metal-organic compounds
A salen-type trinuclear Zn2Gd complex
aKey Laboratory of Functional Inorganic Material Chemistry (HLJU), Ministry of Education, School of Chemistry and Materials Science, Heilongjiang University, Harbin 150080, People's Republic of China
*Correspondence e-mail: sunwbchem@gmail.com
In the trinuclear title complex, di-μ-acetato-1:2κ2O:O′;2:3κ2O:O′-bis{μ-6,6′-dimethoxy-2,2′-[cyclohexane-1,2-diylbis(methanylylidene)]diphenolato}-1:2κ6O1,N,N′,O1′:O6,O6′;2:3κ6O6,O6′:O1,N,N′,O1′-2-gadolinium(III)-1,3-dizinc hexafluoridophosphate methanol monosolvate monohydrate, [GdZn2(C22H24N2O4)2(CH3COO)2]PF6·CH3OH·H2O, the two ZnII ions are located in the inner N2O2 cavities of two 6,6′-dimethoxy-2,2′-[cyclohexane-1,2-diylbis(methanylylidene)]diphenolate (L) ligands. Both ZnII ions are five-coordinated by two O atoms and two N atoms from the L ligand and one O atom of an acetic acid molecule, giving rise to a square-pyramidal geometry around the ZnII ions. The GdIII ion is nine-coordinated by four O atoms from the outer O2O2 sites of one ligand, and three O atoms from another ligand, in which there is one non-coordinating methoxy O atom. Two further O atom from different acetate ligands complete the nine-coordinate environment.
Related literature
For crystal structures of similar trinuclear complexes of salen-type Schiff base ligands, see: Wong et al. (2006); Wang et al. (2009).
Experimental
Crystal data
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Data collection: RAPID-AUTO (Rigaku, 1998); cell RAPID-AUTO; data reduction: CrystalStructure (Rigaku/MSC, 2002); program(s) used to solve structure: SHELXS97 (Sheldrick, 2008); program(s) used to refine structure: SHELXL97 (Sheldrick, 2008); molecular graphics: SHELXTL (Sheldrick, 2008); software used to prepare material for publication: SHELXTL.
Supporting information
10.1107/S160053681204634X/pv2601sup1.cif
contains datablocks I, global. DOI:Structure factors: contains datablock I. DOI: 10.1107/S160053681204634X/pv2601Isup2.hkl
To a 1:1 MeOH/CH2Cl2 solution (20 ml) of the Schiff ligand (L) (0.386 g, 1.0 mmol) was slowly added a solid [Dy(acac)3H2O; acac = acetylacetone] (0.491 g, 1.0 mmol), after stirring for 10 minutes solid [Zn(CH3COO)2H2O] (0.220 g, 1.0 mmol) and NH4PF6 (0.164 g, 1.0 mmol) were added after refluxing and stirring for 1 h, at ambient temperature. After stirring for 5 h, the title complex as yellow solid was collected by filtration and was washed with MeOH; yield = 0.952 g (68%). Single crystals suitable for X-ray determination were obtained by slow diffusion of diethylether into a methanol solution of the powder sample over one week.
H atoms bound to C atoms were placed in calculated positions and treated as riding on their parent atoms, with C—H = 0.93, 0.96, 0.97 and 0.98 Å, for aryl, methyl, methylene and methyne H-atoms, respectively. The Uiso(H) were allowed at 1.5Ueq(C methyl) or 1.2Ueq(C non-methyl). The hydroxyl and water H-atoms were located from a difference map and were included in the
with O—H = 0.85 Å and Uiso(H) = 1.2Ueq(hydroxy O) or 1.5Ueq(water O). The command 'ISOR 0.01 013 014 c72' was used to restrain the ADPs and the distance between O13 and C72 was restrain at 1.50(0.01) Å.Data collection: RAPID-AUTO (Rigaku, 1998); cell
RAPID-AUTO (Rigaku, 1998); data reduction: CrystalStructure (Rigaku/MSC, 2002); program(s) used to solve structure: SHELXS97 (Sheldrick, 2008); program(s) used to refine structure: SHELXL97 (Sheldrick, 2008); molecular graphics: SHELXTL (Sheldrick, 2008); software used to prepare material for publication: SHELXTL (Sheldrick, 2008).Fig. 1. The molecular structure of the title compound showing the atomic numbering and 30% probability displacement ellipsoids. |
[GdZn2(C22H24N2O4)2(C2H3O2)2]PF6·CH4O·H2O | F(000) = 2748 |
Mr = 1361.97 | Dx = 1.644 Mg m−3 |
Monoclinic, P21/n | Mo Kα radiation, λ = 0.71073 Å |
Hall symbol: -p 2yn | Cell parameters from 25271 reflections |
a = 15.8127 (12) Å | θ = 3.0–27.5° |
b = 20.6405 (16) Å | µ = 2.17 mm−1 |
c = 18.5036 (14) Å | T = 296 K |
β = 114.369 (1)° | Prism, yellow |
V = 5501.2 (7) Å3 | 0.20 × 0.18 × 0.16 mm |
Z = 4 |
Rigaku R-AXIS RAPID diffractometer | 13701 independent reflections |
Radiation source: fine-focus sealed tube | 6858 reflections with I > 2σ(I) |
Graphite monochromator | Rint = 0.066 |
Detector resolution: 10.000 pixels mm-1 | θmax = 28.4°, θmin = 1.4° |
ω scans | h = −21→21 |
Absorption correction: multi-scan (ABSCOR; Higashi, 1995) | k = −27→27 |
Tmin = 0.671, Tmax = 0.723 | l = −24→15 |
39974 measured reflections |
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)] = 0.053 | Hydrogen site location: inferred from neighbouring sites |
wR(F2) = 0.157 | H-atom parameters constrained |
S = 0.98 | w = 1/[σ2(Fo2) + (0.0722P)2] where P = (Fo2 + 2Fc2)/3 |
13701 reflections | (Δ/σ)max = 0.002 |
695 parameters | Δρmax = 1.02 e Å−3 |
19 restraints | Δρmin = −0.71 e Å−3 |
[GdZn2(C22H24N2O4)2(C2H3O2)2]PF6·CH4O·H2O | V = 5501.2 (7) Å3 |
Mr = 1361.97 | Z = 4 |
Monoclinic, P21/n | Mo Kα radiation |
a = 15.8127 (12) Å | µ = 2.17 mm−1 |
b = 20.6405 (16) Å | T = 296 K |
c = 18.5036 (14) Å | 0.20 × 0.18 × 0.16 mm |
β = 114.369 (1)° |
Rigaku R-AXIS RAPID diffractometer | 13701 independent reflections |
Absorption correction: multi-scan (ABSCOR; Higashi, 1995) | 6858 reflections with I > 2σ(I) |
Tmin = 0.671, Tmax = 0.723 | Rint = 0.066 |
39974 measured reflections |
R[F2 > 2σ(F2)] = 0.053 | 19 restraints |
wR(F2) = 0.157 | H-atom parameters constrained |
S = 0.98 | Δρmax = 1.02 e Å−3 |
13701 reflections | Δρmin = −0.71 e Å−3 |
695 parameters |
Experimental. Analysis calculated for C49H60Cl0F6GdN4O14PZn2: C, 42.11; H, 4.33; N, 4.01; found: C, 42.01; H, 4.20; N, 3.93%. |
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 | ||
C15 | 0.8093 (5) | 0.5417 (3) | 0.8460 (4) | 0.0542 (15) | |
C17 | 1.0251 (4) | 0.5705 (3) | 0.6400 (4) | 0.0572 (16) | |
C19 | 0.5217 (4) | 0.3534 (3) | 0.6962 (4) | 0.0623 (17) | |
