Supporting information
Crystallographic Information File (CIF) https://doi.org/10.1107/S0108270104032585/gd1354sup1.cif | |
Structure factor file (CIF format) https://doi.org/10.1107/S0108270104032585/gd1354Isup2.hkl |
CCDC reference: 241324
4-Methylbenzoic acid (1.5 mmol, 204 mg) was dissolved in ethanol (20 ml) and the pH of the solution was adjusted to be in the range 5–6 using 2M NaOH. Ethanol solutions of 1,10-phenanthroline (0.5 mmol, 90 mg) and DyCl3·6H2O (0.5 mmol, 189 mg) were successively added. The mixture was heated under reflux with stirring for 2 h and then kept at ambient temperature for 6 d. Crystals of (I) were obtained and used for IR and X-ray diffraction analyses. Analysis calculated: C 57.8, N 3.7, H 3.9%; found: C 58.0, N 3.6, H 3.9%.
All H atoms were initially located in a difference Fourier map. The methyl H atoms were then constrained to an ideal geometry, with C—H distances of 0.97 Å 0.96 Å in CIF? and Uiso(H) = 1.5Ueq(C), but each group was allowed to rotate freely about its C—C bond. All other H atoms were placed in geometrically idealized positions and constrained to ride on their parent atoms, with C—H distances in the range 0.93–?? Å and Uiso(H) = 1.2Ueq(C).
Data collection: SMART (Bruker, 1997); cell refinement: SMART; data reduction: SAINT (Bruker, 1997); program(s) used to solve structure: SHELXS97 (Sheldrick, 1990); program(s) used to refine structure: SHELXL97 (Sheldrick, 1997); molecular graphics: SHELXTL (Bruker, 1998); software used to prepare material for publication: SHELXTL.
[Dy2(C8H7O2)6(C12H8N2)2] | Z = 2 |
Mr = 1496.22 | F(000) = 1492 |
Triclinic, P1 | Dx = 1.559 Mg m−3 |
a = 12.760 (8) Å | Mo Kα radiation, λ = 0.71073 Å |
b = 13.346 (9) Å | Cell parameters from 987 reflections |
c = 19.758 (13) Å | θ = 3.1–23.7° |
α = 91.619 (12)° | µ = 2.39 mm−1 |
β = 97.925 (11)° | T = 293 K |
γ = 106.44 (1)° | Prism, yellow |
V = 3188 (4) Å3 | 0.22 × 0.18 × 0.12 mm |
Bruker SMART CCD area-detector diffractometer | 11165 independent reflections |
Radiation source: fine-focus sealed tube | 7695 reflections with I > 2σ(I) |
Graphite monochromator | Rint = 0.033 |
ϕ and ω scans | θmax = 25.0°, θmin = 1.0° |
Absorption correction: multi-scan (SADABS; Sheldrick, 1996) | h = −15→14 |
Tmin = 0.541, Tmax = 0.750 | k = −13→15 |
16586 measured reflections | l = −20→23 |
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) = 0.121 | H-atom parameters constrained |
S = 1.11 | w = 1/[σ2(Fo2) + (0.0549P)2 + 0.0276P] where P = (Fo2 + 2Fc2)/3 |
11165 reflections | (Δ/σ)max = 0.003 |
811 parameters | Δρmax = 0.86 e Å−3 |
18 restraints | Δρmin = −0.96 e Å−3 |
[Dy2(C8H7O2)6(C12H8N2)2] | γ = 106.44 (1)° |
Mr = 1496.22 | V = 3188 (4) Å3 |
Triclinic, P1 | Z = 2 |
a = 12.760 (8) Å | Mo Kα radiation |
b = 13.346 (9) Å | µ = 2.39 mm−1 |
c = 19.758 (13) Å | T = 293 K |
α = 91.619 (12)° | 0.22 × 0.18 × 0.12 mm |
β = 97.925 (11)° |
Bruker SMART CCD area-detector diffractometer | 11165 independent reflections |
Absorption correction: multi-scan (SADABS; Sheldrick, 1996) | 7695 reflections with I > 2σ(I) |
Tmin = 0.541, Tmax = 0.750 | Rint = 0.033 |
16586 measured reflections |
R[F2 > 2σ(F2)] = 0.043 | 18 restraints |
wR(F2) = 0.121 | H-atom parameters constrained |
S = 1.11 | Δρmax = 0.86 e Å−3 |
11165 reflections | Δρmin = −0.96 e Å−3 |
811 parameters |
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 | ||
Dy1 | 0.71642 (3) | 0.54410 (3) | 0.501141 (17) | 0.03106 (12) | |
Dy2 | 0.38941 (3) | 0.54073 (3) | 0.057315 (16) | 0.02815 (11) | |
O1 | 0.8536 (5) | 0.6978 (4) | 0.4823 (3) | 0.0578 (18) | |
O2 | 0.8443 (4) | 0.6669 (4) | 0.5892 (3) | 0.0496 (15) | |
O3 | 0.8172 (5) | 0.4305 (5) | 0.5402 (3) | 0.0532 (16) | |
O4 | 0.6976 (4) | 0.4510 (4) | 0.6049 (3) | 0.0411 (13) | |
O5 | 0.5737 (4) | 0.4021 (4) | 0.4615 (3) | 0.0471 (15) | |
O6 | 0.3962 (5) | 0.3712 (4) | 0.4604 (3) | 0.0486 (15) | |
O7 | 0.3537 (4) | 0.3629 (4) | 0.0258 (2) | 0.0312 (12) | |
O8 | 0.4491 (4) | 0.3264 (4) | −0.0537 (3) | 0.0437 (14) | |
O9 | 0.3156 (4) | 0.6863 (4) | 0.0381 (3) | 0.0401 (13) | |
O10 | 0.3911 (4) | 0.6790 (4) | 0.1436 (2) | 0.0383 (13) | |
O11 | 0.5110 (4) | 0.4881 (4) | 0.1375 (2) | 0.0359 (13) | |
O12 | 0.6053 (4) | 0.4573 (4) | 0.0573 (2) | 0.0369 (13) | |
N1 | 0.6412 (5) | 0.5955 (5) | 0.3863 (3) | 0.0323 (15) | |
N2 | 0.8044 (5) | 0.4993 (5) | 0.4006 (3) | 0.0351 (15) | |
N3 | 0.1812 (5) | 0.4600 (5) | 0.0148 (3) | 0.0320 (14) | |
N4 | 0.2708 (5) | 0.4507 (5) | 0.1463 (3) | 0.0359 (15) | |
C1 | 0.5529 (7) | 0.6309 (6) | 0.3770 (4) | 0.044 (2) | |
H1A | 0.5112 | 0.6279 | 0.4124 | 0.053* | |
C2 | 0.5209 (7) | 0.6721 (7) | 0.3164 (4) | 0.049 (2) | |
H2A | 0.4578 | 0.6946 | 0.3111 | 0.058* | |
C3 | 0.5824 (7) | 0.6790 (6) | 0.2653 (4) | 0.048 (2) | |
H3A | 0.5628 | 0.7083 | 0.2251 | 0.058* | |
C4 | 0.6766 (6) | 0.6420 (6) | 0.2727 (4) | 0.040 (2) | |
C5 | 0.7461 (8) | 0.6430 (7) | 0.2212 (4) | 0.057 (3) | |
H5A | 0.7338 | 0.6759 | 0.1813 | 0.069* | |
C6 | 0.8274 (7) | 0.5984 (8) | 0.2289 (4) | 0.060 (3) | |
H6A | 0.8709 | 0.6014 | 0.1945 | 0.072* | |
C7 | 0.8498 (6) | 0.5457 (7) | 0.2890 (4) | 0.046 (2) | |
C8 | 0.9287 (7) | 0.4914 (8) | 0.2959 (5) | 0.061 (3) | |
H8A | 0.9705 | 0.4886 | 0.2612 | 0.074* | |
C9 | 0.9431 (7) | 0.4432 (8) | 0.3536 (5) | 0.060 (3) | |
H9A | 0.9952 | 0.4062 | 0.3592 | 0.071* | |
C10 | 0.8803 (7) | 0.4485 (7) | 0.4048 (4) | 0.048 (2) | |
H10A | 0.8921 | 0.4144 | 0.4443 | 0.058* | |
C11 | 0.7873 (6) | 0.5477 (6) | 0.3426 (3) | 0.0324 (18) | |
C12 | 0.7013 (6) | 0.5969 (6) | 0.3348 (4) | 0.0320 (18) | |
C13 | 0.8858 (6) | 0.7240 (6) | 0.5460 (4) | 0.041 (2) | |
C14 | 0.9718 (7) | 0.8250 (6) | 0.5659 (4) | 0.045 (2) | |
C15 | 1.0428 (8) | 0.8727 (8) | 0.5205 (5) | 0.070 (3) | |
H15A | 1.0343 | 0.8413 | 0.4767 | 0.084* | |
