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We have determined the crystal structure of manganese(II) diacetate tetrahydrate at 300 and 14 K by single-crystal neutron diffraction. Proton density distributions for each of the three crystallographically distinct methyl groups have been calculated by Fourier difference. At room temperature the observed densities are those of quasi-free rotors. At low temperature rather well localized protons are observed. Inelastic neutron scattering measurements performed with single crystals allow us to assign each of the three tunnelling lines to a particular crystal site. Classical molecular dynamics simulations give density distributions in qualitative agreement with the observations. With quantum mechanics proton distributions can be represented with rotational wavefunctions convoluted with static distributions of librational coordinates. The effective rotational potentials are temperature dependent.
Supporting information
 | Crystallographic Information File (CIF) https://doi.org/10.1107/S0108768100014695/lc0023sup1.cif |
CCDC references: 159944; 159945
Computing details top
For both compounds, data collection: CAD-4 Software (Enraf-Nonius, 1989). Cell refinement: DIF4 modified version of STOE 4 circle diffractometer control program (1996) for (14K); STOE PW110 for 300K. Data reduction: PRON modified version of REDU4 (STOE) 1996 diffractometer control program (1996) for (14K); PRON modified version of REDU4 (STOE) 1996 for 300K. Program(s) used to refine structure: CRYSTALS Issue 10 (Watkin, Prout, Carruthers & Betteridge, 1996) for (14K); CRYSTALS (Watkin et al., 1996) for 300K. Molecular graphics: CAMERON (Pearce et al., 1996) for (14K); CAMERON (Pearce et al., 1994) for 300K. Software used to prepare material for publication: CRYSTALS (Watkin et al., 1996) for (14K); CRYSTALS Issue 10 (Watkin, Prout, Carruthers & Betteridge, 1996) for 300K.
![[Figure 1]](http://journals.iucr.org/b/issues/2001/01/00/lc0023/lc0023fig1thm.gif)
![[Figure 2]](http://journals.iucr.org/b/issues/2001/01/00/lc0023/lc0023fig2thm.gif)
![[Figure 3]](http://journals.iucr.org/b/issues/2001/01/00/lc0023/lc0023fig3thm.gif)
![[Figure 4]](http://journals.iucr.org/b/issues/2001/01/00/lc0023/lc0023fig4thm.gif)
![[Figure 5]](http://journals.iucr.org/b/issues/2001/01/00/lc0023/lc0023fig5thm.gif)
![[Figure 6]](http://journals.iucr.org/b/issues/2001/01/00/lc0023/lc0023fig6thm.gif)
(14K) manganese acetate tetrahydrate top
Crystal data top
| Mn·2(C2H3O2)·4(D2O) | F(000) = 489.70 |
| Mr = 252.9 | Dx = 1.58 Mg m−3 |
| Monoclinic, P21/c | Melting point: not measured K |
| Hall symbol: -P 2ybc | Neutron radiation, λ = 0.83080 Å |
| a = 10.88 (3) Å | Cell parameters from 14 reflections |
| b = 17.39 (3) Å | θ = 15.7–42.5° |
| c = 9.04 (2) Å | T = 14 K |
| β = 118.8 (2)° | Prism, pink |
| V = 1498.8 Å3 | 3.00 × 3.00 × 3.00 mm |
| Z = 6 |
Data collection top
| Orphée reactor (Saclay, France) : 5C2 four-circle diffractometer | Rint = 0.05 |
| Radiation source: Orphée reactor Saclay France | θmax = 40°, θmin = 2.5° |
| Cu (220) monochromator | h = −17→3 |
| ω scans | k = 0→26 |
| 7656 measured reflections | l = −13→14 |
| 6227 independent reflections | 2 standard reflections every 0 reflections |
| 4686 reflections with > 3.00σ(I) | intensity decay: 0.0% |
Refinement top
| Refinement on F2 | Chebychev polynomial with 4 parameters (Carruthers & Watkin, 1979) 1.23 -1.20 0.899 -0.290 |
| Least-squares matrix: full | (Δ/σ)max = 0.005 |
| R[F2 > 2σ(F2)] = 0.041 | Δρmax = 1.37 e Å−3 |
| wR(F2) = 0.0383 | Δρmin = −2.21 e Å−3 |
| 4686 reflections | Extinction correction: Larson 1970 Crystallographic Computing eq 22 |