C20 | 0.9052 (5) | 0.5368 (3) | 0.8676 (4) | 0.0579 (16) | |
C21 | 0.9314 (4) | 0.3318 (3) | 0.7457 (4) | 0.0562 (16) | |
C22 | 0.6815 (6) | 0.5833 (3) | 0.8827 (5) | 0.072 (2) | |
H22A | 0.6689 | 0.6055 | 0.9209 | 0.086* | |
C23 | 1.0793 (5) | 0.5207 (3) | 0.6260 (4) | 0.0678 (19) | |
H23A | 1.1348 | 0.5343 | 0.6249 | 0.081* | |
C24 | 0.9029 (4) | 0.6117 (3) | 0.6749 (4) | 0.0566 (16) | |
C25 | 0.9460 (4) | 0.5589 (3) | 0.6535 (4) | 0.0511 (15) | |
C26 | 0.4880 (4) | 0.3973 (4) | 0.7390 (4) | 0.0695 (19) | |
H26A | 0.4456 | 0.3807 | 0.7572 | 0.083* | |
C27 | 0.4768 (6) | 0.4935 (4) | 0.8043 (6) | 0.091 (3) | |
H27A | 0.5041 | 0.4747 | 0.8577 | 0.110* | |
C28 | 0.5987 (4) | 0.3649 (3) | 0.6782 (4) | 0.0534 (15) | |
C29 | 0.9993 (5) | 0.2873 (3) | 0.7438 (4) | 0.0678 (19) | |
C30 | 0.5880 (4) | 0.5536 (3) | 0.5878 (4) | 0.0557 (16) | |
C31 | 0.4745 (5) | 0.2935 (3) | 0.6750 (5) | 0.075 (2) | |
H31A | 0.4245 | 0.2855 | 0.6878 | 0.091* | |
C32 | 1.0496 (5) | 0.2956 (3) | 0.6943 (5) | 0.077 (2) | |
H32A | 1.0969 | 0.2661 | 0.7013 | 0.092* | |
C33 | 1.0239 (5) | 0.4909 (4) | 0.8334 (4) | 0.080 (2) | |
H33A | 1.0610 | 0.5090 | 0.8846 | 0.119* | |
H33B | 1.0375 | 0.5128 | 0.7937 | 0.119* | |
H33C | 1.0376 | 0.4456 | 0.8333 | 0.119* | |
C34 | 0.8923 (4) | 0.3213 (3) | 0.8004 (4) | 0.0589 (16) | |
C35 | 1.1788 (5) | 0.4331 (4) | 0.5599 (5) | 0.079 (2) | |
H35A | 1.1320 | 0.4382 | 0.5062 | 0.094* | |
H35B | 1.2102 | 0.4743 | 0.5769 | 0.094* | |
C36 | 0.7696 (4) | 0.4078 (3) | 0.4995 (4) | 0.0546 (16) | |
C37 | 0.7737 (5) | 0.6472 (3) | 0.6979 (5) | 0.077 (2) | |
H37A | 0.8047 | 0.6874 | 0.6987 | 0.116* | |
H37B | 0.7660 | 0.6425 | 0.7464 | 0.116* | |
H37C | 0.7140 | 0.6471 | 0.6539 | 0.116* | |
C38 | 0.8443 (6) | 0.6068 (3) | 0.9634 (4) | 0.075 (2) | |
H38A | 0.8246 | 0.6299 | 0.9968 | 0.091* | |
C39 | 0.5368 (5) | 0.5861 (3) | 0.5091 (4) | 0.075 (2) | |
H39A | 0.4794 | 0.6035 | 0.5068 | 0.112* | |
H39B | 0.5239 | 0.5551 | 0.4673 | 0.112* | |
H39C | 0.5741 | 0.6205 | 0.5030 | 0.112* | |
C40 | 0.5009 (5) | 0.2480 (4) | 0.6365 (5) | 0.083 (2) | |
H40A | 0.4661 | 0.2103 | 0.6196 | 0.099* | |
C41 | 1.0587 (5) | 0.6350 (4) | 0.6450 (5) | 0.086 (2) | |
H41A | 1.1123 | 0.6430 | 0.6373 | 0.104* | |
C42 | 0.7775 (5) | 0.5773 (3) | 0.8950 (4) | 0.0636 (18) | |
C43 | 0.7891 (5) | 0.3628 (4) | 0.8530 (4) | 0.083 (2) | |
H43A | 0.8171 | 0.3272 | 0.8883 | 0.124* | |
H43B | 0.7239 | 0.3547 | 0.8242 | 0.124* | |
H43C | 0.7978 | 0.4020 | 0.8832 | 0.124* | |
C44 | 0.9681 (5) | 0.5663 (3) | 0.9334 (4) | 0.0710 (19) | |
H44A | 1.0313 | 0.5628 | 0.9465 | 0.085* | |
C45 | 0.5130 (6) | 0.5643 (4) | 0.8099 (6) | 0.092 (3) | |
H45A | 0.4799 | 0.5833 | 0.7571 | 0.110* | |
C46 | 0.9355 (6) | 0.6026 (3) | 0.9818 (4) | 0.078 (2) | |
H46A | 0.9777 | 0.6236 | 1.0266 | 0.093* | |
C47 | 1.0930 (5) | 0.3472 (4) | 0.5980 (5) | 0.082 (2) | |
H47A | 1.0493 | 0.3471 | 0.5420 | 0.098* | |
C48 | 1.1323 (5) | 0.4146 (4) | 0.6139 (5) | 0.080 (2) | |
H48A | 1.1814 | 0.4141 | 0.6678 | 0.096* | |
C49 | 0.6957 (5) | 0.3883 (4) | 0.4187 (4) | 0.086 (2) | |
H49A | 0.6352 | 0.3957 | 0.4176 | 0.130* | |
H49B | 0.7025 | 0.3432 | 0.4095 | 0.130* | |
H49C | 0.7027 | 0.4137 | 0.3781 | 0.130* | |
C50 | 0.9808 (6) | 0.2245 (4) | 0.8471 (6) | 0.104 (3) | |
H50A | 0.9973 | 0.1887 | 0.8805 | 0.125* | |
C51 | 0.6292 (4) | 0.3143 (3) | 0.6436 (4) | 0.0580 (16) | |
C52 | 0.9369 (5) | 0.6744 (4) | 0.6782 (5) | 0.085 (2) | |
H52A | 0.9084 | 0.7088 | 0.6918 | 0.102* | |
C53 | 0.9153 (5) | 0.2685 (3) | 0.8499 (5) | 0.081 (2) | |
H53A | 0.8876 | 0.2621 | 0.8849 | 0.097* | |
C54 | 0.7392 (5) | 0.2789 (3) | 0.5959 (5) | 0.084 (2) | |
H54A | 0.7950 | 0.2935 | 0.5924 | 0.126* | |
H54B | 0.6924 | 0.2708 | 0.5436 | 0.126* | |
H54C | 0.7517 | 0.2397 | 0.6265 | 0.126* | |
C55 | 1.2101 (6) | 0.3149 (5) | 0.5481 (6) | 0.116 (3) | |
H55A | 1.2603 | 0.2847 | 0.5565 | 0.139* | |
H55B | 1.1648 | 0.3102 | 0.4937 | 0.139* | |
C56 | 1.2477 (6) | 0.3828 (5) | 0.5607 (7) | 0.113 (3) | |
H56A | 1.3013 | 0.3849 | 0.6112 | 0.136* | |
H56B | 1.2685 | 0.3931 | 0.5195 | 0.136* | |
C57 | 1.0206 (5) | 0.2342 (4) | 0.7947 (5) | 0.090 (3) | |
H57A | 1.0636 | 0.2042 | 0.7932 | 0.109* | |
C58 | 1.1641 (5) | 0.2978 (4) | 0.6045 (5) | 0.093 (3) | |
H58A | 1.1351 | 0.2555 | 0.5910 | 0.112* | |
H58B | 1.2108 | 0.2962 | 0.6587 | 0.112* | |
C59 | 0.5801 (5) | 0.2566 (3) | 0.6215 (4) | 0.073 (2) | |
H59A | 0.5996 | 0.2240 | 0.5972 | 0.088* | |
C60 | 1.0131 (6) | 0.6856 (3) | 0.6612 (5) | 0.091 (3) | |
H60A | 1.0335 | 0.7278 | 0.6607 | 0.109* | |
C64 | 0.3833 (7) | 0.6040 (5) | 0.8373 (7) | 0.132 (4) | |
H64A | 0.3552 | 0.6268 | 0.7871 | 0.159* | |
H64B | 0.3672 | 0.6272 | 0.8755 | 0.159* | |
C68 | 0.3431 (8) | 0.5361 (5) | 0.8271 (8) | 0.143 (5) | |
H68A | 0.3623 | 0.5160 | 0.8788 | 0.172* | |
H68B | 0.2759 | 0.5388 | 0.8035 | 0.172* | |
C69 | 0.3723 (6) | 0.4957 (5) | 0.7776 (6) | 0.112 (3) | |
H69A | 0.3441 | 0.5117 | 0.7236 | 0.135* | |
H69B | 0.3498 | 0.4520 | 0.7776 | 0.135* | |
C71 | 0.4879 (6) | 0.6046 (5) | 0.8652 (6) | 0.110 (3) | |
H71A | 0.5095 | 0.6487 | 0.8660 | 0.132* | |
H71B | 0.5173 | 0.5872 | 0.9186 | 0.132* | |
C72 | 0.2937 (6) | 0.1233 (5) | 0.5715 (7) | 0.134 (4) | |
H72A | 0.2939 | 0.1166 | 0.6229 | 0.200* | |
H72B | 0.2667 | 0.1647 | 0.5512 | 0.200* | |
H72C | 0.3563 | 0.1221 | 0.5758 | 0.200* | |
F1 | 0.2731 (10) | 0.3061 (4) | 0.9481 (7) | 0.301 (7) | |
F2 | 0.3984 (7) | 0.2862 (6) | 0.9409 (6) | 0.267 (5) | |
F3 | 0.2290 (6) | 0.3579 (4) | 0.8329 (7) | 0.266 (6) | |
F4 | 0.3428 (7) | 0.3875 (4) | 0.9315 (5) | 0.233 (4) | |
F5 | 0.3559 (9) | 0.3351 (5) | 0.8342 (7) | 0.267 (6) | |
F6 | 0.2767 (6) | 0.2580 (4) | 0.8468 (5) | 0.202 (3) | |
Gd1 | 0.78621 (2) | 0.458889 (15) | 0.683056 (19) | 0.05067 (11) | |
N1 | 0.6122 (4) | 0.5603 (3) | 0.8230 (4) | 0.0769 (17) | |
N2 | 0.5107 (4) | 0.4567 (3) | 0.7546 (4) | 0.0702 (16) | |
N3 | 1.0625 (3) | 0.4607 (2) | 0.6149 (3) | 0.0592 (13) | |
N4 | 1.0354 (4) | 0.3387 (3) | 0.6428 (4) | 0.0648 (15) | |
O1 | 0.7533 (3) | 0.5113 (2) | 0.7804 (3) | 0.0581 (11) | |