C16 | 1.1247 (9) | 0.9651 (9) | 0.5394 (7) | 0.092 (4) | |
H16A | 1.1721 | 0.9955 | 0.5090 | 0.110* | |
C17 | 1.1356 (10) | 1.0120 (8) | 0.6045 (8) | 0.095 (5) | |
C18 | 1.0641 (10) | 0.9649 (8) | 0.6495 (6) | 0.085 (4) | |
H18A | 1.0712 | 0.9968 | 0.6930 | 0.102* | |
C19 | 0.9842 (8) | 0.8726 (7) | 0.6304 (5) | 0.062 (3) | |
H19A | 0.9377 | 0.8417 | 0.6611 | 0.074* | |
C20 | 1.2277 (11) | 1.1152 (10) | 0.6212 (7) | 0.130 (5) | |
H20A | 1.2290 | 1.1412 | 0.6672 | 0.194* | |
H20B | 1.2144 | 1.1656 | 0.5899 | 0.194* | |
H20C | 1.2975 | 1.1037 | 0.6170 | 0.194* | |
C21 | 0.7734 (7) | 0.4141 (7) | 0.5937 (4) | 0.041 (2) | |
C22 | 0.8140 (7) | 0.3464 (7) | 0.6433 (4) | 0.044 (2) | |
C23 | 0.7888 (7) | 0.3412 (7) | 0.7093 (4) | 0.046 (2) | |
H23A | 0.7441 | 0.3798 | 0.7229 | 0.055* | |
C24 | 0.8285 (8) | 0.2802 (8) | 0.7551 (4) | 0.057 (3) | |
H24A | 0.8107 | 0.2793 | 0.7992 | 0.069* | |
C25 | 0.8927 (9) | 0.2214 (8) | 0.7379 (5) | 0.066 (3) | |
C26 | 0.9180 (9) | 0.2251 (8) | 0.6724 (5) | 0.075 (3) | |
H26A | 0.9611 | 0.1845 | 0.6591 | 0.090* | |
C27 | 0.8806 (8) | 0.2883 (8) | 0.6255 (5) | 0.066 (3) | |
H27A | 0.9008 | 0.2910 | 0.5820 | 0.080* | |
C28 | 0.9302 (11) | 0.1478 (10) | 0.7872 (6) | 0.106 (4) | |
H28A | 0.9049 | 0.1547 | 0.8302 | 0.159* | |
H28B | 1.0094 | 0.1656 | 0.7944 | 0.159* | |
H28C | 0.8997 | 0.0769 | 0.7681 | 0.159* | |
C29 | 0.4787 (6) | 0.3427 (6) | 0.4532 (3) | 0.0300 (17) | |
C30 | 0.4641 (6) | 0.2290 (5) | 0.4342 (3) | 0.0297 (17) | |
C31 | 0.5535 (7) | 0.1916 (6) | 0.4397 (4) | 0.048 (2) | |
H31A | 0.6243 | 0.2361 | 0.4542 | 0.057* | |
C32 | 0.5373 (10) | 0.0855 (8) | 0.4234 (5) | 0.070 (3) | |
H32A | 0.5983 | 0.0598 | 0.4280 | 0.084* | |
C33 | 0.4353 (12) | 0.0181 (7) | 0.4008 (5) | 0.074 (3) | |
C34 | 0.3485 (10) | 0.0575 (8) | 0.3947 (6) | 0.084 (4) | |
H34A | 0.2781 | 0.0132 | 0.3791 | 0.100* | |
C35 | 0.3613 (7) | 0.1623 (7) | 0.4111 (5) | 0.062 (3) | |
H35A | 0.2999 | 0.1874 | 0.4063 | 0.074* | |
C36 | 0.4197 (12) | −0.0962 (9) | 0.3833 (6) | 0.103 (4) | |
H36A | 0.4900 | −0.1101 | 0.3912 | 0.155* | |
H36B | 0.3879 | −0.1136 | 0.3361 | 0.155* | |
H36C | 0.3713 | −0.1377 | 0.4117 | 0.155* | |
C37 | 0.1376 (6) | 0.4589 (6) | −0.0504 (4) | 0.040 (2) | |
H37A | 0.1830 | 0.4933 | −0.0807 | 0.048* | |
C38 | 0.0274 (7) | 0.4088 (7) | −0.0754 (4) | 0.051 (2) | |
H38A | 0.0007 | 0.4085 | −0.1216 | 0.062* | |
C39 | −0.0401 (6) | 0.3609 (7) | −0.0322 (4) | 0.047 (2) | |
H39A | −0.1144 | 0.3282 | −0.0485 | 0.057* | |
C40 | 0.0010 (6) | 0.3598 (6) | 0.0374 (4) | 0.040 (2) | |
C41 | −0.0654 (7) | 0.3165 (7) | 0.0870 (5) | 0.057 (3) | |
H41A | −0.1410 | 0.2865 | 0.0737 | 0.068* | |
C42 | −0.0220 (7) | 0.3178 (7) | 0.1523 (5) | 0.053 (2) | |
H42A | −0.0687 | 0.2909 | 0.1838 | 0.064* | |
C43 | 0.0937 (7) | 0.3589 (6) | 0.1757 (4) | 0.044 (2) | |
C44 | 0.1441 (8) | 0.3569 (7) | 0.2425 (4) | 0.055 (2) | |
H44A | 0.1009 | 0.3272 | 0.2751 | 0.066* | |
C45 | 0.2534 (8) | 0.3966 (7) | 0.2609 (4) | 0.052 (2) | |
H45A | 0.2877 | 0.3931 | 0.3051 | 0.062* | |
C46 | 0.3124 (7) | 0.4431 (7) | 0.2110 (4) | 0.047 (2) | |
H46A | 0.3883 | 0.4718 | 0.2236 | 0.056* | |
C47 | 0.1600 (6) | 0.4074 (6) | 0.1290 (4) | 0.0336 (18) | |
C48 | 0.1148 (6) | 0.4097 (6) | 0.0584 (4) | 0.0313 (17) | |
C49 | 0.3662 (6) | 0.3070 (6) | −0.0229 (4) | 0.0294 (17) | |
C50 | 0.2742 (6) | 0.2086 (6) | −0.0483 (4) | 0.0324 (17) | |
C51 | 0.2854 (7) | 0.1372 (7) | −0.0961 (4) | 0.050 (2) | |
H51A | 0.3523 | 0.1469 | −0.1125 | 0.060* | |
C52 | 0.1949 (9) | 0.0488 (7) | −0.1202 (5) | 0.067 (3) | |
H52A | 0.2035 | −0.0001 | −0.1519 | 0.081* | |
C53 | 0.0965 (8) | 0.0337 (7) | −0.0983 (5) | 0.052 (2) | |
C54 | 0.0861 (7) | 0.1048 (6) | −0.0507 (5) | 0.052 (2) | |
H54A | 0.0185 | 0.0955 | −0.0354 | 0.063* | |
C55 | 0.1739 (6) | 0.1904 (6) | −0.0248 (4) | 0.0375 (19) | |
H55A | 0.1653 | 0.2364 | 0.0088 | 0.045* | |
C56 | 0.0010 (8) | −0.0601 (7) | −0.1268 (6) | 0.082 (4) | |
H56A | 0.0242 | −0.1006 | −0.1596 | 0.124* | |
H56B | −0.0591 | −0.0370 | −0.1487 | 0.124* | |
H56C | −0.0227 | −0.1026 | −0.0902 | 0.124* | |
C57 | 0.3539 (6) | 0.7291 (6) | 0.0987 (4) | 0.0341 (18) | |
C58 | 0.3514 (6) | 0.8395 (6) | 0.1140 (4) | 0.0350 (18) | |
C59 | 0.3059 (8) | 0.8935 (7) | 0.0658 (4) | 0.056 (2) | |
H59A | 0.2780 | 0.8622 | 0.0219 | 0.067* | |
C60 | 0.3010 (8) | 0.9938 (7) | 0.0813 (5) | 0.064 (3) | |
H60A | 0.2690 | 1.0284 | 0.0479 | 0.076* | |
C61 | 0.3429 (7) | 1.0426 (7) | 0.1455 (5) | 0.057 (3) | |
C62 | 0.3866 (8) | 0.9884 (7) | 0.1935 (5) | 0.059 (3) | |
H62A | 0.4134 | 1.0194 | 0.2376 | 0.071* | |
C63 | 0.3921 (7) | 0.8892 (7) | 0.1784 (4) | 0.052 (2) | |
H63A | 0.4238 | 0.8550 | 0.2121 | 0.062* | |
C64 | 0.3328 (10) | 1.1510 (7) | 0.1634 (6) | 0.084 (4) | |
H64A | 0.3651 | 1.1726 | 0.2102 | 0.127* | |
H64B | 0.2562 | 1.1486 | 0.1573 | 0.127* | |
H64C | 0.3708 | 1.2000 | 0.1340 | 0.127* | |
C65 | 0.5720 (6) | 0.4423 (6) | 0.1155 (4) | 0.0323 (18) | |
C66 | 0.6086 (5) | 0.3625 (6) | 0.1573 (4) | 0.0323 (18) | |
C67 | 0.6465 (7) | 0.2871 (7) | 0.1281 (5) | 0.054 (2) | |
H67A | 0.6516 | 0.2854 | 0.0816 | 0.065* | |
C68 | 0.6769 (8) | 0.2140 (8) | 0.1684 (6) | 0.073 (3) | |
H68A | 0.7023 | 0.1632 | 0.1485 | 0.088* | |
C69 | 0.6705 (8) | 0.2147 (9) | 0.2370 (6) | 0.073 (3) | |
C70 | 0.6307 (7) | 0.2876 (8) | 0.2649 (5) | 0.059 (3) | |
H70A | 0.6246 | 0.2877 | 0.3113 | 0.071* | |
C71 | 0.5991 (6) | 0.3611 (7) | 0.2268 (4) | 0.043 (2) | |
H71A | 0.5714 | 0.4099 | 0.2472 | 0.051* | |
C72 | 0.7088 (11) | 0.1354 (10) | 0.2794 (6) | 0.108 (4) | |
H72A | 0.7001 | 0.1466 | 0.3263 | 0.162* | |
H72B | 0.7853 | 0.1433 | 0.2768 | 0.162* | |
H72C | 0.6653 | 0.0660 | 0.2622 | 0.162* |
U11 | U22 | U33 | U12 | U13 | U23 | |
Dy1 | 0.0323 (2) | 0.0303 (2) | 0.0294 (2) | 0.00754 (17) | 0.00397 (16) | 0.00138 (16) |
