research communications
The crystal structures of {LnCu5}3+ (Ln = Gd, Dy and Ho) 15-metallacrown-5 complexes and a reevaluation of the isotypic EuIII analogue
aDepartment of Chemistry, Taras Shevchenko National University of Kyiv, Volodymyrska str. 62, Kyiv, 01601, Ukraine, bL.V. Pisarzhevskii Institute of Physical Chemistry of the National Academy of Sciences of the Ukraine, Prospect Nauki 31, Kyiv 03028, Ukraine, cDepartment of Chemistry, Purdue University, 560 Oval Drive, West Lafayette, IN 47907-2084, USA, and dDepartment of Chemistry, Drexel University, Philadelphia, PA 19104-2816, USA
*Correspondence e-mail: annpavlis@ukr.net
Three new isotypic heteropolynuclear complexes, namely pentaaquacarbonatopentakis(glycinehydroxamato)nitratopentacopper(II)lanthanide(III) x-hydrate, [LnCu5(GlyHA)5(CO3)(NO3)(H2O)5]·xH2O (GlyHA2− is glycinehydroxamate, N-hydroxyglycinamidate or aminoacetohydroxamate, C2H4N2O22−), with lanthanide(III) (LnIII) = gadolinium (Gd, 1, x = 3.5), dysprosium (Dy, 2, x = 3.28) and holmium (Ho, 3, x = 3.445), within a 15-metallacrown-5 class were obtained on reaction of lanthanide(III) nitrate, copper(II) acetate and sodium glycinehydroxamate. Complexes 1–3 contain five copper(II) ions and five bridging GlyHA2− anions, forming a [CuGlyHA]5 metallamacrocyclic core. The LnIII ions are coordinated to the metallamacrocycle through five O-donor hydroxamates. The electroneutrality of complexes 1–3 is achieved by a bidentate carbonate anion coordinated to the LnIII ion and a monodentate nitrate anion coordinated apically to one of the copper(II) ions of the metallamacrocycle. The lattice parameters of complexes 1–3 are similar to those previously reported for an EuIII–CuII 15-metallacrown-5 complex with glycinehydroxamate of proposed composition [EuCu5(GlyHA)5(OH)(NO3)2(H2O)4]·3.5H2O [Stemmler et al. (1999). Inorg. Chem. 38, 2807–2817]. High-quality X-ray data obtained for 1–3 have allowed a re-evaluation of the X-ray data solution proposed earlier for the EuCu5 complex and suggest that the formula is actually [EuCu5(GlyHA)5(CO3)(NO3)(H2O)5]·3.5H2O.
1. Chemical context
The numerous studies of 3d–4f metallamacrocyclic complexes in the last few decades arise from their potentially interesting catalytic (Griffiths & Kostakis, 2018), luminescence (Jankolovits et al., 2011; Li et al., 2017) and magnetic properties (Dhers et al., 2016; Zangana et al., 2014). In addition, a number of heteropolynuclear metallacrown complexes have been shown to possess single molecule magnetic (SMM) behaviour (Ostrowska et al., 2016; Wang et al., 2019), bright luminescence with high quantum yields (Nguyen et al., 2018; Martinić et al., 2017) and the ability to serve as building blocks for the generation of supramolecular assemblies and coordination polymers (Pavlishchuk et al., 2014, 2017b). The utilization of heteronuclear cationic 15-metallacrown-5 complexes as initial building blocks has also led to porous structures that are able to absorb various guest molecules (Lim et al., 2010). The selection of the initial building blocks with labile counter-anions (e.g. nitrates) is crucial for the creation of coordination polymers with porous structures. Some of the products of the reactions between glycinehydroxamate-derived 15-metallacrown-5 complexes and polycarboxylates contain carbonate anions (Pavlishchuk et al., 2014, 2017b), which block the apical positions of the LnIII ions and lead to the formation of discrete assemblies instead of coordination polymers. The presence of carbonate anions in such complexes was associated with the capture of atmospheric carbon dioxide (Pavlishchuk et al., 2014, 2017b).
The first examples of 15-metallacrown-5 complexes were reported by Pecoraro and coworkers in 1999 (Stemmler et al., 1999). One of the reported complexes, a EuIII–CuII glycinehydroxamate metallacrown, contains the [CuGlyHA]5 core and encapsulates an EuIII ion through coordination to five hydroxamate oxygen atoms. It was reported that the positive charge of the 15-metallacrown-5 unit, [EuCu5(GlyHA)5]3+, was partly compensated by two nitrate anions coordinated to copper(II) and europium(III). To fully compensate the positive charge of the [EuCu5(GlyHA)5]3+ unit, an oxygen species coordinated apically to EuIII was assigned as a hydroxide anion, to give a reported overall composition [EuCu5(GlyHA)5(OH)(NO3)2(H2O)4]·3.5H2O. The high R-factor of 12.3% for the structure was attributed to the presence of disordered water molecules in the (Stemmler et al., 1999). We report here the crystal structures of three isostructural 15-metallacrown-5 complexes, [LnCu5(GlyHA)5(CO3)(NO3)(H2O)5]·xH2O (LnIII = Gd (1, x = 3.5); Dy (2, x = 3.28) and Ho (3, x = 3.45)). Based on the high-quality diffraction data collected for 1–3, a new formula of [EuCu5(GlyHA)5(CO3)(NO3)(H2O)5]·3.5H2O is proposed for the previously reported Eu compound.
2. Structural commentary and supramolecular features
Complexes 1–3, and the previously reported europium analogue (Stemmler et al., 1999), are isotypic based on the unit-cell parameters obtained (Table 1) and the structure results. The b and c lattice parameters and the unit-cell volumes for these complexes decrease slightly across the lanthanide series as a result of the lanthanide contraction (Pavlishchuk et al., 2011, 2017b, 2018; Stemmler et al., 1999; Zaleski, et al., 2011). All four compounds crystallize in the P and contain two molecular metallamacrocyclic complexes per related to each other through a centre of inversion (Fig. 1). For the convenience of structure description, a common atom-numbering scheme is adopted for 1–3.
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The neutral metallamacrocyclic unit [LnCu5(GlyHA)5(CO3)(NO3)(H2O)5] in 1–3 possesses structural features typical of previously characterized LnIII–CuII hydroxamate 15-metallacrown-5 complexes (Pavlishchuk et al., 2011, 2017a,b, 2018; Stemmler et al., 1999, Zaleski, et al., 2011; Katkova et al., 2015a,b). The metallamacrocyclic core is built from the repeating fragment [CuGlyHA], formed via bridging coordination of GlyHA2− dianions to two adjacent copper(II) ions, forming two five-membered chelate rings (Fig. 2). The coordination environment of the copper(II) ions in 1–3 consists of two nitrogen atoms (from amino and hydroxamate groups) and two oxygen atoms (from carbonyl and hydroxamate groups) in their basal planes. The Cu—O and Cu—N bond lengths in 1–3 are typical for hydroxamate metallacrown complexes (Tables 2–4) and are comparable with the values previously reported for the EuIII analogue (Stemmler et al., 1999). All the copper(II) ions in 1–3 are pentacoordinate, with N2O3 donor sets in slightly distorted square-pyramidal coordination arrangements [τ values (Addison et al., 1984) fall in the range of 0.01–0.20, Tables 5–7]. For all the complexes, a pronounced Jahn-Teller-like distortion is observed, with the Cu—N and Cu—O bonds from glycinehydroxamate in the plane of the metallacrown unit being substantially shorter than the Cu—O bond of the fifth coordination site, the apical position. This site for the Cu2 atom is in each case occupied by the oxygen atom O15 from the monodentate nitrate anions [Cu2—O15 is 2.469 (3) Å in 1, 2.464 (3) Å in 2 and 2.463 (3) Å in 3], while the coordination spheres of the copper(II) ions of Cu1, Cu3, Cu4 and Cu5 ions in 1–3 are completed by oxygen atoms of coordinated water molecules. The Cu—Ow bond distances in 1–3 range from 2.400 (3) to 2.476 (3) Å. The shorter Cu—O and Cu—N bond lengths within the metallacrown plane of 1–3, on the other hand, range from 1.897 (3) to 2.022 (2) Å.
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The centre of the metallamacrocyclic core [CuGlyHA]5 in 1–3 is occupied by GdIII, DyIII and HoIII ions, respectively, which are coordinated through five hydroxamate oxygen atoms from glycinehydroxamate. The equatorial Ln—O bond distances in 1–3 range from 2.381 (2) to 2.484 (2) Å, 2.382 (3) to 2.469 (3) Å and 2.374 (2) to 2.475 (2) Å respectively, paralleling the lanthanide contraction (Table 8). The LnIII ions in 1–3 and the previously reported EuIII analogue are octacoordinate (Fig. 3), and the coordination geometry of the GdIII, DyIII and HoIII ions in 1–3 can be described as triangular dodecahedral (D2d), according to Shape2.1 calculations (Table 9) (Casanova et al., 2005).
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The two LnIII ion apical positions in 1–3 are occupied by oxygen atoms O12 [2.317 (11), 2.27 (2) and 2.304 (16) Å in 1–3] and O13 [2.288 (17), 2.31 (3) and 2.30 (3) Å in 1–3] from the bidentately coordinated carbonate anion, forming the charge-balanced moiety, [LnCu5(GlyHA)5(CO3)(NO3)(H2O)5]. The apical coordination of carbonate dianions to LnIII ions in 15-metallacrown-5 units has been observed previously and can be associated with the capture of atmospheric carbon dioxide (Pavlishchuk et al., 2014, 2017b, 2018). The interpretation of the X-ray data for the previously described isotypic EuIII complex was based on the assumption of bidentate coordination of two nitrates to EuIII ions instead of one nitrate and one carbonate (Stemmler et al., 1999). The reported Ln—O(nitrate) bond distances for the EuIII analogue (Stemmler et al., 1999) are comparable with values for the Ln—O(carbonate) bonds observed in 1–3, and the Eu—O donor previously attributed to a hydroxide ion is assigned here as a water molecule. The third apical position of the LnIII ions in 1–3, trans to the carbonate anion is occupied by an oxygen donor atom, O11w, from a coordinated water molecule [Gd1—O11w = 2.359 (2), Dy1—O11w = 2.357 (3) and Ho1—O11w = 2.358 (2) Å]. The Ln—O bond lengths for terminal Ln—OH and Ln—OH2 are generally very similar, and a clear distinction between water and OH− as the terminal ligand in 1–3 and in the previously reported EuIII analogue cannot reliably be made. Moreover, both Ln—OH and Ln—OH2 bond lengths are strongly dependent on the lanthanide ion radius, its and the coordination geometry (Novitchi et al., 2012; Yang et al., 2013; Yi et al., 2013; Chen et al., 2012; Wang et al., 2012; Gao et al., 2011; Xu et al., 2011; Dai et al., 2011). While no definite conclusions can therefore be drawn from the bond distances involving Ln—O11, the hydrogen-bonding interactions (Tables 10–12) involving O11 are informative. The water molecule, O11w, acts as a hydrogen bonding donor to two water molecules: forming an intramolecular hydrogen bond with coordinated water molecule O24w, as O11w—H11B⋯O24w, and with the non-coordinated water molecule, O25w, via O11w—H11A⋯O25w bond (shown for 1 in Fig. 4). Hydrogen atoms for all three water molecules are clearly resolved in difference electron-density maps (shown for 2 in Fig. 5). In 1–3, one of the non-coordinated water molecules, on the O23w site, was refined as partially occupied [occupancy factors 0.499 (11), 0.280 (14) and 0.445 (11), respectively]. Overall, the observed positions of the H atoms as well as the hydrogen-bonding network itself, based on the positions and distances of the involved oxygen atoms, are incompatible with the assumption of the presence of a hydroxide anion, as previously proposed.
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The LnIII⋯CuII and CuII⋯CuII separations in the metallamacrocyclic cores of 1–3 and their EuIII analogue (Table 8) have values typical of hydroxamate 15-metallacrown-5 complexes (Stemmler et al., 1999). The metallamacrocyclic cores [LnCu5(GlyHA)5]3+ are almost planar: the average deviations of non-hydrogen atoms from the Cu5 mean planes do not exceed 0.2 Å, while the deviations of the Ln ions from the Cu5 mean planes have values typical for 15-metallacrown-5 complexes. (Pavlishchuk et al., 2011, 2017b, 2018; Stemmler et al., 1999; Zaleski, et al., 2011; Katkova et al., 2015a,b). The largest deviations from the Cu5 mean planes are observed for nitrogen atoms N8 from amino groups located on the periphery of the metallamacrocyclic [LnCu5(GlyHA)5]3+ cores (Table 8).
The 15-metallacrown-5 units [LnCu5(GlyHA)5]3+ in 1–3 are non-oligomerised, as is typical for heteropolynuclear 15-metallacrown-5 complexes. The [LnCu5(GlyHA)5(CO3)(NO3)(H2O)5] fragments are linked to each other through an extended system of hydrogen bonds. Carbonates coordinated to LnIII ions link each [LnCu5(GlyHA)5(CO3)(NO3)(H2O)5] unit with two adjacent metallamacrocycles through O13i⋯H2A—N2 [symmetry code: (i) 2 − x, 1 − y, 1 − z] and O13B⋯H18B—O18w bonds. Nitrate anions in [LnCu5(GlyHA)5(CO3)(NO3)(H2O)5] also connect each metallamacrocyclic unit with neighbouring cations via O17ii⋯H10A—N10 hydrogen bonds [symmetry code: (ii) x + 1, y, z]. In addition, water molecules coordinated to the CuII ions in 1–3 also link {LnCu5}3+ cores with adjacent fragments (O18wiii⋯H19B—O19 [symmetry code: (iii) x − 1, y, z], O18w—H18A⋯O4i, O19w—H19A⋯O8iv [symmetry code: (iv) −x + 1, −y, −z], O20w—H20A⋯O10v [symmetry code: (v) −x + 2, −y, −z], O20w—H20B⋯O14vi [symmetry code: (vi) −x + 2, −y + 1, −z], O24w—H24A⋯O2vii [symmetry code: (vii) −x + 2, −y, −z + 1]. Multiple hydrogen bonds connect 15-metallacrown-5 units with non-coordinated water molecules. As mentioned above, one of the the non-coordinated water molecule positions, O23w, is partially occupied, inducing disorder for the nearby carbonate anion, with refined occupancy factors of 0.499 (11), 0.280 (14) and 0.445 (11) in 1–3, respectively (see the Refinement section for details). Bond distances within the anion are biased because of the disorder, so no assignment of nitrate vs carbonate can be made based on expected N—O or C—O bond distances. However, despite this disorder involving the anions neighbouring the partially occupied water molecule, the nature of the entity as a carbonate anion is clearly resolved in difference electron-density maps. Replacement of the carbonate carbon atom, C11, with a nitrogen atom results only in a marginal increase in R value (e.g. 3.10 vs 3.07% for compound 2). Thermal parameters of the `nitrogen' atoms do however become unreasonably large, compared to the neighbouring oxygen atoms, and a positive residual electron density is clearly visible around the central atoms of the anion when refined as nitrogen (Fig. 6).
For the other O3X anion, coordinated to Cu4, the opposite observation can be made, and this anion matches the electron density requirements of a nitrate anion.
In summary, we have synthesized three new metallamacrocyclic (Ln = Gd, Dy and Ho) complexes with glycinehydroxamate, which are isotypic with the first representative of the 15-metallacrown-5 family reported in 1999. The better quality of the new structural data allow us to propose an alternative composition [LnCu5(GlyHA)5(CO3)(NO3)(H2O)5]·xH2O [LnIII = Gd (1, x = 3.5), Dy (2, x = 3.28) and Ho (3, x = 3.45)] for this series of compounds and the previously reported Eu complex (x = 3.5). The cationic charge of the {LnCu5}3+ metallamacrocyclic cores in 1–3 is compensated by a monodentate nitrate anion coordinated to a CuII ion and a bidentate carbonate ion linked to the LnIII ions. The presence of capping carbonate anions in metallacrown building blocks can prevent the formation of coordination polymers based on the metallacrown complex.
3. Synthesis and crystallization
Complexes 1–3 were prepared and isolated as dark-blue single crystals according to the previously reported procedure for the EuIII analogue, using Gd(NO3)3·6H2O, Dy(NO3)3·6H2O and Ho(NO3)3·5H2O, respectively (Stemmler et al., 1999).
4. Refinement
Crystal data, data collection and structure . The three structures are isotypic and were refined using a common structural model.
details are summarized in Table 13
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All carbon- and nitrogen-bound H atoms, while observed in difference density maps, were placed in calculated positions, with C—H distances of 0.99 Å and N—H distances of 0.91 Å. All H-atom positions of the ordered water molecules were clearly resolved in difference electron-density maps and their positions were refined with O—H and H⋯H distances restrained to 0.84 (2) and 1.36 (2) Å, respectively. The H-atom positions of the disordered water moieties were further restrained based on hydrogen-bonding considerations. In the final Uiso values of all H atoms were set to a multiple of their respective with Uiso(H) = 1.2Ueq(C/N) or 1.5Ueq(O).
cycles, the partially occupied H atoms were set to ride on their carrier oxygen atoms.In all three structures, one water molecule position is partially occupied, inducing disorder for the nearby carbonate anion. The two disordered carbonate moieties were restrained to have similar geometries (using SHELXL SAME restraints, esd = 0.02 Å). Uij components of ADPs for disordered atoms closer to each other than 2.0 Å were restrained to be similar within a standard deviation of 0.01 Å2 (SIMU restraint of SHELXL). In 1 and 3, the distance of the water oxygen to one of the carbonate oxygen atoms was restrained to be at least 2.80 (2) Å for the moiety that contains the water molecule [2.75 (2) Å for 2]. Subject to these conditions, the occupancy ratios refined to 0.499 (11) to 0.501 (11) for 1, 0.280 (14) to 0.720 (14) for 2 and 0.445 (11) to 0.555 (11) for 3.