O2 | 0.6459 (3) | 0.42001 (19) | 0.6928 (3) | 0.0596 (11) | |
O3 | 0.9274 (3) | 0.4990 (2) | 0.8165 (3) | 0.0650 (12) | |
O4 | 0.7073 (3) | 0.3274 (2) | 0.6334 (3) | 0.0687 (12) | |
O5 | 0.9064 (3) | 0.50117 (18) | 0.6495 (2) | 0.0510 (10) | |
O6 | 0.9029 (3) | 0.38335 (19) | 0.6990 (2) | 0.0566 (10) | |
O7 | 0.8278 (3) | 0.59487 (19) | 0.6900 (3) | 0.0623 (11) | |
O8 | 0.8311 (3) | 0.3694 (2) | 0.7990 (3) | 0.0659 (12) | |
O9 | 0.5511 (3) | 0.5546 (2) | 0.6358 (3) | 0.0659 (12) | |
O10 | 0.6651 (3) | 0.5276 (2) | 0.6023 (3) | 0.0599 (11) | |
O11 | 0.7443 (3) | 0.4268 (2) | 0.5507 (3) | 0.0613 (11) | |
O12 | 0.8534 (3) | 0.4006 (2) | 0.5098 (3) | 0.0630 (12) | |
O13 | 0.2345 (9) | 0.0677 (6) | 0.5128 (7) | 0.257 (5) | |
H131 | 0.1778 | 0.0631 | 0.4813 | 0.386* | |
O14 | 0.1290 (6) | 0.1453 (5) | 0.4517 (6) | 0.217 (4) | |
H142 | 0.1215 | 0.1713 | 0.4139 | 0.325* | |
H141 | 0.0880 | 0.1261 | 0.4623 | 0.325* | |
P1 | 0.3108 (2) | 0.32265 (15) | 0.88998 (18) | 0.1102 (8) | |
Zn2 | 0.94810 (4) | 0.41679 (3) | 0.61748 (4) | 0.05187 (19) | |
Zn3 | 0.61201 (5) | 0.50326 (4) | 0.73265 (5) | 0.0604 (2) |
U11 | U22 | U33 | U12 | U13 | U23 | |
C15 | 0.072 (4) | 0.045 (3) | 0.045 (4) | 0.001 (3) | 0.024 (3) | 0.000 (3) |
C17 | 0.061 (4) | 0.052 (4) | 0.062 (4) | −0.007 (3) | 0.029 (3) | 0.000 (3) |
C19 | 0.059 (4) | 0.058 (4) | 0.066 (5) | −0.003 (3) | 0.022 (4) | 0.010 (3) |
C20 | 0.073 (4) | 0.048 (3) | 0.049 (4) | 0.001 (3) | 0.020 (4) | 0.006 (3) |
C21 | 0.059 (4) | 0.047 (3) | 0.057 (4) | −0.004 (3) | 0.019 (3) | 0.004 (3) |
C22 | 0.101 (6) | 0.062 (4) | 0.076 (5) | −0.004 (4) | 0.061 (5) | −0.009 (4) |
C23 | 0.060 (4) | 0.068 (5) | 0.081 (5) | −0.014 (3) | 0.034 (4) | 0.001 (4) |
C24 | 0.065 (4) | 0.046 (3) | 0.061 (4) | −0.005 (3) | 0.028 (3) | 0.001 (3) |
C25 | 0.056 (3) | 0.047 (3) | 0.044 (4) | −0.011 (3) | 0.014 (3) | 0.004 (3) |
C26 | 0.061 (4) | 0.070 (5) | 0.087 (5) | −0.009 (4) | 0.040 (4) | 0.009 (4) |
C27 | 0.105 (6) | 0.070 (5) | 0.133 (8) | −0.005 (4) | 0.083 (6) | −0.009 (5) |
C28 | 0.045 (3) | 0.057 (4) | 0.052 (4) | −0.005 (3) | 0.013 (3) | 0.003 (3) |
C29 | 0.067 (4) | 0.049 (4) | 0.087 (5) | 0.012 (3) | 0.032 (4) | 0.014 (4) |
C30 | 0.054 (4) | 0.047 (4) | 0.065 (4) | −0.004 (3) | 0.023 (3) | −0.004 (3) |
C31 | 0.065 (4) | 0.062 (4) | 0.101 (6) | −0.008 (4) | 0.035 (4) | 0.010 (4) |
C32 | 0.059 (4) | 0.063 (4) | 0.117 (7) | 0.016 (3) | 0.044 (5) | 0.016 (5) |
C33 | 0.063 (4) | 0.106 (6) | 0.063 (5) | 0.002 (4) | 0.019 (4) | 0.005 (5) |
C34 | 0.060 (4) | 0.050 (4) | 0.060 (4) | −0.001 (3) | 0.019 (3) | 0.010 (3) |
C35 | 0.056 (4) | 0.097 (5) | 0.094 (6) | 0.005 (4) | 0.041 (4) | 0.013 (5) |
C36 | 0.055 (4) | 0.048 (3) | 0.056 (4) | −0.010 (3) | 0.017 (3) | −0.004 (3) |
C37 | 0.081 (5) | 0.065 (4) | 0.094 (6) | 0.001 (4) | 0.044 (5) | −0.009 (4) |
C38 | 0.112 (6) | 0.061 (4) | 0.056 (5) | 0.000 (4) | 0.038 (5) | −0.001 (4) |
C39 | 0.069 (4) | 0.079 (5) | 0.077 (5) | 0.013 (4) | 0.031 (4) | 0.011 (4) |
C40 | 0.073 (5) | 0.059 (4) | 0.108 (7) | −0.019 (4) | 0.029 (5) | 0.000 (5) |
C41 | 0.092 (5) | 0.078 (5) | 0.108 (7) | −0.030 (4) | 0.060 (5) | −0.014 (5) |
C42 | 0.092 (5) | 0.044 (4) | 0.052 (4) | −0.004 (3) | 0.027 (4) | −0.003 (3) |
C43 | 0.088 (5) | 0.095 (6) | 0.076 (5) | 0.006 (4) | 0.046 (5) | 0.016 (5) |
C44 | 0.069 (4) | 0.063 (4) | 0.067 (5) | −0.001 (4) | 0.014 (4) | 0.007 (4) |
C45 | 0.087 (5) | 0.102 (6) | 0.120 (7) | −0.010 (5) | 0.075 (6) | −0.022 (6) |
C46 | 0.095 (6) | 0.064 (5) | 0.056 (5) | −0.014 (4) | 0.013 (4) | −0.007 (4) |
C47 | 0.078 (5) | 0.071 (5) | 0.117 (7) | 0.010 (4) | 0.061 (5) | 0.003 (5) |
C48 | 0.076 (5) | 0.078 (5) | 0.108 (6) | 0.009 (4) | 0.061 (5) | 0.006 (5) |
C49 | 0.064 (4) | 0.127 (7) | 0.060 (5) | −0.018 (4) | 0.016 (4) | −0.023 (5) |
C50 | 0.101 (6) | 0.084 (6) | 0.140 (8) | 0.034 (5) | 0.061 (6) | 0.068 (6) |
C51 | 0.059 (4) | 0.052 (4) | 0.060 (4) | 0.000 (3) | 0.021 (3) | −0.003 (3) |
C52 | 0.096 (6) | 0.057 (4) | 0.106 (7) | −0.011 (4) | 0.047 (5) | −0.018 (4) |
C53 | 0.084 (5) | 0.066 (5) | 0.094 (6) | −0.011 (4) | 0.039 (5) | 0.016 (4) |
C54 | 0.091 (5) | 0.061 (4) | 0.110 (7) | −0.004 (4) | 0.051 (5) | −0.023 (4) |
C55 | 0.089 (6) | 0.142 (9) | 0.137 (9) | 0.024 (6) | 0.066 (6) | −0.006 (7) |
C56 | 0.100 (6) | 0.117 (8) | 0.150 (9) | 0.018 (6) | 0.079 (7) | 0.015 (7) |
C57 | 0.089 (5) | 0.068 (5) | 0.125 (7) | 0.029 (4) | 0.054 (6) | 0.040 (5) |
C58 | 0.083 (5) | 0.086 (5) | 0.130 (8) | 0.016 (4) | 0.064 (6) | 0.010 (5) |
C59 | 0.068 (4) | 0.058 (4) | 0.084 (5) | −0.010 (3) | 0.023 (4) | 0.000 (4) |
C60 | 0.108 (6) | 0.052 (4) | 0.140 (8) | −0.033 (4) | 0.079 (6) | −0.023 (5) |
C64 | 0.104 (7) | 0.129 (9) | 0.182 (12) | 0.006 (6) | 0.076 (8) | −0.032 (8) |
C68 | 0.132 (9) | 0.125 (9) | 0.213 (14) | −0.020 (7) | 0.113 (10) | −0.027 (9) |
C69 | 0.108 (7) | 0.115 (7) | 0.145 (9) | −0.029 (6) | 0.084 (7) | −0.041 (7) |
C71 | 0.111 (7) | 0.113 (7) | 0.117 (8) | 0.004 (6) | 0.057 (6) | −0.022 (6) |
C72 | 0.083 (5) | 0.135 (7) | 0.198 (9) | −0.013 (5) | 0.073 (6) | 0.013 (7) |
F1 | 0.56 (2) | 0.176 (8) | 0.393 (15) | 0.020 (10) | 0.424 (16) | 0.004 (8) |
F2 | 0.237 (10) | 0.314 (13) | 0.179 (8) | 0.091 (10) | 0.013 (8) | 0.008 (9) |
F3 | 0.206 (8) | 0.193 (9) | 0.272 (12) | 0.078 (7) | −0.030 (8) | −0.040 (8) |
F4 | 0.324 (11) | 0.155 (7) | 0.159 (7) | −0.036 (7) | 0.039 (7) | −0.061 (6) |
F5 | 0.399 (15) | 0.215 (9) | 0.345 (14) | −0.019 (10) | 0.311 (13) | 0.025 (9) |
F6 | 0.254 (9) | 0.143 (6) | 0.236 (9) | −0.032 (6) | 0.127 (8) | −0.059 (6) |
Gd1 | 0.05211 (18) | 0.05026 (18) | 0.0530 (2) | 0.00167 (14) | 0.02512 (15) | −0.00155 (16) |
N1 | 0.087 (4) | 0.070 (4) | 0.089 (5) | −0.010 (3) | 0.051 (4) | −0.020 (4) |
N2 | 0.074 (4) | 0.065 (4) | 0.087 (4) | −0.001 (3) | 0.049 (3) | −0.004 (3) |
N3 | 0.059 (3) | 0.056 (3) | 0.071 (4) | −0.001 (3) | 0.035 (3) | 0.003 (3) |
N4 | 0.061 (3) | 0.055 (3) | 0.088 (4) | 0.010 (3) | 0.041 (3) | 0.015 (3) |
O1 | 0.058 (2) | 0.064 (3) | 0.055 (3) | −0.011 (2) | 0.026 (2) | −0.014 (2) |