| 380 parameters | Extinction coefficient: 5.1 (4) |
Crystal data top
| Mn·2(C2H3O2)·4(D2O) | β = 118.8 (2)° |
| Mr = 252.9 | V = 1498.8 Å3 |
| Monoclinic, P21/c | Z = 6 |
| a = 10.88 (3) Å | Neutron radiation, λ = 0.83080 Å |
| b = 17.39 (3) Å | T = 14 K |
| c = 9.04 (2) Å | 3.00 × 3.00 × 3.00 mm |
Data collection top
| Orphée reactor (Saclay, France) : 5C2 four-circle diffractometer | Rint = 0.05 |
| 7656 measured reflections | 2 standard reflections every 0 reflections |
| 6227 independent reflections | intensity decay: 0.0% |
| 4686 reflections with > 3.00σ(I) |
Refinement top
| R[F2 > 2σ(F2)] = 0.041 | 380 parameters |
| wR(F2) = 0.0383 | Δρmax = 1.37 e Å−3 |
| 4686 reflections | Δρmin = −2.21 e Å−3 |
Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top
| x | y | z | Uiso*/Ueq | Occ. (<1) | |
| Mn1 | 0.0000 | 0.0000 | 0.0000 | 0.0025 | 0.5000 |
| Mn2 | 0.02154 (11) | 0.20154 (6) | −0.06542 (13) | 0.0030 | |
| C1 | 0.01292 (6) | 0.14148 (3) | 0.23988 (8) | 0.0043 | |
| C2 | 0.00188 (9) | 0.08678 (4) | 0.3620 (1) | 0.0111 | |
| C3 | 0.22184 (6) | 0.07847 (3) | −0.09365 (8) | 0.0046 | |
| C4 | 0.34013 (7) | 0.06109 (4) | −0.1308 (1) | 0.0101 | |
| C5 | −0.20164 (6) | 0.08814 (3) | −0.34227 (8) | 0.0046 | |
| C6 | −0.32383 (7) | 0.07815 (4) | −0.51660 (9) | 0.0101 | |
| O1 | 0.00886 (7) | 0.11501 (4) | 0.10470 (9) | 0.0048 | |
| O2 | 0.02565 (8) | 0.21165 (4) | 0.27019 (9) | 0.0058 | |
| O3 | 0.17622 (8) | 0.14658 (4) | −0.1164 (1) | 0.0067 | |
| O4 | 0.17694 (8) | 0.02440 (4) | −0.0399 (1) | 0.0064 | |
| O5 | −0.16643 (8) | 0.03147 (4) | −0.24337 (9) | 0.0062 | |
| O6 | −0.13990 (8) | 0.15245 (4) | −0.30394 (9) | 0.0065 | |
| O7 | 0.21127 (8) | 0.25320 (4) | 0.1522 (1) | 0.0066 | |
| O8 | −0.16399 (7) | 0.25437 (4) | −0.0662 (1) | 0.0063 | |
| O9 | 0.43410 (8) | 0.31484 (5) | 0.1240 (1) | 0.0084 | |
| O10 | 0.61599 (8) | 0.19110 (5) | 0.1568 (1) | 0.0089 | |
| O11 | 0.67021 (8) | 0.37674 (5) | 0.4130 (1) | 0.0078 | |
| O12 | 0.33359 (8) | 0.10676 (5) | 0.33137 (11) | 0.0095 | |
| D4 | 0.28484 (16) | 0.14675 (9) | 0.2505 (2) | 0.0200 | 0.620 (8) |
| D5 | 0.27648 (15) | 0.06085 (8) | 0.29290 (19) | 0.0186 | 0.634 (7) |
| D9 | 0.62528 (15) | 0.17151 (8) | 0.06256 (17) | 0.0172 | 0.637 (7) |
| D10 | 0.54302 (15) | 0.22961 (9) | 0.11824 (18) | 0.0174 | 0.625 (7) |
| D14 | 0.71476 (15) | 0.42692 (8) | 0.4417 (2) | 0.0170 | 0.606 (7) |
| D15 | 0.74182 (14) | 0.34085 (8) | 0.42256 (18) | 0.0173 | 0.652 (7) |
| D16 | −0.15549 (13) | 0.28483 (7) | 0.02927 (16) | 0.0138 | 0.641 (7) |
| D17 | −0.23923 (12) | 0.27682 (7) | −0.17069 (16) | 0.0135 | 0.655 (7) |
| D18 | 0.39924 (14) | 0.34739 (8) | 0.02314 (17) | 0.0150 | 0.635 (7) |
| D19 | 0.50747 (14) | 0.34354 (8) | 0.21567 (17) | 0.0178 | 0.673 (7) |
| D20 | 0.19968 (14) | 0.28371 (8) | 0.23478 (17) | 0.0154 | 0.640 (7) |
| D21 | 0.28795 (13) | 0.27595 (8) | 0.13958 (17) | 0.0141 | 0.646 (7) |
| H21 | 0.0088 (4) | 0.11561 (13) | 0.4696 (3) | 0.0390 | |
| H22 | −0.0957 (6) | 0.0582 (4) | 0.3010 (5) | 0.1003 | |
| H23 | 0.0764 (7) | 0.0432 (3) | 0.3961 (8) | 0.0986 | |
| H41 | 0.3572 (2) | −0.00001 (11) | −0.1320 (3) | 0.0298 | |
| H42 | 0.4348 (2) | 0.08776 (19) | −0.0346 (5) | 0.0460 | |
| H43 | 0.3191 (4) | 0.08614 (18) | −0.2511 (4) | 0.0462 | |
| H61 | −0.3937 (4) | 0.1263 (2) | −0.5502 (5) | 0.0600 | |
| H62 | −0.3777 (4) | 0.0257 (2) | −0.5301 (4) | 0.0686 | |
| H63 | −0.2886 (4) | 0.0808 (3) | −0.6083 (3) | 0.0598 |
Atomic displacement parameters (Å2) top
| U11 | U22 | U33 | U12 | U13 | U23 | |
| Mn1 | 0.0031 (5) | 0.0019 (5) | 0.0031 (5) | −0.0004 (4) | 0.0018 (4) | 0.0003 (4) |
| Mn2 | 0.0036 (3) | 0.0022 (4) | 0.0040 (4) | −0.0000 (3) | 0.0026 (3) | 0.0005 (3) |