There is an indication of additional disorder involving the partially ordered water molecule nearby the carbonate ion. This additional disorder is not well enough resolved to be independently refined and may cause the B alerts in the 1–3. We opted to not attempt to refine additional potentially highly ambiguous disorder.
files ofSupporting information
https://doi.org/10.1107/S205698901900999X/cq2031sup1.cif
contains datablocks Complex_1, Complex_2, Complex_3, global. DOI:Structure factors: contains datablock Complex_1. DOI: https://doi.org/10.1107/S205698901900999X/cq2031Complex_1sup2.hkl
Structure factors: contains datablock Complex_2. DOI: https://doi.org/10.1107/S205698901900999X/cq2031Complex_2sup3.hkl
Structure factors: contains datablock Complex_3. DOI: https://doi.org/10.1107/S205698901900999X/cq2031Complex_3sup4.hkl
For all structures, data collection: APEX3 (Bruker, 2017); cell
SAINT (Bruker, 2017); data reduction: SAINT (Bruker, 2017); program(s) used to solve structure: SHELXS97 (Sheldrick, 2008); program(s) used to refine structure: SHELXL2018/3 (Sheldrick, 2015), SHELXLE (Hübschle et al., 2011); software used to prepare material for publication: publCIF (Westrip, 2010).[Cu5Gd(C2H4N2O2)5(CO3)(NO3)(H2O)5]·3.5H2O | Z = 2 |
Mr = 1190.49 | F(000) = 1170 |
Triclinic, P1 | Dx = 2.440 Mg m−3 |
a = 11.2057 (15) Å | Mo Kα radiation, λ = 0.71073 Å |
b = 11.5054 (15) Å | Cell parameters from 9949 reflections |
c = 13.2983 (10) Å | θ = 3.1–32.5° |
α = 94.026 (4)° | µ = 5.35 mm−1 |
β = 94.942 (3)° | T = 150 K |
γ = 107.558 (3)° | Rod, blue |
V = 1620.2 (3) Å3 | 0.15 × 0.10 × 0.05 mm |
Bruker AXS D8 Quest CMOS diffractometer | 12399 independent reflections |
Radiation source: sealed tube X-ray source | 9545 reflections with I > 2σ(I) |
Triumph curved graphite crystal monochromator | Rint = 0.056 |
ω and phi scans | θmax = 33.2°, θmin = 3.1° |
Absorption correction: multi-scan (SADABS; Krause et al., 2015) | h = −17→17 |
Tmin = 0.599, Tmax = 0.747 | k = −17→17 |
118155 measured reflections | l = −19→20 |
Refinement on F2 | Secondary atom site location: difference Fourier map |
Least-squares matrix: full | Hydrogen site location: mixed |
R[F2 > 2σ(F2)] = 0.034 | H atoms treated by a mixture of independent and constrained refinement |
wR(F2) = 0.076 | w = 1/[σ2(Fo2) + (0.0346P)2 + 2.5135P] where P = (Fo2 + 2Fc2)/3 |
S = 1.05 | (Δ/σ)max = 0.001 |
12399 reflections | Δρmax = 2.06 e Å−3 |
570 parameters | Δρmin = −1.40 e Å−3 |
135 restraints | Extinction correction: SHELXL-2018/3 (Sheldrick 2015), Fc*=kFc[1+0.001xFc2λ3/sin(2θ)]-1/4 |
Primary atom site location: structure-invariant direct methods | Extinction coefficient: 0.00141 (15) |
Geometry. All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. |
Refinement. A water molecule is partially occupied, inducing disorder for the nearby carbonate anion. The two disordered moieties were restrained to have similar geometries. Uij components of ADPs for disordered atoms closer to each other than 2.0 Angstrom were restrained to be similar. The distance of the water oxygen to one of the carbonate oxygen atoms was restrained to be at least 2.8 Angstrom for the moiety that contains the water molecule. Water H atom positions were refined and O-H and H···H distances were restrained to 0.84 (2) and 1.36 (2) Angstrom, respectively. The water H atom positions of the disordered moiety were further restrained based on hydrogen bonding considerations. Subject to these conditions the occupancy ratio refined to 0.499 (11) to 0.501 (11). |
x | y | z | Uiso*/Ueq | Occ. (<1) | |
C1 | 1.0282 (3) | 0.3071 (3) | 0.5735 (2) | 0.0169 (5) | |
C2 | 1.0133 (3) | 0.3907 (3) | 0.6602 (2) | 0.0198 (6) | |
H2C | 1.011450 | 0.350005 | 0.723478 | 0.024* | |
H2D | 1.085802 | 0.466751 | 0.669686 | 0.024* | |
C3 | 0.6601 (3) | 0.4525 (3) | 0.3876 (2) | 0.0184 (5) | |
C4 | 0.5624 (3) | 0.5110 (3) | 0.3531 (2) | 0.0237 (6) | |
H4C | 0.492326 | 0.489577 | 0.395853 | 0.028* | |
H4D | 0.600253 | 0.601279 | 0.361189 | 0.028* | |
C5 | 0.5301 (3) | 0.2146 (3) | 0.0120 (2) | 0.0180 (5) | |
C6 | 0.4908 (3) | 0.1751 (3) | −0.0995 (2) | 0.0211 (6) | |
H6C | 0.398256 | 0.136861 | −0.110988 | 0.025* | |
H6D | 0.513050 | 0.247914 | −0.137828 | 0.025* | |
C7 | 0.8131 (3) | −0.0807 (3) | −0.0320 (2) | 0.0158 (5) | |
C8 | 0.8535 (3) | −0.1924 (3) | −0.0560 (2) | 0.0185 (5) | |
H8C | 0.778171 | −0.265599 | −0.071359 | 0.022* | |
H8D | 0.899628 | −0.182227 | −0.116646 | 0.022* | |
C9 | 1.1071 (3) | −0.0372 (3) | 0.3184 (2) | 0.0155 (5) | |
C10 | 1.2060 (3) | −0.0372 (3) | 0.4025 (2) | 0.0182 (5) | |
H10C | 1.183398 | −0.118107 | 0.429579 | 0.022* | |
H10D | 1.288131 | −0.023541 | 0.375327 | 0.022* | |
C11 | 1.0002 (9) | 0.3923 (10) | 0.1657 (8) | 0.0187 (17) | 0.499 (11) |
O12 | 0.8812 (8) | 0.3500 (10) | 0.1377 (9) | 0.0268 (16) | 0.499 (11) |
O13 | 1.0398 (17) | 0.3359 (17) | 0.2371 (11) | 0.0221 (18) | 0.499 (11) |
O14 | 1.0726 (7) | 0.4812 (8) | 0.1298 (7) | 0.0296 (16) | 0.499 (11) |
O23 | 1.3130 (8) | 0.5342 (7) | 0.1998 (11) | 0.100 (5) | 0.499 (11) |
H23A | 1.324 (17) | 0.608 (5) | 0.223 (7) | 0.150* | 0.499 (11) |
H23B | 1.242 (5) | 0.491 (7) | 0.171 (13) | 0.150* | 0.499 (11) |
C11B | 1.0371 (9) | 0.3913 (10) | 0.1761 (9) | 0.0210 (18) | 0.501 (11) |
O12B | 0.9211 (8) | 0.3493 (10) | 0.1322 (8) | 0.0280 (16) | 0.501 (11) |
O13B | 1.0555 (17) | 0.3350 (16) | 0.2552 (11) | 0.0231 (19) | 0.501 (11) |
O14B | 1.1203 (8) | 0.4785 (8) | 0.1474 (6) | 0.0319 (18) | 0.501 (11) |
N1 | 0.9476 (2) | 0.2923 (2) | 0.49334 (18) | 0.0184 (5) | |
N2 | 0.8943 (3) | 0.4211 (3) | 0.6387 (2) | 0.0242 (5) | |
H2A | 0.909529 | 0.503064 | 0.653694 | 0.029* | |
H2B | 0.836962 | 0.381155 | 0.679007 | 0.029* | |
N3 | 0.6792 (3) | 0.3745 (2) | 0.32041 (19) | 0.0194 (5) | |
N4 | 0.5128 (3) | 0.4690 (3) | 0.2453 (2) | 0.0321 (7) | |
H4A | 0.541406 | 0.531489 | 0.206441 | 0.038* | |
H4B | 0.427124 | 0.446800 | 0.238524 | 0.038* | |
N5 | 0.6111 (2) | 0.1674 (2) | 0.05484 (18) | 0.0177 (5) | |
N6 | 0.5532 (2) | 0.0865 (2) | −0.13735 (18) | 0.0190 (5) | |
H6A | 0.585643 | 0.108822 | −0.196056 | 0.023* | |
H6B | 0.496054 | 0.010374 | −0.150377 | 0.023* | |
N7 | 0.8504 (2) | −0.0252 (2) | 0.05833 (18) | 0.0161 (4) | |
N8 | 0.9361 (2) | −0.2106 (2) | 0.03158 (19) | 0.0193 (5) | |
H8A | 1.014048 | −0.203019 | 0.012836 | 0.023* | |
H8B | 0.903608 | −0.287467 | 0.050144 | 0.023* | |
N9 | 1.0599 (2) | 0.0527 (2) | 0.32669 (17) | 0.0157 (4) | |
N10 | 1.2174 (3) | 0.0598 (3) | 0.4855 (2) | 0.0236 (5) | |
H10A | 1.297991 | 0.111081 | 0.495577 | 0.028* | |
H10B | 1.199114 | 0.025111 | 0.543971 | 0.028* | |
N11 | 0.5782 (3) | 0.2254 (3) | 0.6118 (2) | 0.0282 (6) | |
Cu1 | 1.09871 (3) | 0.15598 (3) | 0.45052 (3) | 0.01629 (7) | |
Cu2 | 0.82345 (3) | 0.37425 (3) | 0.49429 (3) | 0.01666 (7) | |
Cu3 | 0.56789 (4) | 0.32576 (3) | 0.19730 (3) | 0.01924 (8) | |
Cu4 | 0.69162 (3) | 0.08373 (3) | −0.03230 (3) | 0.01653 (7) | |
Cu5 | 0.95028 (3) | −0.08613 (3) | 0.15079 (3) | 0.01552 (7) | |
Gd1 | 0.84770 (2) | 0.19381 (2) | 0.24301 (2) | 0.01278 (4) | |
O1 | 0.9539 (2) | 0.2085 (2) | 0.41509 (15) | 0.0205 (4) | |
O2 | 1.1140 (2) | 0.2528 (2) | 0.57995 (15) | 0.0193 (4) | |
O3 | 0.7698 (2) | 0.31983 (19) | 0.35249 (15) | 0.0186 (4) | |
O4 | 0.7179 (2) | 0.47939 (19) | 0.47886 (16) | 0.0204 (4) | |
O5 | 0.6439 (2) | 0.2014 (2) | 0.15887 (15) | 0.0208 (4) | |
O6 | 0.4844 (2) | 0.2916 (2) | 0.05861 (16) | 0.0213 (4) | |
O7 | 0.8123 (2) | 0.07808 (19) | 0.07923 (15) | 0.0188 (4) | |
O8 | 0.7441 (2) | −0.04598 (19) | −0.09994 (15) | 0.0184 (4) | |
O9 | 0.97139 (19) | 0.05463 (18) | 0.24655 (15) | 0.0164 (4) | |
O10 | 1.0746 (2) | −0.12244 (19) | 0.24335 (15) | 0.0178 (4) | |
O11 | 0.7121 (2) | 0.0139 (2) | 0.29536 (17) | 0.0213 (4) | |
H11A | 0.643 (3) | 0.014 (4) | 0.316 (3) | 0.032* | |
H11B | 0.719 (4) | −0.056 (2) | 0.281 (3) | 0.032* | |
O15 | 0.6328 (2) | 0.2178 (2) | 0.53415 (19) | 0.0310 (5) | |
O16 | 0.6467 (3) | 0.2508 (4) | 0.6961 (2) | 0.0585 (10) | |
O17 | 0.4642 (3) | 0.2055 (3) | 0.6078 (3) | 0.0426 (7) | |
O18 | 1.2479 (2) | 0.3217 (2) | 0.37422 (18) | 0.0241 (5) | |
H18A | 1.266 (4) | 0.378 (3) | 0.421 (2) | 0.036* | |
H18B | 1.192 (3) | 0.336 (4) | 0.336 (3) | 0.036* | |
O19 | 0.3869 (2) | 0.1932 (2) | 0.26751 (17) | 0.0235 (5) | |
H19A | 0.338 (3) | 0.154 (4) | 0.216 (2) | 0.035* | |
H19B | 0.348 (4) | 0.234 (3) | 0.297 (3) | 0.035* | |
O20 | 0.8216 (2) | 0.2497 (2) | −0.11207 (19) | 0.0283 (5) | |
H20A | 0.844 (4) | 0.221 (4) | −0.165 (2) | 0.042* | |
H20B | 0.839 (4) | 0.3266 (19) | −0.113 (4) | 0.042* | |
O21 | 0.6426 (3) | 0.6180 (2) | 0.0939 (2) | 0.0357 (6) | |
H21A | 0.599 (4) | 0.629 (5) | 0.043 (3) | 0.054* | |
H21B | 0.685 (4) | 0.572 (4) | 0.075 (4) | 0.054* | |
O22 | 0.8172 (4) | 0.5178 (3) | 0.0465 (3) | 0.0538 (9) | |
H22A | 0.824 (6) | 0.514 (6) | −0.0174 (18) | 0.081* | |
H22B | 0.850 (6) | 0.468 (5) | 0.076 (4) | 0.081* | |
O24 | 0.7763 (2) | −0.1972 (2) | 0.24123 (17) | 0.0213 (4) | |
H24A | 0.805 (4) | −0.228 (4) | 0.289 (2) | 0.032* | |
H24B | 0.739 (4) | −0.264 (2) | 0.206 (3) | 0.032* | |
O25 | 0.5128 (2) | 0.0541 (2) | 0.36852 (19) | 0.0266 (5) | |
H25A | 0.477 (4) | 0.102 (4) | 0.340 (3) | 0.040* | |
H25B | 0.541 (4) | 0.095 (4) | 0.425 (2) | 0.040* |
U11 | U22 | U33 | U12 | U13 | U23 | |
C1 | 0.0204 (13) | 0.0140 (12) | 0.0141 (12) | 0.0016 (10) | 0.0034 (10) | 0.0020 (9) |
C2 | 0.0288 (15) | 0.0167 (13) | 0.0115 (12) | 0.0042 (11) | 0.0009 (11) | −0.0007 (10) |
C3 | 0.0241 (14) | 0.0139 (12) | 0.0158 (12) | 0.0040 (11) | 0.0028 (11) | −0.0003 (10) |
C4 | 0.0318 (17) | 0.0204 (14) | 0.0204 (14) | 0.0120 (13) | 0.0012 (12) | −0.0030 (11) |
C5 | 0.0200 (13) | 0.0194 (13) | 0.0147 (12) | 0.0062 (11) | 0.0016 (10) | 0.0022 (10) |
C6 | 0.0246 (15) | 0.0286 (15) | 0.0134 (12) | 0.0143 (12) | −0.0004 (11) | −0.0001 (11) |