O2 | 0.066 (3) | 0.049 (2) | 0.072 (3) | −0.009 (2) | 0.036 (2) | −0.007 (2) |
O3 | 0.062 (3) | 0.071 (3) | 0.061 (3) | −0.001 (2) | 0.024 (2) | −0.001 (3) |
O4 | 0.075 (3) | 0.054 (3) | 0.087 (4) | −0.005 (2) | 0.043 (3) | −0.010 (3) |
O5 | 0.055 (2) | 0.044 (2) | 0.058 (3) | −0.0039 (18) | 0.028 (2) | 0.002 (2) |
O6 | 0.061 (2) | 0.051 (2) | 0.064 (3) | 0.006 (2) | 0.032 (2) | 0.009 (2) |
O7 | 0.066 (3) | 0.049 (2) | 0.080 (3) | 0.004 (2) | 0.037 (2) | 0.000 (2) |
O8 | 0.082 (3) | 0.063 (3) | 0.066 (3) | 0.004 (2) | 0.043 (3) | 0.010 (2) |
O9 | 0.069 (3) | 0.062 (3) | 0.075 (3) | 0.009 (2) | 0.037 (3) | 0.002 (2) |
O10 | 0.056 (2) | 0.057 (3) | 0.066 (3) | 0.006 (2) | 0.025 (2) | 0.002 (2) |
O11 | 0.059 (3) | 0.067 (3) | 0.055 (3) | −0.001 (2) | 0.022 (2) | −0.010 (2) |
O12 | 0.055 (3) | 0.072 (3) | 0.061 (3) | −0.004 (2) | 0.023 (2) | −0.015 (2) |
O13 | 0.309 (9) | 0.271 (9) | 0.243 (9) | −0.026 (8) | 0.165 (8) | 0.022 (7) |
O14 | 0.206 (7) | 0.276 (9) | 0.183 (7) | 0.028 (7) | 0.095 (6) | −0.033 (6) |
P1 | 0.135 (2) | 0.115 (2) | 0.098 (2) | 0.0004 (19) | 0.065 (2) | −0.0109 (18) |
Zn2 | 0.0487 (4) | 0.0502 (4) | 0.0584 (5) | 0.0007 (3) | 0.0239 (4) | 0.0012 (3) |
Zn3 | 0.0629 (5) | 0.0566 (4) | 0.0713 (5) | −0.0020 (4) | 0.0374 (4) | −0.0042 (4) |
C15—O1 | 1.328 (7) | C47—N4 | 1.473 (8) |
C15—C20 | 1.403 (9) | C47—C58 | 1.485 (9) |
C15—C42 | 1.411 (9) | C47—C48 | 1.502 (10) |
C17—C25 | 1.394 (8) | C47—H47A | 0.9800 |
C17—C41 | 1.424 (9) | C48—N3 | 1.464 (8) |
C17—C23 | 1.428 (9) | C48—H48A | 0.9800 |
C19—C28 | 1.410 (8) | C49—H49A | 0.9600 |
C19—C31 | 1.412 (9) | C49—H49B | 0.9600 |
C19—C26 | 1.443 (9) | C49—H49C | 0.9600 |
C20—C44 | 1.358 (9) | C50—C57 | 1.370 (11) |
C20—O3 | 1.379 (7) | C50—C53 | 1.394 (10) |
C21—O6 | 1.326 (7) | C50—H50A | 0.9300 |
C21—C34 | 1.404 (9) | C51—O4 | 1.351 (7) |
C21—C29 | 1.425 (9) | C51—C59 | 1.388 (8) |
C22—N1 | 1.282 (9) | C52—C60 | 1.384 (10) |
C22—C42 | 1.444 (10) | C52—H52A | 0.9300 |
C22—H22A | 0.9300 | C53—H53A | 0.9300 |
C23—N3 | 1.265 (8) | C54—O4 | 1.422 (7) |
C23—H23A | 0.9300 | C54—H54A | 0.9600 |
C24—O7 | 1.371 (7) | C54—H54B | 0.9600 |
C24—C52 | 1.393 (9) | C54—H54C | 0.9600 |
C24—C25 | 1.426 (8) | C55—C56 | 1.503 (12) |
C25—O5 | 1.333 (6) | C55—C58 | 1.539 (11) |
C26—N2 | 1.277 (8) | C55—H55A | 0.9700 |
C26—H26A | 0.9300 | C55—H55B | 0.9700 |
C27—N2 | 1.457 (9) | C56—H56A | 0.9700 |
C27—C69 | 1.517 (11) | C56—H56B | 0.9700 |
C27—C45 | 1.558 (11) | C57—H57A | 0.9300 |
C27—H27A | 0.9800 | C58—H58A | 0.9700 |
C28—O2 | 1.326 (7) | C58—H58B | 0.9700 |
C28—C51 | 1.408 (8) | C59—H59A | 0.9300 |
C29—C57 | 1.393 (9) | C60—H60A | 0.9300 |
C29—C32 | 1.450 (10) | C64—C71 | 1.517 (12) |
C30—O9 | 1.248 (7) | C64—C68 | 1.518 (13) |
C30—O10 | 1.254 (7) | C64—H64A | 0.9700 |
C30—C39 | 1.501 (9) | C64—H64B | 0.9700 |
C31—C40 | 1.345 (10) | C68—C69 | 1.448 (12) |
C31—H31A | 0.9300 | C68—H68A | 0.9700 |
C32—N4 | 1.255 (8) | C68—H68B | 0.9700 |
C32—H32A | 0.9300 | C69—H69A | 0.9700 |
C33—O3 | 1.434 (7) | C69—H69B | 0.9700 |
C33—H33A | 0.9600 | C71—H71A | 0.9700 |
C33—H33B | 0.9600 | C71—H71B | 0.9700 |
C33—H33C | 0.9600 | C72—O13 | 1.592 (8) |
C34—C53 | 1.373 (9) | C72—H72A | 0.9600 |
C34—O8 | 1.379 (7) | C72—H72B | 0.9600 |
C35—C56 | 1.500 (10) | C72—H72C | 0.9600 |
C35—C48 | 1.512 (10) | F1—P1 | 1.469 (8) |
C35—H35A | 0.9700 | F2—P1 | 1.515 (9) |
C35—H35B | 0.9700 | F3—P1 | 1.480 (8) |
C36—O11 | 1.234 (7) | F4—P1 | 1.522 (8) |
C36—O12 | 1.267 (7) | F5—P1 | 1.499 (8) |
C36—C49 | 1.524 (8) | F6—P1 | 1.534 (7) |
C37—O7 | 1.422 (7) | Gd1—O1 | 2.337 (4) |
C37—H37A | 0.9600 | Gd1—O6 | 2.340 (4) |
C37—H37B | 0.9600 | Gd1—O11 | 2.353 (4) |
C37—H37C | 0.9600 | Gd1—O10 | 2.356 (4) |
C38—C46 | 1.341 (10) | Gd1—O5 | 2.394 (4) |
C38—C42 | 1.409 (9) | Gd1—O2 | 2.435 (4) |
C38—H38A | 0.9300 | Gd1—O3 | 2.686 (4) |
C39—H39A | 0.9600 | Gd1—O8 | 2.696 (4) |
C39—H39B | 0.9600 | Gd1—O7 | 2.874 (4) |
C39—H39C | 0.9600 | Gd1—Zn2 | 3.3679 (8) |
C40—C59 | 1.401 (10) | Gd1—Zn3 | 3.3697 (8) |
C40—H40A | 0.9300 | N1—Zn3 | 2.044 (6) |
C41—C60 | 1.369 (10) | N2—Zn3 | 2.046 (6) |
C41—H41A | 0.9300 | N3—Zn2 | 2.041 (5) |
C43—O8 | 1.415 (8) | N4—Zn2 | 2.047 (5) |
C43—H43A | 0.9600 | O1—Zn3 | 2.042 (4) |
C43—H43B | 0.9600 | O2—Zn3 | 2.027 (4) |
C43—H43C | 0.9600 | O5—Zn2 | 2.035 (4) |
C44—C46 | 1.417 (10) | O6—Zn2 | 2.038 (4) |
C44—H44A | 0.9300 | O9—Zn3 | 1.960 (5) |
C45—N1 | 1.488 (9) | O12—Zn2 | 1.965 (4) |
C45—C71 | 1.492 (11) | O13—H131 | 0.8500 |
C45—H45A | 0.9800 | O14—H142 | 0.8500 |
C46—H46A | 0.9300 | O14—H141 | 0.8500 |
O1—C15—C20 | 117.5 (6) | C41—C60—H60A | 119.7 |
O1—C15—C42 | 123.5 (6) | C52—C60—H60A | 119.7 |
C20—C15—C42 | 119.0 (6) | C71—C64—C68 | 113.0 (9) |
C25—C17—C41 | 119.2 (6) | C71—C64—H64A | 109.0 |
C25—C17—C23 | 124.0 (6) | C68—C64—H64A | 109.0 |
C41—C17—C23 | 116.7 (6) | C71—C64—H64B | 109.0 |
C28—C19—C31 | 119.4 (7) | C68—C64—H64B | 109.0 |
C28—C19—C26 | 125.1 (6) | H64A—C64—H64B | 107.8 |
C31—C19—C26 | 115.5 (6) | C69—C68—C64 | 112.6 (9) |
C44—C20—O3 | 124.7 (6) | C69—C68—H68A | 109.1 |
C44—C20—C15 | 121.9 (7) | C64—C68—H68A | 109.1 |
O3—C20—C15 | 113.4 (6) | C69—C68—H68B | 109.1 |
O6—C21—C34 | 117.5 (6) | C64—C68—H68B | 109.1 |
O6—C21—C29 | 123.9 (6) | H68A—C68—H68B | 107.8 |
C34—C21—C29 | 118.6 (6) | C68—C69—C27 | 113.6 (9) |
N1—C22—C42 | 125.0 (7) | C68—C69—H69A | 108.9 |
N1—C22—H22A | 117.5 | C27—C69—H69A | 108.9 |
C42—C22—H22A | 117.5 | C68—C69—H69B | 108.9 |
N3—C23—C17 | 129.2 (6) | C27—C69—H69B | 108.9 |
N3—C23—H23A | 115.4 | H69A—C69—H69B | 107.7 |
C17—C23—H23A | 115.4 | C45—C71—C64 | 108.9 (8) |
O7—C24—C52 | 125.3 (6) | C45—C71—H71A | 109.9 |
O7—C24—C25 | 114.6 (5) | C64—C71—H71A | 109.9 |
C52—C24—C25 | 120.1 (6) | C45—C71—H71B | 109.9 |
O5—C25—C17 | 125.4 (6) | C64—C71—H71B | 109.9 |
O5—C25—C24 | 115.5 (5) | H71A—C71—H71B | 108.3 |
C17—C25—C24 | 119.0 (5) | O13—C72—H72A | 109.5 |
N2—C26—C19 | 126.4 (6) | O13—C72—H72B | 109.5 |
N2—C26—H26A | 116.8 | H72A—C72—H72B | 109.5 |
C19—C26—H26A | 116.8 | O13—C72—H72C | 109.5 |