| C1 | 0.0066 (2) | 0.0030 (2) | 0.0047 (2) | −0.00014 (16) | 0.00365 (18) | −0.00028 (17) |
| C2 | 0.0226 (3) | 0.0055 (2) | 0.0103 (3) | −0.0009 (2) | 0.0120 (3) | 0.0008 (2) |
| C3 | 0.0053 (2) | 0.0034 (2) | 0.0063 (2) | 0.00027 (16) | 0.00368 (18) | 0.00009 (17) |
| C4 | 0.0108 (3) | 0.0066 (3) | 0.0181 (3) | 0.00149 (19) | 0.0112 (2) | 0.0015 (2) |
| C5 | 0.0054 (2) | 0.0038 (2) | 0.0045 (2) | −0.00045 (16) | 0.00221 (18) | −0.00009 (17) |
| C6 | 0.0092 (2) | 0.0096 (3) | 0.0066 (3) | −0.0029 (2) | −0.0001 (2) | 0.0014 (2) |
| O1 | 0.0081 (3) | 0.0032 (2) | 0.0047 (3) | −0.00024 (19) | 0.0042 (2) | −0.00047 (19) |
| O2 | 0.0092 (3) | 0.0028 (3) | 0.0068 (3) | −0.00050 (19) | 0.0050 (2) | −0.0009 (2) |
| O3 | 0.0085 (3) | 0.0043 (3) | 0.0099 (3) | 0.0015 (2) | 0.0065 (2) | 0.0013 (2) |
| O4 | 0.0079 (3) | 0.0051 (3) | 0.0091 (3) | −0.0004 (2) | 0.0064 (2) | 0.0013 (2) |
| O5 | 0.0076 (3) | 0.0043 (3) | 0.0052 (3) | −0.00005 (19) | 0.0019 (2) | 0.0011 (2) |
| O6 | 0.0082 (3) | 0.0044 (3) | 0.0062 (3) | −0.0018 (2) | 0.0029 (2) | −0.0002 (2) |
| O7 | 0.0075 (3) | 0.0065 (3) | 0.0067 (3) | −0.0016 (2) | 0.0042 (2) | −0.0017 (2) |
| O8 | 0.0070 (3) | 0.0059 (3) | 0.0063 (3) | 0.00130 (19) | 0.0034 (2) | −0.0001 (2) |
| O9 | 0.0083 (3) | 0.0086 (3) | 0.0086 (3) | −0.0005 (2) | 0.0043 (2) | −0.0001 (2) |
| O10 | 0.0095 (3) | 0.0094 (3) | 0.0076 (3) | 0.0000 (2) | 0.0038 (2) | −0.0014 (2) |
| O11 | 0.0074 (3) | 0.0071 (3) | 0.0096 (3) | −0.0007 (2) | 0.0048 (2) | −0.0001 (2) |
| O12 | 0.0086 (3) | 0.0081 (3) | 0.0089 (3) | −0.0005 (2) | 0.0020 (2) | −0.0004 (2) |
| D4 | 0.0209 (7) | 0.0165 (7) | 0.0179 (7) | 0.0014 (4) | 0.0056 (5) | 0.0054 (4) |
| D5 | 0.0188 (6) | 0.0132 (6) | 0.0205 (7) | −0.0037 (4) | 0.0069 (5) | −0.0028 (4) |
| D9 | 0.0198 (6) | 0.0200 (7) | 0.0137 (6) | 0.0003 (4) | 0.0095 (5) | −0.0035 (4) |
| D10 | 0.0159 (6) | 0.0187 (7) | 0.0172 (7) | 0.0043 (4) | 0.0077 (5) | 0.0008 (4) |
| D14 | 0.0181 (6) | 0.0108 (6) | 0.0226 (7) | −0.0037 (4) | 0.0102 (5) | −0.0017 (4) |
| D15 | 0.0160 (6) | 0.0162 (6) | 0.0217 (7) | 0.0041 (4) | 0.0107 (5) | 0.0000 (4) |
| D16 | 0.0161 (6) | 0.0148 (6) | 0.0112 (6) | 0.0007 (4) | 0.0070 (4) | −0.0029 (4) |
| D17 | 0.0126 (5) | 0.0149 (6) | 0.0111 (6) | 0.0022 (3) | 0.0041 (4) | 0.0020 (4) |
| D18 | 0.0164 (6) | 0.0143 (6) | 0.0132 (6) | 0.0014 (4) | 0.0061 (4) | 0.0027 (4) |
| D19 | 0.0163 (6) | 0.0191 (6) | 0.0151 (6) | −0.0028 (4) | 0.0052 (4) | −0.0025 (4) |
| D20 | 0.0178 (6) | 0.0164 (6) | 0.0149 (6) | −0.0009 (4) | 0.0101 (5) | −0.0039 (4) |
| D21 | 0.0134 (5) | 0.0154 (6) | 0.0169 (6) | −0.0039 (4) | 0.0100 (4) | −0.0016 (4) |
| H21 | 0.0790 (19) | 0.0256 (9) | 0.028 (1) | −0.005 (1) | 0.0388 (12) | −0.0048 (7) |
| H22 | 0.122 (4) | 0.130 (5) | 0.0348 (15) | −0.106 (4) | 0.027 (2) | −0.006 (2) |
| H23 | 0.171 (5) | 0.077 (3) | 0.121 (4) | 0.097 (4) | 0.129 (4) | 0.081 (3) |
| H41 | 0.0356 (9) | 0.0156 (7) | 0.0501 (12) | 0.0052 (6) | 0.0302 (9) | 0.0012 (7) |
| H42 | 0.0195 (8) | 0.0488 (14) | 0.0677 (18) | −0.0117 (8) | 0.019 (1) | −0.0268 (13) |
| H43 | 0.0637 (17) | 0.0524 (15) | 0.0504 (15) | 0.0305 (13) | 0.0496 (14) | 0.0320 (12) |
| H61 | 0.0393 (14) | 0.0534 (18) | 0.0488 (17) | 0.0240 (13) | −0.0093 (12) | −0.0107 (14) |
| H62 | 0.071 (2) | 0.0476 (16) | 0.0368 (13) | −0.0440 (17) | −0.0143 (14) | 0.0156 (12) |
| H63 | 0.0440 (14) | 0.116 (3) | 0.021 (1) | −0.0219 (18) | 0.017 (1) | −0.0137 (14) |
Geometric parameters (Å, º) top
| Mn1—O1 | 2.1948 (7) | C4—H41 | 1.080 (2) |
| Mn1—O1i | 2.1948 (7) | C4—H42 | 1.081 (3) |
| Mn1—O4 | 2.1644 (7) | C4—H43 | 1.089 (2) |
| Mn1—O4i | 2.1644 (7) | C5—C6 | 1.5042 (9) |
| Mn1—O5 | 2.1402 (7) | C5—O5 | 1.2599 (9) |