C7 | 0.0177 (13) | 0.0158 (12) | 0.0133 (12) | 0.0046 (10) | 0.0019 (10) | 0.0000 (9) |
C8 | 0.0252 (14) | 0.0177 (13) | 0.0133 (12) | 0.0089 (11) | 0.0009 (10) | −0.0027 (10) |
C9 | 0.0164 (12) | 0.0152 (12) | 0.0142 (12) | 0.0040 (10) | 0.0010 (10) | 0.0024 (9) |
C10 | 0.0190 (13) | 0.0186 (13) | 0.0181 (13) | 0.0075 (11) | −0.0003 (10) | 0.0037 (10) |
C11 | 0.019 (4) | 0.021 (3) | 0.016 (3) | 0.006 (3) | 0.003 (3) | −0.002 (2) |
O12 | 0.019 (4) | 0.027 (2) | 0.030 (3) | 0.000 (3) | 0.002 (3) | 0.011 (2) |
O13 | 0.021 (4) | 0.023 (3) | 0.019 (4) | 0.003 (3) | −0.001 (3) | 0.005 (3) |
O14 | 0.027 (4) | 0.027 (3) | 0.028 (3) | −0.003 (3) | 0.003 (3) | 0.006 (2) |
O23 | 0.047 (5) | 0.050 (5) | 0.203 (13) | 0.028 (4) | −0.018 (6) | −0.007 (6) |
C11B | 0.024 (4) | 0.019 (2) | 0.017 (3) | 0.005 (3) | 0.002 (3) | −0.005 (2) |
O12B | 0.026 (4) | 0.027 (2) | 0.024 (3) | −0.003 (3) | 0.001 (3) | 0.011 (2) |
O13B | 0.022 (4) | 0.020 (3) | 0.023 (5) | 0.001 (3) | −0.005 (3) | 0.001 (3) |
O14B | 0.036 (4) | 0.026 (3) | 0.020 (3) | −0.010 (3) | 0.009 (3) | −0.002 (2) |
N1 | 0.0251 (13) | 0.0185 (11) | 0.0115 (10) | 0.0072 (10) | 0.0040 (9) | −0.0032 (9) |
N2 | 0.0282 (14) | 0.0270 (13) | 0.0164 (12) | 0.0092 (11) | −0.0003 (10) | −0.0054 (10) |
N3 | 0.0264 (13) | 0.0174 (11) | 0.0168 (11) | 0.0109 (10) | 0.0008 (10) | 0.0010 (9) |
N4 | 0.056 (2) | 0.0267 (14) | 0.0207 (13) | 0.0252 (14) | −0.0001 (13) | 0.0008 (11) |
N5 | 0.0210 (12) | 0.0238 (12) | 0.0102 (10) | 0.0106 (10) | −0.0005 (9) | −0.0003 (9) |
N6 | 0.0215 (12) | 0.0231 (12) | 0.0123 (10) | 0.0076 (10) | 0.0003 (9) | −0.0002 (9) |
N7 | 0.0213 (12) | 0.0164 (11) | 0.0131 (10) | 0.0106 (9) | −0.0004 (9) | −0.0011 (8) |
N8 | 0.0221 (12) | 0.0195 (12) | 0.0177 (11) | 0.0098 (10) | −0.0006 (9) | −0.0011 (9) |
N9 | 0.0177 (11) | 0.0159 (11) | 0.0130 (10) | 0.0054 (9) | −0.0021 (8) | 0.0007 (8) |
N10 | 0.0225 (13) | 0.0275 (13) | 0.0199 (12) | 0.0088 (11) | −0.0050 (10) | 0.0003 (10) |
N11 | 0.0271 (14) | 0.0270 (14) | 0.0263 (14) | 0.0020 (11) | 0.0040 (11) | 0.0032 (11) |
Cu1 | 0.01724 (16) | 0.01941 (16) | 0.01143 (15) | 0.00596 (13) | −0.00150 (12) | −0.00123 (12) |
Cu2 | 0.02216 (18) | 0.01550 (16) | 0.01149 (15) | 0.00558 (13) | 0.00110 (13) | −0.00207 (12) |
Cu3 | 0.02855 (19) | 0.01987 (17) | 0.01282 (15) | 0.01423 (15) | −0.00091 (14) | −0.00107 (13) |
Cu4 | 0.01952 (17) | 0.02133 (17) | 0.01026 (15) | 0.01014 (14) | −0.00125 (12) | −0.00179 (12) |
Cu5 | 0.01973 (17) | 0.01519 (15) | 0.01250 (15) | 0.00790 (13) | −0.00066 (12) | −0.00106 (12) |
Gd1 | 0.01725 (7) | 0.01235 (6) | 0.00865 (6) | 0.00532 (5) | −0.00028 (4) | −0.00060 (4) |
O1 | 0.0234 (11) | 0.0277 (11) | 0.0114 (9) | 0.0128 (9) | −0.0023 (8) | −0.0074 (8) |
O2 | 0.0218 (10) | 0.0217 (10) | 0.0135 (9) | 0.0064 (8) | −0.0011 (8) | 0.0008 (8) |
O3 | 0.0256 (11) | 0.0203 (10) | 0.0129 (9) | 0.0124 (8) | 0.0000 (8) | 0.0001 (7) |
O4 | 0.0254 (11) | 0.0190 (10) | 0.0159 (9) | 0.0065 (8) | 0.0025 (8) | −0.0031 (8) |
O5 | 0.0281 (11) | 0.0277 (11) | 0.0102 (9) | 0.0170 (9) | −0.0026 (8) | −0.0049 (8) |
O6 | 0.0283 (11) | 0.0263 (11) | 0.0142 (9) | 0.0169 (9) | −0.0010 (8) | 0.0004 (8) |
O7 | 0.0251 (11) | 0.0193 (10) | 0.0150 (9) | 0.0139 (8) | −0.0021 (8) | −0.0036 (7) |
O8 | 0.0233 (10) | 0.0213 (10) | 0.0119 (9) | 0.0107 (8) | −0.0013 (8) | −0.0025 (7) |
O9 | 0.0198 (10) | 0.0170 (9) | 0.0125 (9) | 0.0083 (8) | −0.0047 (7) | −0.0016 (7) |
O10 | 0.0209 (10) | 0.0176 (9) | 0.0163 (9) | 0.0090 (8) | 0.0005 (8) | 0.0003 (7) |
O11 | 0.0194 (10) | 0.0185 (10) | 0.0254 (11) | 0.0043 (8) | 0.0041 (9) | 0.0024 (8) |
O15 | 0.0318 (13) | 0.0314 (13) | 0.0280 (12) | 0.0052 (10) | 0.0081 (10) | 0.0059 (10) |
O16 | 0.0445 (18) | 0.087 (3) | 0.0234 (14) | −0.0098 (17) | 0.0007 (13) | 0.0051 (15) |
O17 | 0.0271 (13) | 0.0321 (14) | 0.070 (2) | 0.0112 (11) | 0.0091 (13) | −0.0005 (14) |
O18 | 0.0274 (12) | 0.0211 (11) | 0.0230 (11) | 0.0090 (9) | −0.0002 (9) | −0.0060 (9) |
O19 | 0.0230 (11) | 0.0295 (12) | 0.0177 (10) | 0.0101 (9) | −0.0006 (8) | −0.0041 (9) |
O20 | 0.0317 (13) | 0.0248 (12) | 0.0303 (13) | 0.0103 (10) | 0.0089 (10) | 0.0017 (10) |
O21 | 0.0499 (17) | 0.0296 (13) | 0.0284 (13) | 0.0187 (12) | −0.0119 (12) | 0.0000 (10) |
O22 | 0.091 (3) | 0.0470 (18) | 0.0389 (17) | 0.0372 (18) | 0.0265 (18) | 0.0148 (15) |
O24 | 0.0249 (11) | 0.0196 (10) | 0.0181 (10) | 0.0060 (9) | −0.0014 (8) | 0.0027 (8) |
O25 | 0.0262 (12) | 0.0255 (12) | 0.0279 (12) | 0.0083 (10) | 0.0031 (10) | 0.0008 (9) |
C1—O2 | 1.296 (4) | N5—Cu4 | 1.906 (2) |
C1—N1 | 1.303 (4) | N6—Cu4 | 2.005 (2) |
C1—C2 | 1.501 (4) | N6—H6A | 0.9100 |
C2—N2 | 1.488 (4) | N6—H6B | 0.9100 |
C2—H2C | 0.9900 | N7—O7 | 1.397 (3) |
C2—H2D | 0.9900 | N7—Cu5 | 1.901 (2) |
C3—O4 | 1.295 (4) | N8—Cu5 | 2.022 (2) |
C3—N3 | 1.298 (4) | N8—H8A | 0.9100 |
C3—C4 | 1.505 (4) | N8—H8B | 0.9100 |
C4—N4 | 1.483 (4) | N9—O9 | 1.398 (3) |
C4—H4C | 0.9900 | N9—Cu1 | 1.898 (2) |
C4—H4D | 0.9900 | N10—Cu1 | 2.016 (3) |
C5—O6 | 1.298 (4) | N10—H10A | 0.9100 |
C5—N5 | 1.302 (4) | N10—H10B | 0.9100 |
C5—C6 | 1.506 (4) | N11—O17 | 1.223 (4) |
C6—N6 | 1.485 (4) | N11—O15 | 1.255 (4) |
C6—H6C | 0.9900 | N11—O16 | 1.266 (4) |
C6—H6D | 0.9900 | Cu1—O1 | 1.929 (2) |
C7—N7 | 1.292 (4) | Cu1—O2 | 1.949 (2) |
C7—O8 | 1.301 (3) | Cu1—O18 | 2.470 (3) |
C7—C8 | 1.509 (4) | Cu2—O3 | 1.929 (2) |
C8—N8 | 1.490 (4) | Cu2—O4 | 1.939 (2) |
C8—H8C | 0.9900 | Cu2—O15 | 2.469 (3) |
C8—H8D | 0.9900 | Cu3—O5 | 1.935 (2) |
C9—O10 | 1.294 (3) | Cu3—O6 | 1.952 (2) |
C9—N9 | 1.298 (4) | Cu3—O19 | 2.444 (2) |
C9—C10 | 1.506 (4) | Cu4—O7 | 1.938 (2) |
C10—N10 | 1.482 (4) | Cu4—O8 | 1.953 (2) |
C10—H10C | 0.9900 | Cu4—O20 | 2.401 (3) |
C10—H10D | 0.9900 | Cu5—O9 | 1.931 (2) |
C11—O14 | 1.252 (9) | Cu5—O10 | 1.939 (2) |
C11—O12 | 1.284 (9) | Cu5—O24 | 2.449 (2) |
C11—O13 | 1.307 (10) | Gd1—O11 | 2.359 (2) |
C11—Gd1 | 2.733 (10) | Gd1—O3 | 2.381 (2) |
O12—Gd1 | 2.317 (11) | Gd1—O7 | 2.408 (2) |
O13—Gd1 | 2.288 (17) | Gd1—O9 | 2.414 (2) |
O23—H23A | 0.851 (19) | Gd1—O1 | 2.457 (2) |
O23—H23B | 0.84 (2) | Gd1—O5 | 2.483 (2) |
C11B—O14B | 1.253 (9) | O11—H11A | 0.840 (19) |
C11B—O13B | 1.307 (10) | O11—H11B | 0.838 (19) |
C11B—O12B | 1.310 (10) | O18—H18A | 0.829 (19) |
C11B—Gd1 | 2.857 (10) | O18—H18B | 0.830 (19) |
O12B—Gd1 | 2.396 (10) | O19—H19A | 0.844 (19) |
O13B—Gd1 | 2.388 (17) | O19—H19B | 0.836 (19) |
N1—O1 | 1.389 (3) | O20—H20A | 0.847 (19) |
N1—Cu2 | 1.902 (3) | O20—H20B | 0.849 (19) |
N2—Cu2 | 1.985 (3) | O21—H21A | 0.840 (19) |
N2—H2A | 0.9100 | O21—H21B | 0.849 (19) |
N2—H2B | 0.9100 | O22—H22A | 0.86 (2) |
N3—O3 | 1.399 (3) | O22—H22B | 0.87 (2) |
N3—Cu3 | 1.910 (3) | O24—H24A | 0.833 (19) |
N4—Cu3 | 2.010 (3) | O24—H24B | 0.839 (19) |
N4—H4A | 0.9100 | O25—H25A | 0.861 (19) |
N4—H4B | 0.9100 | O25—H25B | 0.845 (19) |
N5—O5 | 1.397 (3) | ||
O2—C1—N1 | 123.2 (3) | O4—Cu2—O15 | 86.11 (9) |
O2—C1—C2 | 121.7 (3) | N2—Cu2—O15 | 93.88 (11) |
N1—C1—C2 | 115.1 (3) | N3—Cu3—O5 | 90.98 (10) |
N2—C2—C1 | 109.7 (2) | N3—Cu3—O6 | 168.46 (11) |
N2—C2—H2C | 109.7 | O5—Cu3—O6 | 85.44 (9) |
C1—C2—H2C | 109.7 | N3—Cu3—N4 | 82.70 (12) |
N2—C2—H2D | 109.7 | O5—Cu3—N4 | 172.15 (13) |
C1—C2—H2D | 109.7 | O6—Cu3—N4 | 99.85 (11) |
H2C—C2—H2D | 108.2 | N3—Cu3—O19 | 97.56 (10) |
O4—C3—N3 | 124.2 (3) | O5—Cu3—O19 | 97.57 (9) |
O4—C3—C4 | 120.7 (3) | O6—Cu3—O19 | 93.78 (9) |
N3—C3—C4 | 115.1 (3) | N4—Cu3—O19 | 87.90 (12) |
N4—C4—C3 | 110.7 (2) | N5—Cu4—O7 | 91.39 (9) |
N4—C4—H4C | 109.5 | N5—Cu4—O8 | 161.67 (10) |
C3—C4—H4C | 109.5 | O7—Cu4—O8 | 84.56 (8) |
N4—C4—H4D | 109.5 | N5—Cu4—N6 | 83.88 (10) |
C3—C4—H4D | 109.5 | O7—Cu4—N6 | 174.00 (10) |
H4C—C4—H4D | 108.1 | O8—Cu4—N6 | 98.79 (9) |
O6—C5—N5 | 124.4 (3) | N5—Cu4—O20 | 101.61 (10) |
O6—C5—C6 | 120.0 (3) | O7—Cu4—O20 | 99.20 (9) |
N5—C5—C6 | 115.6 (3) | O8—Cu4—O20 | 96.69 (9) |
N6—C6—C5 | 111.2 (2) | N6—Cu4—O20 | 85.40 (10) |
N6—C6—H6C | 109.4 | N7—Cu5—O9 | 89.59 (9) |
C5—C6—H6C | 109.4 | N7—Cu5—O10 | 170.23 (10) |
N6—C6—H6D | 109.4 | O9—Cu5—O10 | 85.57 (8) |
C5—C6—H6D | 109.4 | N7—Cu5—N8 | 83.14 (10) |
H6C—C6—H6D | 108.0 | O9—Cu5—N8 | 169.38 (10) |
N7—C7—O8 | 123.8 (3) | O10—Cu5—N8 | 100.42 (9) |
N7—C7—C8 | 116.0 (2) | N7—Cu5—O24 | 95.81 (9) |
O8—C7—C8 | 120.2 (2) | O9—Cu5—O24 | 87.44 (8) |
N8—C8—C7 | 110.4 (2) | O10—Cu5—O24 | 92.45 (8) |
N8—C8—H8C | 109.6 | N8—Cu5—O24 | 100.96 (9) |
C7—C8—H8C | 109.6 | O13—Gd1—O12 | 56.4 (3) |
N8—C8—H8D | 109.6 | O13—Gd1—O11 | 153.9 (3) |
C7—C8—H8D | 109.6 | O12—Gd1—O11 | 149.4 (2) |
H8C—C8—H8D | 108.1 | O13—Gd1—O3 | 96.0 (6) |
O10—C9—N9 | 123.9 (3) | O12—Gd1—O3 | 86.3 (3) |
O10—C9—C10 | 120.3 (2) | O11—Gd1—O3 | 91.62 (8) |
N9—C9—C10 | 115.8 (2) | O11—Gd1—O13B | 147.7 (3) |
N10—C10—C9 | 110.9 (2) | O3—Gd1—O13B | 95.0 (5) |
N10—C10—H10C | 109.5 | O11—Gd1—O12B | 156.6 (2) |
C9—C10—H10C | 109.5 | O3—Gd1—O12B | 94.1 (3) |
N10—C10—H10D | 109.5 | O13B—Gd1—O12B | 54.1 (3) |
C9—C10—H10D | 109.5 | O13—Gd1—O7 | 102.1 (5) |
H10C—C10—H10D | 108.0 | O12—Gd1—O7 | 79.3 (3) |
O14—C11—O12 | 123.6 (9) | O11—Gd1—O7 | 85.23 (8) |
O14—C11—O13 | 122.2 (9) | O3—Gd1—O7 | 144.85 (7) |
O12—C11—O13 | 114.2 (9) | O13B—Gd1—O7 | 106.2 (5) |
O14—C11—Gd1 | 178.1 (8) | O12B—Gd1—O7 | 77.1 (3) |
O12—C11—Gd1 | 57.7 (6) | O13—Gd1—O9 | 82.7 (5) |
O13—C11—Gd1 | 56.5 (7) | O12—Gd1—O9 | 122.3 (2) |
C11—O12—Gd1 | 94.3 (7) | O11—Gd1—O9 | 75.95 (7) |
C11—O13—Gd1 | 95.0 (8) | O3—Gd1—O9 | 141.57 (7) |
H23A—O23—H23B | 119 (10) | O13B—Gd1—O9 | 79.4 (5) |
O14B—C11B—O13B | 123.7 (10) | O12B—Gd1—O9 | 111.8 (3) |
O14B—C11B—O12B | 123.8 (9) | O7—Gd1—O9 | 71.27 (6) |
O13B—C11B—O12B | 112.5 (9) | O13—Gd1—O1 | 76.8 (3) |
O14B—C11B—Gd1 | 179.5 (9) | O12—Gd1—O1 | 125.7 (3) |
O13B—C11B—Gd1 | 56.1 (7) | O11—Gd1—O1 | 81.98 (8) |
O12B—C11B—Gd1 | 56.4 (5) | O3—Gd1—O1 | 71.71 (7) |
C11B—O12B—Gd1 | 96.5 (7) | O13B—Gd1—O1 | 70.3 (3) |
C11B—O13B—Gd1 | 96.9 (8) | O12B—Gd1—O1 | 121.3 (2) |
C1—N1—O1 | 116.0 (2) | O7—Gd1—O1 | 141.68 (7) |
C1—N1—Cu2 | 119.25 (19) | O9—Gd1—O1 | 70.62 (7) |