N2—C27—C69 | 116.4 (8) | H72A—C72—H72C | 109.5 |
N2—C27—C45 | 108.1 (6) | H72B—C72—H72C | 109.5 |
C69—C27—C45 | 108.3 (7) | O1—Gd1—O6 | 128.77 (15) |
N2—C27—H27A | 107.9 | O1—Gd1—O11 | 151.18 (15) |
C69—C27—H27A | 107.9 | O6—Gd1—O11 | 79.19 (15) |
C45—C27—H27A | 107.9 | O1—Gd1—O10 | 80.13 (15) |
O2—C28—C51 | 117.3 (5) | O6—Gd1—O10 | 150.90 (15) |
O2—C28—C19 | 124.4 (6) | O11—Gd1—O10 | 72.75 (15) |
C51—C28—C19 | 118.2 (6) | O1—Gd1—O5 | 118.96 (14) |
C57—C29—C21 | 117.7 (7) | O6—Gd1—O5 | 66.83 (13) |
C57—C29—C32 | 118.6 (6) | O11—Gd1—O5 | 75.26 (14) |
C21—C29—C32 | 123.7 (6) | O10—Gd1—O5 | 98.10 (14) |
O9—C30—O10 | 123.6 (6) | O1—Gd1—O2 | 66.18 (14) |
O9—C30—C39 | 117.3 (6) | O6—Gd1—O2 | 117.80 (13) |
O10—C30—C39 | 119.1 (6) | O11—Gd1—O2 | 96.33 (14) |
C40—C31—C19 | 120.9 (7) | O10—Gd1—O2 | 73.61 (14) |
C40—C31—H31A | 119.5 | O5—Gd1—O2 | 169.83 (14) |
C19—C31—H31A | 119.5 | O1—Gd1—O3 | 60.92 (14) |
N4—C32—C29 | 126.2 (6) | O6—Gd1—O3 | 77.05 (14) |
N4—C32—H32A | 116.9 | O11—Gd1—O3 | 144.44 (14) |
C29—C32—H32A | 116.9 | O10—Gd1—O3 | 123.19 (14) |
O3—C33—H33A | 109.5 | O5—Gd1—O3 | 71.23 (13) |
O3—C33—H33B | 109.5 | O2—Gd1—O3 | 118.10 (14) |
H33A—C33—H33B | 109.5 | O1—Gd1—O8 | 76.86 (14) |
O3—C33—H33C | 109.5 | O6—Gd1—O8 | 60.53 (13) |
H33A—C33—H33C | 109.5 | O11—Gd1—O8 | 120.28 (14) |
H33B—C33—H33C | 109.5 | O10—Gd1—O8 | 142.69 (14) |
C53—C34—O8 | 125.1 (7) | O5—Gd1—O8 | 118.69 (13) |
C53—C34—C21 | 121.9 (6) | O2—Gd1—O8 | 70.35 (14) |
O8—C34—C21 | 113.0 (5) | O3—Gd1—O8 | 68.51 (14) |
C56—C35—C48 | 111.6 (7) | O1—Gd1—O7 | 68.47 (14) |
C56—C35—H35A | 109.3 | O6—Gd1—O7 | 119.41 (13) |
C48—C35—H35A | 109.3 | O11—Gd1—O7 | 106.41 (14) |
C56—C35—H35B | 109.3 | O10—Gd1—O7 | 63.37 (13) |
C48—C35—H35B | 109.3 | O5—Gd1—O7 | 57.58 (12) |
H35A—C35—H35B | 108.0 | O2—Gd1—O7 | 121.16 (13) |
O11—C36—O12 | 124.8 (6) | O3—Gd1—O7 | 64.52 (13) |
O11—C36—C49 | 118.5 (6) | O8—Gd1—O7 | 130.82 (13) |
O12—C36—C49 | 116.7 (6) | O1—Gd1—Zn2 | 147.29 (10) |
O7—C37—H37A | 109.5 | O6—Gd1—Zn2 | 36.53 (10) |
O7—C37—H37B | 109.5 | O11—Gd1—Zn2 | 58.79 (10) |
H37A—C37—H37B | 109.5 | O10—Gd1—Zn2 | 117.82 (11) |
O7—C37—H37C | 109.5 | O5—Gd1—Zn2 | 36.68 (9) |
H37A—C37—H37C | 109.5 | O2—Gd1—Zn2 | 142.45 (10) |
H37B—C37—H37C | 109.5 | O3—Gd1—Zn2 | 86.76 (10) |
C46—C38—C42 | 122.0 (7) | O8—Gd1—Zn2 | 96.93 (9) |
C46—C38—H38A | 119.0 | O7—Gd1—Zn2 | 94.24 (9) |
C42—C38—H38A | 119.0 | O1—Gd1—Zn3 | 36.59 (10) |
C30—C39—H39A | 109.5 | O6—Gd1—Zn3 | 146.88 (10) |
C30—C39—H39B | 109.5 | O11—Gd1—Zn3 | 116.70 (10) |
H39A—C39—H39B | 109.5 | O10—Gd1—Zn3 | 57.79 (11) |
C30—C39—H39C | 109.5 | O5—Gd1—Zn3 | 142.85 (9) |
H39A—C39—H39C | 109.5 | O2—Gd1—Zn3 | 36.61 (9) |
H39B—C39—H39C | 109.5 | O3—Gd1—Zn3 | 97.40 (10) |
C31—C40—C59 | 120.9 (7) | O8—Gd1—Zn3 | 86.88 (9) |
C31—C40—H40A | 119.5 | O7—Gd1—Zn3 | 85.43 (9) |
C59—C40—H40A | 119.5 | Zn2—Gd1—Zn3 | 175.19 (2) |
C60—C41—C17 | 120.7 (7) | C22—N1—C45 | 126.0 (7) |
C60—C41—H41A | 119.6 | C22—N1—Zn3 | 129.0 (5) |
C17—C41—H41A | 119.6 | C45—N1—Zn3 | 104.7 (5) |
C38—C42—C15 | 117.9 (7) | C26—N2—C27 | 120.0 (6) |
C38—C42—C22 | 117.1 (7) | C26—N2—Zn3 | 125.2 (5) |
C15—C42—C22 | 125.0 (6) | C27—N2—Zn3 | 113.8 (5) |
O8—C43—H43A | 109.5 | C23—N3—C48 | 121.9 (6) |
O8—C43—H43B | 109.5 | C23—N3—Zn2 | 124.1 (5) |
H43A—C43—H43B | 109.5 | C48—N3—Zn2 | 113.1 (4) |
O8—C43—H43C | 109.5 | C32—N4—C47 | 123.6 (6) |
H43A—C43—H43C | 109.5 | C32—N4—Zn2 | 128.7 (5) |
H43B—C43—H43C | 109.5 | C47—N4—Zn2 | 107.0 (4) |
C20—C44—C46 | 118.8 (7) | C15—O1—Zn3 | 129.2 (4) |
C20—C44—H44A | 120.6 | C15—O1—Gd1 | 130.3 (4) |
C46—C44—H44A | 120.6 | Zn3—O1—Gd1 | 100.39 (17) |
N1—C45—C71 | 118.7 (7) | C28—O2—Zn3 | 126.2 (4) |
N1—C45—C27 | 107.0 (6) | C28—O2—Gd1 | 136.1 (4) |
C71—C45—C27 | 111.9 (7) | Zn3—O2—Gd1 | 97.65 (15) |
N1—C45—H45A | 106.1 | C20—O3—C33 | 117.7 (5) |
C71—C45—H45A | 106.1 | C20—O3—Gd1 | 117.0 (4) |
C27—C45—H45A | 106.1 | C33—O3—Gd1 | 124.8 (4) |
C38—C46—C44 | 120.5 (7) | C51—O4—C54 | 117.2 (5) |
C38—C46—H46A | 119.8 | C25—O5—Zn2 | 125.4 (4) |
C44—C46—H46A | 119.8 | C25—O5—Gd1 | 135.8 (4) |
N4—C47—C58 | 119.7 (7) | Zn2—O5—Gd1 | 98.68 (15) |
N4—C47—C48 | 107.6 (6) | C21—O6—Zn2 | 128.7 (4) |
C58—C47—C48 | 112.5 (6) | C21—O6—Gd1 | 130.9 (4) |
N4—C47—H47A | 105.3 | Zn2—O6—Gd1 | 100.36 (16) |
C58—C47—H47A | 105.3 | C24—O7—C37 | 115.9 (5) |
C48—C47—H47A | 105.3 | C24—O7—Gd1 | 116.1 (3) |
N3—C48—C47 | 110.5 (6) | C37—O7—Gd1 | 127.6 (4) |
N3—C48—C35 | 114.9 (6) | C34—O8—C43 | 116.6 (5) |
C47—C48—C35 | 112.2 (7) | C34—O8—Gd1 | 117.4 (4) |
N3—C48—H48A | 106.2 | C43—O8—Gd1 | 125.6 (4) |
C47—C48—H48A | 106.2 | C30—O9—Zn3 | 116.3 (4) |
C35—C48—H48A | 106.2 | C30—O10—Gd1 | 148.9 (4) |
C36—C49—H49A | 109.5 | C36—O11—Gd1 | 147.9 (4) |
C36—C49—H49B | 109.5 | C36—O12—Zn2 | 116.5 (4) |
H49A—C49—H49B | 109.5 | C72—O13—H131 | 134.9 |
C36—C49—H49C | 109.5 | H142—O14—H141 | 128.6 |
H49A—C49—H49C | 109.5 | F1—P1—F3 | 97.9 (7) |
H49B—C49—H49C | 109.5 | F1—P1—F5 | 174.9 (7) |
C57—C50—C53 | 119.7 (7) | F3—P1—F5 | 87.1 (7) |
C57—C50—H50A | 120.2 | F1—P1—F2 | 88.4 (7) |
C53—C50—H50A | 120.2 | F3—P1—F2 | 173.5 (7) |
O4—C51—C59 | 124.2 (6) | F5—P1—F2 | 86.6 (6) |
O4—C51—C28 | 114.8 (5) | F1—P1—F4 | 89.2 (6) |
C59—C51—C28 | 121.0 (6) | F3—P1—F4 | 86.4 (5) |
C60—C52—C24 | 120.2 (7) | F5—P1—F4 | 92.4 (6) |
C60—C52—H52A | 119.9 | F2—P1—F4 | 95.4 (6) |
C24—C52—H52A | 119.9 | F1—P1—F6 | 91.0 (6) |
C34—C53—C50 | 119.3 (7) | F3—P1—F6 | 92.3 (5) |
C34—C53—H53A | 120.3 | F5—P1—F6 | 87.5 (5) |
C50—C53—H53A | 120.3 | F2—P1—F6 | 85.8 (6) |
O4—C54—H54A | 109.5 | F4—P1—F6 | 178.8 (6) |
O4—C54—H54B | 109.5 | O12—Zn2—O5 | 103.75 (17) |
H54A—C54—H54B | 109.5 | O12—Zn2—O6 | 109.85 (18) |
O4—C54—H54C | 109.5 | O5—Zn2—O6 | 79.60 (16) |
H54A—C54—H54C | 109.5 | O12—Zn2—N3 | 111.4 (2) |
H54B—C54—H54C | 109.5 | O5—Zn2—N3 | 91.34 (18) |
C56—C55—C58 | 112.1 (8) | O6—Zn2—N3 | 138.8 (2) |
C56—C55—H55A | 109.2 | O12—Zn2—N4 | 105.0 (2) |
C58—C55—H55A | 109.2 | O5—Zn2—N4 | 151.2 (2) |
C56—C55—H55B | 109.2 | O6—Zn2—N4 | 88.47 (19) |
C58—C55—H55B | 109.2 | N3—Zn2—N4 | 80.5 (2) |
