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The macrocyclic metallacrown complex DyNa(2-PV)4[12-MCMnIIINshi-4](H2O)4·4DMF, where MC is metallacrown, shi3− is salicyl­hydroximate, 2-PV is 2-propyl­valerate, and DMF is N,N-di­methyl­formamide, contains an [MnIII—N—O] repeat unit. A DyIII ion is captured on the convex side of the central MC cavity, while an Na+ ion is captured on the concave side. Four 2-propyl­valerate anions bridge between each ring MnIII ion and the central DyIII ion.

Supporting information

cif

Crystallographic Information File (CIF) https://doi.org/10.1107/S2056989022010489/ex2062sup1.cif
Contains datablocks I, global

hkl

Structure factor file (CIF format) https://doi.org/10.1107/S2056989022010489/ex2062Isup3.hkl
Contains datablock I

CCDC reference: 2216645

Computing details top

Data collection: APEX4 (Bruker, 2022); cell refinement: SAINT (Bruker, 2022); data reduction: SAINT (Bruker, 2022); program(s) used to solve structure: SHELXT (Sheldrick, 2015a); program(s) used to refine structure: SHELXL2018/3 (Sheldrick, 2015b), ShelXle (Hübschle et al., 2011); molecular graphics: Mercury (Macrae et al., 2020); software used to prepare material for publication: publCIF (Westrip, 2010).

Tetraaquatetrakis(µ-2-propylvalerato)tetrakis(µ4-salicylhydroximato)dysprosiumtetramanganesesodium dimethylformamide tetrasolvate, top
Crystal data top
[DyMn4Na(C7H4NO3)4(C8H15O2)4(H2O)4]·4C3H7NODx = 1.441 Mg m3
Mr = 1942.94Mo Kα radiation, λ = 0.71073 Å
Tetragonal, P4/nCell parameters from 9870 reflections
a = 18.2654 (9) Åθ = 2.5–32.0°
c = 13.4219 (9) ŵ = 1.45 mm1
V = 4477.9 (5) Å3T = 150 K
Z = 2Plate, brown
F(000) = 2002.20.45 × 0.43 × 0.15 mm
Data collection top
Bruker AXS D8 Quest
diffractometer
7801 independent reflections
Radiation source: fine focus sealed tube X-ray source5435 reflections with I > 2σ(I)
Triumph curved graphite crystal monochromatorRint = 0.070
Detector resolution: 7.4074 pixels mm-1θmax = 32.1°, θmin = 2.2°
ω and phi scansh = 2724
Absorption correction: multi-scan
(SADABS; Krause et al., 2015)
k = 2727
Tmin = 0.020, Tmax = 0.060l = 1919
87812 measured reflections
Refinement top
Refinement on F2Primary atom site location: dual
Least-squares matrix: fullSecondary atom site location: difference Fourier map
R[F2 > 2σ(F2)] = 0.072Hydrogen site location: mixed
wR(F2) = 0.257H atoms treated by a mixture of independent and constrained refinement
S = 1.07 w = 1/[σ2(Fo2) + (0.1326P)2 + 7.8338P]
where P = (Fo2 + 2Fc2)/3
7801 reflections(Δ/σ)max = 0.013
708 parametersΔρmax = 1.36 e Å3
2628 restraintsΔρmin = 1.96 e Å3
Special details top

Geometry. All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes.

Refinement. Minor whole molecule disorder was detected for the metallacrown molecule and all organic fragments (excluding the dysprosium and sodium ions), and the disorder was refined. The metallacrown is disordered by clockwise vs counterclockwise rotation orientation of the metallacycle, as are the 2-propylvalerate anion and the interstitial DMF molecule (main moiety and B-moiety). In addition, the alkyl chain of the 2-propylvalerate of the main moiety is disordered over two additional sites, and the interstitial DMF molecule of the main moiety is disordered over one additional site. The Uij components of ADPs for disordered atoms closer to each other than 2.7 Angstrom were restrained to be similar (SIMU command of Shelxl). Occupancies were constrained to sum up to unity for all sites using SUMP commands.

The major and minor (B-moiety) metallacrown units were restrained to have similar geometries. For the B-moiety benzene ring of the salicylhydroximate, the C atoms were restrained to be close to planar (FLAT command of Shelxl).

For the 2-propylvalerate anion, the major (including the additional alkyl chain disorder) and B moieties were restrained to have similar geometries. The C atoms positions 2-propylvalerate were further restrained based on typical carbon-carbon bond distances and angles. The B-moiety carboxylate carbon atom (C8B) was restrained to planarity (CHIV command of Shelxl).

For the interstitial DMF molecule, the N atom was restrained to be equidistant from both carbon atoms of the methyl groups. In addition, the major (including the additional disorder) and B moieties were restrained to have similar geometries.

H atom positions of the water molecule coordinated to the sodium ion were refined and O-H and H···H distances were restrained to 0.84 (2) and 1.36 (2) Angstrom, respectively. The water O and H atom positions were further restrained based on hydrogen bonding considerations to the interstitial DMF molecule and distances of all water H atoms to the sodium ion were restrained to be similar.

All other hydrogen atoms were placed in calculated positions and refined as riding on their carrier atoms with C-H distances of 0.95 Angstrom for sp2 carbon atoms. The Uiso values for hydrogen atoms were set to a multiple of the Ueq value of the carrying carbon atom (1.2 times for sp2 hybridized carbon atoms, 1.5 for water molecules and methyl groups).

Subject to these conditions the occupancy ratios were refined as follows:

main metallacrown unit: 0.9030 (14) B-moiety metallacrown unit: 0.0971 (14)

main alkyl chain of 2-propylvalerate: 0.287 (3): 0.309 (3): 0.307 (3) B-moiety alkyl chain: 0.0971 (14)

main interstitial DMF: 0.549 (3): 0.354 (3) B-moiety DMF: 0.0971 (14)

Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top
xyzUiso*/UeqOcc. (<1)
Dy10.2500000.2500000.78820 (3)0.05635 (17)
Na10.2500000.2500000.5233 (3)0.0524 (8)
Mn10.14036 (4)0.39036 (4)0.64460 (7)0.0514 (2)0.9030 (14)
O10.23534 (18)0.34977 (18)0.6685 (3)0.0490 (7)0.9030 (14)
O20.19756 (19)0.4788 (2)0.6261 (3)0.0563 (8)0.9030 (14)
O30.4255 (2)0.4468 (2)0.5953 (4)0.0683 (11)0.9030 (14)
N10.2918 (3)0.4000 (2)0.6508 (9)0.0499 (9)0.9030 (14)
C10.2672 (3)0.4663 (3)0.6306 (4)0.0504 (9)0.9030 (14)
C20.3191 (3)0.5252 (3)0.6105 (5)0.0563 (11)0.9030 (14)
C30.2920 (3)0.5972 (3)0.6059 (6)0.0631 (12)0.9030 (14)
H30.2416450.6059350.6187110.076*0.9030 (14)
C40.3373 (4)0.6556 (3)0.5831 (7)0.0696 (15)0.9030 (14)
H40.3180070.7038110.5792810.084*0.9030 (14)
C50.4104 (4)0.6431 (3)0.5662 (7)0.0706 (16)0.9030 (14)
H50.4416140.6831170.5505660.085*0.9030 (14)
C60.4391 (3)0.5732 (3)0.5714 (5)0.0664 (14)0.9030 (14)
H60.4898160.5658430.5590090.080*0.9030 (14)
C70.3947 (3)0.5131 (3)0.5948 (5)0.0581 (11)0.9030 (14)
O40.1581 (3)0.3123 (3)0.8654 (4)0.0740 (12)0.9030 (14)
O50.1146 (3)0.4144 (3)0.7956 (4)0.0773 (12)0.9030 (14)
C80.1192 (5)0.3701 (5)0.8633 (6)0.0876 (18)0.9030 (14)
C90.0809 (12)0.3783 (19)0.9652 (13)0.104 (3)0.287 (3)
H90.0830890.3277580.9936590.125*0.287 (3)
C100.0002 (12)0.3888 (18)0.943 (2)0.107 (4)0.287 (3)
H10A0.0261530.3923951.0075400.128*0.287 (3)
H10B0.0059160.4362070.9085090.128*0.287 (3)
C110.0354 (14)0.3317 (19)0.883 (3)0.112 (4)0.287 (3)
H11A0.0244960.2838240.9141160.135*0.287 (3)
H11B0.0121640.3318050.8164300.135*0.287 (3)
C120.1184 (14)0.336 (2)0.868 (3)0.134 (8)0.287 (3)
H12A0.1347360.2953660.8267350.201*0.287 (3)
H12B0.1429030.3344830.9328440.201*0.287 (3)
H12C0.1305150.3826830.8347130.201*0.287 (3)
C130.1196 (14)0.4221 (16)1.0385 (17)0.110 (3)0.287 (3)
H13A0.1020730.4731931.0322170.132*0.287 (3)
H13B0.1721130.4220041.0203700.132*0.287 (3)
C140.1138 (17)0.401 (2)1.1475 (15)0.118 (4)0.287 (3)
H14A0.0656660.3775461.1598670.142*0.287 (3)
H14B0.1172930.4450421.1895320.142*0.287 (3)
C150.177 (2)0.345 (2)1.177 (2)0.126 (7)0.287 (3)
H15A0.1557960.2981781.1975040.188*0.287 (3)
H15B0.2057570.3653581.2326590.188*0.287 (3)
H15C0.2096320.3372121.1198680.188*0.287 (3)
O60.1794 (2)0.3562 (3)0.4701 (3)0.0613 (9)0.9030 (14)
H6A0.207 (2)0.383 (3)0.433 (5)0.092*0.9030 (14)
H6E0.144 (3)0.343 (3)0.435 (5)0.092*0.9030 (14)
C9C0.0715 (15)0.3936 (16)0.9511 (19)0.101 (3)0.309 (3)
H9C0.1066910.3702990.9985200.122*0.309 (3)
C10C0.0167 (16)0.3347 (15)0.9718 (19)0.109 (4)0.309 (3)
H10C0.0391800.3026121.0228950.131*0.309 (3)
H10D0.0253230.3590391.0044380.131*0.309 (3)
C11C0.0138 (15)0.2868 (18)0.898 (2)0.111 (4)0.309 (3)
H11C0.0099710.2385350.9075500.133*0.309 (3)
H11D0.0028980.3053480.8326150.133*0.309 (3)
C12C0.0956 (15)0.272 (2)0.888 (3)0.122 (7)0.309 (3)
H12D0.1034220.2287170.8466720.183*0.309 (3)
H12E0.1194440.3145010.8572900.183*0.309 (3)
H12F0.1166900.2637790.9544390.183*0.309 (3)
C13C0.0880 (15)0.4648 (13)0.992 (2)0.109 (3)0.309 (3)
H13C0.0479670.4810261.0366520.131*0.309 (3)
H13D0.0935630.5011760.9379930.131*0.309 (3)
C14C0.1596 (16)0.4577 (15)1.051 (2)0.115 (4)0.309 (3)
H14C0.1575640.4852401.1142400.138*0.309 (3)
H14D0.2020820.4747351.0112020.138*0.309 (3)
C15C0.162 (2)0.3702 (17)1.070 (3)0.120 (6)0.309 (3)
H15D0.2120860.3521871.0566240.180*0.309 (3)
H15E0.1279340.3457351.0246150.180*0.309 (3)
H15F0.1490290.3596661.1387770.180*0.309 (3)
C9D0.0619 (11)0.375 (2)0.9491 (15)0.103 (3)0.307 (3)
H9D0.0646600.4284300.9642430.124*0.307 (3)
C10D0.0186 (13)0.3685 (16)0.922 (2)0.105 (4)0.307 (3)
H10E0.0467880.3882080.9791300.126*0.307 (3)
H10F0.0272810.4019420.8653130.126*0.307 (3)
C11D0.0511 (17)0.2995 (18)0.896 (3)0.118 (5)0.307 (3)
H11E0.0348980.2638080.9473760.142*0.307 (3)
H11F0.0287190.2840030.8326060.142*0.307 (3)
C12D0.1338 (17)0.290 (2)0.885 (4)0.132 (8)0.307 (3)
H12G0.1531740.2640010.9432120.198*0.307 (3)
H12H0.1441370.2617310.8246550.198*0.307 (3)
H12I0.1570150.3382280.8800810.198*0.307 (3)
C13D0.0917 (15)0.3450 (15)1.0424 (18)0.108 (3)0.307 (3)
H13E0.1141510.2966431.0293560.130*0.307 (3)
H13F0.0514480.3380781.0909340.130*0.307 (3)
C14D0.1487 (15)0.3961 (19)1.086 (2)0.113 (4)0.307 (3)
H14E0.1745490.4236231.0334580.136*0.307 (3)
H14F0.1849330.3687831.1266390.136*0.307 (3)
C15D0.100 (2)0.4496 (19)1.155 (3)0.130 (7)0.307 (3)
H15G0.0954460.4972421.1217710.194*0.307 (3)
H15H0.1241770.4559431.2193880.194*0.307 (3)