O1—N1—Cu2 | 124.58 (18) | O13—Gd1—O5 | 125.4 (3) |
C2—N2—Cu2 | 111.49 (18) | O12—Gd1—O5 | 69.6 (2) |
C2—N2—H2A | 109.3 | O11—Gd1—O5 | 80.69 (8) |
Cu2—N2—H2A | 109.3 | O3—Gd1—O5 | 72.08 (7) |
C2—N2—H2B | 109.3 | O13B—Gd1—O5 | 131.3 (3) |
Cu2—N2—H2B | 109.3 | O12B—Gd1—O5 | 79.6 (2) |
H2A—N2—H2B | 108.0 | O7—Gd1—O5 | 72.87 (7) |
C3—N3—O3 | 115.2 (2) | O9—Gd1—O5 | 138.36 (7) |
C3—N3—Cu3 | 118.8 (2) | O1—Gd1—O5 | 139.11 (7) |
O3—N3—Cu3 | 125.28 (18) | O13—Gd1—C11 | 28.5 (3) |
C4—N4—Cu3 | 110.4 (2) | O12—Gd1—C11 | 27.9 (2) |
C4—N4—H4A | 109.6 | O11—Gd1—C11 | 175.0 (3) |
Cu3—N4—H4A | 109.6 | O3—Gd1—C11 | 92.2 (3) |
C4—N4—H4B | 109.6 | O7—Gd1—C11 | 89.8 (3) |
Cu3—N4—H4B | 109.6 | O9—Gd1—C11 | 102.9 (2) |
H4A—N4—H4B | 108.1 | O1—Gd1—C11 | 102.3 (2) |
C5—N5—O5 | 115.2 (2) | O5—Gd1—C11 | 97.4 (2) |
C5—N5—Cu4 | 117.2 (2) | O11—Gd1—C11B | 171.5 (2) |
O5—N5—Cu4 | 126.74 (18) | O3—Gd1—C11B | 95.6 (2) |
C6—N6—Cu4 | 109.20 (18) | O13B—Gd1—C11B | 27.0 (2) |
C6—N6—H6A | 109.8 | O12B—Gd1—C11B | 27.1 (2) |
Cu4—N6—H6A | 109.8 | O7—Gd1—C11B | 91.4 (2) |
C6—N6—H6B | 109.8 | O9—Gd1—C11B | 95.6 (2) |
Cu4—N6—H6B | 109.8 | O1—Gd1—C11B | 96.0 (2) |
H6A—N6—H6B | 108.3 | O5—Gd1—C11B | 105.8 (2) |
C7—N7—O7 | 115.2 (2) | N1—O1—Cu1 | 107.85 (16) |
C7—N7—Cu5 | 119.6 (2) | N1—O1—Gd1 | 123.02 (16) |
O7—N7—Cu5 | 125.20 (17) | Cu1—O1—Gd1 | 125.67 (9) |
C8—N8—Cu5 | 110.78 (17) | C1—O2—Cu1 | 107.29 (17) |
C8—N8—H8A | 109.5 | N3—O3—Cu2 | 107.71 (15) |
Cu5—N8—H8A | 109.5 | N3—O3—Gd1 | 123.98 (15) |
C8—N8—H8B | 109.5 | Cu2—O3—Gd1 | 128.20 (10) |
Cu5—N8—H8B | 109.5 | C3—O4—Cu2 | 106.89 (18) |
H8A—N8—H8B | 108.1 | N5—O5—Cu3 | 107.81 (16) |
C9—N9—O9 | 115.5 (2) | N5—O5—Gd1 | 120.57 (16) |
C9—N9—Cu1 | 118.54 (19) | Cu3—O5—Gd1 | 123.24 (10) |
O9—N9—Cu1 | 125.47 (17) | C5—O6—Cu3 | 106.60 (18) |
C10—N10—Cu1 | 110.37 (18) | N7—O7—Cu4 | 107.98 (15) |
C10—N10—H10A | 109.6 | N7—O7—Gd1 | 124.61 (15) |
Cu1—N10—H10A | 109.6 | Cu4—O7—Gd1 | 125.52 (9) |
C10—N10—H10B | 109.6 | C7—O8—Cu4 | 106.96 (17) |
Cu1—N10—H10B | 109.6 | N9—O9—Cu5 | 107.74 (15) |
H10A—N10—H10B | 108.1 | N9—O9—Gd1 | 125.05 (15) |
O17—N11—O15 | 122.5 (3) | Cu5—O9—Gd1 | 126.68 (9) |
O17—N11—O16 | 120.9 (3) | C9—O10—Cu5 | 107.26 (17) |
O15—N11—O16 | 116.5 (3) | Gd1—O11—H11A | 120 (3) |
N9—Cu1—O1 | 89.32 (9) | Gd1—O11—H11B | 122 (3) |
N9—Cu1—O2 | 172.09 (10) | H11A—O11—H11B | 115 (4) |
O1—Cu1—O2 | 85.28 (9) | N11—O15—Cu2 | 124.8 (2) |
N9—Cu1—N10 | 83.70 (10) | Cu1—O18—H18A | 101 (3) |
O1—Cu1—N10 | 165.70 (11) | Cu1—O18—H18B | 94 (3) |
O2—Cu1—N10 | 100.27 (10) | H18A—O18—H18B | 104 (4) |
N9—Cu1—O18 | 91.70 (9) | Cu3—O19—H19A | 105 (3) |
O1—Cu1—O18 | 95.08 (9) | Cu3—O19—H19B | 111 (3) |
O2—Cu1—O18 | 94.54 (8) | H19A—O19—H19B | 106 (4) |
N10—Cu1—O18 | 97.58 (10) | Cu4—O20—H20A | 109 (3) |
N1—Cu2—O3 | 90.48 (9) | Cu4—O20—H20B | 140 (3) |
N1—Cu2—O4 | 168.71 (10) | H20A—O20—H20B | 108 (4) |
O3—Cu2—O4 | 85.63 (9) | H21A—O21—H21B | 110 (5) |
N1—Cu2—N2 | 82.87 (11) | H22A—O22—H22B | 111 (6) |
O3—Cu2—N2 | 173.32 (10) | Cu5—O24—H24A | 109 (3) |
O4—Cu2—N2 | 100.83 (10) | Cu5—O24—H24B | 107 (3) |
N1—Cu2—O15 | 104.38 (10) | H24A—O24—H24B | 95 (4) |
O3—Cu2—O15 | 88.22 (9) | H25A—O25—H25B | 100 (4) |
O2—C1—C2—N2 | −169.6 (3) | C10—C9—N9—Cu1 | −9.9 (3) |
N1—C1—C2—N2 | 9.2 (4) | C9—C10—N10—Cu1 | −1.5 (3) |
O4—C3—C4—N4 | 178.1 (3) | C9—N9—Cu1—O1 | −160.3 (2) |
N3—C3—C4—N4 | −2.6 (4) | O9—N9—Cu1—O1 | 11.1 (2) |
O6—C5—C6—N6 | −179.6 (3) | C9—N9—Cu1—N10 | 7.2 (2) |
N5—C5—C6—N6 | 0.9 (4) | O9—N9—Cu1—N10 | 178.6 (2) |
N7—C7—C8—N8 | −3.0 (4) | C9—N9—Cu1—O18 | 104.6 (2) |
O8—C7—C8—N8 | 177.5 (2) | O9—N9—Cu1—O18 | −84.0 (2) |
O10—C9—C10—N10 | −173.5 (3) | C1—N1—O1—Cu1 | −6.3 (3) |
N9—C9—C10—N10 | 7.1 (4) | Cu2—N1—O1—Cu1 | 178.65 (14) |
O14—C11—O12—Gd1 | 178.3 (11) | C1—N1—O1—Gd1 | −166.34 (19) |
O13—C11—O12—Gd1 | −3.1 (13) | Cu2—N1—O1—Gd1 | 18.6 (3) |
O14—C11—O13—Gd1 | −178.2 (10) | N1—C1—O2—Cu1 | 1.7 (3) |
O12—C11—O13—Gd1 | 3.2 (13) | C2—C1—O2—Cu1 | −179.6 (2) |
O14B—C11B—O12B—Gd1 | −179.5 (10) | C3—N3—O3—Cu2 | 4.8 (3) |
O13B—C11B—O12B—Gd1 | −1.7 (13) | Cu3—N3—O3—Cu2 | −165.22 (15) |
O14B—C11B—O13B—Gd1 | 179.5 (10) | C3—N3—O3—Gd1 | −171.5 (2) |
O12B—C11B—O13B—Gd1 | 1.7 (13) | Cu3—N3—O3—Gd1 | 18.4 (3) |
O2—C1—N1—O1 | 3.2 (4) | N3—C3—O4—Cu2 | −3.9 (4) |
C2—C1—N1—O1 | −175.5 (2) | C4—C3—O4—Cu2 | 175.3 (2) |
O2—C1—N1—Cu2 | 178.5 (2) | C5—N5—O5—Cu3 | −6.9 (3) |
C2—C1—N1—Cu2 | −0.2 (3) | Cu4—N5—O5—Cu3 | 161.96 (15) |
C1—C2—N2—Cu2 | −13.4 (3) | C5—N5—O5—Gd1 | −156.0 (2) |
O4—C3—N3—O3 | −0.6 (4) | Cu4—N5—O5—Gd1 | 12.8 (3) |
C4—C3—N3—O3 | −179.9 (2) | N5—C5—O6—Cu3 | 3.2 (4) |
O4—C3—N3—Cu3 | 170.1 (2) | C6—C5—O6—Cu3 | −176.2 (2) |
C4—C3—N3—Cu3 | −9.1 (4) | C7—N7—O7—Cu4 | 9.2 (3) |
C3—C4—N4—Cu3 | 11.8 (3) | Cu5—N7—O7—Cu4 | −171.09 (14) |
O6—C5—N5—O5 | 2.5 (4) | C7—N7—O7—Gd1 | 174.27 (19) |
C6—C5—N5—O5 | −178.0 (2) | Cu5—N7—O7—Gd1 | −6.0 (3) |
O6—C5—N5—Cu4 | −167.4 (2) | N7—C7—O8—Cu4 | −8.2 (3) |
C6—C5—N5—Cu4 | 12.1 (4) | C8—C7—O8—Cu4 | 171.2 (2) |
C5—C6—N6—Cu4 | −12.1 (3) | C9—N9—O9—Cu5 | 1.1 (3) |
O8—C7—N7—O7 | −0.7 (4) | Cu1—N9—O9—Cu5 | −170.58 (13) |
C8—C7—N7—O7 | 179.9 (2) | C9—N9—O9—Gd1 | 173.21 (19) |
O8—C7—N7—Cu5 | 179.6 (2) | Cu1—N9—O9—Gd1 | 1.5 (3) |
C8—C7—N7—Cu5 | 0.2 (4) | N9—C9—O10—Cu5 | 1.1 (3) |
C7—C8—N8—Cu5 | 4.2 (3) | C10—C9—O10—Cu5 | −178.2 (2) |
O10—C9—N9—O9 | −1.6 (4) | O17—N11—O15—Cu2 | 131.9 (3) |
C10—C9—N9—O9 | 177.8 (2) | O16—N11—O15—Cu2 | −50.5 (4) |
O10—C9—N9—Cu1 | 170.7 (2) |
D—H···A | D—H | H···A | D···A | D—H···A |
O23—H23A···O16i | 0.85 (2) | 1.81 (2) | 2.642 (10) | 165 (10) |
O23—H23B···O14 | 0.84 (2) | 1.90 (2) | 2.644 (10) | 148 (5) |
N2—H2A···O13i | 0.91 | 2.17 | 3.00 (2) | 151 |
N2—H2A···O13Bi | 0.91 | 2.06 | 2.92 (2) | 157 |
N2—H2B···O16 | 0.91 | 2.25 | 3.068 (4) | 150 |
N4—H4A···O21 | 0.91 | 2.08 | 2.932 (4) | 155 |
N4—H4B···O23ii | 0.91 | 1.91 | 2.604 (8) | 132 |
N6—H6A···O16iii | 0.91 | 2.24 | 3.061 (4) | 150 |
N6—H6B···N5iv | 0.91 | 2.53 | 3.268 (4) | 139 |
N6—H6B···O5iv | 0.91 | 2.46 | 3.357 (4) | 171 |
N8—H8A···O7v | 0.91 | 2.51 | 3.299 (4) | 145 |
N8—H8A···O20v | 0.91 | 2.39 | 3.005 (4) | 125 |
N8—H8B···O22vi | 0.91 | 2.15 | 3.033 (4) | 163 |
N10—H10A···O17vii | 0.91 | 2.22 | 3.025 (4) | 146 |
N10—H10B···O11viii | 0.91 | 2.41 | 3.192 (4) | 145 |
O11—H11A···O25 | 0.84 (2) | 1.84 (2) | 2.662 (3) | 166 (4) |
O11—H11B···O24 | 0.84 (2) | 1.98 (2) | 2.798 (3) | 167 (4) |
O18—H18A···O4i | 0.83 (2) | 1.99 (2) | 2.813 (3) | 169 (4) |
O18—H18B···O13 | 0.83 (2) | 2.07 (2) | 2.886 (14) | 170 (4) |
O18—H18B···O13B | 0.83 (2) | 1.79 (2) | 2.612 (14) | 169 (5) |
O19—H19A···O8iv | 0.84 (2) | 1.89 (2) | 2.719 (3) | 167 (4) |
O19—H19B···O18ii | 0.84 (2) | 2.01 (2) | 2.847 (3) | 176 (4) |
O20—H20A···O10v | 0.85 (2) | 1.96 (3) | 2.750 (3) | 156 (5) |
O20—H20B···O14ix | 0.85 (2) | 2.17 (2) | 2.997 (9) | 165 (4) |
O20—H20B···O14Bix | 0.85 (2) | 2.24 (2) | 3.075 (9) | 169 (4) |
O21—H21A···O6x | 0.84 (2) | 2.00 (2) | 2.813 (3) | 163 (5) |
O21—H21B···O22 | 0.85 (2) | 1.83 (2) | 2.650 (5) | 162 (5) |
O22—H22A···O14ix | 0.86 (2) | 1.96 (4) | 2.742 (9) | 150 (6) |
O22—H22A···O14Bix | 0.86 (2) | 1.89 (3) | 2.730 (8) | 166 (6) |
O22—H22B···O12 | 0.87 (2) | 1.74 (3) | 2.594 (12) | 168 (6) |
O22—H22B···O14 | 0.87 (2) | 2.49 (5) | 3.137 (9) | 131 (5) |
O22—H22B···O12B | 0.87 (2) | 1.94 (2) | 2.803 (11) | 176 (6) |
O24—H24A···O2viii | 0.83 (2) | 1.98 (2) | 2.785 (3) | 163 (4) |
O24—H24B···O21vi | 0.84 (2) | 1.95 (2) | 2.755 (3) | 161 (4) |
O25—H25A···O19 | 0.86 (2) | 1.92 (2) | 2.773 (3) | 173 (5) |
O25—H25B···O15 | 0.85 (2) | 1.93 (2) | 2.754 (4) | 166 (4) |
Symmetry codes: (i) −x+2, −y+1, −z+1; (ii) x−1, y, z; (iii) x, y, z−1; (iv) −x+1, −y, −z; (v) −x+2, −y, −z; (vi) x, y−1, z; (vii) x+1, y, z; (viii) −x+2, −y, −z+1; (ix) −x+2, −y+1, −z; (x) −x+1, −y+1, −z. |
[Cu5Dy(C2H4N2O2)5(CO3)(NO3)(H2O)5]·3.28H2O | Z = 2 |
Mr = 1191.77 | F(000) = 1170 |
Triclinic, P1 | Dx = 2.460 Mg m−3 |
a = 11.1083 (5) Å | Mo Kα radiation, λ = 0.71073 Å |
b = 11.4991 (5) Å | Cell parameters from 9708 reflections |
c = 13.2894 (6) Å | θ = 3.1–28.6° |
α = 93.9235 (16)° | µ = 5.65 mm−1 |
β = 94.7713 (17)° | T = 150 K |
γ = 107.1470 (17)° | Block, blue |
V = 1608.73 (13) Å3 | 0.25 × 0.21 × 0.11 mm |
Bruker AXS D8 Quest CMOS diffractometer | 8274 independent reflections |
Radiation source: sealed tube X-ray source | 6997 reflections with I > 2σ(I) |
Triumph curved graphite crystal monochromator | Rint = 0.048 |
ω and phi scans | θmax = 28.7°, θmin = 3.1° |
Absorption correction: multi-scan (SADABS; Krause et al., 2015) | h = −14→14 |
Tmin = 0.648, Tmax = 0.754 | k = −15→15 |
74286 measured reflections | l = −17→17 |
Refinement on F2 | Secondary atom site location: difference Fourier map |
Least-squares matrix: full | Hydrogen site location: mixed |
R[F2 > 2σ(F2)] = 0.031 | H atoms treated by a mixture of independent and constrained refinement |
wR(F2) = 0.076 | w = 1/[σ2(Fo2) + (0.0283P)2 + 7.9239P] where P = (Fo2 + 2Fc2)/3 |
S = 1.08 | (Δ/σ)max = 0.001 |
8274 reflections | Δρmax = 0.99 e Å−3 |
564 parameters | Δρmin = −1.26 e Å−3 |
133 restraints | Extinction correction: SHELXL-2018/3 (Sheldrick 2015), Fc*=kFc[1+0.001xFc2λ3/sin(2θ)]-1/4 |
Primary atom site location: structure-invariant direct methods | Extinction coefficient: 0.00073 (12) |
Geometry. All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. |
Refinement. The structure is isotypic to its Gd analogue, AVP815, and was solved by isomorphous replacement. A water molecule is partially occupied, inducing disorder for the nearby carbonate anion. The two disordered moieties were restrained to have similar geometries. Uij components of ADPs for disordered atoms closer to each other than 2.0 Angstrom were restrained to be similar. The distance of the water oxygen to one of the carbonate oxygen atoms was restrained to be at least 2.75 Angstrom for the moiety that contains the water molecule. Water H atom positions were refined and O-H and H···H distances were restrained to 0.84 (2) and 1.36 (2) Angstrom, respectively. The water H atom positions of the disordered moiety were further restrained based on hydrogen bonding considerations. In the final refinement cycles the partially occupied H atoms were set to ride on their carrier oxygen atom. Subject to these conditions the occupancy ratio refined to 0.280 (14) to 0.720 (14). |