H55A—C55—H55B | 107.9 | O12—Zn2—Gd1 | 91.96 (13) |
C35—C56—C55 | 113.8 (7) | O5—Zn2—Gd1 | 44.64 (10) |
C35—C56—H56A | 108.8 | O6—Zn2—Gd1 | 43.11 (11) |
C55—C56—H56A | 108.8 | N3—Zn2—Gd1 | 134.92 (15) |
C35—C56—H56B | 108.8 | N4—Zn2—Gd1 | 131.45 (16) |
C55—C56—H56B | 108.8 | O9—Zn3—O2 | 103.26 (18) |
H56A—C56—H56B | 107.7 | O9—Zn3—O1 | 112.88 (18) |
C50—C57—C29 | 122.7 (7) | O2—Zn3—O1 | 79.67 (17) |
C50—C57—H57A | 118.6 | O9—Zn3—N1 | 105.7 (2) |
C29—C57—H57A | 118.6 | O2—Zn3—N1 | 151.0 (2) |
C47—C58—C55 | 110.0 (7) | O1—Zn3—N1 | 88.1 (2) |
C47—C58—H58A | 109.7 | O9—Zn3—N2 | 107.8 (2) |
C55—C58—H58A | 109.7 | O2—Zn3—N2 | 91.1 (2) |
C47—C58—H58B | 109.7 | O1—Zn3—N2 | 139.3 (2) |
C55—C58—H58B | 109.7 | N1—Zn3—N2 | 81.1 (2) |
H58A—C58—H58B | 108.2 | O9—Zn3—Gd1 | 92.65 (13) |
C51—C59—C40 | 119.2 (7) | O2—Zn3—Gd1 | 45.74 (11) |
C51—C59—H59A | 120.4 | O1—Zn3—Gd1 | 43.02 (12) |
C40—C59—H59A | 120.4 | N1—Zn3—Gd1 | 130.82 (18) |
C41—C60—C52 | 120.5 (7) | N2—Zn3—Gd1 | 136.11 (16) |
O1—C15—C20—C44 | 179.7 (6) | O3—Gd1—O7—C24 | 78.4 (4) |
C42—C15—C20—C44 | −1.3 (9) | O8—Gd1—O7—C24 | 97.0 (4) |
O1—C15—C20—O3 | −1.1 (8) | Zn2—Gd1—O7—C24 | −6.0 (4) |
C42—C15—C20—O3 | 177.9 (5) | Zn3—Gd1—O7—C24 | 178.9 (4) |
C25—C17—C23—N3 | 8.3 (12) | O1—Gd1—O7—C37 | −42.7 (5) |
C41—C17—C23—N3 | −175.8 (8) | O6—Gd1—O7—C37 | −166.1 (5) |
C41—C17—C25—O5 | 178.9 (6) | O11—Gd1—O7—C37 | 107.3 (5) |
C23—C17—C25—O5 | −5.2 (10) | O10—Gd1—O7—C37 | 46.8 (5) |
C41—C17—C25—C24 | −2.3 (10) | O5—Gd1—O7—C37 | 167.2 (6) |
C23—C17—C25—C24 | 173.5 (6) | O2—Gd1—O7—C37 | −0.9 (6) |
O7—C24—C25—O5 | 1.4 (8) | O3—Gd1—O7—C37 | −109.7 (5) |
C52—C24—C25—O5 | −177.8 (6) | O8—Gd1—O7—C37 | −91.1 (5) |
O7—C24—C25—C17 | −177.5 (5) | Zn2—Gd1—O7—C37 | 165.9 (5) |
C52—C24—C25—C17 | 3.3 (10) | Zn3—Gd1—O7—C37 | −9.2 (5) |
C28—C19—C26—N2 | 13.6 (12) | C53—C34—O8—C43 | −0.3 (9) |
C31—C19—C26—N2 | −169.6 (7) | C21—C34—O8—C43 | −179.4 (6) |
C31—C19—C28—O2 | 177.4 (6) | C53—C34—O8—Gd1 | −173.0 (5) |
C26—C19—C28—O2 | −5.8 (10) | C21—C34—O8—Gd1 | 7.8 (7) |
C31—C19—C28—C51 | −3.6 (9) | O1—Gd1—O8—C34 | −157.9 (4) |
C26—C19—C28—C51 | 173.1 (6) | O6—Gd1—O8—C34 | −7.4 (4) |
O6—C21—C29—C57 | −178.2 (6) | O11—Gd1—O8—C34 | 47.2 (4) |
C34—C21—C29—C57 | 2.3 (10) | O10—Gd1—O8—C34 | 148.7 (4) |
O6—C21—C29—C32 | 4.3 (11) | O5—Gd1—O8—C34 | −41.9 (4) |
C34—C21—C29—C32 | −175.2 (7) | O2—Gd1—O8—C34 | 133.0 (4) |
C28—C19—C31—C40 | −1.4 (11) | O3—Gd1—O8—C34 | −94.3 (4) |
C26—C19—C31—C40 | −178.4 (7) | O7—Gd1—O8—C34 | −112.3 (4) |
C57—C29—C32—N4 | 176.2 (8) | Zn2—Gd1—O8—C34 | −10.6 (4) |
C21—C29—C32—N4 | −6.3 (13) | Zn3—Gd1—O8—C34 | 166.5 (4) |
O6—C21—C34—C53 | 178.3 (6) | O1—Gd1—O8—C43 | 30.0 (5) |
C29—C21—C34—C53 | −2.1 (10) | O6—Gd1—O8—C43 | −179.5 (6) |
O6—C21—C34—O8 | −2.6 (8) | O11—Gd1—O8—C43 | −124.9 (5) |
C29—C21—C34—O8 | 177.0 (6) | O10—Gd1—O8—C43 | −23.4 (6) |
C19—C31—C40—C59 | 4.8 (12) | O5—Gd1—O8—C43 | 146.1 (5) |
C25—C17—C41—C60 | −1.4 (12) | O2—Gd1—O8—C43 | −39.0 (5) |
C23—C17—C41—C60 | −177.6 (8) | O3—Gd1—O8—C43 | 93.6 (5) |
C46—C38—C42—C15 | 1.0 (10) | O7—Gd1—O8—C43 | 75.6 (5) |
C46—C38—C42—C22 | 178.0 (7) | Zn2—Gd1—O8—C43 | 177.4 (5) |
O1—C15—C42—C38 | 179.5 (6) | Zn3—Gd1—O8—C43 | −5.6 (5) |
C20—C15—C42—C38 | 0.5 (9) | O10—C30—O9—Zn3 | −7.7 (8) |
O1—C15—C42—C22 | 2.7 (10) | C39—C30—O9—Zn3 | 173.1 (4) |
C20—C15—C42—C22 | −176.2 (6) | O9—C30—O10—Gd1 | 13.5 (12) |
N1—C22—C42—C38 | 178.8 (7) | C39—C30—O10—Gd1 | −167.3 (5) |
N1—C22—C42—C15 | −4.4 (11) | O1—Gd1—O10—C30 | −39.6 (8) |
O3—C20—C44—C46 | −178.6 (6) | O6—Gd1—O10—C30 | 146.4 (7) |
C15—C20—C44—C46 | 0.6 (10) | O11—Gd1—O10—C30 | 130.5 (8) |
N2—C27—C45—N1 | −43.8 (9) | O5—Gd1—O10—C30 | −157.8 (8) |
C69—C27—C45—N1 | −170.8 (7) | O2—Gd1—O10—C30 | 28.3 (8) |
N2—C27—C45—C71 | −175.5 (7) | O3—Gd1—O10—C30 | −84.9 (8) |
C69—C27—C45—C71 | 57.6 (11) | O8—Gd1—O10—C30 | 12.9 (9) |
C42—C38—C46—C44 | −1.8 (11) | O7—Gd1—O10—C30 | −110.4 (8) |
C20—C44—C46—C38 | 1.0 (11) | Zn2—Gd1—O10—C30 | 169.5 (7) |
N4—C47—C48—N3 | −40.2 (9) | Zn3—Gd1—O10—C30 | −8.2 (7) |
C58—C47—C48—N3 | −174.1 (7) | O12—C36—O11—Gd1 | −3.1 (12) |
N4—C47—C48—C35 | −169.9 (6) | C49—C36—O11—Gd1 | 173.7 (6) |
C58—C47—C48—C35 | 56.2 (10) | O1—Gd1—O11—C36 | 160.9 (7) |
C56—C35—C48—N3 | −178.7 (7) | O6—Gd1—O11—C36 | −31.8 (8) |
C56—C35—C48—C47 | −51.3 (10) | O10—Gd1—O11—C36 | 140.4 (8) |
O2—C28—C51—O4 | 3.6 (8) | O5—Gd1—O11—C36 | 36.8 (8) |
C19—C28—C51—O4 | −175.4 (6) | O2—Gd1—O11—C36 | −149.0 (8) |
O2—C28—C51—C59 | −175.7 (6) | O3—Gd1—O11—C36 | 16.9 (9) |
C19—C28—C51—C59 | 5.3 (10) | O8—Gd1—O11—C36 | −78.1 (8) |
O7—C24—C52—C60 | −179.6 (7) | O7—Gd1—O11—C36 | 85.9 (8) |
C25—C24—C52—C60 | −0.5 (12) | Zn2—Gd1—O11—C36 | 1.0 (7) |
O8—C34—C53—C50 | −177.8 (7) | Zn3—Gd1—O11—C36 | 179.0 (7) |
C21—C34—C53—C50 | 1.2 (11) | O11—C36—O12—Zn2 | 3.3 (8) |
C57—C50—C53—C34 | −0.5 (13) | C49—C36—O12—Zn2 | −173.5 (5) |
C48—C35—C56—C55 | 49.7 (12) | C36—O12—Zn2—O5 | −45.7 (5) |
C58—C55—C56—C35 | −51.2 (12) | C36—O12—Zn2—O6 | 38.0 (5) |
C53—C50—C57—C29 | 0.7 (14) | C36—O12—Zn2—N3 | −142.7 (4) |
C21—C29—C57—C50 | −1.6 (13) | C36—O12—Zn2—N4 | 131.9 (4) |
C32—C29—C57—C50 | 176.0 (8) | C36—O12—Zn2—Gd1 | −2.1 (4) |
N4—C47—C58—C55 | 176.0 (7) | C25—O5—Zn2—O12 | −105.7 (4) |
C48—C47—C58—C55 | −56.2 (11) | Gd1—O5—Zn2—O12 | 78.60 (18) |
C56—C55—C58—C47 | 53.5 (11) | C25—O5—Zn2—O6 | 146.2 (5) |
O4—C51—C59—C40 | 178.7 (6) | Gd1—O5—Zn2—O6 | −29.49 (15) |
C28—C51—C59—C40 | −2.1 (10) | C25—O5—Zn2—N3 | 6.6 (5) |
C31—C40—C59—C51 | −3.1 (11) | Gd1—O5—Zn2—N3 | −169.00 (19) |
C17—C41—C60—C52 | 4.3 (14) | C25—O5—Zn2—N4 | 79.1 (6) |
C24—C52—C60—C41 | −3.4 (14) | Gd1—O5—Zn2—N4 | −96.5 (4) |
C71—C64—C68—C69 | −52.3 (15) | C25—O5—Zn2—Gd1 | 175.7 (5) |
C64—C68—C69—C27 | 52.9 (14) | C21—O6—Zn2—O12 | 107.7 (5) |
N2—C27—C69—C68 | −176.6 (8) | Gd1—O6—Zn2—O12 | −70.6 (2) |
C45—C27—C69—C68 | −54.6 (12) | C21—O6—Zn2—O5 | −151.3 (5) |
N1—C45—C71—C64 | 177.0 (8) | Gd1—O6—Zn2—O5 | 30.40 (16) |
C27—C45—C71—C64 | −57.6 (11) | C21—O6—Zn2—N3 | −71.3 (6) |
C68—C64—C71—C45 | 54.2 (13) | Gd1—O6—Zn2—N3 | 110.4 (3) |