| Mn1—O5i | 2.1402 (7) | C5—O6 | 1.2641 (9) |
| Mn2—O1 | 2.2029 (12) | C6—H61 | 1.072 (3) |
| Mn2—O2ii | 2.1339 (12) | C6—H62 | 1.058 (3) |
| Mn2—O3 | 2.1693 (12) | C6—H63 | 1.069 (3) |
| Mn2—O6 | 2.1941 (13) | O7—D20 | 0.9725 (15) |
| Mn2—O7 | 2.2417 (13) | O7—D21 | 0.9784 (14) |
| Mn2—O8 | 2.2149 (12) | O8—D16 | 0.9780 (15) |
| C1—C2 | 1.5051 (9) | O8—D17 | 0.9850 (15) |
| C1—O1 | 1.2866 (9) | O9—D18 | 0.9808 (16) |
| C1—O2 | 1.2437 (9) | O9—D19 | 0.9673 (16) |
| C2—H21 | 1.065 (2) | O10—D9 | 0.9667 (16) |
| C2—H22 | 1.055 (4) | O10—D10 | 0.9663 (17) |
| C2—H23 | 1.042 (3) | O11—D14 | 0.9710 (17) |
| C3—C4 | 1.5092 (9) | O11—D15 | 0.9691 (15) |
| C3—O3 | 1.2623 (9) | O12—D4 | 0.9624 (18) |
| C3—O4 | 1.2600 (9) | O12—D5 | 0.9675 (17) |
| O1—Mn1—O1i | 179.995 | H22—C2—H23 | 104.8 (6) |
| O1—Mn1—O4 | 92.03 (3) | C4—C3—O3 | 117.52 (6) |
| O1i—Mn1—O4 | 87.97 (3) | C4—C3—O4 | 117.85 (6) |
| O1—Mn1—O4i | 87.97 (3) | O3—C3—O4 | 124.62 (6) |
| O1i—Mn1—O4i | 92.03 (3) | C3—C4—H41 | 111.64 (12) |
| O4—Mn1—O4i | 179.995 | C3—C4—H42 | 108.56 (16) |
| O1—Mn1—O5 | 92.86 (3) | H41—C4—H42 | 109.2 (2) |
| O1i—Mn1—O5 | 87.14 (3) | C3—C4—H43 | 110.55 (15) |
| O4—Mn1—O5 | 99.12 (3) | H41—C4—H43 | 109.8 (2) |
| O4i—Mn1—O5 | 80.88 (3) | H42—C4—H43 | 107.0 (3) |
| O1—Mn1—O5i | 87.14 (3) | C6—C5—O5 | 117.79 (6) |
| O1i—Mn1—O5i | 92.86 (3) | C6—C5—O6 | 118.30 (6) |
| O4—Mn1—O5i | 80.88 (3) | O5—C5—O6 | 123.91 (7) |
| O4i—Mn1—O5i | 99.12 (3) | C5—C6—H61 | 110.80 (18) |
| O5—Mn1—O5i | 179.995 | C5—C6—H62 | 112.40 (16) |
| O1—Mn2—O2ii | 177.19 (6) | H61—C6—H62 | 111.2 (4) |
| O1—Mn2—O3 | 99.40 (5) | C5—C6—H63 | 109.96 (18) |
| O2ii—Mn2—O3 | 83.39 (4) | H61—C6—H63 | 102.5 (4) |
| O1—Mn2—O6 | 97.50 (5) | H62—C6—H63 | 109.5 (4) |
| O2ii—Mn2—O6 | 82.31 (5) | Mn1—O1—Mn2 | 109.02 (4) |
| O3—Mn2—O6 | 87.45 (5) | Mn1—O1—C1 | 135.23 (5) |
| O1—Mn2—O7 | 90.12 (5) | Mn2—O1—C1 | 115.69 (6) |
| O2ii—Mn2—O7 | 90.47 (5) | Mn2iii—O2—C1 | 144.10 (6) |
| O3—Mn2—O7 | 83.25 (4) | Mn2—O3—C3 | 131.54 (6) |
| O6—Mn2—O7 | 168.83 (6) | Mn1—O4—C3 | 138.75 (6) |
| O1—Mn2—O8 | 85.52 (4) | Mn1—O5—C5 | 138.33 (6) |
| O2ii—Mn2—O8 | 91.68 (5) | Mn2—O6—C5 | 132.98 (6) |
| O3—Mn2—O8 | 168.91 (6) | Mn2—O7—D20 | 119.2 (1) |
| O6—Mn2—O8 | 82.04 (4) | Mn2—O7—D21 | 122.4 (1) |
| O7—Mn2—O8 | 106.80 (5) | D20—O7—D21 | 107.59 (13) |
| C2—C1—O1 | 119.47 (6) | Mn2—O8—D16 | 121.5 (1) |
| C2—C1—O2 | 119.90 (6) | Mn2—O8—D17 | 120.15 (9) |
| O1—C1—O2 | 120.64 (6) | D16—O8—D17 | 108.25 (13) |
| C1—C2—H21 | 112.14 (13) | D18—O9—D19 | 106.79 (14) |
| C1—C2—H22 | 109.3 (2) | D9—O10—D10 | 110.07 (14) |
| H21—C2—H22 | 108.0 (4) | D14—O11—D15 | 106.17 (14) |
| C1—C2—H23 | 110.6 (2) | D4—O12—D5 | 107.44 (15) |
| H21—C2—H23 | 111.7 (4) |
| Symmetry codes: (i) −x, −y, −z; (ii) x, −y+1/2, z−1/2; (iii) x, −y+1/2, z+1/2. |
(300K) manganese acetate tetrahydrate top
Crystal data top
| Mn·2(C2H3O2)·4(D2O) | Z = 6 |
| Mr = 252.9 | F(000) = 483.17 |
| Monoclinic, P21/c | Dx = 1.53 Mg m−3 |
| Hall symbol: -P 2ybc | Neutron radiation, λ = 0.8308 Å |
| a = 11.10 (3) Å | Cell parameters from 14 reflections |
| b = 17.51 (3) Å | θ = 14.6–25° |
| c = 9.09 (2) Å | T = 300 K |
| β = 118.6 (2)° | Prism, pink |
| V = 1551.2 Å3 | 3.00 × 3.00 × 3.00 mm |
Data collection top
| Orphée reactor (Saclay, France) : 5C2 four-circle diffractometer | Rint = 0.05 |
| Radiation source: Orphée reactor Saclay France | θmax = 22.5°, θmin = 2.5° |
| Cu (220) monochromator | h = −12→4 |
| ω scans, | k = −10→19 |
| 3536 measured reflections | l = −9→10 |
| 2222 independent reflections | 2 standard reflections every 0 reflections |
| 1570 reflections with > 3.00σ(I) | intensity decay: 0.0% |
Refinement top