x | y | z | Uiso*/Ueq | Occ. (<1) | |
C1 | 1.0262 (4) | 0.3060 (4) | 0.5723 (3) | 0.0144 (7) | |
C2 | 1.0110 (4) | 0.3901 (4) | 0.6587 (3) | 0.0179 (8) | |
H2C | 1.008419 | 0.349470 | 0.722153 | 0.022* | |
H2D | 1.084243 | 0.465387 | 0.668060 | 0.022* | |
C3 | 0.6572 (4) | 0.4541 (4) | 0.3859 (3) | 0.0165 (8) | |
C4 | 0.5587 (4) | 0.5142 (4) | 0.3520 (3) | 0.0212 (9) | |
H4C | 0.489368 | 0.495117 | 0.396268 | 0.025* | |
H4D | 0.597517 | 0.604064 | 0.358082 | 0.025* | |
C5 | 0.5288 (4) | 0.2157 (4) | 0.0107 (3) | 0.0161 (8) | |
C6 | 0.4890 (4) | 0.1761 (4) | −0.0999 (3) | 0.0191 (8) | |
H6C | 0.395896 | 0.138873 | −0.110990 | 0.023* | |
H6D | 0.511706 | 0.248396 | −0.138941 | 0.023* | |
C7 | 0.8143 (4) | −0.0808 (4) | −0.0313 (3) | 0.0137 (7) | |
C8 | 0.8543 (4) | −0.1927 (4) | −0.0548 (3) | 0.0167 (8) | |
H8C | 0.778401 | −0.265253 | −0.068936 | 0.020* | |
H8D | 0.899991 | −0.183663 | −0.116018 | 0.020* | |
C9 | 1.1083 (4) | −0.0375 (4) | 0.3189 (3) | 0.0139 (7) | |
C10 | 1.2074 (4) | −0.0386 (4) | 0.4026 (3) | 0.0174 (8) | |
H10C | 1.185344 | −0.119834 | 0.429057 | 0.021* | |
H10D | 1.290439 | −0.024000 | 0.375591 | 0.021* | |
C11 | 0.999 (2) | 0.391 (2) | 0.165 (2) | 0.022 (3) | 0.280 (14) |
O12 | 0.8801 (17) | 0.350 (2) | 0.1404 (16) | 0.023 (3) | 0.280 (14) |
O13 | 1.045 (3) | 0.334 (3) | 0.2344 (18) | 0.024 (3) | 0.280 (14) |
O14 | 1.0694 (15) | 0.4834 (17) | 0.1307 (14) | 0.029 (4) | 0.280 (14) |
O23 | 1.3131 (16) | 0.5344 (19) | 0.198 (2) | 0.111 (13) | 0.280 (14) |
H23A | 1.298662 | 0.593330 | 0.230452 | 0.167* | 0.280 (14) |
H23B | 1.243199 | 0.486108 | 0.171835 | 0.167* | 0.280 (14) |
C11B | 1.0347 (8) | 0.3924 (8) | 0.1751 (7) | 0.0201 (16) | 0.720 (14) |
O12B | 0.9201 (8) | 0.3484 (8) | 0.1307 (6) | 0.0274 (15) | 0.720 (14) |
O13B | 1.0523 (12) | 0.3364 (10) | 0.2565 (6) | 0.0217 (15) | 0.720 (14) |
O14B | 1.1204 (8) | 0.4780 (6) | 0.1476 (5) | 0.0304 (17) | 0.720 (14) |
N1 | 0.9464 (3) | 0.2917 (3) | 0.4929 (2) | 0.0162 (7) | |
N2 | 0.8921 (4) | 0.4220 (4) | 0.6368 (3) | 0.0227 (8) | |
H2A | 0.907785 | 0.503939 | 0.651335 | 0.027* | |
H2B | 0.834002 | 0.382947 | 0.677305 | 0.027* | |
N3 | 0.6771 (4) | 0.3763 (3) | 0.3186 (3) | 0.0180 (7) | |
N4 | 0.5064 (4) | 0.4693 (4) | 0.2446 (3) | 0.0269 (9) | |
H4A | 0.532037 | 0.531124 | 0.204512 | 0.032* | |
H4B | 0.420256 | 0.445419 | 0.239699 | 0.032* | |
N5 | 0.6108 (3) | 0.1700 (3) | 0.0538 (2) | 0.0163 (7) | |
N6 | 0.5516 (3) | 0.0862 (3) | −0.1372 (2) | 0.0163 (7) | |
H6A | 0.583639 | 0.107148 | −0.196466 | 0.020* | |
H6B | 0.494036 | 0.010417 | −0.148883 | 0.020* | |
N7 | 0.8515 (3) | −0.0248 (3) | 0.0586 (2) | 0.0140 (6) | |
N8 | 0.9383 (3) | −0.2107 (3) | 0.0324 (2) | 0.0161 (7) | |
H8A | 1.016697 | −0.203291 | 0.013173 | 0.019* | |
H8B | 0.906275 | −0.287305 | 0.051533 | 0.019* | |
N9 | 1.0612 (3) | 0.0525 (3) | 0.3265 (2) | 0.0140 (6) | |
N10 | 1.2167 (4) | 0.0571 (4) | 0.4862 (3) | 0.0211 (7) | |
H10A | 1.297672 | 0.107865 | 0.497466 | 0.025* | |
H10B | 1.196810 | 0.021431 | 0.544138 | 0.025* | |
N11 | 0.5764 (4) | 0.2266 (4) | 0.6120 (3) | 0.0249 (8) | |
Cu1 | 1.09805 (5) | 0.15432 (4) | 0.45064 (3) | 0.01439 (10) | |
Cu2 | 0.82144 (5) | 0.37532 (4) | 0.49270 (3) | 0.01460 (10) | |
Cu3 | 0.56561 (5) | 0.32746 (5) | 0.19608 (4) | 0.01661 (11) | |
Cu4 | 0.69158 (5) | 0.08435 (5) | −0.03239 (3) | 0.01462 (10) | |
Cu5 | 0.95212 (5) | −0.08593 (4) | 0.15104 (3) | 0.01321 (10) | |
Dy1 | 0.84875 (2) | 0.19510 (2) | 0.24230 (2) | 0.01371 (6) | |
O1 | 0.9519 (3) | 0.2074 (3) | 0.4149 (2) | 0.0176 (6) | |
O2 | 1.1124 (3) | 0.2513 (3) | 0.5797 (2) | 0.0169 (6) | |
O3 | 0.7689 (3) | 0.3219 (3) | 0.3506 (2) | 0.0160 (6) | |
O4 | 0.7152 (3) | 0.4811 (3) | 0.4763 (2) | 0.0189 (6) | |
O5 | 0.6460 (3) | 0.2048 (3) | 0.1576 (2) | 0.0190 (6) | |
O6 | 0.4823 (3) | 0.2928 (3) | 0.0572 (2) | 0.0191 (6) | |
O7 | 0.8131 (3) | 0.0785 (3) | 0.0789 (2) | 0.0168 (6) | |
O8 | 0.7442 (3) | −0.0466 (3) | −0.0994 (2) | 0.0158 (6) | |
O9 | 0.9731 (3) | 0.0552 (3) | 0.2462 (2) | 0.0145 (5) | |
O10 | 1.0775 (3) | −0.1224 (3) | 0.2439 (2) | 0.0156 (6) | |
O11 | 0.7120 (3) | 0.0153 (3) | 0.2935 (2) | 0.0202 (6) | |
H11A | 0.646 (3) | 0.008 (5) | 0.322 (4) | 0.030* | |
H11B | 0.720 (5) | −0.054 (3) | 0.284 (4) | 0.030* | |
O15 | 0.6305 (3) | 0.2204 (3) | 0.5340 (3) | 0.0289 (7) | |
O16 | 0.6442 (4) | 0.2556 (5) | 0.6960 (3) | 0.0562 (13) | |
O17 | 0.4608 (3) | 0.2031 (3) | 0.6087 (3) | 0.0378 (9) | |
O18 | 1.2494 (3) | 0.3207 (3) | 0.3755 (2) | 0.0222 (6) | |
H18A | 1.272 (5) | 0.377 (4) | 0.422 (3) | 0.033* | |
H18B | 1.197 (4) | 0.334 (5) | 0.333 (3) | 0.033* | |
O19 | 0.3864 (3) | 0.1929 (3) | 0.2659 (2) | 0.0208 (6) | |
H19A | 0.337 (4) | 0.153 (5) | 0.218 (3) | 0.031* | |
H19B | 0.340 (5) | 0.225 (5) | 0.295 (4) | 0.031* | |
O20 | 0.8193 (3) | 0.2509 (3) | −0.1131 (3) | 0.0244 (7) | |
H20A | 0.848 (5) | 0.225 (5) | −0.162 (3) | 0.037* | |
H20B | 0.838 (6) | 0.3269 (19) | −0.105 (5) | 0.037* | |
O21 | 0.6433 (4) | 0.6160 (3) | 0.0964 (3) | 0.0301 (8) | |
H21A | 0.606 (6) | 0.639 (6) | 0.048 (3) | 0.045* | |
H21B | 0.685 (5) | 0.573 (5) | 0.070 (5) | 0.045* | |
O22 | 0.8208 (5) | 0.5167 (4) | 0.0461 (3) | 0.0469 (11) | |
H22A | 0.847 (7) | 0.523 (7) | −0.012 (3) | 0.070* | |
H22B | 0.852 (7) | 0.466 (6) | 0.073 (6) | 0.070* | |
O24 | 0.7778 (3) | −0.1964 (3) | 0.2415 (2) | 0.0181 (6) | |
H24A | 0.806 (5) | −0.226 (5) | 0.290 (3) | 0.027* | |
H24B | 0.739 (5) | −0.259 (3) | 0.204 (3) | 0.027* | |
O25 | 0.5139 (3) | 0.0557 (3) | 0.3692 (3) | 0.0248 (7) | |
H25A | 0.474 (5) | 0.101 (5) | 0.347 (4) | 0.037* | |
H25B | 0.538 (6) | 0.097 (5) | 0.425 (3) | 0.037* |
U11 | U22 | U33 | U12 | U13 | U23 | |
C1 | 0.0170 (19) | 0.0133 (18) | 0.0110 (17) | 0.0007 (15) | 0.0037 (14) | 0.0030 (14) |
C2 | 0.024 (2) | 0.0163 (19) | 0.0109 (17) | 0.0026 (16) | 0.0017 (15) | −0.0023 (14) |
C3 | 0.021 (2) | 0.0118 (18) | 0.0153 (18) | 0.0030 (15) | 0.0036 (15) | −0.0001 (14) |
C4 | 0.031 (2) | 0.016 (2) | 0.019 (2) | 0.0121 (18) | −0.0001 (17) | −0.0009 (16) |
C5 | 0.021 (2) | 0.0170 (19) | 0.0109 (17) | 0.0061 (16) | 0.0002 (15) | 0.0021 (14) |
C6 | 0.024 (2) | 0.026 (2) | 0.0105 (18) | 0.0138 (18) | −0.0013 (15) | −0.0009 (15) |
C7 | 0.0146 (18) | 0.0150 (18) | 0.0117 (17) | 0.0045 (15) | 0.0026 (14) | 0.0015 (14) |
C8 | 0.022 (2) | 0.0159 (19) | 0.0127 (18) | 0.0078 (16) | 0.0009 (15) | −0.0016 (14) |
C9 | 0.0141 (18) | 0.0138 (18) | 0.0132 (17) | 0.0031 (14) | 0.0018 (14) | 0.0025 (14) |
C10 | 0.0170 (19) | 0.0191 (19) | 0.0174 (19) | 0.0078 (16) | 0.0005 (15) | 0.0011 (15) |
C11 | 0.028 (5) | 0.022 (4) | 0.016 (4) | 0.006 (5) | 0.006 (5) | 0.000 (4) |
O12 | 0.022 (6) | 0.026 (4) | 0.019 (5) | 0.003 (5) | 0.010 (5) | 0.006 (4) |
O13 | 0.027 (5) | 0.023 (4) | 0.015 (5) | −0.002 (4) | 0.008 (5) | 0.001 (5) |
O14 | 0.030 (7) | 0.029 (6) | 0.020 (6) | −0.003 (6) | 0.002 (6) | 0.004 (5) |
O23 | 0.052 (13) | 0.058 (13) | 0.23 (4) | 0.042 (11) | −0.013 (16) | −0.019 (16) |
C11B | 0.029 (4) | 0.017 (2) | 0.013 (3) | 0.006 (3) | 0.006 (3) | −0.002 (2) |
O12B | 0.031 (4) | 0.026 (2) | 0.022 (3) | 0.001 (3) | 0.007 (3) | 0.0090 (19) |
O13B | 0.025 (3) | 0.021 (2) | 0.015 (4) | 0.002 (2) | 0.000 (3) | 0.001 (3) |
O14B | 0.041 (4) | 0.023 (3) | 0.018 (3) | −0.004 (3) | 0.009 (3) | −0.001 (2) |
N1 | 0.0246 (18) | 0.0153 (16) | 0.0084 (15) | 0.0058 (14) | 0.0042 (13) | −0.0038 (12) |
N2 | 0.027 (2) | 0.026 (2) | 0.0151 (17) | 0.0114 (16) | −0.0011 (14) | −0.0049 (14) |
N3 | 0.0274 (19) | 0.0159 (16) | 0.0140 (16) | 0.0114 (14) | 0.0019 (14) | 0.0022 (13) |
N4 | 0.045 (3) | 0.0235 (19) | 0.0176 (18) | 0.0205 (18) | −0.0008 (17) | 0.0010 (15) |
N5 | 0.0189 (17) | 0.0201 (17) | 0.0112 (15) | 0.0095 (14) | −0.0016 (13) | −0.0013 (13) |
N6 | 0.0184 (17) | 0.0213 (17) | 0.0107 (15) | 0.0092 (14) | 0.0001 (13) | −0.0008 (13) |
N7 | 0.0200 (17) | 0.0120 (15) | 0.0125 (15) | 0.0088 (13) | 0.0030 (13) | −0.0008 (12) |
N8 | 0.0201 (17) | 0.0165 (16) | 0.0130 (15) | 0.0080 (14) | 0.0007 (13) | 0.0002 (12) |
N9 | 0.0139 (16) | 0.0185 (16) | 0.0087 (14) | 0.0048 (13) | −0.0035 (12) | 0.0003 (12) |
N10 | 0.0219 (19) | 0.028 (2) | 0.0145 (16) | 0.0113 (15) | −0.0035 (14) | 0.0008 (14) |
N11 | 0.024 (2) | 0.026 (2) | 0.0220 (19) | 0.0033 (16) | 0.0022 (15) | 0.0022 (15) |
Cu1 | 0.0158 (2) | 0.0178 (2) | 0.0092 (2) | 0.00580 (19) | −0.00147 (17) | −0.00123 (17) |
Cu2 | 0.0202 (2) | 0.0138 (2) | 0.0094 (2) | 0.00534 (19) | 0.00115 (18) | −0.00185 (17) |
Cu3 | 0.0250 (3) | 0.0173 (2) | 0.0107 (2) | 0.0125 (2) | −0.00060 (19) | −0.00092 (18) |
Cu4 | 0.0181 (2) | 0.0191 (2) | 0.0083 (2) | 0.00965 (19) | −0.00130 (17) | −0.00176 (17) |
Cu5 | 0.0177 (2) | 0.0126 (2) | 0.0102 (2) | 0.00695 (18) | −0.00060 (17) | −0.00128 (17) |
Dy1 | 0.01860 (10) | 0.01323 (9) | 0.00956 (9) | 0.00606 (7) | −0.00016 (6) | −0.00055 (6) |
O1 | 0.0217 (15) | 0.0213 (15) | 0.0108 (13) | 0.0110 (12) | −0.0017 (11) | −0.0079 (11) |
O2 | 0.0203 (15) | 0.0198 (14) | 0.0106 (13) | 0.0067 (12) | −0.0002 (11) | 0.0003 (11) |
O3 | 0.0210 (15) | 0.0171 (14) | 0.0130 (13) | 0.0116 (12) | 0.0002 (11) | −0.0009 (11) |
O4 | 0.0242 (16) | 0.0183 (14) | 0.0143 (13) | 0.0071 (12) | 0.0024 (11) | −0.0016 (11) |
O5 | 0.0279 (16) | 0.0280 (16) | 0.0053 (12) | 0.0174 (13) | −0.0034 (11) | −0.0037 (11) |
O6 | 0.0248 (16) | 0.0220 (15) | 0.0141 (13) | 0.0140 (13) | −0.0017 (11) | 0.0010 (11) |
O7 | 0.0244 (15) | 0.0170 (14) | 0.0130 (13) | 0.0145 (12) | −0.0024 (11) | −0.0041 (11) |