H15I0.0515710.4281701.1643850.194*0.307 (3)
Mn1B0.4210 (3)0.3002 (3)0.6438 (6)0.0469 (15)0.0971 (14)
O1B0.3183 (10)0.3217 (11)0.655 (3)0.050 (4)0.0971 (14)
O2B0.4248 (12)0.4055 (10)0.618 (3)0.052 (3)0.0971 (14)
O3B0.2210 (14)0.5183 (15)0.620 (3)0.058 (4)0.0971 (14)
N1B0.304 (2)0.3966 (16)0.648 (11)0.054 (4)0.0971 (14)
C1B0.3622 (14)0.4357 (11)0.627 (4)0.054 (3)0.0971 (14)
C2B0.3539 (14)0.5138 (11)0.608 (2)0.056 (3)0.0971 (14)
C3B0.4195 (17)0.5499 (18)0.584 (4)0.060 (3)0.0971 (14)
H3B0.4639640.5228610.5828590.073*0.0971 (14)
C4B0.421 (2)0.6238 (19)0.563 (5)0.062 (4)0.0971 (14)
H4B0.4650520.6482910.5461110.074*0.0971 (14)
C5B0.355 (2)0.660 (2)0.567 (5)0.063 (4)0.0971 (14)
H5B0.3550610.7111490.5523980.076*0.0971 (14)
C6B0.290 (2)0.6277 (15)0.591 (4)0.060 (4)0.0971 (14)
H6B0.2466630.6565430.5956480.072*0.0971 (14)
C7B0.2863 (14)0.5516 (15)0.609 (4)0.058 (3)0.0971 (14)
O4B0.249 (3)0.352 (2)0.881 (3)0.090 (5)0.0971 (14)
O5B0.190 (3)0.437 (3)0.793 (3)0.075 (6)0.0971 (14)
C8B0.215 (2)0.414 (2)0.872 (2)0.091 (5)0.0971 (14)
C9B0.212 (3)0.450 (3)0.976 (3)0.105 (4)0.0971 (14)
H9B0.2443920.4937220.9710600.126*0.0971 (14)
C10B0.135 (3)0.480 (4)0.988 (4)0.106 (4)0.0971 (14)
H10G0.1021550.4368960.9903540.127*0.0971 (14)
H10H0.1332320.5029941.0541690.127*0.0971 (14)
C11B0.102 (3)0.531 (4)0.920 (6)0.107 (5)0.0971 (14)
H11G0.1266550.5245950.8548980.128*0.0971 (14)
H11H0.1143770.5804420.9440080.128*0.0971 (14)
C12B0.020 (3)0.531 (5)0.899 (6)0.109 (11)0.0971 (14)
H12J0.0079780.5695670.8509480.163*0.0971 (14)
H12K0.0051710.4832750.8712380.163*0.0971 (14)
H12L0.0072040.5395600.9610480.163*0.0971 (14)
C13B0.245 (3)0.404 (4)1.054 (4)0.107 (5)0.0971 (14)
H13G0.2756330.4347151.0978270.128*0.0971 (14)
H13H0.2770730.3667521.0225370.128*0.0971 (14)
C14B0.187 (4)0.365 (5)1.116 (7)0.112 (5)0.0971 (14)
H14G0.1466560.3478731.0737540.135*0.0971 (14)
H14H0.1671720.3989591.1672250.135*0.0971 (14)
C15B0.227 (6)0.297 (4)1.169 (6)0.115 (10)0.0971 (14)
H15J0.1917480.2704521.2105490.173*0.0971 (14)
H15K0.2468300.2640501.1182370.173*0.0971 (14)
H15L0.2672510.3148981.2112730.173*0.0971 (14)
O6B0.2072 (19)0.383 (3)0.472 (3)0.065 (6)0.0971 (14)
H6C0.178 (4)0.368 (3)0.428 (7)0.097*0.0971 (14)
H6D0.247 (3)0.393 (4)0.443 (7)0.097*0.0971 (14)
O70.2905 (12)0.4390 (12)0.371 (2)0.071 (4)0.549 (3)
C160.3400 (8)0.4850 (8)0.3568 (10)0.086 (3)0.549 (3)
H160.3819010.4821460.3985820.104*0.549 (3)
N20.3391 (8)0.5377 (9)0.2882 (13)0.082 (3)0.549 (3)
C170.4050 (11)0.5828 (11)0.2738 (15)0.120 (5)0.549 (3)
H17A0.4467420.5510470.2583630.179*0.549 (3)
H17B0.4152040.6104330.3348030.179*0.549 (3)
H17C0.3969900.6169540.2185130.179*0.549 (3)
C180.2743 (11)0.5436 (12)0.2230 (15)0.122 (5)0.549 (3)
H18A0.2723510.5927180.1937680.183*0.549 (3)
H18B0.2299110.5348440.2621630.183*0.549 (3)
H18C0.2777330.5070790.1696770.183*0.549 (3)
O7B0.338 (2)0.417 (2)0.366 (4)0.086 (7)0.0971 (14)
C16B0.293 (3)0.467 (3)0.352 (7)0.088 (5)0.0971 (14)
H16B0.2428890.4595120.3703840.105*0.0971 (14)
N2B0.313 (3)0.532 (2)0.311 (5)0.089 (5)0.0971 (14)
C17B0.255 (4)0.588 (3)0.313 (7)0.097 (8)0.0971 (14)
H17D0.2735330.6331740.2830040.145*0.0971 (14)
H17E0.2127370.5702710.2763910.145*0.0971 (14)
H17F0.2414860.5974650.3827690.145*0.0971 (14)
C18B0.392 (3)0.546 (4)0.323 (7)0.095 (7)0.0971 (14)
H18D0.4042400.5933940.2919200.142*0.0971 (14)
H18E0.4043570.5477360.3936830.142*0.0971 (14)
H18F0.4200590.5072290.2901400.142*0.0971 (14)
O7C0.296 (2)0.441 (2)0.386 (4)0.077 (6)0.354 (3)
C16C0.2949 (12)0.4984 (12)0.3350 (17)0.087 (4)0.354 (3)
H16C0.2500260.5228090.3213760.104*0.354 (3)
N2C0.3591 (11)0.5251 (12)0.299 (2)0.080 (4)0.354 (3)
C17C0.3557 (17)0.5992 (13)0.257 (2)0.112 (6)0.354 (3)
H17G0.4043470.6135880.2333490.168*0.354 (3)
H17H0.3211430.5997780.2010640.168*0.354 (3)
H17I0.3391920.6337060.3082160.168*0.354 (3)
C18C0.4231 (14)0.4784 (15)0.303 (2)0.118 (6)0.354 (3)
H18G0.4651490.5045630.2749640.176*0.354 (3)
H18H0.4333990.4651720.3723090.176*0.354 (3)
H18I0.4139160.4339360.2641120.176*0.354 (3)
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
Dy10.0591 (2)0.0591 (2)0.0508 (3)0.0000.0000.000
Na10.0498 (10)0.0498 (10)0.058 (2)0.0000.0000.000
Mn10.0453 (4)0.0447 (4)0.0641 (5)0.0015 (2)0.0072 (3)0.0063 (3)
O10.0445 (15)0.0446 (15)0.0580 (19)0.0001 (12)0.0063 (13)0.0018 (13)
O20.0482 (16)0.0458 (17)0.075 (2)0.0004 (13)0.0103 (16)0.0038 (16)
O30.0549 (19)0.0484 (18)0.102 (3)0.0038 (15)0.022 (2)0.0030 (19)
