Supporting information
Crystallographic Information File (CIF) https://doi.org/10.1107/S1600536805018246/lh6434sup1.cif | |
Structure factor file (CIF format) https://doi.org/10.1107/S1600536805018246/lh6434Isup2.hkl |
CCDC reference: 277715
Key indicators
- Single-crystal X-ray study
- T = 173 K
- Mean (C-C) = 0.007 Å
- Disorder in main residue
- R factor = 0.029
- wR factor = 0.079
- Data-to-parameter ratio = 18.5
checkCIF/PLATON results
No syntax errors found
Alert level B REFLT01_ALERT_1_B The number of symmetry-independent reflections cannot exceed the total number of reflections measured Number of symmetry-independent reflections = 3139 Total number of reflections = 3106
Alert level C PLAT030_ALERT_1_C _diffrn_reflns_number .LE. _reflns_number_total ? PLAT066_ALERT_1_C Predicted and Reported Transmissions Identical . ? PLAT301_ALERT_3_C Main Residue Disorder ......................... 9.00 Perc. PLAT601_ALERT_2_C Structure Contains Solvent Accessible VOIDS of . 40.00 A 3 PLAT764_ALERT_4_C Overcomplete CIF Bond List Detected (Rep/Expd) . 1.12 Ratio
0 ALERT level A = In general: serious problem 1 ALERT level B = Potentially serious problem 5 ALERT level C = Check and explain 0 ALERT level G = General alerts; check 3 ALERT type 1 CIF construction/syntax error, inconsistent or missing data 1 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 1 ALERT type 4 Improvement, methodology, query or suggestion
Data collection: SMART (Bruker, 1998); cell refinement: SAINT (Bruker, 2002); data reduction: SAINT; program(s) used to solve structure: SIR97 (Altomare et al., 1999); program(s) used to refine structure: SHELXTL (Bruker, 2000); molecular graphics: SHELXTL; software used to prepare material for publication: SHELXTL.
[Dy(C9H16O8)] | F(000) = 800 |
Mr = 414.72 | Dx = 2.020 Mg m−3 |
Monoclinic, P21/c | Mo Kα radiation, λ = 0.71073 Å |
Hall symbol: -P 2ybc | Cell parameters from 1890 reflections |
a = 11.651 (2) Å | θ = 1.9–27.5° |
b = 13.942 (2) Å | µ = 5.51 mm−1 |
c = 8.981 (2) Å | T = 173 K |
β = 110.837 (3)° | Plate, colorless |
V = 1363.4 (4) Å3 | 0.26 × 0.20 × 0.10 mm |
Z = 4 |
Bruker SMART Platform CCD diffractometer | 3139 independent reflections |