Dy2 | 0.02508 (19) | 0.0355 (2) | 0.0242 (2) | 0.00896 (16) | 0.00428 (15) | 0.00333 (15) |
O1 | 0.067 (4) | 0.046 (4) | 0.039 (3) | −0.016 (3) | 0.002 (3) | 0.002 (3) |
O2 | 0.050 (3) | 0.046 (4) | 0.039 (3) | −0.005 (3) | 0.001 (3) | 0.008 (3) |
O3 | 0.061 (4) | 0.075 (5) | 0.043 (4) | 0.042 (3) | 0.020 (3) | 0.024 (3) |
O4 | 0.041 (3) | 0.046 (4) | 0.043 (3) | 0.017 (3) | 0.015 (3) | 0.010 (3) |
O5 | 0.044 (3) | 0.032 (3) | 0.057 (4) | 0.000 (3) | 0.004 (3) | −0.004 (3) |
O6 | 0.045 (3) | 0.048 (4) | 0.057 (4) | 0.022 (3) | 0.007 (3) | −0.012 (3) |
O7 | 0.028 (3) | 0.029 (3) | 0.033 (3) | 0.005 (2) | 0.002 (2) | 0.000 (2) |
O8 | 0.034 (3) | 0.047 (4) | 0.050 (3) | 0.008 (3) | 0.014 (3) | −0.001 (3) |
O9 | 0.040 (3) | 0.046 (3) | 0.035 (3) | 0.017 (3) | 0.002 (2) | 0.001 (3) |
O10 | 0.050 (3) | 0.043 (3) | 0.029 (3) | 0.024 (3) | 0.008 (2) | 0.005 (2) |
O11 | 0.032 (3) | 0.052 (4) | 0.028 (3) | 0.019 (3) | 0.005 (2) | 0.006 (2) |
O12 | 0.041 (3) | 0.044 (3) | 0.028 (3) | 0.013 (3) | 0.005 (2) | 0.010 (2) |
N1 | 0.028 (3) | 0.033 (4) | 0.033 (4) | 0.005 (3) | 0.002 (3) | 0.001 (3) |
N2 | 0.032 (3) | 0.043 (4) | 0.032 (4) | 0.017 (3) | 0.002 (3) | −0.001 (3) |
N3 | 0.025 (3) | 0.043 (4) | 0.031 (3) | 0.014 (3) | 0.006 (3) | 0.002 (3) |
N4 | 0.041 (4) | 0.037 (4) | 0.030 (4) | 0.010 (3) | 0.011 (3) | 0.002 (3) |
C1 | 0.043 (5) | 0.045 (5) | 0.041 (5) | 0.009 (4) | 0.001 (4) | 0.000 (4) |
C2 | 0.044 (5) | 0.047 (6) | 0.052 (6) | 0.015 (4) | −0.006 (4) | −0.004 (4) |
C3 | 0.054 (5) | 0.039 (5) | 0.039 (5) | 0.008 (4) | −0.024 (4) | 0.003 (4) |
C4 | 0.036 (4) | 0.041 (5) | 0.030 (4) | −0.003 (4) | −0.008 (4) | −0.002 (4) |
C5 | 0.069 (6) | 0.064 (7) | 0.028 (5) | 0.005 (5) | −0.002 (4) | 0.013 (4) |
C6 | 0.045 (5) | 0.101 (8) | 0.030 (5) | 0.011 (6) | 0.014 (4) | 0.011 (5) |
C7 | 0.036 (5) | 0.062 (6) | 0.029 (4) | 0.000 (4) | 0.003 (4) | −0.007 (4) |
C8 | 0.041 (5) | 0.103 (9) | 0.045 (6) | 0.029 (5) | 0.010 (4) | −0.006 (5) |
C9 | 0.050 (6) | 0.080 (8) | 0.054 (6) | 0.032 (5) | 0.000 (5) | 0.006 (5) |
C10 | 0.051 (5) | 0.066 (6) | 0.034 (5) | 0.029 (5) | 0.001 (4) | 0.002 (4) |
C11 | 0.025 (4) | 0.043 (5) | 0.021 (4) | 0.001 (3) | −0.003 (3) | −0.004 (3) |
C12 | 0.029 (4) | 0.027 (4) | 0.031 (4) | −0.002 (3) | −0.006 (3) | −0.001 (3) |
C13 | 0.035 (4) | 0.039 (5) | 0.043 (5) | 0.011 (4) | −0.006 (4) | −0.007 (4) |
C14 | 0.042 (5) | 0.041 (5) | 0.047 (5) | 0.013 (4) | −0.008 (4) | 0.001 (4) |
C15 | 0.073 (7) | 0.053 (7) | 0.070 (7) | −0.005 (5) | 0.016 (6) | −0.009 (5) |
C16 | 0.069 (7) | 0.053 (7) | 0.130 (11) | −0.021 (6) | 0.012 (7) | 0.025 (7) |
C17 | 0.076 (8) | 0.029 (6) | 0.149 (13) | 0.002 (6) | −0.060 (8) | −0.005 (7) |
C18 | 0.108 (9) | 0.043 (7) | 0.079 (8) | 0.009 (7) | −0.040 (7) | −0.014 (6) |
C19 | 0.074 (7) | 0.043 (6) | 0.057 (6) | 0.011 (5) | −0.016 (5) | −0.011 (5) |
C20 | 0.118 (8) | 0.093 (8) | 0.151 (9) | 0.006 (7) | −0.020 (7) | 0.008 (7) |
C21 | 0.046 (5) | 0.045 (5) | 0.033 (5) | 0.014 (4) | 0.005 (4) | 0.008 (4) |
C22 | 0.045 (5) | 0.051 (6) | 0.038 (5) | 0.014 (4) | 0.007 (4) | 0.009 (4) |
C23 | 0.047 (5) | 0.053 (6) | 0.035 (5) | 0.009 (4) | 0.011 (4) | 0.009 (4) |
C24 | 0.060 (6) | 0.074 (7) | 0.036 (5) | 0.013 (5) | 0.010 (4) | 0.021 (5) |
C25 | 0.077 (7) | 0.072 (8) | 0.053 (6) | 0.029 (6) | 0.006 (5) | 0.032 (5) |
C26 | 0.097 (8) | 0.084 (8) | 0.072 (7) | 0.069 (7) | 0.019 (6) | 0.016 (6) |
C27 | 0.093 (8) | 0.091 (8) | 0.040 (5) | 0.060 (7) | 0.019 (5) | 0.026 (5) |
C28 | 0.131 (11) | 0.112 (11) | 0.094 (9) | 0.067 (9) | 0.008 (8) | 0.049 (8) |
C29 | 0.041 (5) | 0.026 (4) | 0.020 (4) | 0.009 (4) | −0.001 (3) | −0.001 (3) |
C30 | 0.035 (4) | 0.026 (4) | 0.027 (4) | 0.006 (3) | 0.007 (3) | −0.001 (3) |
C31 | 0.060 (6) | 0.036 (5) | 0.050 (5) | 0.021 (4) | 0.005 (4) | −0.004 (4) |
C32 | 0.105 (9) | 0.052 (7) | 0.063 (7) | 0.039 (6) | 0.014 (6) | 0.002 (5) |
C33 | 0.140 (11) | 0.030 (6) | 0.052 (6) | 0.019 (7) | 0.027 (7) | −0.006 (5) |
C34 | 0.097 (9) | 0.037 (6) | 0.101 (9) | −0.012 (6) | 0.032 (7) | −0.023 (6) |
C35 | 0.047 (5) | 0.046 (6) | 0.080 (7) | −0.002 (5) | 0.010 (5) | −0.022 (5) |
C36 | 0.153 (9) | 0.062 (6) | 0.093 (7) | 0.027 (6) | 0.024 (7) | −0.009 (6) |
C37 | 0.025 (4) | 0.054 (6) | 0.043 (5) | 0.014 (4) | 0.006 (4) | 0.004 (4) |
C38 | 0.038 (5) | 0.074 (7) | 0.043 (5) | 0.023 (5) | −0.005 (4) | −0.007 (5) |
C39 | 0.023 (4) | 0.053 (6) | 0.065 (6) | 0.012 (4) | 0.004 (4) | −0.006 (5) |
C40 | 0.024 (4) | 0.048 (5) | 0.052 (5) | 0.013 (4) | 0.011 (4) | −0.002 (4) |
C41 | 0.028 (4) | 0.057 (6) | 0.085 (7) | 0.004 (4) | 0.025 (5) | −0.003 (5) |
C42 | 0.043 (5) | 0.052 (6) | 0.070 (7) | 0.010 (4) | 0.035 (5) | 0.006 (5) |
C43 | 0.046 (5) | 0.037 (5) | 0.052 (6) | 0.008 (4) | 0.028 (4) | 0.001 (4) |
C44 | 0.075 (7) | 0.055 (6) | 0.038 (5) | 0.015 (5) | 0.032 (5) | −0.001 (4) |
C45 | 0.074 (7) | 0.056 (6) | 0.026 (4) | 0.018 (5) | 0.013 (4) | 0.004 (4) |
C46 | 0.054 (5) | 0.051 (6) | 0.031 (5) | 0.009 (4) | 0.008 (4) | −0.002 (4) |
C47 | 0.032 (4) | 0.038 (5) | 0.034 (4) | 0.013 (4) | 0.012 (3) | −0.002 (3) |
C48 | 0.027 (4) | 0.034 (4) | 0.038 (4) | 0.013 (3) | 0.013 (3) | 0.000 (3) |
C49 | 0.029 (4) | 0.025 (4) | 0.033 (4) | 0.008 (3) | 0.002 (3) | 0.009 (3) |
C50 | 0.036 (4) | 0.027 (4) | 0.033 (4) | 0.007 (3) | 0.005 (3) | 0.001 (3) |
C51 | 0.050 (5) | 0.045 (6) | 0.056 (6) | 0.015 (4) | 0.013 (4) | 0.002 (4) |
C52 | 0.101 (9) | 0.036 (6) | 0.057 (6) | 0.017 (6) | −0.004 (6) | −0.012 (5) |
C53 | 0.053 (6) | 0.032 (5) | 0.063 (6) | 0.004 (4) | −0.001 (5) | 0.010 (4) |
C54 | 0.037 (5) | 0.033 (5) | 0.083 (7) | 0.004 (4) | 0.009 (5) | 0.011 (5) |
C55 | 0.033 (4) | 0.027 (4) | 0.051 (5) | 0.005 (3) | 0.009 (4) | 0.003 (4) |
C56 | 0.080 (7) | 0.036 (6) | 0.104 (9) | −0.007 (5) | −0.025 (6) | 0.000 (6) |