O8 | 0.0198 (14) | 0.0192 (14) | 0.0091 (12) | 0.0089 (12) | −0.0025 (10) | −0.0025 (10) |
O9 | 0.0177 (14) | 0.0164 (13) | 0.0092 (12) | 0.0071 (11) | −0.0055 (10) | −0.0007 (10) |
O10 | 0.0195 (14) | 0.0149 (13) | 0.0136 (13) | 0.0081 (11) | 0.0005 (11) | −0.0012 (10) |
O11 | 0.0186 (15) | 0.0170 (14) | 0.0247 (16) | 0.0042 (12) | 0.0051 (12) | 0.0019 (12) |
O15 | 0.0303 (18) | 0.0313 (18) | 0.0233 (17) | 0.0047 (15) | 0.0068 (14) | 0.0064 (14) |
O16 | 0.042 (2) | 0.088 (4) | 0.0178 (18) | −0.011 (2) | 0.0019 (17) | 0.003 (2) |
O17 | 0.0249 (18) | 0.0300 (19) | 0.058 (3) | 0.0085 (15) | 0.0077 (17) | −0.0026 (17) |
O18 | 0.0247 (17) | 0.0192 (15) | 0.0212 (16) | 0.0075 (13) | −0.0009 (13) | −0.0087 (12) |
O19 | 0.0212 (16) | 0.0255 (16) | 0.0157 (14) | 0.0091 (13) | 0.0000 (12) | −0.0042 (12) |
O20 | 0.0289 (18) | 0.0234 (16) | 0.0233 (16) | 0.0108 (14) | 0.0079 (13) | 0.0005 (13) |
O21 | 0.044 (2) | 0.0262 (18) | 0.0204 (16) | 0.0149 (16) | −0.0072 (15) | 0.0016 (13) |
O22 | 0.076 (3) | 0.044 (2) | 0.035 (2) | 0.034 (2) | 0.021 (2) | 0.0123 (19) |
O24 | 0.0230 (16) | 0.0172 (14) | 0.0130 (14) | 0.0053 (12) | −0.0016 (11) | 0.0026 (11) |
O25 | 0.0210 (16) | 0.0276 (17) | 0.0270 (17) | 0.0094 (13) | 0.0027 (13) | 0.0016 (14) |
C1—N1 | 1.289 (5) | N5—Cu4 | 1.904 (3) |
C1—O2 | 1.293 (5) | N6—Cu4 | 2.005 (3) |
C1—C2 | 1.503 (5) | N6—H6A | 0.9100 |
C2—N2 | 1.484 (6) | N6—H6B | 0.9100 |
C2—H2C | 0.9900 | N7—O7 | 1.393 (4) |
C2—H2D | 0.9900 | N7—Cu5 | 1.899 (3) |
C3—O4 | 1.288 (5) | N8—Cu5 | 2.021 (3) |
C3—N3 | 1.299 (5) | N8—H8A | 0.9100 |
C3—C4 | 1.512 (6) | N8—H8B | 0.9100 |
C4—N4 | 1.492 (6) | N9—O9 | 1.395 (4) |
C4—H4C | 0.9900 | N9—Cu1 | 1.897 (3) |
C4—H4D | 0.9900 | N10—Cu1 | 2.012 (4) |
C5—N5 | 1.293 (5) | N10—H10A | 0.9100 |
C5—O6 | 1.298 (5) | N10—H10B | 0.9100 |
C5—C6 | 1.499 (5) | N11—O17 | 1.228 (5) |
C6—N6 | 1.486 (5) | N11—O15 | 1.249 (5) |
C6—H6C | 0.9900 | N11—O16 | 1.260 (5) |
C6—H6D | 0.9900 | Cu1—O1 | 1.931 (3) |
C7—N7 | 1.292 (5) | Cu1—O2 | 1.949 (3) |
C7—O8 | 1.301 (5) | Cu1—O18 | 2.476 (3) |
C7—C8 | 1.501 (5) | Cu2—O3 | 1.931 (3) |
C8—N8 | 1.491 (5) | Cu2—O4 | 1.939 (3) |
C8—H8C | 0.9900 | Cu2—O15 | 2.464 (3) |
C8—H8D | 0.9900 | Cu3—O5 | 1.941 (3) |
C9—N9 | 1.293 (5) | Cu3—O6 | 1.954 (3) |
C9—O10 | 1.295 (5) | Cu3—O19 | 2.430 (3) |
C9—C10 | 1.502 (5) | Cu4—O7 | 1.936 (3) |
C10—N10 | 1.484 (5) | Cu4—O8 | 1.956 (3) |
C10—H10C | 0.9900 | Cu4—O20 | 2.400 (3) |
C10—H10D | 0.9900 | Cu5—O9 | 1.932 (3) |
C11—O14 | 1.256 (15) | Cu5—O10 | 1.941 (3) |
C11—O12 | 1.275 (16) | Cu5—O24 | 2.440 (3) |
C11—O13 | 1.318 (16) | Dy1—O11 | 2.357 (3) |
C11—Dy1 | 2.704 (19) | Dy1—O3 | 2.382 (3) |
O12—Dy1 | 2.27 (2) | Dy1—O9 | 2.410 (3) |
O13—Dy1 | 2.31 (3) | Dy1—O7 | 2.412 (3) |
O23—H23A | 0.8410 | Dy1—O1 | 2.453 (3) |
O23—H23B | 0.8398 | Dy1—O5 | 2.469 (3) |
C11B—O14B | 1.251 (8) | O11—H11A | 0.83 (2) |
C11B—O12B | 1.295 (9) | O11—H11B | 0.82 (2) |
C11B—O13B | 1.326 (8) | O18—H18A | 0.83 (2) |
C11B—Dy1 | 2.834 (8) | O18—H18B | 0.83 (2) |
O12B—Dy1 | 2.380 (8) | O19—H19A | 0.82 (2) |
O13B—Dy1 | 2.347 (12) | O19—H19B | 0.82 (2) |
N1—O1 | 1.387 (4) | O20—H20A | 0.82 (2) |
N1—Cu2 | 1.907 (4) | O20—H20B | 0.83 (2) |
N2—Cu2 | 1.983 (4) | O21—H21A | 0.84 (2) |
N2—H2A | 0.9100 | O21—H21B | 0.84 (2) |
N2—H2B | 0.9100 | O22—H22A | 0.85 (2) |
N3—O3 | 1.398 (4) | O22—H22B | 0.85 (2) |
N3—Cu3 | 1.905 (4) | O24—H24A | 0.83 (2) |
N4—Cu3 | 2.017 (4) | O24—H24B | 0.83 (2) |
N4—H4A | 0.9100 | O25—H25A | 0.83 (2) |
N4—H4B | 0.9100 | O25—H25B | 0.83 (2) |
N5—O5 | 1.399 (4) | ||
N1—C1—O2 | 123.5 (4) | O4—Cu2—O15 | 86.41 (12) |
N1—C1—C2 | 115.2 (4) | N2—Cu2—O15 | 93.60 (15) |
O2—C1—C2 | 121.2 (3) | N3—Cu3—O5 | 90.67 (13) |
N2—C2—C1 | 109.7 (3) | N3—Cu3—O6 | 168.26 (15) |
N2—C2—H2C | 109.7 | O5—Cu3—O6 | 85.39 (12) |
C1—C2—H2C | 109.7 | N3—Cu3—N4 | 82.79 (15) |
N2—C2—H2D | 109.7 | O5—Cu3—N4 | 171.97 (16) |
C1—C2—H2D | 109.7 | O6—Cu3—N4 | 100.11 (14) |
H2C—C2—H2D | 108.2 | N3—Cu3—O19 | 97.68 (13) |
O4—C3—N3 | 124.3 (4) | O5—Cu3—O19 | 97.42 (12) |
O4—C3—C4 | 120.1 (4) | O6—Cu3—O19 | 93.80 (12) |
N3—C3—C4 | 115.6 (4) | N4—Cu3—O19 | 88.10 (15) |
N4—C4—C3 | 110.0 (3) | N5—Cu4—O7 | 91.62 (13) |
N4—C4—H4C | 109.7 | N5—Cu4—O8 | 161.94 (14) |
C3—C4—H4C | 109.7 | O7—Cu4—O8 | 84.56 (11) |
N4—C4—H4D | 109.7 | N5—Cu4—N6 | 83.78 (14) |
C3—C4—H4D | 109.7 | O7—Cu4—N6 | 173.83 (14) |
H4C—C4—H4D | 108.2 | O8—Cu4—N6 | 98.55 (13) |
N5—C5—O6 | 123.9 (4) | N5—Cu4—O20 | 100.27 (13) |
N5—C5—C6 | 116.2 (4) | O7—Cu4—O20 | 99.73 (12) |
O6—C5—C6 | 119.9 (4) | O8—Cu4—O20 | 97.78 (12) |
N6—C6—C5 | 111.0 (3) | N6—Cu4—O20 | 85.18 (13) |
N6—C6—H6C | 109.4 | N7—Cu5—O9 | 89.53 (12) |
C5—C6—H6C | 109.4 | N7—Cu5—O10 | 170.19 (14) |
N6—C6—H6D | 109.4 | O9—Cu5—O10 | 85.47 (11) |
C5—C6—H6D | 109.4 | N7—Cu5—N8 | 83.23 (14) |
H6C—C6—H6D | 108.0 | O9—Cu5—N8 | 169.36 (13) |
N7—C7—O8 | 123.7 (4) | O10—Cu5—N8 | 100.49 (13) |
N7—C7—C8 | 116.3 (3) | N7—Cu5—O24 | 95.86 (13) |
O8—C7—C8 | 120.0 (3) | O9—Cu5—O24 | 87.84 (11) |
N8—C8—C7 | 110.4 (3) | O10—Cu5—O24 | 92.38 (11) |
N8—C8—H8C | 109.6 | N8—Cu5—O24 | 100.61 (13) |
C7—C8—H8C | 109.6 | O12—Dy1—O13 | 57.1 (6) |
N8—C8—H8D | 109.6 | O12—Dy1—O11 | 148.9 (5) |
C7—C8—H8D | 109.6 | O13—Dy1—O11 | 153.5 (6) |
H8C—C8—H8D | 108.1 | O13B—Dy1—O11 | 148.4 (2) |
N9—C9—O10 | 124.2 (4) | O13B—Dy1—O12B | 54.7 (2) |
N9—C9—C10 | 116.1 (3) | O11—Dy1—O12B | 155.6 (2) |
O10—C9—C10 | 119.6 (3) | O12—Dy1—O3 | 85.0 (5) |
N10—C10—C9 | 110.6 (3) | O13—Dy1—O3 | 97.2 (8) |
N10—C10—H10C | 109.5 | O13B—Dy1—O3 | 93.6 (3) |
C9—C10—H10C | 109.5 | O11—Dy1—O3 | 92.12 (10) |
N10—C10—H10D | 109.5 | O12B—Dy1—O3 | 93.8 (2) |
C9—C10—H10D | 109.5 | O12—Dy1—O9 | 123.4 (5) |
H10C—C10—H10D | 108.1 | O13—Dy1—O9 | 81.7 (8) |
O14—C11—O12 | 123.4 (18) | O13B—Dy1—O9 | 80.7 (3) |
O14—C11—O13 | 121.3 (19) | O11—Dy1—O9 | 75.78 (10) |
O12—C11—O13 | 115.3 (18) | O12B—Dy1—O9 | 112.1 (2) |
O14—C11—Dy1 | 179 (2) | O3—Dy1—O9 | 141.93 (9) |
O12—C11—Dy1 | 56.8 (11) | O12—Dy1—O7 | 80.3 (5) |
O13—C11—Dy1 | 58.5 (14) | O13—Dy1—O7 | 101.5 (7) |
C11—O12—Dy1 | 95.2 (13) | O13B—Dy1—O7 | 107.8 (3) |
C11—O13—Dy1 | 92.3 (16) | O11—Dy1—O7 | 84.36 (11) |
H23A—O23—H23B | 107.9 | O12B—Dy1—O7 | 77.1 (2) |
O14B—C11B—O12B | 125.8 (7) | O3—Dy1—O7 | 144.46 (9) |
O14B—C11B—O13B | 122.3 (8) | O9—Dy1—O7 | 71.21 (9) |
O12B—C11B—O13B | 111.8 (7) | O12—Dy1—O1 | 126.0 (5) |
O14B—C11B—Dy1 | 177.4 (6) | O13—Dy1—O1 | 77.8 (5) |
O12B—C11B—Dy1 | 56.6 (4) | O13B—Dy1—O1 | 70.69 (19) |
O13B—C11B—Dy1 | 55.3 (5) | O11—Dy1—O1 | 81.73 (11) |
C11B—O12B—Dy1 | 96.4 (5) | O12B—Dy1—O1 | 122.6 (2) |
C11B—O13B—Dy1 | 97.0 (6) | O3—Dy1—O1 | 71.77 (9) |
C1—N1—O1 | 116.4 (3) | O9—Dy1—O1 | 70.83 (9) |
C1—N1—Cu2 | 119.4 (3) | O7—Dy1—O1 | 141.70 (9) |
O1—N1—Cu2 | 124.0 (3) | O12—Dy1—O5 | 68.7 (5) |
C2—N2—Cu2 | 111.6 (3) | O13—Dy1—O5 | 125.6 (6) |
C2—N2—H2A | 109.3 | O13B—Dy1—O5 | 130.3 (2) |
Cu2—N2—H2A | 109.3 | O11—Dy1—O5 | 80.88 (11) |
C2—N2—H2B | 109.3 | O12B—Dy1—O5 | 78.5 (2) |
Cu2—N2—H2B | 109.3 | O3—Dy1—O5 | 71.92 (9) |
H2A—N2—H2B | 108.0 | O9—Dy1—O5 | 138.36 (9) |
C3—N3—O3 | 115.0 (3) | O7—Dy1—O5 | 72.60 (9) |
C3—N3—Cu3 | 119.0 (3) | O1—Dy1—O5 | 138.84 (9) |
O3—N3—Cu3 | 125.2 (2) | O12—Dy1—C11 | 28.0 (4) |
C4—N4—Cu3 | 110.8 (3) | O13—Dy1—C11 | 29.1 (4) |
C4—N4—H4A | 109.5 | O11—Dy1—C11 | 174.5 (7) |
Cu3—N4—H4A | 109.5 | O3—Dy1—C11 | 91.8 (7) |
C4—N4—H4B | 109.5 | O9—Dy1—C11 | 103.3 (6) |
Cu3—N4—H4B | 109.5 | O7—Dy1—C11 | 90.2 (7) |
H4A—N4—H4B | 108.1 | O1—Dy1—C11 | 103.2 (6) |
C5—N5—O5 | 116.2 (3) | O5—Dy1—C11 | 96.7 (5) |
C5—N5—Cu4 | 117.2 (3) | O13B—Dy1—C11B | 27.67 (19) |
O5—N5—Cu4 | 125.8 (2) | O11—Dy1—C11B | 172.4 (2) |
C6—N6—Cu4 | 109.1 (2) | O12B—Dy1—C11B | 27.0 (2) |
C6—N6—H6A | 109.9 | O3—Dy1—C11B | 94.7 (2) |
Cu4—N6—H6A | 109.9 | O9—Dy1—C11B | 96.7 (2) |
C6—N6—H6B | 109.9 | O7—Dy1—C11B | 92.0 (2) |
Cu4—N6—H6B | 109.9 | O1—Dy1—C11B | 97.2 (2) |
H6A—N6—H6B | 108.3 | O5—Dy1—C11B | 104.4 (2) |
C7—N7—O7 | 115.4 (3) | N1—O1—Cu1 | 107.4 (2) |
C7—N7—Cu5 | 119.3 (3) | N1—O1—Dy1 | 123.3 (2) |
O7—N7—Cu5 | 125.3 (2) | Cu1—O1—Dy1 | 125.28 (13) |
C8—N8—Cu5 | 110.6 (2) | C1—O2—Cu1 | 107.0 (2) |
C8—N8—H8A | 109.5 | N3—O3—Cu2 | 107.7 (2) |
Cu5—N8—H8A | 109.5 | N3—O3—Dy1 | 124.3 (2) |
C8—N8—H8B | 109.5 | Cu2—O3—Dy1 | 127.93 (13) |
Cu5—N8—H8B | 109.5 | C3—O4—Cu2 | 107.0 (3) |
H8A—N8—H8B | 108.1 | N5—O5—Cu3 | 107.2 (2) |
C9—N9—O9 | 115.5 (3) | N5—O5—Dy1 | 121.8 (2) |
C9—N9—Cu1 | 118.3 (3) | Cu3—O5—Dy1 | 123.95 (13) |
O9—N9—Cu1 | 125.6 (2) | C5—O6—Cu3 | 106.9 (2) |
C10—N10—Cu1 | 110.4 (2) | N7—O7—Cu4 | 108.0 (2) |
C10—N10—H10A | 109.6 | N7—O7—Dy1 | 124.6 (2) |
Cu1—N10—H10A | 109.6 | Cu4—O7—Dy1 | 125.53 (13) |
C10—N10—H10B | 109.6 | C7—O8—Cu4 | 106.9 (2) |
Cu1—N10—H10B | 109.6 | N9—O9—Cu5 | 107.8 (2) |
H10A—N10—H10B | 108.1 | N9—O9—Dy1 | 124.9 (2) |
O17—N11—O15 | 122.1 (4) | Cu5—O9—Dy1 | 126.77 (12) |
O17—N11—O16 | 120.1 (4) | C9—O10—Cu5 | 107.0 (2) |
O15—N11—O16 | 117.8 (4) | Dy1—O11—H11A | 128 (4) |
N9—Cu1—O1 | 89.39 (13) | Dy1—O11—H11B | 125 (4) |
N9—Cu1—O2 | 172.56 (14) | H11A—O11—H11B | 107 (6) |
O1—Cu1—O2 | 85.19 (12) | N11—O15—Cu2 | 125.3 (3) |
N9—Cu1—N10 | 83.73 (14) | Cu1—O18—H18A | 103 (4) |
O1—Cu1—N10 | 165.35 (15) | Cu1—O18—H18B | 97 (4) |
O2—Cu1—N10 | 100.37 (13) | H18A—O18—H18B | 111 (6) |
N9—Cu1—O18 | 91.67 (12) | Cu3—O19—H19A | 107 (4) |
O1—Cu1—O18 | 95.28 (12) | Cu3—O19—H19B | 117 (4) |
O2—Cu1—O18 | 93.90 (11) | H19A—O19—H19B | 101 (6) |
N10—Cu1—O18 | 97.82 (14) | Cu4—O20—H20A | 110 (4) |
N1—Cu2—O3 | 90.66 (13) | Cu4—O20—H20B | 136 (4) |
N1—Cu2—O4 | 168.94 (14) | H20A—O20—H20B | 114 (6) |
O3—Cu2—O4 | 85.41 (12) | H21A—O21—H21B | 106 (6) |
N1—Cu2—N2 | 82.65 (15) | H22A—O22—H22B | 106 (7) |
O3—Cu2—N2 | 173.24 (14) | Cu5—O24—H24A | 110 (4) |
O4—Cu2—N2 | 101.00 (14) | Cu5—O24—H24B | 106 (4) |
N1—Cu2—O15 | 103.87 (14) | H24A—O24—H24B | 101 (5) |
O3—Cu2—O15 | 88.90 (12) | H25A—O25—H25B | 95 (6) |
N1—C1—C2—N2 | 9.0 (5) | O9—N9—Cu1—O1 | 11.1 (3) |
O2—C1—C2—N2 | −169.9 (4) | C9—N9—Cu1—N10 | 7.5 (3) |