Radiation source: normal-focus sealed tube | 2657 reflections with I > 2σ(I) |
Graphite monochromator | Rint = 0.066 |
ω scans | θmax = 27.5°, θmin = 1.9° |
Absorption correction: multi-scan TWINABS (Blessing, 1995; Sheldrick, 2002) | h = −15→14 |
Tmin = 0.277, Tmax = 0.576 | k = 0→18 |
3106 measured reflections | l = 0→11 |
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)] = 0.029 | Hydrogen site location: inferred from neighbouring sites |
wR(F2) = 0.080 | H-atom parameters constrained |
S = 1.02 | w = 1/[σ2(Fo2) + (0.0544P)2 + 0.5P] where P = (Fo2 + 2Fc2)/3 |
3106 reflections | (Δ/σ)max = 0.001 |
168 parameters | Δρmax = 1.53 e Å−3 |
1 restraint | Δρmin = −1.40 e Å−3 |
Experimental. A crystal (0.26 x 0.20 x 0.10 mm3) was selected for single-crystal X-ray diffraction. Data were collected on a Bruker SMART Platform CCD diffractometer at 173 (2) K. The data collection was conducted using Mo Kα radiation at a frame time of 20 s and a detector distance of 4.94 cm. Data was collected to a resolution of 0.77 Å. Frames were collected at 0.30° steps in ω at four different φ settings and a detector position of -28° in 2Θ. Absorption and intensity data were corrected for through use of the TWINABS program. After integrating the data with SAINT, final cell constants were calculated from the xyz centroids of 1890 strong reflections from the actual data collection. The structure was solved using SIR97 and refined using SHELXL97. Based on systematic absences and intensities, P21/c was determined as the space group. Most non-hydrogen atoms were calculated using direct-methods. The remaining non-hydrogen atoms were located through conducting full-matrix least squares / difference Fourier cycles. All non-hydrogen atoms were refined anisotropically. |
Geometry. All e.s.d.'s (except the e.s.d. in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell e.s.d.'s are taken into account individually in the estimation of e.s.d.'s in distances, angles and torsion angles; correlations between e.s.d.'s in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell e.s.d.'s is used for estimating e.s.d.'s involving l.s. planes. |