C42—C22—N1—C45 | 178.3 (7) | C21—O6—Zn2—N4 | 2.4 (5) |
C42—C22—N1—Zn3 | 5.4 (11) | Gd1—O6—Zn2—N4 | −176.0 (2) |
C71—C45—N1—C22 | 7.3 (13) | C21—O6—Zn2—Gd1 | 178.3 (6) |
C27—C45—N1—C22 | −120.5 (8) | C23—N3—Zn2—O12 | 101.1 (6) |
C71—C45—N1—Zn3 | −178.4 (7) | C48—N3—Zn2—O12 | −89.8 (5) |
C27—C45—N1—Zn3 | 53.9 (7) | C23—N3—Zn2—O5 | −4.3 (6) |
C19—C26—N2—C27 | −174.8 (7) | C48—N3—Zn2—O5 | 164.9 (5) |
C19—C26—N2—Zn3 | −6.9 (11) | C23—N3—Zn2—O6 | −79.9 (7) |
C69—C27—N2—C26 | −55.9 (11) | C48—N3—Zn2—O6 | 89.2 (5) |
C45—C27—N2—C26 | −178.0 (7) | C23—N3—Zn2—N4 | −156.5 (6) |
C69—C27—N2—Zn3 | 134.9 (7) | C48—N3—Zn2—N4 | 12.7 (5) |
C45—C27—N2—Zn3 | 12.7 (9) | C23—N3—Zn2—Gd1 | −15.2 (7) |
C17—C23—N3—C48 | −170.2 (7) | C48—N3—Zn2—Gd1 | 154.0 (4) |
C17—C23—N3—Zn2 | −1.9 (11) | C32—N4—Zn2—O12 | −114.3 (7) |
C47—C48—N3—C23 | −178.9 (7) | C47—N4—Zn2—O12 | 75.2 (5) |
C35—C48—N3—C23 | −50.6 (10) | C32—N4—Zn2—O5 | 60.8 (8) |
C47—C48—N3—Zn2 | 11.7 (8) | C47—N4—Zn2—O5 | −109.7 (5) |
C35—C48—N3—Zn2 | 139.9 (6) | C32—N4—Zn2—O6 | −4.1 (7) |
C29—C32—N4—C47 | 175.8 (7) | C47—N4—Zn2—O6 | −174.7 (5) |
C29—C32—N4—Zn2 | 6.7 (12) | C32—N4—Zn2—N3 | 136.0 (7) |
C58—C47—N4—C32 | 8.7 (12) | C47—N4—Zn2—N3 | −34.5 (5) |
C48—C47—N4—C32 | −121.3 (8) | C32—N4—Zn2—Gd1 | −7.8 (8) |
C58—C47—N4—Zn2 | 179.8 (6) | C47—N4—Zn2—Gd1 | −178.3 (4) |
C48—C47—N4—Zn2 | 49.9 (7) | O1—Gd1—Zn2—O12 | −161.5 (2) |
C20—C15—O1—Zn3 | 176.8 (4) | O6—Gd1—Zn2—O12 | 117.4 (2) |
C42—C15—O1—Zn3 | −2.2 (8) | O11—Gd1—Zn2—O12 | 0.70 (18) |
C20—C15—O1—Gd1 | −8.2 (8) | O10—Gd1—Zn2—O12 | −43.91 (17) |
C42—C15—O1—Gd1 | 172.9 (4) | O5—Gd1—Zn2—O12 | −107.7 (2) |
O6—Gd1—O1—C15 | 47.8 (5) | O2—Gd1—Zn2—O12 | 55.5 (2) |
O11—Gd1—O1—C15 | −148.3 (4) | O3—Gd1—Zn2—O12 | −170.07 (16) |
O10—Gd1—O1—C15 | −128.4 (5) | O8—Gd1—Zn2—O12 | 122.05 (16) |
O5—Gd1—O1—C15 | −34.6 (5) | O7—Gd1—Zn2—O12 | −105.94 (16) |
O2—Gd1—O1—C15 | 155.2 (5) | O1—Gd1—Zn2—O5 | −53.8 (3) |
O3—Gd1—O1—C15 | 8.6 (4) | O6—Gd1—Zn2—O5 | −134.9 (2) |
O8—Gd1—O1—C15 | 81.1 (5) | O11—Gd1—Zn2—O5 | 108.4 (2) |
O7—Gd1—O1—C15 | −63.3 (5) | O10—Gd1—Zn2—O5 | 63.8 (2) |
Zn2—Gd1—O1—C15 | −1.1 (6) | O2—Gd1—Zn2—O5 | 163.2 (2) |
Zn3—Gd1—O1—C15 | −176.1 (6) | O3—Gd1—Zn2—O5 | −62.39 (19) |
O6—Gd1—O1—Zn3 | −136.08 (16) | O8—Gd1—Zn2—O5 | −130.27 (19) |
O11—Gd1—O1—Zn3 | 27.8 (4) | O7—Gd1—Zn2—O5 | 1.75 (18) |
O10—Gd1—O1—Zn3 | 47.67 (17) | O1—Gd1—Zn2—O6 | 81.1 (3) |
O5—Gd1—O1—Zn3 | 141.52 (15) | O11—Gd1—Zn2—O6 | −116.7 (2) |
O2—Gd1—O1—Zn3 | −28.66 (15) | O10—Gd1—Zn2—O6 | −161.3 (2) |
O3—Gd1—O1—Zn3 | −175.2 (2) | O5—Gd1—Zn2—O6 | 134.9 (2) |
O8—Gd1—O1—Zn3 | −102.74 (18) | O2—Gd1—Zn2—O6 | −61.9 (2) |
O7—Gd1—O1—Zn3 | 112.81 (19) | O3—Gd1—Zn2—O6 | 72.5 (2) |
Zn2—Gd1—O1—Zn3 | 174.96 (5) | O8—Gd1—Zn2—O6 | 4.6 (2) |
C51—C28—O2—Zn3 | 174.1 (4) | O7—Gd1—Zn2—O6 | 136.64 (19) |
C19—C28—O2—Zn3 | −6.9 (9) | O1—Gd1—Zn2—N3 | −38.2 (3) |
C51—C28—O2—Gd1 | −5.0 (9) | O6—Gd1—Zn2—N3 | −119.3 (3) |
C19—C28—O2—Gd1 | 173.9 (4) | O11—Gd1—Zn2—N3 | 124.0 (3) |
O1—Gd1—O2—C28 | −152.0 (6) | O10—Gd1—Zn2—N3 | 79.4 (2) |
O6—Gd1—O2—C28 | −29.3 (6) | O5—Gd1—Zn2—N3 | 15.6 (3) |
O11—Gd1—O2—C28 | 51.8 (6) | O2—Gd1—Zn2—N3 | 178.8 (3) |
O10—Gd1—O2—C28 | 121.7 (6) | O3—Gd1—Zn2—N3 | −46.8 (2) |
O5—Gd1—O2—C28 | 85.6 (9) | O8—Gd1—Zn2—N3 | −114.6 (2) |
O3—Gd1—O2—C28 | −119.0 (5) | O7—Gd1—Zn2—N3 | 17.4 (2) |
O8—Gd1—O2—C28 | −68.1 (5) | O1—Gd1—Zn2—N4 | 86.5 (3) |
O7—Gd1—O2—C28 | 165.3 (5) | O6—Gd1—Zn2—N4 | 5.4 (3) |
Zn2—Gd1—O2—C28 | 7.1 (6) | O11—Gd1—Zn2—N4 | −111.3 (3) |
Zn3—Gd1—O2—C28 | 179.3 (7) | O10—Gd1—Zn2—N4 | −155.9 (2) |
O1—Gd1—O2—Zn3 | 28.65 (16) | O5—Gd1—Zn2—N4 | 140.3 (3) |
O6—Gd1—O2—Zn3 | 151.40 (15) | O2—Gd1—Zn2—N4 | −56.5 (3) |
O11—Gd1—O2—Zn3 | −127.51 (17) | O3—Gd1—Zn2—N4 | 77.9 (2) |
O10—Gd1—O2—Zn3 | −57.60 (17) | O8—Gd1—Zn2—N4 | 10.0 (2) |
O5—Gd1—O2—Zn3 | −93.8 (7) | O7—Gd1—Zn2—N4 | 142.0 (2) |
O3—Gd1—O2—Zn3 | 61.7 (2) | C30—O9—Zn3—O2 | −42.1 (5) |
O8—Gd1—O2—Zn3 | 112.56 (19) | C30—O9—Zn3—O1 | 42.1 (5) |
O7—Gd1—O2—Zn3 | −14.0 (2) | C30—O9—Zn3—N1 | 136.8 (5) |
Zn2—Gd1—O2—Zn3 | −172.17 (4) | C30—O9—Zn3—N2 | −137.7 (4) |
C44—C20—O3—C33 | −0.8 (9) | C30—O9—Zn3—Gd1 | 2.9 (4) |
C15—C20—O3—C33 | 180.0 (6) | C28—O2—Zn3—O9 | −98.8 (5) |
C44—C20—O3—Gd1 | −173.2 (5) | Gd1—O2—Zn3—O9 | 80.60 (19) |
C15—C20—O3—Gd1 | 7.6 (6) | C28—O2—Zn3—O1 | 149.9 (5) |
O1—Gd1—O3—C20 | −8.0 (4) | Gd1—O2—Zn3—O1 | −30.69 (16) |
O6—Gd1—O3—C20 | −157.7 (4) | C28—O2—Zn3—N1 | 83.4 (6) |
O11—Gd1—O3—C20 | 153.1 (4) | Gd1—O2—Zn3—N1 | −97.2 (4) |
O10—Gd1—O3—C20 | 45.3 (4) | C28—O2—Zn3—N2 | 9.8 (5) |
O5—Gd1—O3—C20 | 132.7 (4) | Gd1—O2—Zn3—N2 | −170.8 (2) |
O2—Gd1—O3—C20 | −42.8 (4) | C28—O2—Zn3—Gd1 | −179.4 (6) |
O8—Gd1—O3—C20 | −94.5 (4) | C15—O1—Zn3—O9 | 108.4 (5) |
O7—Gd1—O3—C20 | 70.5 (4) | Gd1—O1—Zn3—O9 | −67.8 (2) |
Zn2—Gd1—O3—C20 | 166.7 (4) | C15—O1—Zn3—O2 | −151.4 (5) |
Zn3—Gd1—O3—C20 | −10.9 (4) | Gd1—O1—Zn3—O2 | 32.39 (17) |
O1—Gd1—O3—C33 | −179.8 (5) | C15—O1—Zn3—N1 | 2.1 (5) |
O6—Gd1—O3—C33 | 30.6 (5) | Gd1—O1—Zn3—N1 | −174.0 (2) |
O11—Gd1—O3—C33 | −18.7 (6) | C15—O1—Zn3—N2 | −71.9 (6) |
O10—Gd1—O3—C33 | −126.5 (5) | Gd1—O1—Zn3—N2 | 112.0 (3) |
O5—Gd1—O3—C33 | −39.1 (5) | C15—O1—Zn3—Gd1 | 176.2 (6) |
O2—Gd1—O3—C33 | 145.4 (5) | C22—N1—Zn3—O9 | −117.0 (7) |
O8—Gd1—O3—C33 | 93.7 (5) | C45—N1—Zn3—O9 | 68.9 (5) |
O7—Gd1—O3—C33 | −101.3 (5) | C22—N1—Zn3—O2 | 60.8 (8) |
Zn2—Gd1—O3—C33 | −5.1 (5) | C45—N1—Zn3—O2 | −113.3 (6) |
Zn3—Gd1—O3—C33 | 177.4 (5) | C22—N1—Zn3—O1 | −3.7 (7) |
C59—C51—O4—C54 | 1.6 (10) | C45—N1—Zn3—O1 | −177.9 (5) |
C28—C51—O4—C54 | −177.7 (6) | C22—N1—Zn3—N2 | 136.9 (7) |
C17—C25—O5—Zn2 | −3.1 (8) | C45—N1—Zn3—N2 | −37.2 (5) |
C24—C25—O5—Zn2 | 178.0 (4) | C22—N1—Zn3—Gd1 | −9.1 (8) |
C17—C25—O5—Gd1 | 170.7 (4) | C45—N1—Zn3—Gd1 | 176.8 (4) |
C24—C25—O5—Gd1 | −8.1 (8) | C26—N2—Zn3—O9 | 101.2 (6) |
O1—Gd1—O5—C25 | −24.8 (5) | C27—N2—Zn3—O9 | −90.2 (6) |
O6—Gd1—O5—C25 | −147.6 (5) | C26—N2—Zn3—O2 | −3.1 (7) |
O11—Gd1—O5—C25 | 128.0 (5) | C27—N2—Zn3—O2 | 165.5 (5) |
O10—Gd1—O5—C25 | 58.3 (5) | C26—N2—Zn3—O1 | −78.5 (7) |
O2—Gd1—O5—C25 | 93.2 (9) | C27—N2—Zn3—O1 | 90.1 (6) |