C57 | 0.026 (4) | 0.044 (5) | 0.035 (4) | 0.010 (4) | 0.014 (3) | 0.006 (4) |
C58 | 0.037 (4) | 0.027 (4) | 0.040 (5) | 0.007 (3) | 0.005 (4) | 0.000 (3) |
C59 | 0.072 (6) | 0.050 (6) | 0.040 (5) | 0.019 (5) | −0.009 (5) | −0.002 (4) |
C60 | 0.078 (7) | 0.035 (6) | 0.072 (7) | 0.016 (5) | −0.010 (6) | 0.014 (5) |
C61 | 0.056 (6) | 0.032 (5) | 0.079 (7) | 0.009 (4) | 0.004 (5) | 0.007 (5) |
C62 | 0.079 (7) | 0.042 (6) | 0.051 (6) | 0.016 (5) | −0.005 (5) | −0.011 (4) |
C63 | 0.066 (6) | 0.052 (6) | 0.035 (5) | 0.018 (5) | 0.003 (4) | 0.006 (4) |
C64 | 0.105 (9) | 0.034 (6) | 0.110 (9) | 0.019 (6) | 0.005 (7) | −0.003 (6) |
C65 | 0.028 (4) | 0.042 (5) | 0.023 (4) | 0.005 (4) | 0.002 (3) | 0.003 (3) |
C66 | 0.019 (4) | 0.040 (5) | 0.037 (4) | 0.003 (3) | 0.010 (3) | 0.014 (4) |
C67 | 0.065 (6) | 0.063 (6) | 0.052 (6) | 0.033 (5) | 0.029 (5) | 0.021 (5) |
C68 | 0.076 (7) | 0.082 (8) | 0.096 (8) | 0.057 (6) | 0.048 (6) | 0.049 (7) |
C69 | 0.062 (6) | 0.094 (9) | 0.081 (8) | 0.038 (6) | 0.025 (6) | 0.065 (7) |
C70 | 0.058 (6) | 0.077 (7) | 0.045 (6) | 0.026 (5) | 0.002 (5) | 0.027 (5) |
C71 | 0.049 (5) | 0.050 (6) | 0.031 (4) | 0.018 (4) | 0.000 (4) | 0.011 (4) |
C72 | 0.123 (8) | 0.113 (8) | 0.110 (8) | 0.060 (6) | 0.027 (6) | 0.062 (6) |
Dy1—O5 | 2.256 (5) | C26—C27 | 1.396 (12) |
Dy1—O6i | 2.257 (6) | C26—H26A | 0.9300 |
Dy1—O3 | 2.332 (6) | C27—H27A | 0.9300 |
Dy1—O1 | 2.367 (5) | C28—H28A | 0.9600 |
Dy1—O4 | 2.431 (5) | C28—H28B | 0.9600 |
Dy1—O2 | 2.433 (5) | C28—H28C | 0.9600 |
Dy1—N1 | 2.529 (6) | C29—C30 | 1.506 (10) |
Dy1—N2 | 2.547 (6) | C30—C31 | 1.361 (11) |
Dy1—C21 | 2.722 (8) | C30—C35 | 1.369 (10) |
Dy1—C13 | 2.763 (8) | C31—C32 | 1.393 (12) |
Dy2—O12ii | 2.276 (5) | C31—H31A | 0.9300 |
Dy2—O8ii | 2.318 (5) | C32—C33 | 1.363 (15) |
Dy2—O11 | 2.328 (5) | C32—H32A | 0.9300 |
Dy2—O7 | 2.335 (5) | C33—C34 | 1.347 (15) |
Dy2—O9 | 2.405 (5) | C33—C36 | 1.505 (14) |
Dy2—O10 | 2.471 (5) | C34—C35 | 1.384 (13) |
Dy2—N3 | 2.576 (6) | C34—H34A | 0.9300 |
Dy2—N4 | 2.579 (6) | C35—H35A | 0.9300 |
Dy2—C57 | 2.798 (8) | C36—H36A | 0.9600 |
O1—C13 | 1.276 (9) | C36—H36B | 0.9600 |
O2—C13 | 1.234 (9) | C36—H36C | 0.9600 |
O3—C21 | 1.259 (9) | C37—C38 | 1.387 (10) |
O4—C21 | 1.245 (9) | C37—H37A | 0.9300 |
O5—C29 | 1.232 (8) | C38—C39 | 1.341 (11) |
O6—C29 | 1.240 (9) | C38—H38A | 0.9300 |
O6—Dy1i | 2.257 (6) | C39—C40 | 1.405 (11) |
O7—C49 | 1.257 (8) | C39—H39A | 0.9300 |
O8—C49 | 1.259 (8) | C40—C48 | 1.412 (10) |
O8—Dy2ii | 2.318 (5) | C40—C41 | 1.414 (11) |
O9—C57 | 1.281 (8) | C41—C42 | 1.330 (12) |
O10—C57 | 1.248 (8) | C41—H41A | 0.9300 |
O11—C65 | 1.231 (9) | C42—C43 | 1.427 (11) |
O12—C65 | 1.281 (8) | C42—H42A | 0.9300 |
O12—Dy2ii | 2.276 (5) | C43—C47 | 1.387 (10) |
N1—C1 | 1.333 (10) | C43—C44 | 1.391 (12) |
N1—C12 | 1.354 (9) | C44—C45 | 1.337 (12) |
N2—C10 | 1.326 (10) | C44—H44A | 0.9300 |
N2—C11 | 1.354 (9) | C45—C46 | 1.379 (11) |
N3—C37 | 1.329 (9) | C45—H45A | 0.9300 |
N3—C48 | 1.350 (9) | C46—H46A | 0.9300 |
N4—C46 | 1.332 (9) | C47—C48 | 1.439 (10) |
N4—C47 | 1.357 (9) | C49—C50 | 1.511 (9) |
C1—C2 | 1.390 (11) | C50—C51 | 1.372 (11) |
C1—H1A | 0.9300 | C50—C55 | 1.381 (10) |
C2—C3 | 1.352 (11) | C51—C52 | 1.414 (12) |
C2—H2A | 0.9300 | C51—H51A | 0.9300 |
C3—C4 | 1.414 (11) | C52—C53 | 1.348 (13) |
C3—H3A | 0.9300 | C52—H52A | 0.9300 |
C4—C12 | 1.417 (10) | C53—C54 | 1.362 (12) |
C4—C5 | 1.436 (12) | C53—C56 | 1.509 (11) |
C5—C6 | 1.330 (13) | C54—C55 | 1.381 (10) |
C5—H5A | 0.9300 | C54—H54A | 0.9300 |
C6—C7 | 1.431 (12) | C55—H55A | 0.9300 |
C6—H6A | 0.9300 | C56—H56A | 0.9600 |
C7—C8 | 1.392 (12) | C56—H56B | 0.9600 |
C7—C11 | 1.414 (10) | C56—H56C | 0.9600 |
C8—C9 | 1.340 (12) | C57—C58 | 1.505 (10) |
C8—H8A | 0.9300 | C58—C59 | 1.374 (11) |
C9—C10 | 1.387 (12) | C58—C63 | 1.381 (10) |
C9—H9A | 0.9300 | C59—C60 | 1.385 (12) |
C10—H10A | 0.9300 | C59—H59A | 0.9300 |
C11—C12 | 1.424 (11) | C60—C61 | 1.376 (12) |
C13—C14 | 1.480 (11) | C60—H60A | 0.9300 |
C14—C19 | 1.376 (12) | C61—C62 | 1.362 (12) |
C14—C15 | 1.401 (12) | C61—C64 | 1.525 (12) |
C15—C16 | 1.374 (13) | C62—C63 | 1.371 (12) |
C15—H15A | 0.9300 | C62—H62A | 0.9300 |
C16—C17 | 1.386 (17) | C63—H63A | 0.9300 |
C16—H16A | 0.9300 | C64—H64A | 0.9600 |
C17—C18 | 1.397 (17) | C64—H64B | 0.9600 |
C17—C20 | 1.529 (15) | C64—H64C | 0.9600 |
C18—C19 | 1.362 (13) | C65—C66 | 1.502 (10) |
C18—H18A | 0.9300 | C66—C67 | 1.378 (11) |
C19—H19A | 0.9300 | C66—C71 | 1.396 (10) |
C20—H20A | 0.9600 | C67—C68 | 1.382 (12) |
C20—H20B | 0.9600 | C67—H67A | 0.9300 |
C20—H20C | 0.9600 | C68—C69 | 1.368 (14) |
C21—C22 | 1.491 (11) | C68—H68A | 0.9300 |
C22—C27 | 1.374 (12) | C69—C70 | 1.355 (14) |
C22—C23 | 1.383 (10) | C69—C72 | 1.514 (13) |
C23—C24 | 1.374 (12) | C70—C71 | 1.369 (11) |
C23—H23A | 0.9300 | C70—H70A | 0.9300 |
C24—C25 | 1.351 (14) | C71—H71A | 0.9300 |
C24—H24A | 0.9300 | C72—H72A | 0.9600 |
C25—C26 | 1.375 (13) | C72—H72B | 0.9600 |
C25—C28 | 1.528 (13) | C72—H72C | 0.9600 |
O5—Dy1—O6i | 92.3 (2) | O4—C21—Dy1 | 63.3 (4) |
O5—Dy1—O3 | 88.1 (2) | O3—C21—Dy1 | 58.8 (4) |
O6i—Dy1—O3 | 139.1 (2) | C22—C21—Dy1 | 175.3 (6) |
O5—Dy1—O1 | 150.90 (19) | C27—C22—C23 | 117.3 (8) |
O6i—Dy1—O1 | 95.3 (2) | C27—C22—C21 | 120.8 (8) |
O3—Dy1—O1 | 103.9 (2) | C23—C22—C21 | 121.8 (8) |
O5—Dy1—O4 | 79.63 (19) | C24—C23—C22 | 121.4 (9) |
O6i—Dy1—O4 | 85.2 (2) | C24—C23—H23A | 119.3 |
O3—Dy1—O4 | 54.66 (18) | C22—C23—H23A | 119.3 |
O1—Dy1—O4 | 128.94 (18) | C25—C24—C23 | 121.9 (9) |
O5—Dy1—O2 | 155.07 (19) | C25—C24—H24A | 119.1 |
O6i—Dy1—O2 | 78.9 (2) | C23—C24—H24A | 119.1 |
O3—Dy1—O2 | 83.7 (2) | C24—C25—C26 | 117.6 (9) |
O1—Dy1—O2 | 53.94 (18) | C24—C25—C28 | 121.9 (10) |
O4—Dy1—O2 | 76.43 (18) | C26—C25—C28 | 120.5 (10) |
O5—Dy1—N1 | 76.99 (19) | C25—C26—C27 | 121.5 (9) |