| Refinement on F2 | Hydrogen site location: inferred from neighbouring sites |
| Least-squares matrix: full | |
| R[F2 > 2σ(F2)] = 0.066 | (Δ/σ)max = 0.069 |
| wR(F2) = 0.0456 | Δρmax = 1.32 e Å−3 |
| 1570 reflections | Δρmin = −1.50 e Å−3 |
| 314 parameters | Extinction correction: Larson 1970 Crystallographic Computing eq 22, equ(22) p292 "Larson, Crystallographic Computing" (1969) |
| Primary atom site location: structure-invariant direct methods | Extinction coefficient: 5.1 (4) |
Crystal data top
| Mn·2(C2H3O2)·4(D2O) | β = 118.6 (2)° |
| Mr = 252.9 | V = 1551.2 Å3 |
| Monoclinic, P21/c | Z = 6 |
| a = 11.10 (3) Å | Neutron radiation, λ = 0.8308 Å |
| b = 17.51 (3) Å | T = 300 K |
| c = 9.09 (2) Å | 3.00 × 3.00 × 3.00 mm |
Data collection top
| Orphée reactor (Saclay, France) : 5C2 four-circle diffractometer | Rint = 0.05 |
| 3536 measured reflections | θmax = 22.5° |
| 2222 independent reflections | 2 standard reflections every 0 reflections |
| 1570 reflections with > 3.00σ(I) | intensity decay: 0.0% |
Refinement top
| R[F2 > 2σ(F2)] = 0.066 | 314 parameters |
| wR(F2) = 0.0456 | Δρmax = 1.32 e Å−3 |
| 1570 reflections | Δρmin = −1.50 e Å−3 |
Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top
| x | y | z | Uiso*/Ueq | Occ. (<1) | |
| Mn1 | 0.0000 | 0.0000 | 0.0000 | 0.0219 | 0.5000 |
| Mn2 | 0.0208 (5) | 0.2015 (3) | −0.0667 (6) | 0.0232 | |
| C1 | 0.0131 (3) | 0.14135 (16) | 0.2390 (4) | 0.0253 | |
| C2 | 0.0036 (5) | 0.0871 (2) | 0.3609 (5) | 0.0501 | |
| C3 | 0.2194 (3) | 0.07975 (17) | −0.0884 (4) | 0.0275 | |
| C4 | 0.3385 (5) | 0.0625 (2) | −0.1176 (8) | 0.0678 | |
| C5 | −0.1988 (3) | 0.08875 (16) | −0.3406 (4) | 0.0272 | |
| C6 | −0.3200 (4) | 0.0784 (3) | −0.5113 (5) | 0.0571 | |
| O1 | 0.0098 (4) | 0.11565 (17) | 0.1055 (4) | 0.0258 | |
| O2 | 0.0237 (4) | 0.21124 (19) | 0.2680 (5) | 0.0327 | |
| O3 | 0.1734 (4) | 0.1470 (2) | −0.1130 (5) | 0.0379 | |
| O4 | 0.1719 (4) | 0.0261 (2) | −0.0413 (5) | 0.0354 | |
| O5 | −0.1634 (4) | 0.0332 (2) | −0.2416 (5) | 0.0368 | |
| O6 | −0.1368 (4) | 0.1520 (2) | −0.3052 (4) | 0.0365 | |
| O7 | 0.2060 (5) | 0.2547 (2) | 0.1497 (6) | 0.0381 | |
| O8 | −0.1620 (5) | 0.2535 (2) | −0.0677 (8) | 0.0340 | |
| O9 | 0.4282 (8) | 0.3165 (3) | 0.1235 (12) | 0.0542 | |
| O10 | 0.6174 (9) | 0.1951 (5) | 0.1532 (9) | 0.0660 | |
| O11 | 0.6678 (6) | 0.3776 (5) | 0.4119 (6) | 0.0458 | |
| O12 | 0.3347 (6) | 0.1044 (5) | 0.3305 (8) | 0.0604 | |
| D4 | 0.288 (1) | 0.1441 (6) | 0.2511 (12) | 0.0735 | 0.63 (3) |
| D5 | 0.2757 (9) | 0.0589 (6) | 0.2926 (11) | 0.0599 | 0.58 (3) |
| D9 | 0.6223 (8) | 0.1728 (5) | 0.0588 (13) | 0.0615 | 0.60 (3) |
| D10 | 0.5432 (14) | 0.2295 (7) | 0.1161 (12) | 0.0724 | 0.59 (3) |
| D14 | 0.7119 (9) | 0.4261 (6) | 0.437 (1) | 0.0661 | 0.66 (3) |
| D15 | 0.738 (1) | 0.3429 (6) | 0.4211 (11) | 0.0686 | 0.65 (3) |
| D16 | −0.1540 (6) | 0.2837 (4) | 0.0263 (9) | 0.0405 | 0.64 (2) |
| D17 | −0.2362 (8) | 0.2750 (4) | −0.170 (1) | 0.0489 | 0.63 (2) |
| D18 | 0.3956 (7) | 0.3489 (5) | 0.0233 (12) | 0.0573 | 0.63 (3) |
| D19 | 0.5020 (11) | 0.3442 (6) | 0.2147 (13) | 0.0632 | 0.59 (3) |
| D20 | 0.1950 (6) | 0.2834 (4) | 0.2337 (9) | 0.0442 | 0.63 (2) |
| D21 | 0.2802 (7) | 0.2776 (4) | 0.1372 (8) | 0.0420 | 0.60 (2) |
Atomic displacement parameters (Å2) top
| U11 | U22 | U33 | U12 | U13 | U23 | |
| Mn1 | 0.032 (4) | 0.011 (3) | 0.029 (4) | −0.002 (3) | 0.020 (3) | −0.004 (3) |
| Mn2 | 0.027 (3) | 0.016 (2) | 0.030 (3) | 0.0008 (19) | 0.016 (2) | 0.0004 (19) |
| C1 | 0.0364 (17) | 0.0167 (15) | 0.0277 (15) | −0.0006 (11) | 0.0194 (13) | −0.0035 (12) |
| C2 | 0.103 (3) | 0.0222 (17) | 0.047 (2) | −0.0046 (18) | 0.054 (2) | 0.0043 (15) |