O3—Gd1—O5—C25 | −64.0 (5) | C26—N2—Zn3—N1 | −155.0 (7) |
O8—Gd1—O5—C25 | −115.2 (5) | C27—N2—Zn3—N1 | 13.6 (6) |
O7—Gd1—O5—C25 | 7.1 (5) | C26—N2—Zn3—Gd1 | −12.6 (8) |
Zn2—Gd1—O5—C25 | −174.9 (6) | C27—N2—Zn3—Gd1 | 156.0 (5) |
Zn3—Gd1—O5—C25 | 13.1 (6) | O1—Gd1—Zn3—O9 | 121.4 (2) |
O1—Gd1—O5—Zn2 | 150.10 (15) | O6—Gd1—Zn3—O9 | −156.8 (2) |
O6—Gd1—O5—Zn2 | 27.30 (15) | O11—Gd1—Zn3—O9 | −44.04 (18) |
O11—Gd1—O5—Zn2 | −57.05 (16) | O10—Gd1—Zn3—O9 | 0.79 (18) |
O10—Gd1—O5—Zn2 | −126.74 (16) | O5—Gd1—Zn3—O9 | 57.0 (2) |
O2—Gd1—O5—Zn2 | −91.9 (7) | O2—Gd1—Zn3—O9 | −106.0 (2) |
O3—Gd1—O5—Zn2 | 110.87 (18) | O3—Gd1—Zn3—O9 | 125.58 (16) |
O8—Gd1—O5—Zn2 | 59.71 (19) | O8—Gd1—Zn3—O9 | −166.57 (16) |
O7—Gd1—O5—Zn2 | −177.9 (2) | O7—Gd1—Zn3—O9 | 62.04 (16) |
Zn3—Gd1—O5—Zn2 | −172.02 (4) | O1—Gd1—Zn3—O2 | −132.6 (2) |
C34—C21—O6—Zn2 | 176.5 (4) | O6—Gd1—Zn3—O2 | −50.8 (3) |
C29—C21—O6—Zn2 | −3.1 (9) | O11—Gd1—Zn3—O2 | 62.0 (2) |
C34—C21—O6—Gd1 | −5.7 (8) | O10—Gd1—Zn3—O2 | 106.8 (2) |
C29—C21—O6—Gd1 | 174.7 (5) | O5—Gd1—Zn3—O2 | 163.0 (2) |
O1—Gd1—O6—C21 | 45.0 (5) | O3—Gd1—Zn3—O2 | −128.4 (2) |
O11—Gd1—O6—C21 | −127.2 (5) | O8—Gd1—Zn3—O2 | −60.6 (2) |
O10—Gd1—O6—C21 | −142.7 (5) | O7—Gd1—Zn3—O2 | 168.0 (2) |
O5—Gd1—O6—C21 | 154.3 (5) | O6—Gd1—Zn3—O1 | 81.8 (3) |
O2—Gd1—O6—C21 | −35.7 (5) | O11—Gd1—Zn3—O1 | −165.4 (2) |
O3—Gd1—O6—C21 | 79.4 (5) | O10—Gd1—Zn3—O1 | −120.6 (2) |
O8—Gd1—O6—C21 | 7.0 (5) | O5—Gd1—Zn3—O1 | −64.3 (2) |
O7—Gd1—O6—C21 | 129.9 (5) | O2—Gd1—Zn3—O1 | 132.6 (2) |
Zn2—Gd1—O6—C21 | −178.3 (6) | O3—Gd1—Zn3—O1 | 4.2 (2) |
Zn3—Gd1—O6—C21 | −4.2 (6) | O8—Gd1—Zn3—O1 | 72.0 (2) |
O1—Gd1—O6—Zn2 | −136.78 (16) | O7—Gd1—Zn3—O1 | −59.3 (2) |
O11—Gd1—O6—Zn2 | 51.05 (17) | O1—Gd1—Zn3—N1 | 7.9 (3) |
O10—Gd1—O6—Zn2 | 35.6 (4) | O6—Gd1—Zn3—N1 | 89.7 (3) |
O5—Gd1—O6—Zn2 | −27.41 (15) | O11—Gd1—Zn3—N1 | −157.5 (3) |
O2—Gd1—O6—Zn2 | 142.55 (15) | O10—Gd1—Zn3—N1 | −112.7 (3) |
O3—Gd1—O6—Zn2 | −102.29 (17) | O5—Gd1—Zn3—N1 | −56.5 (3) |
O8—Gd1—O6—Zn2 | −174.7 (2) | O2—Gd1—Zn3—N1 | 140.5 (3) |
O7—Gd1—O6—Zn2 | −51.8 (2) | O3—Gd1—Zn3—N1 | 12.1 (3) |
Zn3—Gd1—O6—Zn2 | 174.04 (4) | O8—Gd1—Zn3—N1 | 79.9 (3) |
C52—C24—O7—C37 | 9.7 (10) | O7—Gd1—Zn3—N1 | −51.5 (3) |
C25—C24—O7—C37 | −169.5 (6) | O1—Gd1—Zn3—N2 | −119.3 (3) |
C52—C24—O7—Gd1 | −177.5 (6) | O6—Gd1—Zn3—N2 | −37.5 (3) |
C25—C24—O7—Gd1 | 3.4 (7) | O11—Gd1—Zn3—N2 | 75.3 (3) |
O1—Gd1—O7—C24 | 145.4 (4) | O10—Gd1—Zn3—N2 | 120.1 (3) |
O6—Gd1—O7—C24 | 22.0 (4) | O5—Gd1—Zn3—N2 | 176.4 (3) |
O11—Gd1—O7—C24 | −64.6 (4) | O2—Gd1—Zn3—N2 | 13.3 (3) |
O10—Gd1—O7—C24 | −125.1 (4) | O3—Gd1—Zn3—N2 | −115.1 (3) |
O5—Gd1—O7—C24 | −4.7 (4) | O8—Gd1—Zn3—N2 | −47.2 (3) |
O2—Gd1—O7—C24 | −172.8 (4) | O7—Gd1—Zn3—N2 | −178.6 (3) |
Experimental details
Crystal data | |
Chemical formula | [GdZn2(C22H24N2O4)2(C2H3O2)2]PF6·CH4O·H2O |
Mr | 1361.97 |
Crystal system, space group | Monoclinic, P21/n |
Temperature (K) | 296 |
a, b, c (Å) | 15.8127 (12), 20.6405 (16), 18.5036 (14) |
β (°) | 114.369 (1) |
V (Å3) | 5501.2 (7) |
Z | 4 |
Radiation type | Mo Kα |
µ (mm−1) | 2.17 |
Crystal size (mm) | 0.20 × 0.18 × 0.16 |
Data collection | |
Diffractometer | Rigaku R-AXIS RAPID diffractometer |
Absorption correction | Multi-scan (ABSCOR; Higashi, 1995) |
Tmin, Tmax | 0.671, 0.723 |
No. of measured, independent and observed [I > 2σ(I)] reflections | 39974, 13701, 6858 |
Rint | 0.066 |
(sin θ/λ)max (Å−1) | 0.668 |
Refinement | |
R[F2 > 2σ(F2)], wR(F2), S | 0.053, 0.157, 0.98 |
No. of reflections | 13701 |
No. of parameters | 695 |
No. of restraints | 19 |
H-atom treatment | H-atom parameters constrained |
Δρmax, Δρmin (e Å−3) | 1.02, −0.71 |
Computer programs: RAPID-AUTO (Rigaku, 1998), CrystalStructure (Rigaku/MSC, 2002), SHELXS97 (Sheldrick, 2008), SHELXL97 (Sheldrick, 2008), SHELXTL (Sheldrick, 2008).
Acknowledgements
The authors gratefully acknowledge financial support from the NSFC of China (No. 21102039), Heilongjiang Province (Nos. 11551336 and 11521205), the Undergraduate Open Experiment Programme of Heilongjiang University and the Undergraduate Science and Technique Innovation Programme of Students and Heilongjiang University (No. QL201021).
References
Higashi, T. (1995). ABSCOR. Rigaku Corporation, Tokyo, Japan. Google Scholar
Rigaku (1998). RAPID-AUTO. Rigaku Corporation, Tokyo, Japan. Google Scholar
Rigaku/MSC (2002). CrystalStructure. Rigaku/MSC Inc., The Woodlands, Texas, USA. Google Scholar
Sheldrick, G. M. (2008). Acta Cryst. A64, 112–122. Web of Science CrossRef CAS IUCr Journals Google Scholar
Wang, H. L., Zhang, D. P., Ni, Z. H., Li, X. Y., Tian, L. J. & Jiang, J. Z. (2009). Inorg. Chem. 48, 5946–5956. Web of Science CSD CrossRef PubMed CAS Google Scholar
Wong, W. K., Yang, X. P., Jones, R. A., Rivers, J. H., Lynch, V., Lo, W. K., Xiao, D., Oye, M. M. & Holmes, A. (2006). Inorg. Chem. 45, 4340–4345. Web of Science CSD CrossRef PubMed CAS Google Scholar
This is an open-access article distributed under the terms of the Creative Commons Attribution (CC-BY) Licence, which permits unrestricted use, distribution, and reproduction in any medium, provided the original authors and source are cited.
The Schiff base heteronuclear M—Ln complexes (M = transition metal and Ln = rare earth) have attracted much attention for their magnetic properties. Several mutinuclear complexes are reported that have been derived from aromatic salen type Schiff base ligands (Wong et al., 2006; Wang et al., 2009). In this article, we report the preparation and crystal structure of a Zn—Gd—Zn trinuclear coordination complex of the ligand N,N'-bis(3-methoxysalicylidene)propane-1,2-cyclohexanediamine.
The hexadentate Schiff base ligand (L) links Zn and Gd atoms into a trinuclear complex (Fig. 1). The GdIII centre in the complex is nine-coordinated by seven oxygen atoms from ligand L and two oxygen atoms from two acetic acid molecules. The ZnII center is five-coordinated by two nitrogen atoms and two oxygen atoms from the ligand and one oxygen atom from acetic acid and result in a square-pyramidal coordination geometry.