O6i—Dy1—N1 | 82.7 (2) | C25—C26—H26A | 119.2 |
O3—Dy1—N1 | 136.7 (2) | C27—C26—H26A | 119.2 |
O1—Dy1—N1 | 76.20 (19) | C22—C27—C26 | 120.3 (9) |
O4—Dy1—N1 | 153.11 (18) | C22—C27—H27A | 119.8 |
O2—Dy1—N1 | 124.11 (19) | C26—C27—H27A | 119.8 |
O5—Dy1—N2 | 85.6 (2) | C25—C28—H28A | 109.5 |
O6i—Dy1—N2 | 147.3 (2) | C25—C28—H28B | 109.5 |
O3—Dy1—N2 | 73.6 (2) | H28A—C28—H28B | 109.5 |
O1—Dy1—N2 | 72.9 (2) | C25—C28—H28C | 109.5 |
O4—Dy1—N2 | 126.2 (2) | H28A—C28—H28C | 109.5 |
O2—Dy1—N2 | 114.3 (2) | H28B—C28—H28C | 109.5 |
N1—Dy1—N2 | 65.0 (2) | O5—C29—O6 | 123.9 (7) |
O5—Dy1—C21 | 84.2 (2) | O5—C29—C30 | 117.1 (7) |
O6i—Dy1—C21 | 111.9 (2) | O6—C29—C30 | 119.1 (7) |
O3—Dy1—C21 | 27.5 (2) | C31—C30—C35 | 119.3 (8) |
O1—Dy1—C21 | 118.4 (2) | C31—C30—C29 | 120.1 (7) |
O4—Dy1—C21 | 27.2 (2) | C35—C30—C29 | 120.5 (7) |
O2—Dy1—C21 | 77.7 (2) | C30—C31—C32 | 118.9 (9) |
N1—Dy1—C21 | 156.7 (2) | C30—C31—H31A | 120.6 |
N2—Dy1—C21 | 100.4 (2) | C32—C31—H31A | 120.6 |
O5—Dy1—C13 | 177.2 (2) | C33—C32—C31 | 122.4 (10) |
O6i—Dy1—C13 | 86.0 (2) | C33—C32—H32A | 118.8 |
O3—Dy1—C13 | 94.7 (2) | C31—C32—H32A | 118.8 |
O1—Dy1—C13 | 27.4 (2) | C34—C33—C32 | 117.5 (10) |
O4—Dy1—C13 | 102.5 (2) | C34—C33—C36 | 121.1 (12) |
O2—Dy1—C13 | 26.5 (2) | C32—C33—C36 | 121.4 (12) |
N1—Dy1—C13 | 100.5 (2) | C33—C34—C35 | 121.8 (10) |
N2—Dy1—C13 | 94.6 (2) | C33—C34—H34A | 119.1 |
C21—Dy1—C13 | 98.6 (2) | C35—C34—H34A | 119.1 |
O12ii—Dy2—O8ii | 78.43 (18) | C30—C35—C34 | 120.1 (10) |
O12ii—Dy2—O11 | 125.54 (18) | C30—C35—H35A | 120.0 |
O8ii—Dy2—O11 | 79.83 (19) | C34—C35—H35A | 120.0 |
O12ii—Dy2—O7 | 78.31 (17) | C33—C36—H36A | 109.5 |
O8ii—Dy2—O7 | 127.43 (18) | C33—C36—H36B | 109.5 |
O11—Dy2—O7 | 76.68 (17) | H36A—C36—H36B | 109.5 |
O12ii—Dy2—O9 | 83.15 (18) | C33—C36—H36C | 109.5 |
O8ii—Dy2—O9 | 79.76 (19) | H36A—C36—H36C | 109.5 |
O11—Dy2—O9 | 139.83 (18) | H36B—C36—H36C | 109.5 |
O7—Dy2—O9 | 141.94 (16) | N3—C37—C38 | 123.0 (8) |
O12ii—Dy2—O10 | 131.68 (18) | N3—C37—H37A | 118.5 |
O8ii—Dy2—O10 | 74.40 (18) | C38—C37—H37A | 118.5 |
O11—Dy2—O10 | 87.87 (18) | C39—C38—C37 | 119.5 (8) |
O7—Dy2—O10 | 148.95 (17) | C39—C38—H38A | 120.3 |
O9—Dy2—O10 | 53.35 (17) | C37—C38—H38A | 120.3 |
O12ii—Dy2—N3 | 81.72 (18) | C38—C39—C40 | 120.2 (7) |
O8ii—Dy2—N3 | 148.82 (19) | C38—C39—H39A | 119.9 |
O11—Dy2—N3 | 131.34 (19) | C40—C39—H39A | 119.9 |
O7—Dy2—N3 | 70.48 (18) | C39—C40—C48 | 117.0 (7) |
O9—Dy2—N3 | 74.18 (18) | C39—C40—C41 | 123.9 (7) |
O10—Dy2—N3 | 102.34 (18) | C48—C40—C41 | 119.1 (8) |
O12ii—Dy2—N4 | 142.40 (18) | C42—C41—C40 | 121.3 (8) |
O8ii—Dy2—N4 | 139.13 (19) | C42—C41—H41A | 119.3 |
O11—Dy2—N4 | 75.01 (19) | C40—C41—H41A | 119.3 |
O7—Dy2—N4 | 77.03 (18) | C41—C42—C43 | 122.2 (8) |
O9—Dy2—N4 | 99.51 (19) | C41—C42—H42A | 118.9 |
O10—Dy2—N4 | 72.99 (19) | C43—C42—H42A | 118.9 |
N3—Dy2—N4 | 63.47 (19) | C47—C43—C44 | 117.8 (8) |
O12ii—Dy2—C57 | 106.9 (2) | C47—C43—C42 | 117.6 (8) |
O8ii—Dy2—C57 | 72.5 (2) | C44—C43—C42 | 124.6 (8) |
O11—Dy2—C57 | 113.0 (2) | C45—C44—C43 | 121.5 (8) |
O7—Dy2—C57 | 159.96 (18) | C45—C44—H44A | 119.3 |
O9—Dy2—C57 | 27.20 (18) | C43—C44—H44A | 119.3 |
O10—Dy2—C57 | 26.47 (18) | C44—C45—C46 | 116.5 (8) |
N3—Dy2—C57 | 90.8 (2) | C44—C45—H45A | 121.7 |
N4—Dy2—C57 | 88.3 (2) | C46—C45—H45A | 121.7 |
C13—O1—Dy1 | 93.8 (5) | N4—C46—C45 | 126.0 (8) |
C13—O2—Dy1 | 91.8 (5) | N4—C46—H46A | 117.0 |
C21—O3—Dy1 | 93.7 (5) | C45—C46—H46A | 117.0 |
C21—O4—Dy1 | 89.5 (5) | N4—C47—C43 | 122.3 (7) |
C29—O5—Dy1 | 158.2 (5) | N4—C47—C48 | 116.5 (6) |
C29—O6—Dy1i | 162.4 (5) | C43—C47—C48 | 121.1 (7) |
C49—O7—Dy2 | 138.1 (5) | N3—C48—C40 | 122.2 (7) |
C49—O8—Dy2ii | 139.3 (5) | N3—C48—C47 | 119.5 (6) |
C57—O9—Dy2 | 93.7 (4) | C40—C48—C47 | 118.3 (7) |
C57—O10—Dy2 | 91.5 (4) | O7—C49—O8 | 125.6 (7) |
C65—O11—Dy2 | 117.2 (5) | O7—C49—C50 | 118.2 (6) |
C65—O12—Dy2ii | 162.9 (4) | O8—C49—C50 | 116.3 (7) |
C1—N1—C12 | 119.5 (7) | C51—C50—C55 | 118.2 (7) |
C1—N1—Dy1 | 122.8 (5) | C51—C50—C49 | 122.1 (7) |
C12—N1—Dy1 | 117.3 (5) | C55—C50—C49 | 119.6 (7) |
C10—N2—C11 | 117.5 (7) | C50—C51—C52 | 119.7 (8) |
C10—N2—Dy1 | 124.8 (5) | C50—C51—H51A | 120.2 |
C11—N2—Dy1 | 116.5 (5) | C52—C51—H51A | 120.2 |
C37—N3—C48 | 118.1 (6) | C53—C52—C51 | 121.4 (9) |
C37—N3—Dy2 | 122.1 (5) | C53—C52—H52A | 119.3 |
C48—N3—Dy2 | 119.6 (4) | C51—C52—H52A | 119.3 |
C46—N4—C47 | 115.9 (7) | C52—C53—C54 | 118.5 (8) |
C46—N4—Dy2 | 123.3 (5) | C52—C53—C56 | 119.8 (9) |
C47—N4—Dy2 | 120.8 (5) | C54—C53—C56 | 121.7 (9) |
N1—C1—C2 | 122.4 (8) | C53—C54—C55 | 121.4 (8) |
N1—C1—H1A | 118.8 | C53—C54—H54A | 119.3 |
C2—C1—H1A | 118.8 | C55—C54—H54A | 119.3 |
C3—C2—C1 | 119.3 (8) | C54—C55—C50 | 120.8 (8) |
C3—C2—H2A | 120.3 | C54—C55—H55A | 119.6 |
C1—C2—H2A | 120.3 | C50—C55—H55A | 119.6 |
C2—C3—C4 | 120.3 (8) | C53—C56—H56A | 109.5 |
C2—C3—H3A | 119.8 | C53—C56—H56B | 109.5 |
C4—C3—H3A | 119.8 | H56A—C56—H56B | 109.5 |
C3—C4—C12 | 117.1 (8) | C53—C56—H56C | 109.5 |
C3—C4—C5 | 125.0 (8) | H56A—C56—H56C | 109.5 |
C12—C4—C5 | 117.9 (8) | H56B—C56—H56C | 109.5 |
C6—C5—C4 | 122.0 (8) | O10—C57—O9 | 120.0 (7) |
C6—C5—H5A | 119.0 | O10—C57—C58 | 121.6 (7) |
C4—C5—H5A | 119.0 | O9—C57—C58 | 118.5 (7) |
C5—C6—C7 | 121.6 (8) | O10—C57—Dy2 | 62.0 (4) |
C5—C6—H6A | 119.2 | O9—C57—Dy2 | 59.1 (4) |
C7—C6—H6A | 119.2 | C58—C57—Dy2 | 169.7 (5) |
C8—C7—C11 | 119.1 (8) | C59—C58—C63 | 117.3 (8) |
C8—C7—C6 | 122.6 (8) | C59—C58—C57 | 122.0 (7) |
C11—C7—C6 | 118.3 (8) | C63—C58—C57 | 120.7 (7) |
C9—C8—C7 | 118.6 (9) | C58—C59—C60 | 121.3 (8) |
C9—C8—H8A | 120.7 | C58—C59—H59A | 119.3 |
C7—C8—H8A | 120.7 | C60—C59—H59A | 119.3 |
C8—C9—C10 | 119.9 (9) | C61—C60—C59 | 120.6 (9) |
C8—C9—H9A | 120.1 | C61—C60—H60A | 119.7 |
C10—C9—H9A | 120.1 | C59—C60—H60A | 119.7 |
N2—C10—C9 | 123.8 (8) | C62—C61—C60 | 118.0 (9) |