Refinement. Refinement of F2 against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F2, conventional R-factors R are based on F, with F set to zero for negative F2. The threshold expression of F2 > σ(F2) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F2 are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. |
x | y | z | Uiso*/Ueq | Occ. (<1) | |
Dy1 | 0.130714 (16) | 0.108170 (13) | 0.55683 (2) | 0.01036 (9) | |
O1 | 0.2391 (3) | 0.1228 (2) | 0.8515 (4) | 0.0171 (7) | |
O2 | 0.2095 (3) | −0.0226 (2) | 0.7524 (4) | 0.0158 (6) | |
C1 | 0.2572 (4) | 0.0332 (3) | 0.8684 (5) | 0.0113 (8) | |
C2 | 0.3403 (4) | −0.0061 (3) | 1.0257 (5) | 0.0179 (9) | 0.709 (9) |
H2A | 0.3337 | −0.0770 | 1.0247 | 0.021* | 0.709 (9) |
H2B | 0.3140 | 0.0185 | 1.1119 | 0.021* | 0.709 (9) |
C3 | 0.4756 (5) | 0.0230 (5) | 1.0594 (7) | 0.0160 (12) | 0.709 (9) |
H3A | 0.4811 | 0.0936 | 1.0532 | 0.019* | 0.709 (9) |
H3B | 0.5268 | 0.0028 | 1.1686 | 0.019* | 0.709 (9) |
C2' | 0.3403 (4) | −0.0061 (3) | 1.0257 (5) | 0.0179 (9) | 0.291 (9) |
H2C | 0.2996 | −0.0606 | 1.0577 | 0.021* | 0.291 (9) |
H2D | 0.3572 | 0.0442 | 1.1086 | 0.021* | 0.291 (9) |
C3' | 0.4634 (10) | −0.0406 (11) | 1.0114 (17) | 0.0160 (12) | 0.291 (9) |
H3C | 0.5117 | −0.0759 | 1.1092 | 0.019* | 0.291 (9) |
H3D | 0.4453 | −0.0852 | 0.9202 | 0.019* | 0.291 (9) |
O3 | 0.2322 (3) | 0.1361 (2) | 0.3565 (3) | 0.0128 (6) | |
O4 | 0.3470 (3) | 0.0930 (3) | 0.5979 (4) | 0.0229 (8) | |
C4 | 0.3369 (4) | 0.1270 (3) | 0.4632 (5) | 0.0132 (8) | |
C5 | 0.4512 (4) | 0.1576 (3) | 0.4320 (5) | 0.0171 (9) | |
H5A | 0.4445 | 0.2265 | 0.4039 | 0.021* | |
H5B | 0.4560 | 0.1212 | 0.3397 | 0.021* | |
C6 | 0.5687 (4) | 0.1412 (4) | 0.5745 (6) | 0.0209 (10) | |
H6A | 0.5714 | 0.1879 | 0.6587 | 0.025* | |
H6B | 0.5658 | 0.0762 | 0.6173 | 0.025* | |
O5 | −0.0640 (3) | 0.0389 (2) | 0.5868 (3) | 0.0106 (6) | |
O6 | −0.0153 (3) | 0.1861 (2) | 0.6675 (4) | 0.0174 (7) | |
C7 | −0.0874 (4) | 0.1163 (3) | 0.6456 (5) | 0.0115 (8) | |
C8 | −0.2029 (4) | 0.1232 (3) | 0.6838 (5) | 0.0164 (9) | |
H8A | −0.1912 | 0.1717 | 0.7684 | 0.020* | |
H8B | −0.2185 | 0.0606 | 0.7252 | 0.020* | |
C9 | −0.3141 (4) | 0.1506 (4) | 0.5385 (6) | 0.0179 (9) | |
H9A | −0.3050 | 0.2176 | 0.5075 | 0.022* | |
H9B | −0.3186 | 0.1084 | 0.4479 | 0.022* | |