| C3 | 0.0302 (16) | 0.0211 (16) | 0.0385 (16) | 0.0004 (11) | 0.0222 (13) | −0.0003 (12) |
| C4 | 0.057 (3) | 0.044 (2) | 0.142 (5) | 0.0157 (19) | 0.079 (3) | 0.020 (2) |
| C5 | 0.0339 (16) | 0.0221 (16) | 0.0285 (15) | −0.0010 (12) | 0.0171 (13) | 0.0005 (12) |
| C6 | 0.048 (2) | 0.057 (3) | 0.033 (2) | −0.0173 (18) | −0.0077 (17) | 0.0107 (17) |
| O1 | 0.040 (2) | 0.0144 (16) | 0.0270 (17) | 0.0010 (12) | 0.0189 (15) | −0.0036 (13) |
| O2 | 0.052 (2) | 0.0159 (18) | 0.039 (2) | 0.0005 (15) | 0.0288 (18) | −0.0039 (15) |
| O3 | 0.050 (2) | 0.0237 (19) | 0.056 (2) | 0.0107 (16) | 0.038 (2) | 0.0079 (16) |
| O4 | 0.041 (2) | 0.0264 (19) | 0.052 (2) | −0.0017 (15) | 0.0320 (19) | 0.0004 (16) |
| O5 | 0.041 (2) | 0.0237 (18) | 0.035 (2) | −0.0011 (15) | 0.0105 (17) | 0.0053 (15) |
| O6 | 0.046 (2) | 0.028 (2) | 0.0311 (19) | −0.0081 (16) | 0.0154 (16) | −0.0025 (15) |
| O7 | 0.044 (3) | 0.039 (2) | 0.035 (2) | −0.015 (2) | 0.022 (2) | −0.007 (2) |
| O8 | 0.037 (3) | 0.035 (2) | 0.030 (2) | 0.0100 (19) | 0.016 (2) | 0.002 (2) |
| O9 | 0.056 (3) | 0.062 (3) | 0.051 (3) | −0.016 (3) | 0.030 (3) | −0.004 (4) |
| O10 | 0.057 (4) | 0.074 (4) | 0.055 (4) | 0.002 (3) | 0.017 (3) | −0.009 (4) |
| O11 | 0.041 (3) | 0.041 (3) | 0.063 (3) | −0.005 (3) | 0.030 (2) | −0.002 (2) |
| O12 | 0.050 (3) | 0.052 (3) | 0.056 (3) | −0.005 (4) | 0.007 (3) | −0.000 (4) |
| D4 | 0.078 (6) | 0.068 (7) | 0.058 (6) | −0.006 (5) | 0.020 (5) | 0.008 (5) |
| D5 | 0.055 (6) | 0.049 (6) | 0.068 (6) | −0.007 (4) | 0.023 (4) | −0.012 (4) |
| D9 | 0.063 (5) | 0.069 (6) | 0.049 (6) | −0.008 (4) | 0.024 (4) | −0.019 (4) |
| D10 | 0.065 (8) | 0.086 (8) | 0.064 (6) | −0.010 (6) | 0.028 (5) | −0.008 (5) |
| D14 | 0.070 (5) | 0.056 (7) | 0.082 (6) | −0.002 (5) | 0.045 (4) | 0.002 (4) |
| D15 | 0.053 (6) | 0.073 (6) | 0.084 (6) | −0.001 (5) | 0.036 (4) | −0.007 (4) |
| D16 | 0.045 (4) | 0.040 (4) | 0.041 (5) | 0.003 (2) | 0.024 (3) | −0.004 (3) |
| D17 | 0.050 (5) | 0.049 (4) | 0.050 (6) | −0.001 (3) | 0.026 (5) | −0.001 (3) |
| D18 | 0.050 (4) | 0.067 (5) | 0.057 (6) | 0.002 (3) | 0.027 (4) | 0.004 (5) |
| D19 | 0.056 (6) | 0.070 (6) | 0.066 (7) | −0.003 (4) | 0.032 (5) | −0.004 (5) |
| D20 | 0.052 (4) | 0.051 (4) | 0.036 (4) | −0.003 (3) | 0.027 (3) | −0.008 (3) |
| D21 | 0.043 (5) | 0.040 (4) | 0.051 (4) | −0.010 (3) | 0.030 (3) | −0.008 (3) |
Geometric parameters (Å, º) top
| Mn1—O1 | 2.221 (3) | C3—O4 | 1.249 (5) |
| Mn1—O1i | 2.221 (3) | C5—C6 | 1.501 (5) |
| Mn1—O4 | 2.163 (3) | C5—O5 | 1.254 (5) |
| Mn1—O4i | 2.163 (3) | C5—O6 | 1.262 (5) |
| Mn1—O5 | 2.153 (4) | O7—D20 | 0.971 (7) |
| Mn1—O5i | 2.153 (4) | O7—D21 | 0.969 (7) |
| Mn2—O1 | 2.216 (6) | O8—D16 | 0.972 (6) |
| Mn2—O2ii | 2.154 (6) | O8—D17 | 0.976 (7) |
| Mn2—O3 | 2.154 (6) | O9—D18 | 0.984 (8) |
| Mn2—O6 | 2.209 (6) | O9—D19 | 0.972 (9) |
| Mn2—O7 | 2.256 (6) | O10—D9 | 0.968 (9) |
| Mn2—O8 | 2.220 (6) | O10—D10 | 0.943 (11) |
| C1—C2 | 1.501 (4) | O11—D14 | 0.952 (9) |
| C1—O1 | 1.278 (4) | O11—D15 | 0.958 (9) |
| C1—O2 | 1.245 (5) | O12—D4 | 0.956 (9) |
| C3—C4 | 1.498 (5) | O12—D5 | 0.984 (9) |
| C3—O3 | 1.261 (5) | ||
| O1—Mn1—O1i | 179.995 | C2—C1—O1 | 119.9 (3) |
| O1—Mn1—O4 | 91.02 (13) | C2—C1—O2 | 119.9 (3) |
| O1i—Mn1—O4 | 88.98 (13) | O1—C1—O2 | 120.2 (3) |
| O1—Mn1—O4i | 88.98 (13) | C1—C2—H1 | 178.2 (19) |
| O1i—Mn1—O4i | 91.02 (13) | C4—C3—O3 | 118.3 (3) |
| O4—Mn1—O4i | 179.995 | C4—C3—O4 | 117.5 (3) |
| O1—Mn1—O5 | 92.13 (13) | O3—C3—O4 | 124.2 (3) |
| O1i—Mn1—O5 | 87.87 (13) | C3—C4—H2 | 175 (2) |
| O4—Mn1—O5 | 98.54 (15) | C6—C5—O5 | 117.8 (3) |
| O4i—Mn1—O5 | 81.46 (15) | C6—C5—O6 | 118.6 (3) |
| O1—Mn1—O5i | 87.86 (13) | O5—C5—O6 | 123.6 (3) |
| O1i—Mn1—O5i | 92.14 (13) | C5—C6—H3 | 179 (2) |