N2—C10—H10A | 118.1 | C62—C61—C64 | 121.4 (9) |
C9—C10—H10A | 118.1 | C60—C61—C64 | 120.5 (9) |
N2—C11—C7 | 121.1 (7) | C61—C62—C63 | 121.7 (8) |
N2—C11—C12 | 118.8 (7) | C61—C62—H62A | 119.2 |
C7—C11—C12 | 120.1 (7) | C63—C62—H62A | 119.2 |
N1—C12—C4 | 121.2 (7) | C62—C63—C58 | 121.1 (8) |
N1—C12—C11 | 118.7 (6) | C62—C63—H63A | 119.4 |
C4—C12—C11 | 120.0 (7) | C58—C63—H63A | 119.4 |
O2—C13—O1 | 120.3 (7) | C61—C64—H64A | 109.5 |
O2—C13—C14 | 121.6 (7) | C61—C64—H64B | 109.5 |
O1—C13—C14 | 118.0 (7) | H64A—C64—H64B | 109.5 |
O2—C13—Dy1 | 61.7 (4) | C61—C64—H64C | 109.5 |
O1—C13—Dy1 | 58.7 (4) | H64A—C64—H64C | 109.5 |
C14—C13—Dy1 | 175.2 (6) | H64B—C64—H64C | 109.5 |
C19—C14—C15 | 119.0 (8) | O11—C65—O12 | 123.5 (7) |
C19—C14—C13 | 120.0 (8) | O11—C65—C66 | 119.5 (7) |
C15—C14—C13 | 121.0 (8) | O12—C65—C66 | 117.0 (7) |
C16—C15—C14 | 121.3 (10) | C67—C66—C71 | 118.7 (8) |
C16—C15—H15A | 119.4 | C67—C66—C65 | 121.8 (7) |
C14—C15—H15A | 119.4 | C71—C66—C65 | 119.4 (7) |
C15—C16—C17 | 118.9 (11) | C66—C67—C68 | 119.6 (9) |
C15—C16—H16A | 120.6 | C66—C67—H67A | 120.2 |
C17—C16—H16A | 120.6 | C68—C67—H67A | 120.2 |
C16—C17—C18 | 119.8 (10) | C69—C68—C67 | 121.5 (10) |
C16—C17—C20 | 115.7 (14) | C69—C68—H68A | 119.2 |
C18—C17—C20 | 124.5 (13) | C67—C68—H68A | 119.2 |
C19—C18—C17 | 120.7 (11) | C70—C69—C68 | 118.5 (9) |
C19—C18—H18A | 119.6 | C70—C69—C72 | 122.0 (10) |
C17—C18—H18A | 119.6 | C68—C69—C72 | 119.4 (11) |
C18—C19—C14 | 120.4 (10) | C69—C70—C71 | 121.9 (9) |
C18—C19—H19A | 119.8 | C69—C70—H70A | 119.1 |
C14—C19—H19A | 119.8 | C71—C70—H70A | 119.1 |
C17—C20—H20A | 109.5 | C70—C71—C66 | 119.7 (9) |
C17—C20—H20B | 109.5 | C70—C71—H71A | 120.1 |
H20A—C20—H20B | 109.5 | C66—C71—H71A | 120.1 |
C17—C20—H20C | 109.5 | C69—C72—H72A | 109.5 |
H20A—C20—H20C | 109.5 | C69—C72—H72B | 109.5 |
H20B—C20—H20C | 109.5 | H72A—C72—H72B | 109.5 |
O4—C21—O3 | 121.9 (8) | C69—C72—H72C | 109.5 |
O4—C21—C22 | 120.5 (7) | H72A—C72—H72C | 109.5 |
O3—C21—C22 | 117.5 (8) | H72B—C72—H72C | 109.5 |
O5—Dy1—O1—C13 | 175.2 (5) | O4—Dy1—C13—C14 | −146 (8) |
O6i—Dy1—O1—C13 | 70.6 (5) | O2—Dy1—C13—C14 | −134 (8) |
O3—Dy1—O1—C13 | −72.9 (5) | N1—Dy1—C13—C14 | 20 (8) |
O4—Dy1—O1—C13 | −17.4 (6) | N2—Dy1—C13—C14 | 86 (8) |
O2—Dy1—O1—C13 | −1.5 (5) | C21—Dy1—C13—C14 | −173 (8) |
N1—Dy1—O1—C13 | 151.8 (5) | O2—C13—C14—C19 | −19.6 (13) |
N2—Dy1—O1—C13 | −140.6 (5) | O1—C13—C14—C19 | 159.1 (8) |
C21—Dy1—O1—C13 | −47.8 (6) | Dy1—C13—C14—C19 | 113 (7) |
O5—Dy1—O2—C13 | −174.6 (5) | O2—C13—C14—C15 | 159.3 (9) |
O6i—Dy1—O2—C13 | −103.5 (5) | O1—C13—C14—C15 | −22.0 (12) |
O3—Dy1—O2—C13 | 113.7 (5) | Dy1—C13—C14—C15 | −68 (8) |
O1—Dy1—O2—C13 | 1.5 (5) | C19—C14—C15—C16 | 0.7 (15) |
O4—Dy1—O2—C13 | 168.8 (5) | C13—C14—C15—C16 | −178.2 (10) |
N1—Dy1—O2—C13 | −30.3 (6) | C14—C15—C16—C17 | −0.9 (18) |
N2—Dy1—O2—C13 | 44.9 (5) | C15—C16—C17—C18 | 0.4 (18) |
C21—Dy1—O2—C13 | 140.9 (5) | C15—C16—C17—C20 | −179.2 (11) |
O5—Dy1—O3—C21 | −81.0 (5) | C16—C17—C18—C19 | 0.5 (18) |
O6i—Dy1—O3—C21 | 10.4 (6) | C20—C17—C18—C19 | −180.0 (11) |
O1—Dy1—O3—C21 | 125.8 (5) | C17—C18—C19—C14 | −0.7 (16) |
O4—Dy1—O3—C21 | −2.4 (4) | C15—C14—C19—C18 | 0.1 (14) |
O2—Dy1—O3—C21 | 75.4 (5) | C13—C14—C19—C18 | 179.1 (9) |
N1—Dy1—O3—C21 | −149.7 (5) | Dy1—O4—C21—O3 | −4.3 (8) |
N2—Dy1—O3—C21 | −167.0 (5) | Dy1—O4—C21—C22 | 176.9 (7) |
C13—Dy1—O3—C21 | 99.6 (5) | Dy1—O3—C21—O4 | 4.5 (8) |
O5—Dy1—O4—C21 | 97.5 (5) | Dy1—O3—C21—C22 | −176.7 (6) |
O6i—Dy1—O4—C21 | −169.3 (5) | O5—Dy1—C21—O4 | −78.6 (5) |
O3—Dy1—O4—C21 | 2.4 (4) | O6i—Dy1—C21—O4 | 11.5 (5) |
O1—Dy1—O4—C21 | −76.3 (5) | O3—Dy1—C21—O4 | −175.8 (8) |
O2—Dy1—O4—C21 | −89.5 (5) | O1—Dy1—C21—O4 | 120.8 (4) |
N1—Dy1—O4—C21 | 127.4 (5) | O2—Dy1—C21—O4 | 84.1 (5) |
N2—Dy1—O4—C21 | 20.8 (5) | N1—Dy1—C21—O4 | −114.5 (6) |
C13—Dy1—O4—C21 | −84.5 (5) | N2—Dy1—C21—O4 | −163.1 (4) |
O6i—Dy1—O5—C29 | −12.5 (14) | C13—Dy1—C21—O4 | 100.6 (5) |
O3—Dy1—O5—C29 | 126.5 (14) | O5—Dy1—C21—O3 | 97.1 (5) |
O1—Dy1—O5—C29 | −117.8 (14) | O6i—Dy1—C21—O3 | −172.7 (4) |
O4—Dy1—O5—C29 | 72.1 (14) | O1—Dy1—C21—O3 | −63.4 (5) |
O2—Dy1—O5—C29 | 55.8 (16) | O4—Dy1—C21—O3 | 175.8 (8) |
N1—Dy1—O5—C29 | −94.5 (14) | O2—Dy1—C21—O3 | −100.1 (5) |
N2—Dy1—O5—C29 | −159.8 (14) | N1—Dy1—C21—O3 | 61.3 (8) |
C21—Dy1—O5—C29 | 99.2 (14) | N2—Dy1—C21—O3 | 12.7 (5) |
C13—Dy1—O5—C29 | −66 (5) | C13—Dy1—C21—O3 | −83.6 (5) |
O12ii—Dy2—O7—C49 | 19.3 (6) | O5—Dy1—C21—C22 | 136 (7) |
O8ii—Dy2—O7—C49 | −46.1 (7) | O6i—Dy1—C21—C22 | −134 (7) |
O11—Dy2—O7—C49 | −112.0 (7) | O3—Dy1—C21—C22 | 39 (7) |
O9—Dy2—O7—C49 | 81.8 (7) | O1—Dy1—C21—C22 | −25 (8) |
O10—Dy2—O7—C49 | −174.1 (6) | O4—Dy1—C21—C22 | −146 (8) |
N3—Dy2—O7—C49 | 104.5 (7) | O2—Dy1—C21—C22 | −62 (7) |
N4—Dy2—O7—C49 | 170.6 (7) | N1—Dy1—C21—C22 | 100 (7) |
C57—Dy2—O7—C49 | 126.6 (8) | N2—Dy1—C21—C22 | 51 (7) |
O12ii—Dy2—O9—C57 | −150.9 (4) | C13—Dy1—C21—C22 | −45 (7) |
O8ii—Dy2—O9—C57 | −71.5 (4) | O4—C21—C22—C27 | 166.6 (9) |
O11—Dy2—O9—C57 | −11.0 (5) | O3—C21—C22—C27 | −12.3 (12) |
O7—Dy2—O9—C57 | 148.1 (4) | Dy1—C21—C22—C27 | −49 (8) |
O10—Dy2—O9—C57 | 6.6 (4) | O4—C21—C22—C23 | −14.9 (12) |
N3—Dy2—O9—C57 | 125.8 (4) | O3—C21—C22—C23 | 166.2 (8) |
N4—Dy2—O9—C57 | 67.0 (4) | Dy1—C21—C22—C23 | 129 (7) |
O12ii—Dy2—O10—C57 | 23.7 (5) | C27—C22—C23—C24 | −0.1 (13) |
O8ii—Dy2—O10—C57 | 81.9 (4) | C21—C22—C23—C24 | −178.7 (8) |
O11—Dy2—O10—C57 | 162.0 (4) | C22—C23—C24—C25 | −0.9 (14) |
O7—Dy2—O10—C57 | −138.6 (4) | C23—C24—C25—C26 | 0.4 (15) |
O9—Dy2—O10—C57 | −6.8 (4) | C23—C24—C25—C28 | −175.7 (10) |
N3—Dy2—O10—C57 | −66.1 (4) | C24—C25—C26—C27 | 1.0 (17) |
N4—Dy2—O10—C57 | −123.1 (4) | C28—C25—C26—C27 | 177.2 (11) |
O12ii—Dy2—O11—C65 | −12.1 (6) | C23—C22—C27—C26 | 1.5 (15) |
O8ii—Dy2—O11—C65 | −79.9 (5) | C21—C22—C27—C26 | −179.9 (9) |