O7 | −0.0352 (3) | 0.1592 (2) | 0.3270 (4) | 0.0194 (7) | |
H7A | −0.0095 | 0.1680 | 0.2507 | 0.029* | |
H7B | −0.0903 | 0.1162 | 0.3019 | 0.029* | |
O8 | 0.1831 (3) | 0.2738 (2) | 0.5760 (4) | 0.0187 (7) | |
H8C | 0.2467 | 0.2816 | 0.5522 | 0.028* | |
H8D | 0.1976 | 0.2928 | 0.6708 | 0.028* |
U11 | U22 | U33 | U12 | U13 | U23 | |
Dy1 | 0.00963 (14) | 0.00924 (12) | 0.01255 (13) | −0.00079 (7) | 0.00438 (9) | 0.00021 (7) |
O1 | 0.0245 (18) | 0.0150 (15) | 0.0107 (14) | 0.0056 (13) | 0.0050 (13) | −0.0004 (12) |
O2 | 0.0166 (15) | 0.0124 (15) | 0.0143 (14) | −0.0039 (12) | 0.0003 (12) | 0.0024 (12) |
C1 | 0.0083 (18) | 0.016 (2) | 0.013 (2) | 0.0010 (16) | 0.0076 (16) | 0.0053 (16) |
C2 | 0.016 (2) | 0.024 (2) | 0.013 (2) | 0.0059 (18) | 0.0044 (17) | 0.0066 (17) |
C3 | 0.012 (3) | 0.022 (3) | 0.011 (3) | 0.005 (3) | 0.000 (2) | −0.001 (2) |
C2' | 0.016 (2) | 0.024 (2) | 0.013 (2) | 0.0059 (18) | 0.0044 (17) | 0.0066 (17) |
C3' | 0.012 (3) | 0.022 (3) | 0.011 (3) | 0.005 (3) | 0.000 (2) | −0.001 (2) |
O3 | 0.0096 (14) | 0.0170 (14) | 0.0125 (14) | −0.0025 (12) | 0.0048 (12) | −0.0004 (12) |
O4 | 0.0108 (16) | 0.042 (2) | 0.0184 (17) | 0.0038 (14) | 0.0084 (13) | 0.0147 (15) |
C4 | 0.011 (2) | 0.015 (2) | 0.018 (2) | 0.0011 (16) | 0.0099 (17) | −0.0002 (17) |
C5 | 0.013 (2) | 0.023 (2) | 0.020 (2) | 0.0004 (18) | 0.0101 (17) | 0.0030 (18) |
C6 | 0.012 (2) | 0.031 (3) | 0.022 (2) | −0.0004 (19) | 0.0085 (18) | 0.001 (2) |
O5 | 0.0132 (14) | 0.0072 (13) | 0.0150 (14) | 0.0003 (11) | 0.0095 (11) | −0.0011 (11) |
O6 | 0.0138 (15) | 0.0114 (15) | 0.0304 (17) | −0.0036 (12) | 0.0121 (13) | −0.0092 (13) |
C7 | 0.010 (2) | 0.014 (2) | 0.011 (2) | 0.0021 (16) | 0.0058 (16) | 0.0011 (15) |
C8 | 0.013 (2) | 0.021 (2) | 0.020 (2) | −0.0015 (17) | 0.0120 (18) | −0.0055 (18) |
C9 | 0.008 (2) | 0.025 (2) | 0.024 (2) | −0.0009 (18) | 0.0091 (18) | 0.0020 (19) |
O7 | 0.0141 (15) | 0.0156 (16) | 0.0220 (16) | −0.0072 (13) | −0.0014 (13) | 0.0081 (13) |
O8 | 0.0329 (18) | 0.0136 (15) | 0.0153 (15) | −0.0119 (14) | 0.0154 (14) | −0.0034 (12) |
Dy1—O8 | 2.380 (3) | O3—C4 | 1.261 (5) |
Dy1—O7 | 2.380 (3) | O4—C4 | 1.265 (6) |
Dy1—O5i | 2.400 (3) | C4—C5 | 1.516 (6) |
Dy1—O4 | 2.423 (3) | C5—C6 | 1.522 (6) |