O4—C3—C4—N4 | 179.4 (4) | O9—N9—Cu1—N10 | 178.1 (3) |
N3—C3—C4—N4 | −0.7 (5) | C9—N9—Cu1—O18 | 105.2 (3) |
N5—C5—C6—N6 | 1.9 (5) | O9—N9—Cu1—O18 | −84.2 (3) |
O6—C5—C6—N6 | −178.9 (4) | C7—N7—Cu5—O9 | 174.1 (3) |
N7—C7—C8—N8 | −3.7 (5) | O7—N7—Cu5—O9 | −5.5 (3) |
O8—C7—C8—N8 | 177.5 (3) | C7—N7—Cu5—N8 | 1.9 (3) |
N9—C9—C10—N10 | 8.5 (5) | O7—N7—Cu5—N8 | −177.7 (3) |
O10—C9—C10—N10 | −173.1 (3) | C7—N7—Cu5—O24 | −98.1 (3) |
O14—C11—O12—Dy1 | −179 (3) | O7—N7—Cu5—O24 | 82.2 (3) |
O13—C11—O12—Dy1 | −2 (3) | C1—N1—O1—Cu1 | −6.8 (4) |
O14—C11—O13—Dy1 | 179 (3) | Cu2—N1—O1—Cu1 | 178.22 (19) |
O12—C11—O13—Dy1 | 2 (3) | C1—N1—O1—Dy1 | −165.3 (3) |
O14B—C11B—O12B—Dy1 | 179.0 (9) | Cu2—N1—O1—Dy1 | 19.7 (4) |
O13B—C11B—O12B—Dy1 | −1.8 (9) | N1—C1—O2—Cu1 | 1.8 (5) |
O14B—C11B—O13B—Dy1 | −178.9 (9) | C2—C1—O2—Cu1 | −179.4 (3) |
O12B—C11B—O13B—Dy1 | 1.9 (9) | C3—N3—O3—Cu2 | 5.3 (4) |
O2—C1—N1—O1 | 3.6 (6) | Cu3—N3—O3—Cu2 | −164.7 (2) |
C2—C1—N1—O1 | −175.2 (3) | C3—N3—O3—Dy1 | −171.9 (3) |
O2—C1—N1—Cu2 | 178.7 (3) | Cu3—N3—O3—Dy1 | 18.1 (4) |
C2—C1—N1—Cu2 | 0.0 (5) | N3—C3—O4—Cu2 | −4.7 (5) |
C1—C2—N2—Cu2 | −13.2 (4) | C4—C3—O4—Cu2 | 175.2 (3) |
O4—C3—N3—O3 | −0.4 (6) | C5—N5—O5—Cu3 | −5.6 (4) |
C4—C3—N3—O3 | 179.7 (3) | Cu4—N5—O5—Cu3 | 163.6 (2) |
O4—C3—N3—Cu3 | 170.3 (3) | C5—N5—O5—Dy1 | −157.2 (3) |
C4—C3—N3—Cu3 | −9.7 (5) | Cu4—N5—O5—Dy1 | 12.0 (4) |
C3—C4—N4—Cu3 | 9.5 (5) | N5—C5—O6—Cu3 | 2.5 (5) |
O6—C5—N5—O5 | 2.2 (6) | C6—C5—O6—Cu3 | −176.5 (3) |
C6—C5—N5—O5 | −178.7 (3) | C7—N7—O7—Cu4 | 9.3 (4) |
O6—C5—N5—Cu4 | −168.0 (3) | Cu5—N7—O7—Cu4 | −171.08 (19) |
C6—C5—N5—Cu4 | 11.1 (5) | C7—N7—O7—Dy1 | 174.4 (3) |
C5—C6—N6—Cu4 | −12.7 (4) | Cu5—N7—O7—Dy1 | −6.0 (4) |
O8—C7—N7—O7 | −1.1 (6) | N7—C7—O8—Cu4 | −7.6 (5) |
C8—C7—N7—O7 | −179.8 (3) | C8—C7—O8—Cu4 | 171.1 (3) |
O8—C7—N7—Cu5 | 179.3 (3) | C9—N9—O9—Cu5 | 1.2 (4) |
C8—C7—N7—Cu5 | 0.5 (5) | Cu1—N9—O9—Cu5 | −169.69 (19) |
C7—C8—N8—Cu5 | 4.8 (4) | C9—N9—O9—Dy1 | 172.9 (3) |
O10—C9—N9—O9 | −0.9 (6) | Cu1—N9—O9—Dy1 | 2.0 (4) |
C10—C9—N9—O9 | 177.5 (3) | N9—C9—O10—Cu5 | 0.1 (5) |
O10—C9—N9—Cu1 | 170.7 (3) | C10—C9—O10—Cu5 | −178.2 (3) |
C10—C9—N9—Cu1 | −11.0 (5) | O17—N11—O15—Cu2 | 134.4 (4) |
C9—C10—N10—Cu1 | −2.5 (4) | O16—N11—O15—Cu2 | −47.2 (6) |
C9—N9—Cu1—O1 | −159.6 (3) |
D—H···A | D—H | H···A | D···A | D—H···A |
O23—H23A···O16i | 0.84 | 1.84 | 2.61 (2) | 150 |
O23—H23B···O14 | 0.84 | 1.95 | 2.657 (17) | 141 |
N2—H2A···O13i | 0.91 | 2.23 | 3.05 (3) | 150 |
N2—H2A···O13Bi | 0.91 | 2.05 | 2.900 (11) | 156 |
N2—H2B···O16 | 0.91 | 2.23 | 3.054 (6) | 150 |
N4—H4A···O21 | 0.91 | 2.08 | 2.912 (6) | 152 |
N4—H4B···O23ii | 0.91 | 1.86 | 2.520 (16) | 128 |
N6—H6A···O16iii | 0.91 | 2.29 | 3.091 (6) | 147 |
N6—H6B···N5iv | 0.91 | 2.54 | 3.287 (5) | 140 |
N6—H6B···O5iv | 0.91 | 2.49 | 3.396 (5) | 171 |
N8—H8A···O7v | 0.91 | 2.48 | 3.262 (5) | 144 |
N8—H8A···O20v | 0.91 | 2.38 | 2.989 (5) | 124 |
N8—H8B···O22vi | 0.91 | 2.17 | 3.045 (6) | 162 |
N10—H10A···O17vii | 0.91 | 2.20 | 3.005 (5) | 147 |
N10—H10B···O11viii | 0.91 | 2.42 | 3.198 (5) | 143 |
O11—H11A···O25 | 0.83 (2) | 1.86 (3) | 2.642 (4) | 157 (6) |
O11—H11B···O24 | 0.82 (2) | 2.00 (3) | 2.800 (4) | 164 (6) |
O18—H18A···O4i | 0.83 (2) | 2.01 (2) | 2.821 (4) | 165 (6) |
O18—H18B···O13 | 0.83 (2) | 2.05 (4) | 2.87 (3) | 169 (6) |
O18—H18B···O13B | 0.83 (2) | 1.84 (3) | 2.650 (10) | 165 (6) |
O19—H19A···O8iv | 0.82 (2) | 1.91 (2) | 2.710 (4) | 167 (6) |
O19—H19B···O18ii | 0.82 (2) | 2.01 (2) | 2.827 (4) | 172 (6) |
O20—H20A···O10v | 0.82 (2) | 1.95 (3) | 2.738 (4) | 160 (6) |
O20—H20B···O14ix | 0.83 (2) | 2.18 (3) | 2.973 (18) | 158 (6) |
O20—H20B···O14Bix | 0.83 (2) | 2.28 (3) | 3.065 (7) | 158 (6) |
O21—H21A···O6x | 0.84 (2) | 1.98 (2) | 2.810 (4) | 174 (7) |
O21—H21B···O22 | 0.84 (2) | 1.85 (3) | 2.660 (6) | 160 (7) |
O22—H22A···O14ix | 0.85 (2) | 1.91 (3) | 2.736 (19) | 166 (8) |
O22—H22A···O14Bix | 0.85 (2) | 1.87 (2) | 2.708 (8) | 171 (8) |
O22—H22B···O12 | 0.85 (2) | 1.74 (4) | 2.57 (2) | 165 (8) |
O22—H22B···O14 | 0.85 (2) | 2.41 (7) | 3.033 (18) | 130 (7) |
O22—H22B···O12B | 0.85 (2) | 1.90 (2) | 2.753 (10) | 179 (9) |
O24—H24A···O2viii | 0.83 (2) | 1.97 (2) | 2.777 (4) | 165 (5) |
O24—H24B···O21vi | 0.83 (2) | 1.95 (2) | 2.767 (5) | 168 (5) |
O25—H25A···O19 | 0.83 (2) | 1.95 (2) | 2.769 (5) | 168 (6) |
O25—H25B···O15 | 0.83 (2) | 1.94 (3) | 2.752 (5) | 163 (6) |
Symmetry codes: (i) −x+2, −y+1, −z+1; (ii) x−1, y, z; (iii) x, y, z−1; (iv) −x+1, −y, −z; (v) −x+2, −y, −z; (vi) x, y−1, z; (vii) x+1, y, z; (viii) −x+2, −y, −z+1; (ix) −x+2, −y+1, −z; (x) −x+1, −y+1, −z. |
[Cu5Ho(C2H4N2O2)5(CO3)(NO3)(H2O)5]·3.445H2O | Z = 2 |
Mr = 1197.21 | F(000) = 1174.9 |
Triclinic, P1 | Dx = 2.467 Mg m−3 |
a = 11.2027 (9) Å | Mo Kα radiation, λ = 0.71073 Å |
b = 11.4955 (9) Å | Cell parameters from 9995 reflections |
c = 13.2467 (10) Å | θ = 2.3–33.2° |
α = 94.001 (3)° | µ = 5.77 mm−1 |
β = 94.784 (3)° | T = 150 K |
γ = 107.518 (3)° | Prism, blue |
V = 1613.0 (2) Å3 | 0.44 × 0.42 × 0.28 mm |
Bruker AXS D8 Quest CMOS diffractometer | 12306 independent reflections |
Radiation source: fine focus sealed tube X-ray source | 10012 reflections with I > 2σ(I) |
Triumph curved graphite crystal monochromator | Rint = 0.042 |
Detector resolution: 10.4167 pixels mm-1 | θmax = 33.2°, θmin = 2.5° |
ω and phi scans | h = −17→17 |
Absorption correction: multi-scan (SADABS; Krause et al., 2015) | k = −17→17 |
Tmin = 0.548, Tmax = 0.747 | l = −20→20 |
50443 measured reflections |
Refinement on F2 | Primary atom site location: isomorphous structure methods |
Least-squares matrix: full | Secondary atom site location: difference Fourier map |
R[F2 > 2σ(F2)] = 0.033 | Hydrogen site location: mixed |
wR(F2) = 0.082 | H atoms treated by a mixture of independent and constrained refinement |
S = 1.05 | w = 1/[σ2(Fo2) + (0.0289P)2 + 5.881P] where P = (Fo2 + 2Fc2)/3 |
12306 reflections | (Δ/σ)max = 0.001 |
563 parameters | Δρmax = 2.80 e Å−3 |
139 restraints | Δρmin = −2.27 e Å−3 |
Geometry. All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. |
Refinement. Solved by isomorphous replacement from its Gd analogue. A water molecule is partially occupied, inducing disorder for the nearby carbonate anion. The two disordered moieties were restrained to have similar geometries. Uij components of ADPs for disordered atoms closer to each other than 2.0 Angstrom were restrained to be similar. The distance of the water oxygen to one of the carbonate oxygen atoms was restrained to be at least 2.8 Angstrom for the moiety that contains the water molecule. Water H atom positions were refined and O-H and H···H distances were restrained to 0.84 (2) and 1.36 (2) Angstrom, respectively. The water H atom positions of the disordered moiety were further restrained based on hydrogen bonding considerations. Subject to these conditions the occupancy ratio refined to 0.445 (11) to 0.555 (11). |
x | y | z | Uiso*/Ueq | Occ. (<1) | |
C1 | 1.0280 (3) | 0.3079 (3) | 0.5731 (2) | 0.0118 (5) | |
C2 | 1.0125 (3) | 0.3910 (3) | 0.6604 (2) | 0.0141 (6) | |
H2C | 1.009297 | 0.349401 | 0.723592 | 0.017* | |
H2D | 1.085438 | 0.466647 | 0.670787 | 0.017* | |
C3 | 0.6597 (3) | 0.4528 (3) | 0.3871 (2) | 0.0138 (5) | |
C4 | 0.5618 (3) | 0.5118 (3) | 0.3530 (3) | 0.0177 (6) | |
H4C | 0.491688 | 0.490089 | 0.395941 | 0.021* | |
H4D | 0.599580 | 0.602076 | 0.361106 | 0.021* | |
C5 | 0.5303 (3) | 0.2146 (3) | 0.0111 (2) | 0.0123 (5) | |
C6 | 0.4901 (3) | 0.1750 (3) | −0.1003 (2) | 0.0173 (6) | |
H6C | 0.397531 | 0.136935 | −0.111278 | 0.021* | |
H6D | 0.512297 | 0.247545 | −0.139250 | 0.021* | |
C7 | 0.8131 (3) | −0.0808 (3) | −0.0328 (2) | 0.0114 (5) | |
C8 | 0.8533 (3) | −0.1924 (3) | −0.0563 (2) | 0.0140 (5) | |
H8C | 0.778056 | −0.265608 | −0.070891 | 0.017* | |
H8D | 0.898930 | −0.182788 | −0.117611 | 0.017* | |
C9 | 1.1067 (3) | −0.0368 (3) | 0.3181 (2) | 0.0098 (5) | |
C10 | 1.2053 (3) | −0.0372 (3) | 0.4021 (2) | 0.0139 (5) | |
H10C | 1.182002 | −0.117768 | 0.429942 | 0.017* | |
H10D | 1.287142 | −0.024697 | 0.374459 | 0.017* | |
C11 | 0.9971 (13) | 0.3886 (16) | 0.1665 (14) | 0.022 (2) | 0.445 (11) |
O12 | 0.8827 (10) | 0.3498 (14) | 0.1383 (12) | 0.0236 (19) | 0.445 (11) |
O13 | 1.042 (3) | 0.334 (2) | 0.2371 (15) | 0.024 (2) | 0.445 (11) |
O14 | 1.0681 (9) | 0.4809 (11) | 0.1285 (9) | 0.030 (2) | 0.445 (11) |
O23 | 1.2942 (11) | 0.5207 (9) | 0.1960 (8) | 0.082 (4) | 0.445 (11) |
H23A | 1.308337 | 0.590634 | 0.233418 | 0.122* | 0.445 (11) |
H23B | 1.233023 | 0.460780 | 0.173402 | 0.122* | 0.445 (11) |
C11B | 1.0297 (10) | 0.3906 (11) | 0.1741 (10) | 0.0202 (19) | 0.555 (11) |
O12B | 0.9181 (9) | 0.3477 (11) | 0.1319 (10) | 0.0282 (19) | 0.555 (11) |
O13B | 1.050 (2) | 0.3358 (17) | 0.2541 (11) | 0.0225 (19) | 0.555 (11) |
O14B | 1.1139 (8) | 0.4780 (8) | 0.1452 (6) | 0.0272 (17) | 0.555 (11) |
N1 | 0.9480 (3) | 0.2936 (2) | 0.49315 (19) | 0.0136 (5) | |
N2 | 0.8953 (3) | 0.4226 (3) | 0.6386 (2) | 0.0216 (6) | |
H2A | 0.911575 | 0.504772 | 0.653058 | 0.026* | |
H2B | 0.837833 | 0.383792 | 0.679653 | 0.026* | |
N3 | 0.6791 (3) | 0.3750 (2) | 0.3201 (2) | 0.0138 (5) | |
N4 | 0.5131 (4) | 0.4698 (3) | 0.2452 (2) | 0.0255 (7) | |
H4A | 0.542034 | 0.532305 | 0.206181 | 0.031* | |
H4B | 0.427458 | 0.447852 | 0.238332 | 0.031* | |
N5 | 0.6111 (3) | 0.1682 (2) | 0.05439 (19) | 0.0122 (5) | |
N6 | 0.5523 (3) | 0.0857 (3) | −0.13800 (19) | 0.0136 (5) | |
H6A | 0.584500 | 0.107440 | −0.197228 | 0.016* | |
H6B | 0.495105 | 0.009616 | −0.150397 | 0.016* | |
N7 | 0.8501 (3) | −0.0247 (2) | 0.05795 (19) | 0.0109 (4) | |
N8 | 0.9364 (3) | −0.2099 (2) | 0.0309 (2) | 0.0141 (5) | |
H8A | 1.014323 | −0.201893 | 0.011654 | 0.017* | |
H8B | 0.904566 | −0.286957 | 0.049667 | 0.017* | |
N9 | 1.0597 (2) | 0.0533 (2) | 0.32597 (19) | 0.0110 (4) | |
N10 | 1.2179 (3) | 0.0612 (3) | 0.4850 (2) | 0.0185 (5) | |