| O4—Mn1—O5i | 81.46 (15) | Mn1—O1—Mn2 | 108.75 (18) |
| O4i—Mn1—O5i | 98.54 (15) | Mn1—O1—C1 | 134.8 (2) |
| O5—Mn1—O5i | 179.995 | Mn2—O1—C1 | 116.5 (3) |
| O1—Mn2—O2ii | 176.9 (3) | Mn2iii—O2—C1 | 144.4 (3) |
| O1—Mn2—O3 | 98.7 (2) | Mn2—O3—C3 | 132.0 (3) |
| O2ii—Mn2—O3 | 84.4 (2) | Mn1—O4—C3 | 140.4 (3) |
| O1—Mn2—O6 | 98.1 (2) | Mn1—O5—C5 | 139.7 (3) |
| O2ii—Mn2—O6 | 82.1 (2) | Mn2—O6—C5 | 132.3 (3) |
| O3—Mn2—O6 | 87.8 (2) | Mn2—O7—D20 | 119.6 (6) |
| O1—Mn2—O7 | 90.0 (2) | Mn2—O7—D21 | 122.6 (6) |
| O2ii—Mn2—O7 | 90.2 (2) | D20—O7—D21 | 108.2 (6) |
| O3—Mn2—O7 | 83.1 (3) | Mn2—O8—D16 | 121.4 (5) |
| O6—Mn2—O7 | 168.6 (3) | Mn2—O8—D17 | 121.0 (6) |
| O1—Mn2—O8 | 85.5 (2) | D16—O8—D17 | 108.0 (6) |
| O2ii—Mn2—O8 | 91.4 (2) | D18—O9—D19 | 106.7 (9) |
| O3—Mn2—O8 | 169.6 (3) | D9—O10—D10 | 110.5 (10) |
| O6—Mn2—O8 | 82.2 (3) | D14—O11—D15 | 103.9 (9) |
| O7—Mn2—O8 | 106.5 (3) | D4—O12—D5 | 107.1 (9) |
| Symmetry codes: (i) −x, −y, −z; (ii) x, −y+1/2, z−1/2; (iii) x, −y+1/2, z+1/2. |
Experimental details
| (14K) | (300K) | |
| Crystal data | ||
| Chemical formula | Mn·2(C2H3O2)·4(D2O) | Mn·2(C2H3O2)·4(D2O) |
| Mr | 252.9 | 252.9 |
| Crystal system, space group | Monoclinic, P21/c | Monoclinic, P21/c |
| Temperature (K) | 14 | 300 |
| a, b, c (Å) | 10.88 (3), 17.39 (3), 9.04 (2) | 11.10 (3), 17.51 (3), 9.09 (2) |
| β (°) | 118.8 (2) | 118.6 (2) |
| V (Å3) | 1498.8 | 1551.2 |
| Z | 6 | 6 |
| Radiation type | Neutron, λ = 0.83080 Å | Neutron, λ = 0.8308 Å |
| µ (mm−1) | ? | ? |
| Crystal size (mm) | 3.00 × 3.00 × 3.00 | 3.00 × 3.00 × 3.00 |
| Data collection | ||
| Diffractometer | Orphée reactor (Saclay, France) : 5C2 four-circle diffractometer | Orphée reactor (Saclay, France) : 5C2 four-circle diffractometer |
| Absorption correction | – | – |
| No. of measured, independent and observed [ > 3.00σ(I)] reflections | 7656, 6227, 4686 | 3536, 2222, 1570 |
| Rint | 0.05 | 0.05 |
| θmax (°) | 40 | 22.5 |
| (sin θ/λ)max (Å−1) | 0.774 | 0.461 |
| Refinement | ||
| R[F2 > 2σ(F2)], wR(F2), S | 0.041, 0.0383, ? | 0.066, 0.0456, ? |
| No. of reflections | 4686 | 1570 |
| No. of parameters | 380 | 314 |
| No. of restraints | ? | ? |
| Δρmax, Δρmin (e Å−3) | 1.37, −2.21 | 1.32, −1.50 |
Computer programs: CAD-4 Software (Enraf-Nonius, 1989), DIF4 modified version of STOE 4 circle diffractometer control program (1996), STOE PW110, PRON modified version of REDU4 (STOE) 1996 diffractometer control program (1996), PRON modified version of REDU4 (STOE) 1996, CRYSTALS Issue 10 (Watkin, Prout, Carruthers & Betteridge, 1996), CRYSTALS (Watkin et al., 1996), CAMERON (Pearce et al., 1996), CAMERON (Pearce et al., 1994).
Selected geometric parameters (Å, º) for (14K) top
| Mn1—O1 | 2.1948 (7) | C3—O4 | 1.2600 (9) |
| Mn1—O1i | 2.1948 (7) | C5—C6 | 1.5042 (9) |
| Mn1—O4 | 2.1644 (7) | C5—O5 | 1.2599 (9) |
| Mn1—O4i | 2.1644 (7) | C5—O6 | 1.2641 (9) |
| Mn1—O5 | 2.1402 (7) | O7—D20 | 0.9725 (15) |
| Mn1—O5i | 2.1402 (7) | O7—D21 | 0.9784 (14) |
| Mn2—O1 | 2.2029 (12) | O8—D16 | 0.9780 (15) |
| Mn2—O2ii | 2.1339 (12) | O8—D17 | 0.9850 (15) |
| Mn2—O3 | 2.1693 (12) | O9—D18 | 0.9808 (16) |
| Mn2—O6 | 2.1941 (13) | O9—D19 | 0.9673 (16) |
| Mn2—O7 | 2.2417 (13) | O10—D9 | 0.9667 (16) |
| Mn2—O8 | 2.2149 (12) | O10—D10 | 0.9663 (17) |
| C1—C2 | 1.5051 (9) | O11—D14 | 0.9710 (17) |
| C1—O1 | 1.2866 (9) | O11—D15 | 0.9691 (15) |
| C1—O2 | 1.2437 (9) | O12—D4 | 0.9624 (18) |
| C3—C4 | 1.5092 (9) | O12—D5 | 0.9675 (17) |
| C3—O3 | 1.2623 (9) | ||
| O1—Mn1—O1i | 179.995 | O7—Mn2—O8 | 106.80 (5) |
| O1—Mn1—O4 | 92.03 (3) | C2—C1—O1 | 119.47 (6) |
| O1i—Mn1—O4 | 87.97 (3) | C2—C1—O2 | 119.90 (6) |
| O1—Mn1—O4i | 87.97 (3) | O1—C1—O2 | 120.64 (6) |