O7—Dy2—O11—C65 | 52.7 (5) | C25—C26—C27—C22 | −2.0 (17) |
O9—Dy2—O11—C65 | −140.4 (5) | Dy1—O5—C29—O6 | 23.8 (19) |
O10—Dy2—O11—C65 | −154.4 (5) | Dy1—O5—C29—C30 | −155.3 (11) |
N3—Dy2—O11—C65 | 101.0 (5) | Dy1i—O6—C29—O5 | −35 (2) |
N4—Dy2—O11—C65 | 132.6 (6) | Dy1i—O6—C29—C30 | 144.3 (15) |
C57—Dy2—O11—C65 | −145.8 (5) | O5—C29—C30—C31 | 12.7 (10) |
O5—Dy1—N1—C1 | 80.5 (6) | O6—C29—C30—C31 | −166.4 (7) |
O6i—Dy1—N1—C1 | −13.6 (6) | O5—C29—C30—C35 | −167.1 (8) |
O3—Dy1—N1—C1 | 153.4 (5) | O6—C29—C30—C35 | 13.7 (11) |
O1—Dy1—N1—C1 | −110.9 (6) | C35—C30—C31—C32 | −1.7 (12) |
O4—Dy1—N1—C1 | 50.3 (8) | C29—C30—C31—C32 | 178.5 (7) |
O2—Dy1—N1—C1 | −84.9 (6) | C30—C31—C32—C33 | 1.2 (14) |
N2—Dy1—N1—C1 | 171.7 (6) | C31—C32—C33—C34 | −0.1 (16) |
C21—Dy1—N1—C1 | 117.2 (7) | C31—C32—C33—C36 | 179.9 (9) |
C13—Dy1—N1—C1 | −98.1 (6) | C32—C33—C34—C35 | −0.4 (17) |
O5—Dy1—N1—C12 | −106.6 (5) | C36—C33—C34—C35 | 179.5 (10) |
O6i—Dy1—N1—C12 | 159.3 (5) | C31—C30—C35—C34 | 1.2 (14) |
O3—Dy1—N1—C12 | −33.7 (6) | C29—C30—C35—C34 | −179.0 (8) |
O1—Dy1—N1—C12 | 61.9 (5) | C33—C34—C35—C30 | −0.1 (17) |
O4—Dy1—N1—C12 | −136.9 (5) | C48—N3—C37—C38 | 0.2 (12) |
O2—Dy1—N1—C12 | 88.0 (5) | Dy2—N3—C37—C38 | 174.9 (6) |
N2—Dy1—N1—C12 | −15.4 (5) | N3—C37—C38—C39 | 1.6 (14) |
C21—Dy1—N1—C12 | −69.9 (8) | C37—C38—C39—C40 | −1.2 (13) |
C13—Dy1—N1—C12 | 74.8 (5) | C38—C39—C40—C48 | −0.8 (12) |
O5—Dy1—N2—C10 | −99.1 (7) | C38—C39—C40—C41 | 176.2 (8) |
O6i—Dy1—N2—C10 | 173.4 (6) | C39—C40—C41—C42 | −179.9 (9) |
O3—Dy1—N2—C10 | −9.8 (6) | C48—C40—C41—C42 | −3.0 (14) |
O1—Dy1—N2—C10 | 100.8 (7) | C40—C41—C42—C43 | −2.5 (15) |
O4—Dy1—N2—C10 | −25.4 (7) | C41—C42—C43—C47 | 6.0 (14) |
O2—Dy1—N2—C10 | 65.3 (7) | C41—C42—C43—C44 | −176.2 (9) |
N1—Dy1—N2—C10 | −176.8 (7) | C47—C43—C44—C45 | −2.5 (14) |
C21—Dy1—N2—C10 | −15.9 (7) | C42—C43—C44—C45 | 179.8 (9) |
C13—Dy1—N2—C10 | 83.7 (7) | C43—C44—C45—C46 | 2.4 (14) |
O5—Dy1—N2—C11 | 93.7 (5) | C47—N4—C46—C45 | −0.6 (13) |
O6i—Dy1—N2—C11 | 6.2 (7) | Dy2—N4—C46—C45 | 179.6 (7) |
O3—Dy1—N2—C11 | −177.0 (5) | C44—C45—C46—N4 | −0.9 (14) |
O1—Dy1—N2—C11 | −66.4 (5) | C46—N4—C47—C43 | 0.5 (11) |
O4—Dy1—N2—C11 | 167.4 (4) | Dy2—N4—C47—C43 | −179.6 (6) |
O2—Dy1—N2—C11 | −101.9 (5) | C46—N4—C47—C48 | −176.5 (7) |
N1—Dy1—N2—C11 | 16.0 (5) | Dy2—N4—C47—C48 | 3.3 (9) |
C21—Dy1—N2—C11 | 176.9 (5) | C44—C43—C47—N4 | 0.9 (12) |
C13—Dy1—N2—C11 | −83.5 (5) | C42—C43—C47—N4 | 178.8 (7) |
O12ii—Dy2—N3—C37 | −10.7 (6) | C44—C43—C47—C48 | 177.9 (8) |
O8ii—Dy2—N3—C37 | 40.1 (8) | C42—C43—C47—C48 | −4.2 (12) |
O11—Dy2—N3—C37 | −141.6 (6) | C37—N3—C48—C40 | −2.3 (11) |
O7—Dy2—N3—C37 | −91.2 (6) | Dy2—N3—C48—C40 | −177.1 (6) |
O9—Dy2—N3—C37 | 74.5 (6) | C37—N3—C48—C47 | 178.6 (7) |
O10—Dy2—N3—C37 | 120.3 (6) | Dy2—N3—C48—C47 | 3.8 (9) |
N4—Dy2—N3—C37 | −176.1 (7) | C39—C40—C48—N3 | 2.6 (12) |
C57—Dy2—N3—C37 | 96.2 (6) | C41—C40—C48—N3 | −174.6 (7) |
O12ii—Dy2—N3—C48 | 163.9 (6) | C39—C40—C48—C47 | −178.3 (7) |
O8ii—Dy2—N3—C48 | −145.3 (5) | C41—C40—C48—C47 | 4.5 (11) |
O11—Dy2—N3—C48 | 33.0 (6) | N4—C47—C48—N3 | −4.6 (11) |
O7—Dy2—N3—C48 | 83.4 (5) | C43—C47—C48—N3 | 178.2 (7) |
O9—Dy2—N3—C48 | −110.9 (5) | N4—C47—C48—C40 | 176.2 (7) |
O10—Dy2—N3—C48 | −65.1 (5) | C43—C47—C48—C40 | −0.9 (11) |
N4—Dy2—N3—C48 | −1.5 (5) | Dy2—O7—C49—O8 | 39.6 (11) |
C57—Dy2—N3—C48 | −89.2 (5) | Dy2—O7—C49—C50 | −139.5 (5) |
O12ii—Dy2—N4—C46 | 154.5 (6) | Dy2ii—O8—C49—O7 | −6.9 (12) |
O8ii—Dy2—N4—C46 | −29.1 (8) | Dy2ii—O8—C49—C50 | 172.2 (5) |
O11—Dy2—N4—C46 | 24.9 (6) | O7—C49—C50—C51 | −172.8 (7) |
O7—Dy2—N4—C46 | 104.3 (6) | O8—C49—C50—C51 | 8.0 (11) |
O9—Dy2—N4—C46 | −114.4 (6) | O7—C49—C50—C55 | 9.4 (10) |
O10—Dy2—N4—C46 | −67.5 (6) | O8—C49—C50—C55 | −169.8 (7) |
N3—Dy2—N4—C46 | 178.8 (7) | C55—C50—C51—C52 | 0.7 (12) |
C57—Dy2—N4—C46 | −89.5 (6) | C49—C50—C51—C52 | −177.2 (7) |
O12ii—Dy2—N4—C47 | −25.3 (7) | C50—C51—C52—C53 | 1.3 (14) |
O8ii—Dy2—N4—C47 | 151.1 (5) | C51—C52—C53—C54 | −1.4 (14) |
O11—Dy2—N4—C47 | −154.9 (6) | C51—C52—C53—C56 | 178.3 (8) |
O7—Dy2—N4—C47 | −75.5 (6) | C52—C53—C54—C55 | −0.3 (14) |
O9—Dy2—N4—C47 | 65.8 (6) | C56—C53—C54—C55 | 179.9 (8) |
O10—Dy2—N4—C47 | 112.7 (6) | C53—C54—C55—C50 | 2.3 (13) |
N3—Dy2—N4—C47 | −1.0 (5) | C51—C50—C55—C54 | −2.4 (12) |
C57—Dy2—N4—C47 | 90.7 (6) | C49—C50—C55—C54 | 175.5 (7) |
C12—N1—C1—C2 | −1.6 (11) | Dy2—O10—C57—O9 | 11.9 (7) |
Dy1—N1—C1—C2 | 171.2 (6) | Dy2—O10—C57—C58 | −168.8 (6) |
N1—C1—C2—C3 | −1.5 (12) | Dy2—O9—C57—O10 | −12.2 (7) |
C1—C2—C3—C4 | 1.8 (12) | Dy2—O9—C57—C58 | 168.5 (6) |
C2—C3—C4—C12 | 0.8 (11) | O12ii—Dy2—C57—O10 | −161.7 (4) |
C2—C3—C4—C5 | 178.4 (8) | O8ii—Dy2—C57—O10 | −90.1 (4) |
C3—C4—C5—C6 | −173.7 (9) | O11—Dy2—C57—O10 | −19.6 (5) |
C12—C4—C5—C6 | 3.8 (13) | O7—Dy2—C57—O10 | 95.9 (7) |
C4—C5—C6—C7 | 0.6 (15) | O9—Dy2—C57—O10 | 168.0 (7) |
C5—C6—C7—C8 | 174.8 (9) | N3—Dy2—C57—O10 | 116.7 (4) |
C5—C6—C7—C11 | −3.9 (13) | N4—Dy2—C57—O10 | 53.3 (4) |
C11—C7—C8—C9 | −0.4 (13) | O12ii—Dy2—C57—O9 | 30.3 (4) |
C6—C7—C8—C9 | −179.1 (9) | O8ii—Dy2—C57—O9 | 101.9 (4) |
C7—C8—C9—C10 | −0.2 (14) | O11—Dy2—C57—O9 | 172.3 (4) |
C11—N2—C10—C9 | 0.6 (12) | O7—Dy2—C57—O9 | −72.1 (7) |
Dy1—N2—C10—C9 | −166.4 (7) | O10—Dy2—C57—O9 | −168.0 (7) |
C8—C9—C10—N2 | 0.1 (14) | N3—Dy2—C57—O9 | −51.3 (4) |
C10—N2—C11—C7 | −1.2 (10) | N4—Dy2—C57—O9 | −114.7 (4) |
Dy1—N2—C11—C7 | 166.9 (5) | O12ii—Dy2—C57—C58 | −49 (3) |
C10—N2—C11—C12 | 175.8 (7) | O8ii—Dy2—C57—C58 | 23 (3) |
Dy1—N2—C11—C12 | −16.0 (8) | O11—Dy2—C57—C58 | 93 (3) |
C8—C7—C11—N2 | 1.1 (11) | O7—Dy2—C57—C58 | −151 (3) |
C6—C7—C11—N2 | 179.9 (7) | O9—Dy2—C57—C58 | −79 (3) |
C8—C7—C11—C12 | −175.9 (7) | O10—Dy2—C57—C58 | 113 (3) |
C6—C7—C11—C12 | 2.9 (11) | N3—Dy2—C57—C58 | −131 (3) |
C1—N1—C12—C4 | 4.4 (10) | N4—Dy2—C57—C58 | 166 (3) |
Dy1—N1—C12—C4 | −168.8 (5) | O10—C57—C58—C59 | −176.9 (7) |