Dy1—O2 | 2.471 (3) | C5—H5A | 0.9900 |
Dy1—O1 | 2.502 (3) | C5—H5B | 0.9900 |
Dy1—O6 | 2.503 (3) | C6—C9iii | 1.518 (6) |
Dy1—O3 | 2.510 (3) | C6—H6A | 0.9900 |
Dy1—O5 | 2.567 (3) | C6—H6B | 0.9900 |
Dy1—C4 | 2.826 (4) | O5—C7 | 1.273 (5) |
Dy1—C1 | 2.857 (4) | O5—Dy1i | 2.400 (3) |
Dy1—C7 | 2.924 (4) | O6—C7 | 1.254 (5) |
O1—C1 | 1.267 (5) | C7—C8 | 1.505 (6) |
O2—C1 | 1.260 (5) | C8—C9 | 1.525 (6) |
C1—C2 | 1.504 (6) | C8—H8A | 0.9900 |
C2—C3 | 1.549 (7) | C8—H8B | 0.9900 |
C2—H2A | 0.9900 | C9—C6iv | 1.518 (6) |
C2—H2B | 0.9900 | C9—H9A | 0.9900 |
C3—C3ii | 1.518 (12) | C9—H9B | 0.9900 |
C3—H3A | 0.9900 | O7—H7A | 0.8484 |
C3—H3B | 0.9900 | O7—H7B | 0.8490 |
C3'—C3'ii | 1.48 (3) | O8—H8C | 0.8485 |
C3'—H3C | 0.9900 | O8—H8D | 0.8487 |
C3'—H3D | 0.9900 | ||
O8—Dy1—O7 | 83.15 (11) | O2—C1—C2 | 119.9 (4) |
O8—Dy1—O5i | 153.37 (10) | O1—C1—C2 | 119.8 (4) |
O7—Dy1—O5i | 77.39 (10) | O2—C1—Dy1 | 59.6 (2) |
O8—Dy1—O4 | 81.25 (12) | O1—C1—Dy1 | 61.0 (2) |
O7—Dy1—O4 | 129.64 (11) | C2—C1—Dy1 | 171.6 (3) |
O5i—Dy1—O4 | 97.32 (11) | C1—C2—C3 | 111.0 (4) |
O8—Dy1—O2 | 130.09 (10) | C1—C2—H2A | 109.4 |
O7—Dy1—O2 | 144.98 (10) | C3—C2—H2A | 109.4 |
O5i—Dy1—O2 | 73.68 (10) | C1—C2—H2B | 109.4 |
O4—Dy1—O2 | 73.98 (10) | C3—C2—H2B | 109.4 |
O8—Dy1—O1 | 79.88 (10) | H2A—C2—H2B | 108.0 |
O7—Dy1—O1 | 147.28 (11) | C3ii—C3—C2 | 111.2 (6) |
O5i—Dy1—O1 | 125.68 (10) | C3ii—C3—H3A | 109.4 |
O4—Dy1—O1 | 74.93 (11) | C2—C3—H3A | 109.4 |
O2—Dy1—O1 | 52.29 (10) | C3ii—C3—H3B | 109.4 |
O8—Dy1—O6 | 75.10 (10) | C2—C3—H3B | 109.4 |
O7—Dy1—O6 | 75.97 (11) | H3A—C3—H3B | 108.0 |
O5i—Dy1—O6 | 116.65 (9) | C3'ii—C3'—H3C | 109.3 |
O4—Dy1—O6 | 142.61 (11) | C3'ii—C3'—H3D | 109.3 |
O2—Dy1—O6 | 99.86 (11) | H3C—C3'—H3D | 107.9 |
O1—Dy1—O6 | 72.74 (11) | C4—O3—Dy1 | 90.8 (2) |
O8—Dy1—O3 | 74.16 (10) | C4—O4—Dy1 | 94.8 (3) |
O7—Dy1—O3 | 77.07 (10) | O3—C4—O4 | 120.0 (4) |
O5i—Dy1—O3 | 83.82 (9) | O3—C4—C5 | 120.4 (4) |
O4—Dy1—O3 | 52.62 (10) | O4—C4—C5 | 119.5 (4) |
O2—Dy1—O3 | 118.26 (10) | O3—C4—Dy1 | 62.7 (2) |
O1—Dy1—O3 | 123.79 (10) | O4—C4—Dy1 | 58.7 (2) |
O6—Dy1—O3 | 141.00 (10) | C5—C4—Dy1 | 167.6 (3) |
O8—Dy1—O5 | 124.83 (10) | C4—C5—C6 | 112.9 (4) |
O7—Dy1—O5 | 74.22 (10) | C4—C5—H5A | 109.0 |