N10.049 (2)0.0442 (18)0.057 (2)0.0025 (15)0.009 (3)0.0048 (17)
C10.051 (2)0.0420 (19)0.058 (2)0.0031 (16)0.0111 (18)0.0014 (17)
C20.055 (2)0.046 (2)0.068 (3)0.0066 (18)0.005 (2)0.006 (2)
C30.057 (2)0.048 (2)0.085 (3)0.003 (2)0.007 (2)0.001 (2)
C40.062 (3)0.045 (2)0.101 (4)0.004 (2)0.011 (3)0.001 (3)
C50.066 (3)0.051 (3)0.095 (4)0.011 (2)0.010 (3)0.000 (3)
C60.059 (3)0.050 (2)0.090 (4)0.011 (2)0.018 (3)0.004 (3)
C70.056 (2)0.044 (2)0.074 (3)0.0055 (18)0.016 (2)0.005 (2)
O40.086 (3)0.076 (3)0.060 (2)0.006 (2)0.019 (2)0.006 (2)
O50.087 (3)0.076 (3)0.069 (3)0.003 (2)0.021 (2)0.002 (2)
C80.100 (4)0.095 (4)0.067 (3)0.010 (4)0.026 (3)0.015 (3)
C90.117 (6)0.113 (6)0.083 (5)0.015 (6)0.024 (5)0.012 (5)
C100.115 (7)0.121 (7)0.084 (6)0.015 (6)0.029 (6)0.011 (6)
C110.121 (8)0.123 (8)0.093 (7)0.006 (8)0.026 (7)0.010 (8)
C120.140 (15)0.155 (16)0.107 (14)0.016 (15)0.038 (13)0.003 (14)
C130.121 (6)0.121 (6)0.087 (6)0.011 (6)0.019 (6)0.013 (6)
C140.132 (8)0.128 (8)0.095 (7)0.008 (8)0.023 (7)0.015 (7)
C150.143 (13)0.146 (13)0.088 (11)0.007 (12)0.018 (12)0.011 (12)
O60.057 (2)0.064 (2)0.063 (2)0.0103 (17)0.0029 (18)0.0144 (19)
C9C0.114 (6)0.110 (6)0.080 (5)0.017 (5)0.025 (5)0.013 (5)
C10C0.119 (7)0.122 (7)0.086 (6)0.013 (7)0.026 (6)0.011 (6)
C11C0.109 (8)0.125 (8)0.098 (7)0.019 (7)0.027 (7)0.013 (7)
C12C0.111 (14)0.145 (15)0.110 (13)0.013 (14)0.036 (13)0.011 (13)
C13C0.123 (7)0.118 (7)0.086 (6)0.013 (6)0.024 (6)0.021 (6)
C14C0.127 (7)0.121 (7)0.096 (7)0.007 (7)0.022 (6)0.014 (6)
C15C0.137 (11)0.126 (11)0.098 (10)0.021 (10)0.023 (10)0.014 (10)
C9D0.114 (6)0.113 (6)0.082 (5)0.019 (6)0.025 (5)0.009 (5)
C10D0.115 (7)0.118 (7)0.083 (7)0.012 (7)0.031 (6)0.013 (7)
C11D0.127 (9)0.131 (9)0.096 (8)0.010 (9)0.025 (9)0.004 (8)
C12D0.136 (16)0.130 (16)0.130 (15)0.016 (15)0.020 (15)0.022 (15)
C13D0.120 (6)0.123 (7)0.082 (6)0.011 (6)0.025 (6)0.011 (6)
C14D0.127 (7)0.121 (7)0.091 (7)0.014 (7)0.022 (6)0.012 (6)
C15D0.140 (13)0.131 (13)0.118 (12)0.018 (12)0.035 (11)0.004 (12)
Mn1B0.036 (3)0.038 (3)0.066 (4)0.001 (2)0.001 (2)0.002 (2)
O1B0.042 (7)0.032 (7)0.075 (8)0.003 (6)0.009 (7)0.007 (7)
O2B0.048 (6)0.035 (6)0.073 (7)0.002 (6)0.006 (6)0.001 (6)
O3B0.054 (7)0.047 (7)0.074 (7)0.004 (7)0.009 (7)0.005 (7)
N1B0.052 (7)0.040 (7)0.070 (7)0.006 (6)0.010 (7)0.000 (7)
C1B0.055 (6)0.037 (6)0.072 (6)0.004 (6)0.012 (6)0.000 (6)
C2B0.052 (5)0.040 (5)0.076 (5)0.006 (5)0.012 (5)0.001 (5)
C3B0.056 (6)0.043 (6)0.083 (6)0.004 (6)0.012 (6)0.002 (6)
C4B0.057 (7)0.045 (7)0.084 (7)0.007 (7)0.011 (7)0.002 (7)
C5B0.058 (7)0.046 (7)0.085 (7)0.012 (7)0.015 (7)0.002 (7)
C6B0.055 (7)0.043 (7)0.081 (7)0.007 (7)0.013 (7)0.001 (7)
C7B0.055 (6)0.042 (6)0.078 (6)0.007 (6)0.010 (6)0.003 (6)
O4B0.104 (10)0.094 (9)0.071 (9)0.012 (9)0.012 (9)0.019 (9)
O5B0.076 (12)0.081 (12)0.068 (12)0.001 (11)0.006 (11)0.009 (11)
C8B0.103 (8)0.097 (8)0.072 (8)0.011 (8)0.019 (8)0.015 (8)
C9B0.118 (7)0.112 (7)0.083 (7)0.012 (7)0.020 (7)0.016 (7)
C10B0.118 (7)0.115 (7)0.084 (6)0.014 (6)0.023 (6)0.015 (6)
C11B0.120 (9)0.115 (10)0.086 (9)0.013 (9)0.023 (9)0.015 (9)
C12B0.12 (2)0.12 (2)0.084 (19)0.02 (2)0.038 (19)0.017 (19)
C13B0.120 (8)0.116 (8)0.085 (8)0.011 (8)0.019 (8)0.014 (8)
C14B0.126 (9)0.122 (9)0.088 (8)0.011 (8)0.023 (8)0.015 (8)
C15B0.132 (19)0.131 (19)0.082 (18)0.005 (19)0.019 (18)0.010 (18)
O6B0.058 (11)0.070 (12)0.066 (12)0.008 (11)0.004 (11)0.012 (11)
O70.071 (6)0.071 (6)0.070 (9)0.005 (5)0.001 (5)0.021 (6)
C160.098 (7)0.089 (6)0.072 (5)0.030 (6)0.022 (5)0.010 (5)
N20.114 (7)0.071 (5)0.062 (6)0.032 (5)0.007 (6)0.012 (4)
C170.133 (11)0.110 (9)0.116 (10)0.054 (9)0.015 (9)0.025 (8)
C180.139 (11)0.117 (10)0.111 (10)0.006 (9)0.001 (9)0.014 (8)
O7B0.100 (13)0.080 (12)0.077 (12)0.026 (12)0.005 (12)0.019 (12)
C16B0.106 (9)0.083 (9)0.074 (9)0.026 (9)0.002 (9)0.013 (9)
N2B0.108 (9)0.083 (8)0.076 (9)0.026 (8)0.003 (8)0.012 (8)
C17B0.118 (15)0.094 (14)0.078 (14)0.025 (14)0.003 (14)0.007 (13)
C18B0.113 (13)0.089 (12)0.082 (12)0.027 (12)0.008 (12)0.018 (12)
O7C0.082 (10)0.075 (9)0.075 (12)0.007 (8)0.001 (9)0.018 (8)
C16C0.110 (8)0.075 (7)0.076 (7)0.016 (7)0.012 (7)0.017 (6)
N2C0.102 (8)0.076 (7)0.062 (7)0.033 (7)0.004 (7)0.004 (6)
C17C0.136 (12)0.095 (11)0.105 (11)0.018 (11)0.012 (11)0.014 (10)
C18C0.126 (11)0.116 (11)0.110 (11)0.026 (10)0.001 (10)0.017 (10)
Geometric parameters (Å, º) top
Dy1—O4B2.24 (4)C10D—C11D1.43 (2)
Dy1—O4i2.277 (5)C10D—H10E0.9900
Dy1—O4ii2.277 (5)C10D—H10F0.9900