C1—N1—C12—C11 | −172.7 (7) | O9—C57—C58—C59 | 2.4 (11) |
Dy1—N1—C12—C11 | 14.2 (8) | Dy2—C57—C58—C59 | 76 (3) |
C3—C4—C12—N1 | −4.0 (10) | O10—C57—C58—C63 | 1.0 (11) |
C5—C4—C12—N1 | 178.3 (7) | O9—C57—C58—C63 | −179.7 (7) |
C3—C4—C12—C11 | 173.0 (6) | Dy2—C57—C58—C63 | −106 (3) |
C5—C4—C12—C11 | −4.7 (10) | C63—C58—C59—C60 | −0.2 (14) |
N2—C11—C12—N1 | 1.4 (10) | C57—C58—C59—C60 | 177.8 (8) |
C7—C11—C12—N1 | 178.5 (7) | C58—C59—C60—C61 | 0.8 (15) |
N2—C11—C12—C4 | −175.7 (6) | C59—C60—C61—C62 | −1.6 (15) |
C7—C11—C12—C4 | 1.4 (10) | C59—C60—C61—C64 | −177.3 (10) |
Dy1—O2—C13—O1 | −2.7 (8) | C60—C61—C62—C63 | 1.8 (15) |
Dy1—O2—C13—C14 | 176.0 (7) | C64—C61—C62—C63 | 177.5 (9) |
Dy1—O1—C13—O2 | 2.8 (9) | C61—C62—C63—C58 | −1.3 (15) |
Dy1—O1—C13—C14 | −176.0 (6) | C59—C58—C63—C62 | 0.4 (13) |
O5—Dy1—C13—O2 | 127 (4) | C57—C58—C63—C62 | −177.7 (8) |
O6i—Dy1—C13—O2 | 73.0 (5) | Dy2—O11—C65—O12 | 28.8 (9) |
O3—Dy1—C13—O2 | −65.9 (5) | Dy2—O11—C65—C66 | −149.8 (5) |
O1—Dy1—C13—O2 | −177.3 (9) | Dy2ii—O12—C65—O11 | −69 (2) |
O4—Dy1—C13—O2 | −11.1 (5) | Dy2ii—O12—C65—C66 | 109.2 (17) |
N1—Dy1—C13—O2 | 154.8 (5) | O11—C65—C66—C67 | 159.6 (7) |
N2—Dy1—C13—O2 | −139.8 (5) | O12—C65—C66—C67 | −19.1 (10) |
C21—Dy1—C13—O2 | −38.5 (5) | O11—C65—C66—C71 | −17.3 (10) |
O5—Dy1—C13—O1 | −56 (5) | O12—C65—C66—C71 | 164.0 (6) |
O6i—Dy1—C13—O1 | −109.7 (5) | C71—C66—C67—C68 | −1.7 (13) |
O3—Dy1—C13—O1 | 111.4 (5) | C65—C66—C67—C68 | −178.6 (8) |
O4—Dy1—C13—O1 | 166.2 (5) | C66—C67—C68—C69 | −0.1 (15) |
O2—Dy1—C13—O1 | 177.3 (9) | C67—C68—C69—C70 | 1.7 (16) |
N1—Dy1—C13—O1 | −27.9 (5) | C67—C68—C69—C72 | −177.8 (10) |
N2—Dy1—C13—O1 | 37.5 (5) | C68—C69—C70—C71 | −1.4 (16) |
C21—Dy1—C13—O1 | 138.8 (5) | C72—C69—C70—C71 | 178.1 (9) |
O5—Dy1—C13—C14 | −8 (11) | C69—C70—C71—C66 | −0.5 (14) |
O6i—Dy1—C13—C14 | −61 (8) | C67—C66—C71—C70 | 2.0 (12) |
O3—Dy1—C13—C14 | 160 (8) | C65—C66—C71—C70 | 179.0 (7) |
O1—Dy1—C13—C14 | 48 (7) |
Symmetry codes: (i) −x+1, −y+1, −z+1; (ii) −x+1, −y+1, −z. |
Experimental details
Crystal data | |
Chemical formula | [Dy2(C8H7O2)6(C12H8N2)2] |
Mr | 1496.22 |
Crystal system, space group | Triclinic, P1 |
Temperature (K) | 293 |
a, b, c (Å) | 12.760 (8), 13.346 (9), 19.758 (13) |
α, β, γ (°) | 91.619 (12), 97.925 (11), 106.44 (1) |
V (Å3) | 3188 (4) |
Z | 2 |
Radiation type | Mo Kα |
µ (mm−1) | 2.39 |
Crystal size (mm) | 0.22 × 0.18 × 0.12 |
Data collection | |
Diffractometer | Bruker SMART CCD area-detector diffractometer |
Absorption correction | Multi-scan (SADABS; Sheldrick, 1996) |
Tmin, Tmax | 0.541, 0.750 |
No. of measured, independent and observed [I > 2σ(I)] reflections | 16586, 11165, 7695 |
Rint | 0.033 |
(sin θ/λ)max (Å−1) | 0.595 |
Refinement | |
R[F2 > 2σ(F2)], wR(F2), S | 0.043, 0.121, 1.11 |
No. of reflections | 11165 |
No. of parameters | 811 |
No. of restraints | 18 |
H-atom treatment | H-atom parameters constrained |
Δρmax, Δρmin (e Å−3) | 0.86, −0.96 |
Computer programs: SMART (Bruker, 1997), SMART, SAINT (Bruker, 1997), SHELXS97 (Sheldrick, 1990), SHELXL97 (Sheldrick, 1997), SHELXTL (Bruker, 1998), SHELXTL.
Lanthanide carboxylate complexes containing 1,10-phenanthroline (phen) or 2,2'-bipyridine (2,2'-bipy) have been widely studied. Complexes of this type display a variety of structural types, with high stability and intense fluorescence. We have synthesized the title novel complex, [Dy(4—CH3C6H4COO)3.phen]2, (I), using 4-methylbenzoic acid and 1,10-phenanthroline (phen) as ligands with dysprosium(III) via a conventional solution reaction method. Two kinds of constitution exist in the complex. Here, we report the crystal structure of (I).
The structure of (I) contains two independent centrosymmtric dimers (Fig. 1), unlike lanthanide complexes of 4-methylbenzoic acid, such as the one-dimensional polymer Eu(4—CH3C6H4COO)3 (Jin et al., 2001), but similar to the binuclear complex Sm2(C8H7O2)6·(C10H8N2)2 (C10H8N2 is 2,2'-bipyridine; Li & Zou, 2003).
Each Dy1 ion is coordinated by two O atoms from two bridging 4-methylbenzoate groups, four O atoms from two chelating 4-methylbenzoate groups and two N atoms from one 1,10-phenanthroline (Fig. 1a), and each Dy2 ion is coordinated by four O atoms from four bridging 4-methylbenzoate groups, two O atoms from one chelating 4-methylbenzoate group and two N atoms from one 1,10-phenanthroline (Fig. 1b). The coordination number of each type of Dy ion is 8, but their coordination environments are different. The coordinated polyhedron of Dy1 is an irregular dodecahedron (Fig. 2a), while that of Dy2 is a square antiprism (Fig. 2 b).
Two carboxylate groups rarely link to the same central ion in chelating coordination mode. The complex containing Dy2, however, is typical of lanthanide carboxylate complexes. For example, Sm2(C8H7O2)6·(C10H8N2)2, [Eu(3—CH3C6H4COO)3.phen](H2O) (Jin et al., 1993) and Eu2(3,4-DMBA)6.(phen)2 (3,4-DMBA is 3,4-dimethylbenzoate; Wang et al., 1999) are of this type.
The Dy1—O distances in (I) range from 2.256 (5) to 2.433 (5) Å, with an average of 2.278 (5) Å. The Dy1—N distances are 2.529 (6) and 2.547 (6) Å, and the distance between two Dy ions is 5.305%A. The Dy2—O distances range from 2.276 (5) to 2.471 (5) Å, with an average of 2.3555 Å. The Dy2—N distances are 2.576 (6) and 2.579 (6) Å, and the distance between the two Dy ions is 4.200 Å.
The Dy—O or Dy—N distances involving Dy1 and Dy2 differ only slightly between the two metal sites, but the Dy—Dy distances are significantly different. The Dy1—Dy1 distance is longer than Dy2—Dy2 because of the different numbers of bridging ligands. The molecular structure and coordination environment of the title complex are quite similar to that observed for the dimer Eu(4—CH3C6H4COO)3.phen (Jin et al., 1994).