| O1i—Mn1—O4i | 92.03 (3) | C4—C3—O3 | 117.52 (6) |
| O4—Mn1—O4i | 179.995 | C4—C3—O4 | 117.85 (6) |
| O1—Mn1—O5 | 92.86 (3) | O3—C3—O4 | 124.62 (6) |
| O1i—Mn1—O5 | 87.14 (3) | C6—C5—O5 | 117.79 (6) |
| O4—Mn1—O5 | 99.12 (3) | C6—C5—O6 | 118.30 (6) |
| O4i—Mn1—O5 | 80.88 (3) | O5—C5—O6 | 123.91 (7) |
| O1—Mn1—O5i | 87.14 (3) | Mn1—O1—Mn2 | 109.02 (4) |
| O1i—Mn1—O5i | 92.86 (3) | Mn1—O1—C1 | 135.23 (5) |
| O4—Mn1—O5i | 80.88 (3) | Mn2—O1—C1 | 115.69 (6) |
| O4i—Mn1—O5i | 99.12 (3) | Mn2iii—O2—C1 | 144.10 (6) |
| O5—Mn1—O5i | 179.995 | Mn2—O3—C3 | 131.54 (6) |
| O1—Mn2—O2ii | 177.19 (6) | Mn1—O4—C3 | 138.75 (6) |
| O1—Mn2—O3 | 99.40 (5) | Mn1—O5—C5 | 138.33 (6) |
| O2ii—Mn2—O3 | 83.39 (4) | Mn2—O6—C5 | 132.98 (6) |
| O1—Mn2—O6 | 97.50 (5) | Mn2—O7—D20 | 119.2 (1) |
| O2ii—Mn2—O6 | 82.31 (5) | Mn2—O7—D21 | 122.4 (1) |
| O3—Mn2—O6 | 87.45 (5) | D20—O7—D21 | 107.59 (13) |
| O1—Mn2—O7 | 90.12 (5) | Mn2—O8—D16 | 121.5 (1) |
| O2ii—Mn2—O7 | 90.47 (5) | Mn2—O8—D17 | 120.15 (9) |
| O3—Mn2—O7 | 83.25 (4) | D16—O8—D17 | 108.25 (13) |
| O6—Mn2—O7 | 168.83 (6) | D18—O9—D19 | 106.79 (14) |
| O1—Mn2—O8 | 85.52 (4) | D9—O10—D10 | 110.07 (14) |
| O2ii—Mn2—O8 | 91.68 (5) | D14—O11—D15 | 106.17 (14) |
| O3—Mn2—O8 | 168.91 (6) | D4—O12—D5 | 107.44 (15) |
| O6—Mn2—O8 | 82.04 (4) |
| Symmetry codes: (i) −x, −y, −z; (ii) x, −y+1/2, z−1/2; (iii) x, −y+1/2, z+1/2. |
Selected geometric parameters (Å, º) for (300K) top
| Mn1—O1 | 2.221 (3) | C3—O4 | 1.249 (5) |
| Mn1—O1i | 2.221 (3) | C5—C6 | 1.501 (5) |
| Mn1—O4 | 2.163 (3) | C5—O5 | 1.254 (5) |
| Mn1—O4i | 2.163 (3) | C5—O6 | 1.262 (5) |
| Mn1—O5 | 2.153 (4) | O7—D20 | 0.971 (7) |
| Mn1—O5i | 2.153 (4) | O7—D21 | 0.969 (7) |
| Mn2—O1 | 2.216 (6) | O8—D16 | 0.972 (6) |
| Mn2—O2ii | 2.154 (6) | O8—D17 | 0.976 (7) |
| Mn2—O3 | 2.154 (6) | O9—D18 | 0.984 (8) |
| Mn2—O6 | 2.209 (6) | O9—D19 | 0.972 (9) |
| Mn2—O7 | 2.256 (6) | O10—D9 | 0.968 (9) |
| Mn2—O8 | 2.220 (6) | O10—D10 | 0.943 (11) |
| C1—C2 | 1.501 (4) | O11—D14 | 0.952 (9) |
| C1—O1 | 1.278 (4) | O11—D15 | 0.958 (9) |
| C1—O2 | 1.245 (5) | O12—D4 | 0.956 (9) |
| C3—C4 | 1.498 (5) | O12—D5 | 0.984 (9) |
| C3—O3 | 1.261 (5) | ||
| O1—Mn1—O1i | 179.995 | O7—Mn2—O8 | 106.5 (3) |
| O1—Mn1—O4 | 91.02 (13) | C2—C1—O1 | 119.9 (3) |
| O1i—Mn1—O4 | 88.98 (13) | C2—C1—O2 | 119.9 (3) |
| O1—Mn1—O4i | 88.98 (13) | O1—C1—O2 | 120.2 (3) |
| O1i—Mn1—O4i | 91.02 (13) | C4—C3—O3 | 118.3 (3) |
| O4—Mn1—O4i | 179.995 | C4—C3—O4 | 117.5 (3) |
| O1—Mn1—O5 | 92.13 (13) | O3—C3—O4 | 124.2 (3) |
| O1i—Mn1—O5 | 87.87 (13) | C6—C5—O5 | 117.8 (3) |
| O4—Mn1—O5 | 98.54 (15) | C6—C5—O6 | 118.6 (3) |
| O4i—Mn1—O5 | 81.46 (15) | O5—C5—O6 | 123.6 (3) |
| O1—Mn1—O5i | 87.86 (13) | Mn1—O1—Mn2 | 108.75 (18) |
| O1i—Mn1—O5i | 92.14 (13) | Mn1—O1—C1 | 134.8 (2) |
| O4—Mn1—O5i | 81.46 (15) | Mn2—O1—C1 | 116.5 (3) |
| O4i—Mn1—O5i | 98.54 (15) | Mn2iii—O2—C1 | 144.4 (3) |
| O5—Mn1—O5i | 179.995 | Mn2—O3—C3 | 132.0 (3) |
| O1—Mn2—O2ii | 176.9 (3) | Mn1—O4—C3 | 140.4 (3) |
| O1—Mn2—O3 | 98.7 (2) | Mn1—O5—C5 | 139.7 (3) |
| O2ii—Mn2—O3 | 84.4 (2) | Mn2—O6—C5 | 132.3 (3) |
| O1—Mn2—O6 | 98.1 (2) | Mn2—O7—D20 | 119.6 (6) |
| O2ii—Mn2—O6 | 82.1 (2) | Mn2—O7—D21 | 122.6 (6) |
| O3—Mn2—O6 | 87.8 (2) | D20—O7—D21 | 108.2 (6) |
| O1—Mn2—O7 | 90.0 (2) | Mn2—O8—D16 | 121.4 (5) |
| O2ii—Mn2—O7 | 90.2 (2) | Mn2—O8—D17 | 121.0 (6) |
| O3—Mn2—O7 | 83.1 (3) | D16—O8—D17 | 108.0 (6) |
| O6—Mn2—O7 | 168.6 (3) | D18—O9—D19 | 106.7 (9) |
| O1—Mn2—O8 | 85.5 (2) | D9—O10—D10 | 110.5 (10) |
| O2ii—Mn2—O8 | 91.4 (2) | D14—O11—D15 | 103.9 (9) |
| O3—Mn2—O8 | 169.6 (3) | D4—O12—D5 | 107.1 (9) |
| O6—Mn2—O8 | 82.2 (3) |
| Symmetry codes: (i) −x, −y, −z; (ii) x, −y+1/2, z−1/2; (iii) x, −y+1/2, z+1/2. |