Dy1—O4iii2.277 (5)C11D—C12D1.53 (2)
Dy1—O42.277 (5)C11D—H11E0.9900
Dy1—O12.444 (3)C11D—H11F0.9900
Dy1—O1ii2.444 (3)C12D—H12G0.9800
Dy1—O1iii2.444 (3)C12D—H12H0.9800
Dy1—O1i2.444 (3)C12D—H12I0.9800
Dy1—O1Biii2.54 (3)C13D—C14D1.52 (2)
Dy1—O1Bii2.54 (3)C13D—H13E0.9900
Dy1—O1Bi2.54 (3)C13D—H13F0.9900
Na1—O62.436 (5)C14D—C15D1.61 (2)
Na1—O6ii2.436 (5)C14D—H14E0.9900
Na1—O6i2.436 (5)C14D—H14F0.9900
Na1—O6iii2.436 (5)C15D—H15G0.9800
Na1—O1Bi2.53 (3)C15D—H15H0.9800
Na1—O1Bii2.53 (3)C15D—H15I0.9800
Na1—O1Biii2.53 (3)Mn1B—O3Bi1.85 (3)
Na1—O1B2.53 (3)Mn1B—O1B1.923 (17)
Na1—O6Bii2.64 (5)Mn1B—N1Bi1.95 (4)
Na1—O6Bi2.64 (5)Mn1B—O2B1.955 (17)
Na1—O6Biii2.64 (5)Mn1B—O6Bi2.41 (4)
Na1—O6B2.64 (5)O1B—N1B1.397 (18)
Mn1—O3ii1.840 (4)O2B—C1B1.275 (18)
Mn1—O11.914 (3)O3B—C7B1.349 (19)
Mn1—O21.939 (4)N1B—C1B1.317 (19)
Mn1—N1ii1.946 (5)C1B—C2B1.459 (17)
Mn1—O52.126 (5)C2B—C3B1.404 (19)
Mn1—O62.527 (5)C2B—C7B1.414 (19)
O1—N11.401 (5)C3B—C4B1.38 (2)
O2—C11.294 (6)C3B—H3B0.9500
O3—C71.335 (7)C4B—C5B1.37 (2)
N1—C11.319 (7)C4B—H4B0.9500
C1—C21.459 (7)C5B—C6B1.37 (2)
C2—C31.406 (8)C5B—H5B0.9500
C2—C71.415 (8)C6B—C7B1.412 (19)
C3—C41.384 (8)C6B—H6B0.9500
C3—H30.9500O4B—C8B1.29 (2)
C4—C51.373 (9)O5B—C8B1.23 (2)
C4—H40.9500C8B—C9B1.54 (2)
C5—C61.383 (9)C9B—C13B1.47 (2)
C5—H50.9500C9B—C10B1.52 (2)
C6—C71.402 (7)C9B—H9B1.0000
C6—H60.9500C10B—C11B1.44 (2)
O4—C81.274 (10)C10B—H10G0.9900
O5—C81.220 (10)C10B—H10H0.9900
C8—C9C1.526 (16)C11B—C12B1.53 (2)
C8—C91.543 (16)C11B—H11G0.9900
C8—C9D1.558 (16)C11B—H11H0.9900
C9—C131.452 (16)C12B—H12J0.9800
C9—C101.515 (15)C12B—H12K0.9800
C9—H91.0000C12B—H12L0.9800
C10—C111.470 (16)C13B—C14B1.52 (2)
C10—H10A0.9900C13B—H13G0.9900
C10—H10B0.9900C13B—H13H0.9900
C11—C121.530 (16)C14B—C15B1.61 (2)
C11—H11A0.9900C14B—H14G0.9900
C11—H11B0.9900C14B—H14H0.9900
C12—H12A0.9800C15B—H15J0.9800
C12—H12B0.9800C15B—H15K0.9800
C12—H12C0.9800C15B—H15L0.9800
C13—C141.517 (17)O6B—H6C0.84 (2)
C13—H13A0.9900O6B—H6D0.850 (18)
C13—H13B0.9900O7—C161.248 (18)
C14—C151.594 (17)C16—N21.333 (15)
C14—H14A0.9900C16—H160.9500
C14—H14B0.9900N2—C171.472 (14)
C15—H15A0.9800N2—C181.475 (16)
C15—H15B0.9800C17—H17A0.9800
C15—H15C0.9800C17—H17B0.9800
O6—H6A0.857 (17)C17—H17C0.9800
O6—H6E0.832 (18)C18—H18A0.9800
C9C—C13C1.44 (2)C18—H18B0.9800
C9C—C10C1.50 (2)C18—H18C0.9800
C9C—H9C1.0000O7B—C16B1.25 (2)
C10C—C11C1.43 (2)C16B—N2B1.36 (2)
C10C—H10C0.9900C16B—H16B0.9500
C10C—H10D0.9900N2B—C18B1.47 (2)
C11C—C12C1.53 (2)N2B—C17B1.47 (2)
C11C—H11C0.9900C17B—H17D0.9800
C11C—H11D0.9900C17B—H17E0.9800
C12C—H12D0.9800C17B—H17F0.9800
C12C—H12E0.9800C18B—H18D0.9800
C12C—H12F0.9800C18B—H18E0.9800
C13C—C14C1.53 (2)C18B—H18F0.9800
C13C—H13C0.9900O7C—C16C1.25 (2)
C13C—H13D0.9900C16C—N2C1.358 (18)
C14C—C15C1.62 (2)C16C—H16C0.9500
C14C—H14C0.9900N2C—C18C1.448 (18)
C14C—H14D0.9900N2C—C17C1.469 (17)
C15C—H15D0.9800C17C—H17G0.9800
C15C—H15E0.9800C17C—H17H0.9800
C15C—H15F0.9800C17C—H17I0.9800
C9D—C13D1.47 (2)C18C—H18G0.9800
C9D—C10D1.52 (2)C18C—H18H0.9800
C9D—H9D1.0000C18C—H18I0.9800
O4B—Dy1—O4ii111.0 (14)C10C—C9C—C8108.9 (16)
O4i—Dy1—O4ii125.9 (3)C13C—C9C—H9C90.3
O4B—Dy1—O4iii99.8 (12)C10C—C9C—H9C90.3
O4i—Dy1—O4iii78.06 (11)C8—C9C—H9C90.3
O4ii—Dy1—O4iii78.06 (11)C11C—C10C—C9C125 (2)
O4i—Dy1—O478.06 (11)C11C—C10C—H10C106.1
O4ii—Dy1—O478.06 (11)C9C—C10C—H10C106.1
O4iii—Dy1—O4125.9 (3)C11C—C10C—H10D106.1
O4i—Dy1—O178.69 (16)C9C—C10C—H10D106.1
O4ii—Dy1—O1142.57 (15)H10C—C10C—H10D106.3
O4iii—Dy1—O1138.77 (16)C10C—C11C—C12C123 (2)
O4—Dy1—O181.14 (15)C10C—C11C—H11C106.5
O4B—Dy1—O1ii116.6 (12)C12C—C11C—H11C106.5
O4i—Dy1—O1ii138.77 (16)C10C—C11C—H11D106.5
O4ii—Dy1—O1ii81.14 (15)C12C—C11C—H11D106.5
O4iii—Dy1—O1ii142.57 (15)H11C—C11C—H11D106.5
O4—Dy1—O1ii78.69 (16)C11C—C12C—H12D109.5
O1—Dy1—O1ii64.39 (9)C11C—C12C—H12E109.5
O4B—Dy1—O1iii170.3 (14)H12D—C12C—H12E109.5
O4i—Dy1—O1iii142.57 (15)C11C—C12C—H12F109.5
O4ii—Dy1—O1iii78.69 (16)H12D—C12C—H12F109.5
O4iii—Dy1—O1iii81.14 (15)H12E—C12C—H12F109.5
O4—Dy1—O1iii138.77 (16)C9C—C13C—C14C107.4 (19)
O1—Dy1—O1iii97.80 (17)C9C—C13C—H13C110.2
O1ii—Dy1—O1iii64.40 (9)C14C—C13C—H13C110.2
O4B—Dy1—O1i106.2 (15)C9C—C13C—H13D110.2
O4i—Dy1—O1i81.14 (15)C14C—C13C—H13D110.2
O4ii—Dy1—O1i138.77 (16)H13C—C13C—H13D108.5
O4iii—Dy1—O1i78.69 (16)C13C—C14C—C15C101.0 (19)
O4—Dy1—O1i142.57 (15)C13C—C14C—H14C111.6
O1—Dy1—O1i64.40 (9)C15C—C14C—H14C111.6
O1ii—Dy1—O1i97.80 (17)C13C—C14C—H14D111.6
O1iii—Dy1—O1i64.40 (9)C15C—C14C—H14D111.6