O5i—Dy1—O5 | 66.78 (10) | C6—C5—H5A | 109.0 |
O4—Dy1—O5 | 149.48 (10) | C4—C5—H5B | 109.0 |
O2—Dy1—O5 | 76.49 (9) | C6—C5—H5B | 109.0 |
O1—Dy1—O5 | 92.99 (10) | H5A—C5—H5B | 107.8 |
O6—Dy1—O5 | 51.00 (9) | C9iii—C6—C5 | 114.6 (4) |
O3—Dy1—O5 | 142.47 (9) | C9iii—C6—H6A | 108.6 |
O8—Dy1—C4 | 73.04 (12) | C5—C6—H6A | 108.6 |
O7—Dy1—C4 | 103.20 (12) | C9iii—C6—H6B | 108.6 |
O5i—Dy1—C4 | 93.80 (11) | C5—C6—H6B | 108.6 |
O4—Dy1—C4 | 26.50 (12) | H6A—C6—H6B | 107.6 |
O2—Dy1—C4 | 98.04 (12) | C7—O5—Dy1i | 150.6 (3) |
O1—Dy1—C4 | 98.31 (12) | C7—O5—Dy1 | 93.0 (2) |
O6—Dy1—C4 | 147.97 (11) | Dy1i—O5—Dy1 | 113.22 (10) |
O3—Dy1—C4 | 26.51 (11) | C7—O6—Dy1 | 96.5 (2) |
O5—Dy1—C4 | 160.56 (11) | O6—C7—O5 | 119.5 (4) |
O8—Dy1—C1 | 104.75 (11) | O6—C7—C8 | 121.2 (4) |
O7—Dy1—C1 | 159.35 (11) | O5—C7—C8 | 119.3 (4) |
O5i—Dy1—C1 | 99.76 (11) | O6—C7—Dy1 | 58.3 (2) |
O4—Dy1—C1 | 70.90 (11) | O5—C7—Dy1 | 61.3 (2) |
O2—Dy1—C1 | 26.10 (11) | C8—C7—Dy1 | 177.2 (3) |
O1—Dy1—C1 | 26.30 (11) | C7—C8—C9 | 112.1 (4) |
O6—Dy1—C1 | 87.51 (11) | C7—C8—H8A | 109.2 |
O3—Dy1—C1 | 123.27 (10) | C9—C8—H8A | 109.2 |
O5—Dy1—C1 | 85.80 (10) | C7—C8—H8B | 109.2 |
C4—Dy1—C1 | 97.39 (12) | C9—C8—H8B | 109.2 |
O8—Dy1—C7 | 99.67 (11) | H8A—C8—H8B | 107.9 |
O7—Dy1—C7 | 73.05 (12) | C6iv—C9—C8 | 110.5 (4) |
O5i—Dy1—C7 | 91.91 (11) | C6iv—C9—H9A | 109.5 |
O4—Dy1—C7 | 156.89 (11) | C8—C9—H9A | 109.5 |
O2—Dy1—C7 | 88.51 (11) | C6iv—C9—H9B | 109.5 |
O1—Dy1—C7 | 82.47 (12) | C8—C9—H9B | 109.5 |
O6—Dy1—C7 | 25.23 (10) | H9A—C9—H9B | 108.1 |
O3—Dy1—C7 | 150.03 (11) | Dy1—O7—H7A | 109.4 |
O5—Dy1—C7 | 25.77 (10) | Dy1—O7—H7B | 108.8 |
C4—Dy1—C7 | 172.32 (12) | H7A—O7—H7B | 109.8 |
C1—Dy1—C7 | 86.71 (11) | Dy1—O8—H8C | 109.2 |
C1—O1—Dy1 | 92.7 (2) | Dy1—O8—H8D | 109.3 |
C1—O2—Dy1 | 94.3 (2) | H8C—O8—H8D | 109.4 |
O2—C1—O1 | 120.3 (4) | ||
O8—Dy1—O1—C1 | −160.9 (3) | O5i—Dy1—C4—O4 | −98.8 (3) |
O7—Dy1—O1—C1 | 139.3 (2) | O2—Dy1—C4—O4 | −24.8 (3) |
O5i—Dy1—O1—C1 | 10.9 (3) | O1—Dy1—C4—O4 | 28.1 (3) |
O4—Dy1—O1—C1 | −77.3 (3) | O6—Dy1—C4—O4 | 98.7 (3) |
O2—Dy1—O1—C1 | 3.9 (2) | O3—Dy1—C4—O4 | −166.8 (4) |
O6—Dy1—O1—C1 | 121.7 (3) | O5—Dy1—C4—O4 | −96.8 (4) |
O3—Dy1—O1—C1 | −97.8 (3) | C1—Dy1—C4—O4 | 1.6 (3) |
O5—Dy1—O1—C1 | 74.3 (2) | O8—Dy1—C4—C5 | 19.3 (14) |
