.03 (3) | 2.880 (5) | 176 (6) |
O6W—H6WB···O7W | 0.85 (3) | 2.22 (5) | 2.800 (16) | 126 (6) |
Symmetry codes: (ii) −x, −y, −z; (iii) x+1, y+1, z; (iv) x, y+1, z; (v) x−1, y−1, z; (vi) x, y−1, z. |