O4B—Dy1—O1Biii144.4 (13)H14C—C14C—H14D109.4
O4i—Dy1—O1Biii160.8 (7)C14C—C15C—H15D109.5
O4ii—Dy1—O1Biii72.2 (7)C14C—C15C—H15E109.5
O4iii—Dy1—O1Biii115.1 (5)H15D—C15C—H15E109.5
O4—Dy1—O1Biii102.4 (5)C14C—C15C—H15F109.5
O1—Dy1—O1Biii82.4 (7)H15D—C15C—H15F109.5
O1ii—Dy1—O1Biii27.9 (4)H15E—C15C—H15F109.5
O1iii—Dy1—O1Biii37.6 (4)C13D—C9D—C10D122 (2)
O1i—Dy1—O1Biii87.7 (7)C13D—C9D—C8111.2 (19)
O4B—Dy1—O1Bii88.6 (13)C10D—C9D—C8118.0 (18)
O4i—Dy1—O1Bii102.4 (5)C13D—C9D—H9D99.9
O4ii—Dy1—O1Bii115.1 (5)C10D—C9D—H9D99.9
O4iii—Dy1—O1Bii160.8 (7)C8—C9D—H9D99.9
O4—Dy1—O1Bii72.2 (7)C11D—C10D—C9D122 (2)
O1—Dy1—O1Bii27.9 (4)C11D—C10D—H10E106.9
O1ii—Dy1—O1Bii37.6 (4)C9D—C10D—H10E106.9
O1iii—Dy1—O1Bii87.7 (7)C11D—C10D—H10F106.9
O1i—Dy1—O1Bii82.4 (7)C9D—C10D—H10F106.9
O1Biii—Dy1—O1Bii60.4 (9)H10E—C10D—H10F106.7
O4B—Dy1—O1Bi143.3 (15)C10D—C11D—C12D122 (2)
O4i—Dy1—O1Bi115.1 (5)C10D—C11D—H11E106.8
O4ii—Dy1—O1Bi102.4 (5)C12D—C11D—H11E106.8
O4iii—Dy1—O1Bi72.2 (7)C10D—C11D—H11F106.8
O4—Dy1—O1Bi160.8 (7)C12D—C11D—H11F106.8
O1—Dy1—O1Bi87.7 (7)H11E—C11D—H11F106.6
O1ii—Dy1—O1Bi82.4 (7)C11D—C12D—H12G109.5
O1iii—Dy1—O1Bi27.9 (4)C11D—C12D—H12H109.5
O1i—Dy1—O1Bi37.6 (4)H12G—C12D—H12H109.5
O1Biii—Dy1—O1Bi60.4 (9)C11D—C12D—H12I109.5
O1Bii—Dy1—O1Bi90.7 (15)H12G—C12D—H12I109.5
O6—Na1—O6ii85.06 (8)H12H—C12D—H12I109.5
O6—Na1—O6i85.06 (8)C9D—C13D—C14D111 (2)
O6ii—Na1—O6i145.9 (3)C9D—C13D—H13E109.5
O6—Na1—O6iii145.9 (3)C14D—C13D—H13E109.5
O6ii—Na1—O6iii85.06 (8)C9D—C13D—H13F109.5
O6i—Na1—O6iii85.06 (8)C14D—C13D—H13F109.5
O6—Na1—O1Bi150.7 (6)H13E—C13D—H13F108.1
O6ii—Na1—O1Bi110.9 (4)C13D—C14D—C15D103 (2)
O6i—Na1—O1Bi93.1 (5)C13D—C14D—H14E111.2
O6iii—Na1—O1Bi62.5 (6)C15D—C14D—H14E111.2
O6—Na1—O1Bii62.5 (6)C13D—C14D—H14F111.2
O6ii—Na1—O1Bii93.1 (5)C15D—C14D—H14F111.2
O6i—Na1—O1Bii110.9 (4)H14E—C14D—H14F109.2
O6iii—Na1—O1Bii150.7 (6)C14D—C15D—H15G109.5
O1Bi—Na1—O1Bii91.4 (12)C14D—C15D—H15H109.5
O6—Na1—O1Biii110.9 (4)H15G—C15D—H15H109.5
O6ii—Na1—O1Biii62.5 (6)C14D—C15D—H15I109.5
O6i—Na1—O1Biii150.7 (6)H15G—C15D—H15I109.5
O6iii—Na1—O1Biii93.1 (5)H15H—C15D—H15I109.5
O1Bi—Na1—O1Biii60.8 (7)O3Bi—Mn1B—O1B174.4 (18)
O1Bii—Na1—O1Biii60.8 (7)O3Bi—Mn1B—O2B98.1 (10)
O1Bi—Na1—O1B60.8 (7)O1B—Mn1B—O2B81.2 (8)
O1Bii—Na1—O1B60.8 (7)N1Bi—Mn1B—O2B166 (3)
O1Biii—Na1—O1B91.4 (12)O3Bi—Mn1B—O6Bi95.9 (17)
O6—Na1—O6Bii71.0 (7)O1B—Mn1B—O6Bi78.5 (16)
O6ii—Na1—O6Bii15.2 (7)N1Bi—Mn1B—O6Bi85 (4)
O6i—Na1—O6Bii144.3 (8)O2B—Mn1B—O6Bi84.1 (14)
O6iii—Na1—O6Bii100.0 (8)O3Bi—Mn1B—Na1134.2 (11)
O1Bi—Na1—O6Bii120.7 (9)O1B—Mn1B—Na141.2 (10)
O1Bii—Na1—O6Bii81.5 (10)N1Bi—Mn1B—Na165 (3)
O1Biii—Na1—O6Bii64.8 (10)O2B—Mn1B—Na1101.6 (9)
O1B—Na1—O6Bii142.0 (10)O6Bi—Mn1B—Na146.4 (12)
O6—Na1—O6Bi100.0 (8)N1B—O1B—Mn1B112.6 (15)
O6ii—Na1—O6Bi144.3 (8)N1B—O1B—Na1112 (6)
O6i—Na1—O6Bi15.2 (7)Mn1B—O1B—Na1108.7 (13)
O6iii—Na1—O6Bi71.0 (7)N1B—O1B—Dy1117 (4)
O1Bi—Na1—O6Bi81.5 (10)Mn1B—O1B—Dy1115.3 (12)
O1Bii—Na1—O6Bi120.7 (9)Na1—O1B—Dy189.0 (6)
O1Biii—Na1—O6Bi142.0 (10)C1B—O2B—Mn1B112.2 (14)
O1B—Na1—O6Bi64.8 (10)C7B—O3B—Mn1Bii130 (2)
O6Bii—Na1—O6Bi149.9 (18)C1B—N1B—O1B113 (2)
O6—Na1—O6Biii144.3 (8)C1B—N1B—Mn1Bii131 (3)
O6ii—Na1—O6Biii71.0 (7)O1B—N1B—Mn1Bii114 (2)
O6i—Na1—O6Biii100.0 (8)O2B—C1B—N1B121.0 (18)
O6iii—Na1—O6Biii15.2 (7)O2B—C1B—C2B119.9 (18)
O1Bi—Na1—O6Biii64.8 (10)N1B—C1B—C2B118.9 (19)
O1Bii—Na1—O6Biii142.0 (10)C3B—C2B—C7B121.2 (19)
O1Biii—Na1—O6Biii81.5 (10)C3B—C2B—C1B114.3 (19)
O1B—Na1—O6Biii120.7 (9)C7B—C2B—C1B124.5 (19)
O6Bii—Na1—O6Biii86.1 (4)C4B—C3B—C2B121 (2)
O6Bi—Na1—O6Biii86.1 (4)C4B—C3B—H3B119.3
O1Bi—Na1—O6B142.0 (10)C2B—C3B—H3B119.3
O1Bii—Na1—O6B64.8 (10)C5B—C4B—C3B117 (3)
O1Biii—Na1—O6B120.7 (9)C5B—C4B—H4B121.6
O1B—Na1—O6B81.5 (10)C3B—C4B—H4B121.6
O6Bii—Na1—O6B86.1 (4)C4B—C5B—C6B124 (3)
O6Bi—Na1—O6B86.1 (4)C4B—C5B—H5B118.0
O6Biii—Na1—O6B149.9 (18)C6B—C5B—H5B118.0
O3ii—Mn1—O1168.5 (2)C5B—C6B—C7B120 (2)
O3ii—Mn1—O297.45 (17)C5B—C6B—H6B119.8
O1—Mn1—O281.70 (15)C7B—C6B—H6B119.8
O3ii—Mn1—N1ii90.57 (19)O3B—C7B—C6B120 (2)
O1—Mn1—N1ii88.75 (16)O3B—C7B—C2B124 (2)
O2—Mn1—N1ii168.3 (3)C6B—C7B—C2B116.1 (19)
O3ii—Mn1—O594.6 (2)C8B—O4B—Dy1133 (3)
O1—Mn1—O596.9 (2)O5B—C8B—O4B124 (3)
O2—Mn1—O594.0 (2)O5B—C8B—C9B128 (3)
N1ii—Mn1—O593.8 (4)O4B—C8B—C9B108 (2)
O3ii—Mn1—O689.8 (2)C13B—C9B—C10B121 (3)
O1—Mn1—O678.68 (15)C13B—C9B—C8B113 (3)
O2—Mn1—O686.28 (16)C10B—C9B—C8B106 (3)
N1ii—Mn1—O685.3 (4)C13B—C9B—H9B105.3
O5—Mn1—O6175.52 (19)C10B—C9B—H9B105.3
O3ii—Mn1—Na1124.15 (18)C8B—C9B—H9B105.3