C4—Dy1—O1—C1 | −89.9 (3) | O7—Dy1—C4—C5 | 97.8 (15) |
C7—Dy1—O1—C1 | 97.9 (3) | O5i—Dy1—C4—C5 | 175.7 (14) |
O8—Dy1—O2—C1 | 15.8 (3) | O4—Dy1—C4—C5 | −85.5 (15) |
O7—Dy1—O2—C1 | −142.5 (2) | O2—Dy1—C4—C5 | −110.3 (15) |
O5i—Dy1—O2—C1 | −178.0 (3) | O1—Dy1—C4—C5 | −57.4 (15) |
O4—Dy1—O2—C1 | 79.2 (2) | O6—Dy1—C4—C5 | 13.2 (16) |
O1—Dy1—O2—C1 | −3.9 (2) | O3—Dy1—C4—C5 | 107.7 (15) |
O6—Dy1—O2—C1 | −62.9 (2) | O5—Dy1—C4—C5 | 177.7 (13) |
O3—Dy1—O2—C1 | 108.6 (2) | C1—Dy1—C4—C5 | −83.9 (15) |
O5—Dy1—O2—C1 | −108.6 (2) | O3—C4—C5—C6 | 179.9 (4) |
C4—Dy1—O2—C1 | 90.4 (3) | O4—C4—C5—C6 | 0.6 (6) |
C7—Dy1—O2—C1 | −85.6 (2) | Dy1—C4—C5—C6 | 78.9 (15) |
Dy1—O2—C1—O1 | 7.1 (4) | C4—C5—C6—C9iii | 167.6 (4) |
Dy1—O2—C1—C2 | −170.3 (3) | O8—Dy1—O5—C7 | −13.9 (3) |
Dy1—O1—C1—O2 | −7.0 (4) | O7—Dy1—O5—C7 | −83.6 (2) |
Dy1—O1—C1—C2 | 170.4 (3) | O5i—Dy1—O5—C7 | −166.4 (3) |
O8—Dy1—C1—O2 | −167.5 (2) | O4—Dy1—O5—C7 | 130.7 (3) |
O7—Dy1—C1—O2 | 82.1 (4) | O2—Dy1—O5—C7 | 115.8 (2) |
O5i—Dy1—C1—O2 | 2.0 (3) | O1—Dy1—O5—C7 | 65.8 (2) |
O4—Dy1—C1—O2 | −92.5 (3) | O6—Dy1—O5—C7 | 0.9 (2) |
O1—Dy1—C1—O2 | 173.0 (4) | O3—Dy1—O5—C7 | −125.0 (2) |
O6—Dy1—C1—O2 | 118.6 (2) | C4—Dy1—O5—C7 | −168.6 (3) |
O3—Dy1—C1—O2 | −87.0 (3) | C1—Dy1—O5—C7 | 91.1 (2) |
O5—Dy1—C1—O2 | 67.5 (2) | O8—Dy1—O5—Dy1i | 152.44 (11) |
C4—Dy1—C1—O2 | −93.2 (2) | O7—Dy1—O5—Dy1i | 82.78 (13) |
C7—Dy1—C1—O2 | 93.3 (2) | O5i—Dy1—O5—Dy1i | 0.0 |
O8—Dy1—C1—O1 | 19.5 (3) | O4—Dy1—O5—Dy1i | −62.9 (2) |
O7—Dy1—C1—O1 | −90.9 (4) | O2—Dy1—O5—Dy1i | −77.79 (12) |
O5i—Dy1—C1—O1 | −171.0 (2) | O1—Dy1—O5—Dy1i | −127.82 (12) |
O4—Dy1—C1—O1 | 94.6 (3) | O6—Dy1—O5—Dy1i | 167.30 (18) |
O2—Dy1—C1—O1 | −173.0 (4) | O3—Dy1—O5—Dy1i | 41.3 (2) |
O6—Dy1—C1—O1 | −54.4 (2) | C4—Dy1—O5—Dy1i | −2.2 (4) |
O3—Dy1—C1—O1 | 100.0 (3) | C1—Dy1—O5—Dy1i | −102.50 (13) |
O5—Dy1—C1—O1 | −105.5 (2) | C7—Dy1—O5—Dy1i | 166.4 (3) |
C4—Dy1—C1—O1 | 93.8 (3) | O8—Dy1—O6—C7 | 166.5 (3) |
C7—Dy1—C1—O1 | −79.6 (3) | O7—Dy1—O6—C7 | 79.9 (3) |
O2—C1—C2—C3 | 109.0 (5) | O5i—Dy1—O6—C7 | 12.1 (3) |
O1—C1—C2—C3 | −68.4 (5) | O4—Dy1—O6—C7 | −141.0 (3) |
C1—C2—C3—C3ii | −65.6 (7) | O2—Dy1—O6—C7 | −64.5 (3) |
O8—Dy1—O3—C4 | 83.6 (3) | O1—Dy1—O6—C7 | −109.7 (3) |