O1—Mn1—Na145.80 (12)C11B—C10B—C9B124 (3)
O2—Mn1—Na1103.48 (11)C11B—C10B—H10G106.3
N1ii—Mn1—Na164.9 (3)C9B—C10B—H10G106.3
O5—Mn1—Na1133.91 (17)C11B—C10B—H10H106.2
O6—Mn1—Na141.91 (11)C9B—C10B—H10H106.2
N1—O1—Mn1112.7 (3)H10G—C10B—H10H106.4
N1—O1—Dy1121.3 (4)C10B—C11B—C12B122 (3)
Mn1—O1—Dy1119.88 (15)C10B—C11B—H11G106.8
N1—O1—Na1104.4 (4)C12B—C11B—H11G106.8
Mn1—O1—Na1103.43 (15)C10B—C11B—H11H106.8
Dy1—O1—Na187.70 (12)C12B—C11B—H11H106.8
C1—O2—Mn1112.1 (3)H11G—C11B—H11H106.6
C7—O3—Mn1i129.8 (3)C11B—C12B—H12J109.5
C1—N1—O1112.6 (5)C11B—C12B—H12K109.5
C1—N1—Mn1i130.9 (4)H12J—C12B—H12K109.5
O1—N1—Mn1i116.1 (3)C11B—C12B—H12L109.5
O2—C1—N1120.4 (4)H12J—C12B—H12L109.5
O2—C1—C2120.0 (4)H12K—C12B—H12L109.5
N1—C1—C2119.6 (5)C9B—C13B—C14B112 (3)
C3—C2—C7118.8 (5)C9B—C13B—H13G109.2
C3—C2—C1118.0 (5)C14B—C13B—H13G109.2
C7—C2—C1123.1 (5)C9B—C13B—H13H109.2
C4—C3—C2121.4 (6)C14B—C13B—H13H109.2
C4—C3—H3119.3H13G—C13B—H13H107.9
C2—C3—H3119.3C13B—C14B—C15B107 (3)
C5—C4—C3119.3 (6)C13B—C14B—H14G110.4
C5—C4—H4120.3C15B—C14B—H14G110.4
C3—C4—H4120.3C13B—C14B—H14H110.4
C4—C5—C6120.9 (6)C15B—C14B—H14H110.4
C4—C5—H5119.5H14G—C14B—H14H108.6
C6—C5—H5119.5C14B—C15B—H15J109.5
C5—C6—C7121.0 (6)C14B—C15B—H15K109.5
C5—C6—H6119.5H15J—C15B—H15K109.5
C7—C6—H6119.5C14B—C15B—H15L109.5
O3—C7—C6117.9 (5)H15J—C15B—H15L109.5
O3—C7—C2123.5 (5)H15K—C15B—H15L109.5
C6—C7—C2118.5 (5)Mn1Bii—O6B—Na192.1 (13)
C8—O4—Dy1144.7 (5)Mn1Bii—O6B—H6C137 (7)
C8—O5—Mn1124.0 (5)Na1—O6B—H6C95 (6)
O5—C8—O4127.1 (7)Mn1Bii—O6B—H6D115 (7)
O5—C8—C9C110.5 (16)Na1—O6B—H6D95 (6)
O4—C8—C9C122.3 (16)H6C—O6B—H6D107 (3)
O5—C8—C9124.4 (14)O7—C16—N2125.5 (16)
O4—C8—C9108.3 (14)O7—C16—H16117.2
O5—C8—C9D117.9 (15)N2—C16—H16117.2
O4—C8—C9D113.9 (16)C16—N2—C17119.0 (13)
C13—C9—C10122.4 (16)C16—N2—C18118.2 (12)
C13—C9—C8115.7 (17)C17—N2—C18122.5 (13)
C10—C9—C8106.3 (18)N2—C17—H17A109.5
C13—C9—H9103.3N2—C17—H17B109.5
C10—C9—H9103.3H17A—C17—H17B109.5
C8—C9—H9103.3N2—C17—H17C109.5
C11—C10—C9116.6 (15)H17A—C17—H17C109.5
C11—C10—H10A108.1H17B—C17—H17C109.5
C9—C10—H10A108.1N2—C18—H18A109.5
C11—C10—H10B108.1N2—C18—H18B109.5
C9—C10—H10B108.1H18A—C18—H18B109.5
H10A—C10—H10B107.3N2—C18—H18C109.5
C10—C11—C12118.1 (17)H18A—C18—H18C109.5
C10—C11—H11A107.8H18B—C18—H18C109.5
C12—C11—H11A107.8O7B—C16B—N2B120 (3)
C10—C11—H11B107.8O7B—C16B—H16B119.8
C12—C11—H11B107.8N2B—C16B—H16B119.8
H11A—C11—H11B107.1C16B—N2B—C18B113 (3)
C11—C12—H12A109.5C16B—N2B—C17B113 (3)
C11—C12—H12B109.5C18B—N2B—C17B125 (3)
H12A—C12—H12B109.5N2B—C17B—H17D109.5
C11—C12—H12C109.5N2B—C17B—H17E109.5
H12A—C12—H12C109.5H17D—C17B—H17E109.5
H12B—C12—H12C109.5N2B—C17B—H17F109.5
C9—C13—C14118.5 (17)H17D—C17B—H17F109.5
C9—C13—H13A107.7H17E—C17B—H17F109.5
C14—C13—H13A107.7N2B—C18B—H18D109.5
C9—C13—H13B107.7N2B—C18B—H18E109.5
C14—C13—H13B107.7H18D—C18B—H18E109.5
H13A—C13—H13B107.1N2B—C18B—H18F109.5
C13—C14—C15110.9 (15)H18D—C18B—H18F109.5
C13—C14—H14A109.5H18E—C18B—H18F109.5
C15—C14—H14A109.5O7C—C16C—N2C119 (2)
C13—C14—H14B109.5O7C—C16C—H16C120.5
C15—C14—H14B109.5N2C—C16C—H16C120.5
H14A—C14—H14B108.1C16C—N2C—C18C118.3 (16)
C14—C15—H15A109.5C16C—N2C—C17C115.5 (18)
C14—C15—H15B109.5C18C—N2C—C17C126.2 (19)
H15A—C15—H15B109.5N2C—C17C—H17G109.5
C14—C15—H15C109.5N2C—C17C—H17H109.5
H15A—C15—H15C109.5H17G—C17C—H17H109.5
H15B—C15—H15C109.5N2C—C17C—H17I109.5
Na1—O6—Mn194.24 (17)H17G—C17C—H17I109.5
Na1—O6—H6A109 (4)H17H—C17C—H17I109.5
Mn1—O6—H6A124 (6)N2C—C18C—H18G109.5
Na1—O6—H6E110 (4)N2C—C18C—H18H109.5
Mn1—O6—H6E112 (5)H18G—C18C—H18H109.5
H6A—O6—H6E107 (3)N2C—C18C—H18I109.5
C13C—C9C—C10C135.8 (18)H18G—C18C—H18I109.5
C13C—C9C—C8115.4 (18)H18H—C18C—H18I109.5
Mn1—O1—N1—C16.0 (10)O5—C8—C9D—C13D153.5 (19)
Dy1—O1—N1—C1146.3 (6)O4—C8—C9D—C13D37 (3)
Na1—O1—N1—C1117.5 (7)O5—C8—C9D—C10D58 (3)
Mn1—O1—N1—Mn1i167.2 (5)O4—C8—C9D—C10D111 (2)
Dy1—O1—N1—Mn1i40.4 (9)C13D—C9D—C10D—C11D70 (4)
Na1—O1—N1—Mn1i55.7 (8)C8—C9D—C10D—C11D75 (4)
Mn1—O2—C1—N13.1 (9)C9D—C10D—C11D—C12D170 (3)
Mn1—O2—C1—C2175.1 (4)C10D—C9D—C13D—C14D141 (3)
O1—N1—C1—O21.9 (12)C8—C9D—C13D—C14D72 (3)
Mn1i—N1—C1—O2170.1 (7)C9D—C13D—C14D—C15D89 (3)
O1—N1—C1—C2179.9 (6)Mn1B—O1B—N1B—C1B5 (12)
Mn1i—N1—C1—C28.2 (14)Na1—O1B—N1B—C1B117 (9)
O2—C1—C2—C312.2 (9)Dy1—O1B—N1B—C1B143 (7)
N1—C1—C2—C3169.5 (8)Mn1B—O1B—N1B—Mn1Bii173 (5)
O2—C1—C2—C7167.2 (6)Na1—O1B—N1B—Mn1Bii51 (9)
N1—C1—C2—C711.0 (11)Dy1—O1B—N1B—Mn1Bii50 (10)
C7—C2—C3—C42.2 (11)Mn1B—O2B—C1B—N1B2 (9)
C1—C2—C3—C4177.3 (7)Mn1B—O2B—C1B—C2B178 (2)
C2—C3—C4—C51.0 (12)O1B—N1B—C1B—O2B2 (14)
C3—C4—C5—C60.1 (13)Mn1Bii—N1B—C1B—O2B167 (8)
C4—C5—C6—C70.4 (12)O1B—N1B—C1B—C2B173 (6)
Mn1i—O3—C7—C6166.9 (5)Mn1Bii—N1B—C1B—C2B8 (15)
Mn1i—O3—C7—C217.1 (10)O2B—C1B—C2B—C3B3 (4)
C5—C6—C7—O3177.8 (7)N1B—C1B—C2B—C3B179 (8)
C5—C6—C7—C21.5 (11)O2B—C1B—C2B—C7B175 (5)
C3—C2—C7—O3178.4 (6)N1B—C1B—C2B—C7B0 (8)
C1—C2—C7—O31.0 (10)C7B—C2B—C3B—C4B1 (3)
C3—C2—C7—C62.4 (10)C1B—C2B—C3B—C4B180 (3)
C1—C2—C7—C6177.0 (6)C2B—C3B—C4B—C5B1 (5)
Mn1—O5—C8—O422.3 (14)C3B—C4B—C5B—C6B0 (7)
Mn1—O5—C8—C9C158.7 (11)C4B—C5B—C6B—C7B3 (7)
Mn1—O5—C8—C9161.6 (12)Mn1Bii—O3B—C7B—C6B180 (3)
Mn1—O5—C8—C9D145.4 (13)Mn1Bii—O3B—C7B—C2B4 (7)
Dy1—O4—C8—O512.0 (18)C5B—C6B—C7B—O3B172 (5)
Dy1—O4—C8—C9C166.8 (12)C5B—C6B—C7B—C2B5 (6)
Dy1—O4—C8—C9164.6 (11)C3B—C2B—C7B—O3B172 (5)
Dy1—O4—C8—C9D179.9 (12)C1B—C2B—C7B—O3B6 (5)
O5—C8—C9—C1384 (2)C3B—C2B—C7B—C6B4 (4)
O4—C8—C9—C1392 (2)C1B—C2B—C7B—C6B178 (3)
O5—C8—C9—C1055 (2)Dy1—O4B—C8B—O5B22 (5)
O4—C8—C9—C10128.2 (18)Dy1—O4B—C8B—C9B158 (4)
C13—C9—C10—C11168 (3)O5B—C8B—C9B—C13B178 (4)
C8—C9—C10—C1156 (4)O4B—C8B—C9B—C13B3 (4)
C9—C10—C11—C12174 (3)O5B—C8B—C9B—C10B43 (5)
C10—C9—C13—C1482 (3)O4B—C8B—C9B—C10B137 (4)
C8—C9—C13—C14146 (2)C13B—C9B—C10B—C11B174 (7)
C9—C13—C14—C1590 (3)C8B—C9B—C10B—C11B57 (8)
O5—C8—C9C—C13C58 (3)C9B—C10B—C11B—C12B148 (7)
O4—C8—C9C—C13C121 (2)C10B—C9B—C13B—C14B25 (8)
O5—C8—C9C—C10C121 (2)C8B—C9B—C13B—C14B102 (6)
O4—C8—C9C—C10C60 (3)C9B—C13B—C14B—C15B160 (6)
C13C—C9C—C10C—C11C148 (4)O7—C16—N2—C17173 (3)
C8—C9C—C10C—C11C31 (4)O7—C16—N2—C180 (4)
C9C—C10C—C11C—C12C131 (4)O7B—C16B—N2B—C18B22 (11)
C10C—C9C—C13C—C14C108 (4)O7B—C16B—N2B—C17B172 (9)
C8—C9C—C13C—C14C74 (3)O7C—C16C—N2C—C18C13 (5)
C9C—C13C—C14C—C15C20 (3)O7C—C16C—N2C—C17C169 (4)
Symmetry codes: (i) y, x+1/2, z; (ii) y+1/2, x, z; (iii) x+1/2, y+1/2, z.
Hydrogen-bond geometry (Å, º) top
D—H···AD—HH···AD···AD—H···A
O6—H6A···O70.86 (2)2.02 (2)2.860 (15)165 (5)
O6—H6E···O7ii0.83 (2)1.99 (2)2.809 (19)167 (5)
O6B—H6C···O7Bii0.84 (2)2.00 (2)2.80 (3)159 (10)
O6B—H6D···O7B0.85 (2)2.01 (2)2.859 (19)177 (10)
Symmetry code: (ii) y+1/2, x, z.
Average bond length (Å) and bond-valence-sum (BVS) values (v.u.) used to support assigned oxidation states of the dysprosium and manganese ions of 1 top
Avg. Bond lengthBVS valueAssigned oxidation state
Dy12.3613.143+
Mn11.9533.023+
Continuous Shape Measure (CShM) values for the geometry about the eight-coordinate central DyIII and Na+ ions of 1 top
ShapeDyIIINa+
Octagon (D8h)32.05632.142
Heptagonal pyramid (C7v)23.66626.075
Hexagonal bipyramid (D6h)16.87013.023
Cube (Oh)9.2535.054
Square antiprism (D4d)0.7473.803
Triangular dodecahedron (D2d)2.7304.048
Johnson gyrobifastigium (J26; D2s)17.55316.887
Johnson elongated triangular bipyramid (J14; D3h)30.39528.728
Johnson biaugmented trigonal prism (J50; C2v)3.0365.420
Biaugmented trigonal prism (C2v)1.9913.667
Johnson snub diphenoid (J84; D2d)5.9718.256
Triakis tetrahedron (Td)10.1185.959
Elongated trigonal bipyramid (D3h)25.70825.581
Continuous Shape Measure (CShM) values for the geometry about the five-coordinate ring MnIII ion of 1 top
ShapePentagon (D5h)Vacant octahedron (C4v)Trigonal bipyramid (D3h)Spherical square pyramid (C4v)Johnson trigonal bipyramid (J12; D3h)
Mn130.5150.8325.4220.7397.504
Structural Feature Comparison of 1 and other DyNa(carboxylate)4[12-MCMnIIIN(shi)-4] compounds (Å, °) top
CompoundMC cavity radiusaAvg. cross cavity MnIII—MnIII distanceaAvg. adjacent MnIII—MnIII DistanceaAvg. cross-cavity Ooxime—Ooxime distanceaDyIII–oxime oxygen mean plane distanceb
DyNa(2-PV)4[12-MC-4], 10.546.514.603.681.6069 (37)
DyNa(OAc)4[12-MC-4]0.556.524.613.711.5918 (7)
DyNa(TMA)4[12-MC-4]0.566.514.603.731.5790 (19)
DyNa(ben)4[12-MC-4]0.546.514.603.691.5811 (18)
DyNa(2-OHben)4[12-MC-4]0.546.474.573.681.5094 (46)
DyNa(3-OHben)4[12-MC-4]0.566.534.623.721.5463 (25)
DyNa(4-OHben)4[12-MC-4]0.546.494.593.691.5925 (66)
DyNa(2-Fben)4[12-MC-4]0.556.514.603.711.5424 (52)
DyNa(3-Fben)4[12-MC-4]0.566.514.603.721.5567 (34)
DyNa(4-Fben)4[12-MC-4]0.546.524.613.681.5589 (45)
DyNa(2-Clben)4[12-MC-4]0.536.504.603.671.5883 (79)
DyNa(4-Clben)4[12-MC-4]0.556.544.623.711.5593 (13)
DyNa(3-Brben)4[12-MC-4]0.566.514.603.711.5685 (13)
DyNa(2-Iben)4[12-MC-4]0.546.504.593.681.5764 (117)
Notes: (a) Measured with Mercury (Macrae et al., 2020); (b) measured with SHELXL (Sheldrick, 2015b).
 

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