O7—Dy1—O3—C4 | 170.1 (3) | O3—Dy1—O6—C7 | 127.5 (3) |
O5i—Dy1—O3—C4 | −111.5 (3) | O5—Dy1—O6—C7 | −1.0 (2) |
O4—Dy1—O3—C4 | −7.4 (2) | C4—Dy1—O6—C7 | 172.5 (2) |
O2—Dy1—O3—C4 | −43.8 (3) | C1—Dy1—O6—C7 | −87.6 (3) |
O1—Dy1—O3—C4 | 17.8 (3) | Dy1—O6—C7—O5 | 1.7 (4) |
O6—Dy1—O3—C4 | 122.8 (3) | Dy1—O6—C7—C8 | −176.7 (4) |
O5—Dy1—O3—C4 | −149.1 (2) | Dy1i—O5—C7—O6 | −155.5 (4) |
C1—Dy1—O3—C4 | −13.9 (3) | Dy1—O5—C7—O6 | −1.7 (4) |
C7—Dy1—O3—C4 | 165.5 (3) | Dy1i—O5—C7—C8 | 23.0 (8) |
O8—Dy1—O4—C4 | −69.3 (3) | Dy1—O5—C7—C8 | 176.8 (3) |
O7—Dy1—O4—C4 | 4.1 (3) | Dy1i—O5—C7—Dy1 | −153.8 (5) |
O5i—Dy1—O4—C4 | 83.8 (3) | O8—Dy1—C7—O6 | −13.3 (3) |
O2—Dy1—O4—C4 | 154.4 (3) | O7—Dy1—C7—O6 | −93.0 (3) |
O1—Dy1—O4—C4 | −151.1 (3) | O5i—Dy1—C7—O6 | −169.2 (3) |
O6—Dy1—O4—C4 | −120.3 (3) | O4—Dy1—C7—O6 | 77.1 (4) |
O3—Dy1—O4—C4 | 7.4 (3) | O2—Dy1—C7—O6 | 117.2 (3) |
O5—Dy1—O4—C4 | 139.4 (3) | O1—Dy1—C7—O6 | 65.1 (3) |
C1—Dy1—O4—C4 | −178.4 (3) | O3—Dy1—C7—O6 | −88.3 (3) |
Dy1—O3—C4—O4 | 13.0 (4) | O5—Dy1—C7—O6 | 178.3 (4) |
Dy1—O3—C4—C5 | −166.3 (4) | C1—Dy1—C7—O6 | 91.1 (3) |
Dy1—O4—C4—O3 | −13.6 (5) | O8—Dy1—C7—O5 | 168.4 (2) |
Dy1—O4—C4—C5 | 165.7 (4) | O7—Dy1—C7—O5 | 88.7 (2) |
O8—Dy1—C4—O3 | −88.4 (3) | O5i—Dy1—C7—O5 | 12.5 (3) |
O7—Dy1—C4—O3 | −9.9 (3) | O4—Dy1—C7—O5 | −101.2 (3) |
O5i—Dy1—C4—O3 | 68.0 (3) | O2—Dy1—C7—O5 | −61.1 (2) |
O4—Dy1—C4—O3 | 166.8 (4) | O1—Dy1—C7—O5 | −113.2 (2) |
O2—Dy1—C4—O3 | 142.0 (2) | O6—Dy1—C7—O5 | −178.3 (4) |
O1—Dy1—C4—O3 | −165.1 (2) | O3—Dy1—C7—O5 | 93.4 (3) |
O6—Dy1—C4—O3 | −94.5 (3) | C1—Dy1—C7—O5 | −87.2 (2) |
O5—Dy1—C4—O3 | 70.0 (4) | O6—C7—C8—C9 | 94.5 (5) |
C1—Dy1—C4—O3 | 168.4 (3) | O5—C7—C8—C9 | −84.0 (5) |
O8—Dy1—C4—O4 | 104.8 (3) | C7—C8—C9—C6iv | 170.9 (4) |
O7—Dy1—C4—O4 | −176.7 (3) |
Symmetry codes: (i) −x, −y, −z+1; (ii) −x+1, −y, −z+2; (iii) x+1, y, z; (iv) x−1, y, z. |
D—H···A | D—H | H···A | D···A | D—H···A |
O7—H7A···O6v | 0.85 | 2.16 | 2.645 (4) | 116 |
O7—H7B···O2i | 0.85 | 1.84 | 2.689 (4) | 180 |
O8—H8C···O1v | 0.85 | 2.22 | 2.740 (4) | 120 |
O8—H8D···O3vi | 0.85 | 1.86 | 2.687 (4) | 166 |
Symmetry codes: (i) −x, −y, −z+1; (v) x, −y+1/2, z−1/2; (vi) x, −y+1/2, z+1/2. |
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