H10A | 1.298457 | 0.112497 | 0.494020 | 0.022* | |
H10B | 1.200453 | 0.027405 | 0.544288 | 0.022* | |
N11 | 0.5792 (3) | 0.2265 (3) | 0.6124 (2) | 0.0229 (6) | |
Cu1 | 1.09880 (4) | 0.15681 (3) | 0.44997 (3) | 0.01166 (7) | |
Cu2 | 0.82339 (4) | 0.37481 (3) | 0.49405 (3) | 0.01165 (7) | |
Cu3 | 0.56785 (4) | 0.32620 (4) | 0.19698 (3) | 0.01405 (8) | |
Cu4 | 0.69119 (4) | 0.08365 (4) | −0.03271 (3) | 0.01185 (7) | |
Cu5 | 0.95011 (4) | −0.08588 (3) | 0.15039 (3) | 0.01067 (7) | |
Ho1 | 0.84737 (2) | 0.19371 (2) | 0.24296 (2) | 0.01295 (4) | |
O1 | 0.9539 (2) | 0.2094 (2) | 0.41456 (17) | 0.0171 (5) | |
O2 | 1.1136 (2) | 0.2531 (2) | 0.57996 (16) | 0.0139 (4) | |
O3 | 0.7699 (2) | 0.3202 (2) | 0.35211 (16) | 0.0136 (4) | |
O4 | 0.7177 (2) | 0.4801 (2) | 0.47858 (17) | 0.0150 (4) | |
O5 | 0.6451 (2) | 0.2021 (2) | 0.15826 (16) | 0.0159 (4) | |
O6 | 0.4839 (2) | 0.2914 (2) | 0.05838 (17) | 0.0159 (4) | |
O7 | 0.8119 (2) | 0.0781 (2) | 0.07896 (17) | 0.0143 (4) | |
O8 | 0.7438 (2) | −0.0459 (2) | −0.10037 (16) | 0.0142 (4) | |
O9 | 0.9714 (2) | 0.0553 (2) | 0.24613 (16) | 0.0120 (4) | |
O10 | 1.0747 (2) | −0.1222 (2) | 0.24305 (17) | 0.0126 (4) | |
O11 | 0.7125 (2) | 0.0137 (2) | 0.2961 (2) | 0.0176 (5) | |
H11A | 0.647 (3) | 0.013 (4) | 0.320 (4) | 0.026* | |
H11B | 0.718 (5) | −0.054 (2) | 0.280 (4) | 0.026* | |
O15 | 0.6333 (3) | 0.2185 (3) | 0.5342 (2) | 0.0257 (6) | |
O16 | 0.6461 (4) | 0.2526 (4) | 0.6963 (2) | 0.0562 (12) | |
O17 | 0.4642 (3) | 0.2061 (3) | 0.6079 (3) | 0.0366 (7) | |
O18 | 1.2491 (3) | 0.3228 (2) | 0.3739 (2) | 0.0212 (5) | |
H18A | 1.265 (5) | 0.370 (4) | 0.426 (2) | 0.032* | |
H18B | 1.193 (4) | 0.332 (5) | 0.333 (3) | 0.032* | |
O19 | 0.3874 (2) | 0.1934 (2) | 0.26731 (19) | 0.0187 (5) | |
H19A | 0.343 (4) | 0.151 (4) | 0.218 (3) | 0.028* | |
H19B | 0.343 (4) | 0.226 (4) | 0.298 (3) | 0.028* | |
O20 | 0.8212 (3) | 0.2497 (2) | −0.1135 (2) | 0.0225 (5) | |
H20A | 0.839 (5) | 0.217 (4) | −0.165 (3) | 0.034* | |
H20B | 0.841 (5) | 0.3242 (18) | −0.108 (4) | 0.034* | |
O21 | 0.6432 (3) | 0.6168 (3) | 0.0936 (2) | 0.0311 (7) | |
H21A | 0.597 (5) | 0.617 (5) | 0.042 (3) | 0.047* | |
H21B | 0.677 (5) | 0.568 (4) | 0.071 (4) | 0.047* | |
O22 | 0.8170 (5) | 0.5170 (4) | 0.0460 (3) | 0.0501 (10) | |
H22A | 0.845 (7) | 0.518 (7) | −0.013 (3) | 0.075* | |
H22B | 0.843 (7) | 0.460 (5) | 0.070 (5) | 0.075* | |
O24 | 0.7767 (2) | −0.1977 (2) | 0.24108 (19) | 0.0173 (5) | |
H24A | 0.801 (4) | −0.226 (4) | 0.290 (3) | 0.026* | |
H24B | 0.737 (4) | −0.256 (3) | 0.201 (3) | 0.026* | |
O25 | 0.5129 (3) | 0.0538 (2) | 0.3694 (2) | 0.0218 (5) | |
H25A | 0.477 (4) | 0.094 (4) | 0.338 (4) | 0.033* | |
H25B | 0.540 (5) | 0.094 (4) | 0.425 (2) | 0.033* |
U11 | U22 | U33 | U12 | U13 | U23 | |
C1 | 0.0147 (13) | 0.0115 (12) | 0.0078 (11) | 0.0018 (10) | 0.0012 (10) | 0.0010 (9) |
C2 | 0.0204 (15) | 0.0121 (13) | 0.0079 (12) | 0.0028 (11) | 0.0018 (11) | −0.0008 (10) |
C3 | 0.0203 (15) | 0.0086 (12) | 0.0119 (13) | 0.0034 (11) | 0.0032 (11) | −0.0004 (10) |
C4 | 0.0232 (16) | 0.0141 (14) | 0.0159 (14) | 0.0078 (12) | −0.0007 (12) | −0.0035 (11) |
C5 | 0.0152 (14) | 0.0140 (13) | 0.0081 (12) | 0.0052 (11) | −0.0004 (10) | 0.0010 (9) |
C6 | 0.0209 (16) | 0.0243 (16) | 0.0093 (12) | 0.0126 (13) | −0.0024 (11) | −0.0001 (11) |
C7 | 0.0139 (13) | 0.0129 (12) | 0.0081 (12) | 0.0053 (11) | 0.0013 (10) | −0.0002 (9) |
C8 | 0.0200 (15) | 0.0124 (13) | 0.0100 (12) | 0.0068 (11) | 0.0005 (11) | −0.0033 (10) |
C9 | 0.0093 (12) | 0.0113 (12) | 0.0087 (11) | 0.0028 (10) | 0.0011 (9) | 0.0015 (9) |
C10 | 0.0138 (13) | 0.0144 (13) | 0.0146 (13) | 0.0059 (11) | 0.0001 (11) | 0.0029 (10) |
C11 | 0.025 (5) | 0.024 (3) | 0.017 (3) | 0.009 (4) | 0.005 (4) | −0.003 (3) |
O12 | 0.022 (4) | 0.026 (3) | 0.022 (3) | 0.004 (4) | 0.003 (4) | 0.008 (3) |
O13 | 0.026 (4) | 0.022 (3) | 0.021 (5) | 0.001 (3) | 0.004 (4) | 0.001 (4) |
O14 | 0.027 (5) | 0.029 (4) | 0.030 (4) | 0.000 (4) | 0.005 (4) | 0.005 (3) |
O23 | 0.145 (10) | 0.061 (6) | 0.075 (7) | 0.088 (7) | 0.012 (7) | 0.002 (5) |
C11B | 0.030 (4) | 0.016 (2) | 0.014 (3) | 0.004 (3) | 0.007 (3) | −0.003 (2) |
O12B | 0.032 (5) | 0.021 (2) | 0.026 (3) | −0.003 (4) | 0.009 (4) | 0.006 (2) |
O13B | 0.025 (4) | 0.019 (3) | 0.018 (4) | −0.002 (2) | 0.001 (3) | 0.002 (3) |
O14B | 0.032 (4) | 0.021 (3) | 0.019 (3) | −0.007 (3) | 0.011 (3) | 0.000 (2) |
N1 | 0.0176 (12) | 0.0149 (12) | 0.0083 (11) | 0.0056 (10) | 0.0029 (9) | −0.0040 (9) |
N2 | 0.0274 (16) | 0.0282 (15) | 0.0106 (12) | 0.0139 (13) | −0.0014 (11) | −0.0083 (11) |
N3 | 0.0199 (13) | 0.0131 (11) | 0.0095 (11) | 0.0081 (10) | −0.0011 (9) | −0.0014 (9) |
N4 | 0.046 (2) | 0.0207 (14) | 0.0164 (13) | 0.0227 (15) | −0.0035 (13) | −0.0010 (11) |
N5 | 0.0145 (12) | 0.0167 (12) | 0.0066 (10) | 0.0080 (10) | −0.0024 (9) | −0.0014 (8) |
N6 | 0.0163 (12) | 0.0169 (12) | 0.0076 (10) | 0.0059 (10) | 0.0004 (9) | −0.0004 (9) |
N7 | 0.0153 (12) | 0.0104 (10) | 0.0088 (10) | 0.0073 (9) | 0.0004 (9) | −0.0012 (8) |
N8 | 0.0170 (12) | 0.0130 (11) | 0.0130 (11) | 0.0072 (10) | −0.0011 (9) | −0.0026 (9) |
N9 | 0.0118 (11) | 0.0115 (11) | 0.0087 (10) | 0.0035 (9) | −0.0031 (8) | −0.0011 (8) |
N10 | 0.0191 (14) | 0.0213 (14) | 0.0147 (12) | 0.0081 (11) | −0.0050 (10) | −0.0014 (10) |
N11 | 0.0229 (15) | 0.0218 (14) | 0.0209 (14) | 0.0027 (12) | 0.0021 (12) | 0.0007 (11) |
Cu1 | 0.01256 (17) | 0.01432 (17) | 0.00767 (15) | 0.00496 (14) | −0.00191 (12) | −0.00186 (12) |
Cu2 | 0.01622 (18) | 0.01112 (16) | 0.00713 (15) | 0.00445 (14) | 0.00047 (13) | −0.00241 (12) |
Cu3 | 0.0221 (2) | 0.01470 (17) | 0.00826 (16) | 0.01148 (15) | −0.00165 (14) | −0.00181 (12) |
Cu4 | 0.01516 (17) | 0.01590 (17) | 0.00609 (15) | 0.00853 (14) | −0.00143 (12) | −0.00185 (12) |
Cu5 | 0.01450 (17) | 0.00999 (15) | 0.00826 (15) | 0.00602 (13) | −0.00087 (12) | −0.00170 (12) |
Ho1 | 0.01760 (7) | 0.01211 (6) | 0.00911 (6) | 0.00536 (5) | −0.00014 (5) | −0.00060 (4) |
O1 | 0.0202 (11) | 0.0247 (12) | 0.0085 (9) | 0.0135 (10) | −0.0027 (8) | −0.0079 (8) |
O2 | 0.0158 (10) | 0.0164 (10) | 0.0085 (9) | 0.0050 (9) | −0.0018 (8) | −0.0016 (8) |
O3 | 0.0185 (11) | 0.0150 (10) | 0.0096 (9) | 0.0102 (9) | −0.0013 (8) | −0.0016 (8) |
O4 | 0.0214 (11) | 0.0133 (10) | 0.0101 (9) | 0.0064 (9) | 0.0003 (8) | −0.0037 (8) |
O5 | 0.0229 (12) | 0.0225 (11) | 0.0050 (9) | 0.0140 (10) | −0.0042 (8) | −0.0049 (8) |
O6 | 0.0222 (12) | 0.0193 (11) | 0.0101 (10) | 0.0135 (9) | −0.0016 (8) | −0.0018 (8) |
O7 | 0.0211 (11) | 0.0143 (10) | 0.0106 (9) | 0.0128 (9) | −0.0033 (8) | −0.0046 (8) |
O8 | 0.0203 (11) | 0.0162 (10) | 0.0079 (9) | 0.0098 (9) | −0.0016 (8) | −0.0023 (7) |
O9 | 0.0159 (10) | 0.0135 (10) | 0.0070 (9) | 0.0076 (8) | −0.0055 (7) | −0.0012 (7) |
O10 | 0.0152 (10) | 0.0116 (9) | 0.0114 (9) | 0.0056 (8) | 0.0001 (8) | −0.0003 (7) |
O11 | 0.0150 (11) | 0.0137 (10) | 0.0236 (12) | 0.0037 (9) | 0.0030 (9) | 0.0003 (9) |
O15 | 0.0262 (14) | 0.0257 (13) | 0.0224 (13) | 0.0025 (11) | 0.0059 (11) | 0.0047 (10) |
O16 | 0.039 (2) | 0.086 (3) | 0.0181 (15) | −0.0168 (19) | 0.0004 (14) | 0.0038 (17) |
O17 | 0.0214 (14) | 0.0286 (15) | 0.059 (2) | 0.0074 (12) | 0.0086 (14) | −0.0025 (14) |
O18 | 0.0242 (13) | 0.0197 (12) | 0.0194 (12) | 0.0088 (10) | 0.0004 (10) | −0.0062 (9) |
O19 | 0.0176 (12) | 0.0233 (12) | 0.0142 (11) | 0.0071 (10) | −0.0017 (9) | −0.0041 (9) |
O20 | 0.0257 (13) | 0.0200 (12) | 0.0240 (13) | 0.0097 (11) | 0.0079 (10) | 0.0001 (10) |
O21 | 0.0443 (19) | 0.0255 (14) | 0.0248 (14) | 0.0174 (13) | −0.0118 (13) | 0.0005 (11) |
O22 | 0.087 (3) | 0.043 (2) | 0.0364 (19) | 0.037 (2) | 0.026 (2) | 0.0151 (16) |
O24 | 0.0195 (12) | 0.0172 (11) | 0.0146 (11) | 0.0050 (9) | −0.0019 (9) | 0.0040 (8) |
O25 | 0.0198 (12) | 0.0216 (12) | 0.0241 (13) | 0.0072 (10) | 0.0019 (10) | −0.0004 (10) |
C1—N1 | 1.296 (4) | N5—Cu4 | 1.903 (3) |
C1—O2 | 1.297 (4) | N6—Cu4 | 2.008 (3) |
C1—C2 | 1.503 (4) | N6—H6A | 0.9100 |
C2—N2 | 1.475 (5) | N6—H6B | 0.9100 |
C2—H2C | 0.9900 | N7—O7 | 1.391 (3) |
C2—H2D | 0.9900 | N7—Cu5 | 1.902 (3) |
C3—N3 | 1.294 (4) | N8—Cu5 | 2.019 (3) |
C3—O4 | 1.297 (4) | N8—H8A | 0.9100 |
C3—C4 | 1.508 (5) | N8—H8B | 0.9100 |
C4—N4 | 1.478 (4) | N9—O9 | 1.393 (3) |
C4—H4C | 0.9900 | N9—Cu1 | 1.897 (2) |
C4—H4D | 0.9900 | N10—Cu1 | 2.013 (3) |
C5—N5 | 1.296 (4) | N10—H10A | 0.9100 |
C5—O6 | 1.302 (4) | N10—H10B | 0.9100 |
C5—C6 | 1.504 (4) | N11—O17 | 1.234 (4) |
C6—N6 | 1.485 (4) | N11—O16 | 1.252 (5) |
C6—H6C | 0.9900 | N11—O15 | 1.253 (4) |
C6—H6D | 0.9900 | Cu1—O1 | 1.930 (2) |
C7—N7 | 1.296 (4) | Cu1—O2 | 1.948 (2) |
C7—O8 | 1.299 (4) | Cu1—O18 | 2.471 (3) |
C7—C8 | 1.504 (4) | Cu2—O3 | 1.926 (2) |
C8—N8 | 1.485 (4) | Cu2—O4 | 1.940 (2) |
C8—H8C | 0.9900 | Cu2—O15 | 2.463 (3) |
C8—H8D | 0.9900 | Cu3—O5 | 1.939 (2) |
C9—O10 | 1.294 (3) | Cu3—O6 | 1.949 (2) |
C9—N9 | 1.297 (4) | Cu3—O19 | 2.437 (3) |
C9—C10 | 1.502 (4) | Cu4—O7 | 1.937 (2) |
C10—N10 | 1.487 (4) | Cu4—O8 | 1.949 (2) |
C10—H10C | 0.9900 | Cu4—O20 | 2.405 (3) |
C10—H10D | 0.9900 | Cu5—O9 | 1.931 (2) |
C11—O12 | 1.239 (11) | Cu5—O10 | 1.941 (2) |
C11—O14 | 1.283 (12) | Cu5—O24 | 2.443 (3) |
C11—O13 | 1.305 (13) | Ho1—O11 | 2.358 (2) |
C11—Ho1 | 2.683 (14) | Ho1—O3 | 2.374 (2) |
O12—Ho1 | 2.304 (16) | Ho1—O7 | 2.404 (2) |
O13—Ho1 | 2.30 (3) | Ho1—O9 | 2.407 (2) |
O23—H23A | 0.8779 | Ho1—O1 | 2.446 (2) |
O23—H23B | 0.8290 | Ho1—O5 | 2.475 (2) |
C11B—O14B | 1.261 (9) | O11—H11A | 0.817 (19) |
C11B—O12B | 1.262 (10) | O11—H11B | 0.813 (19) |
C11B—O13B | 1.309 (10) | O18—H18A | 0.821 (19) |
C11B—Ho1 | 2.817 (10) | O18—H18B | 0.834 (19) |
O12B—Ho1 | 2.374 (12) | O19—H19A | 0.820 (19) |
O13B—Ho1 | 2.35 (2) | O19—H19B | 0.826 (19) |
N1—O1 | 1.391 (3) | O20—H20A | 0.824 (19) |
N1—Cu2 | 1.898 (3) | O20—H20B | 0.814 (19) |
N2—Cu2 | 1.987 (3) | O21—H21A | 0.822 (19) |
N2—H2A | 0.9100 | O21—H21B | 0.827 (19) |
N2—H2B | 0.9100 | O22—H22A | 0.87 (2) |
N3—O3 | 1.400 (3) | O22—H22B | 0.86 (2) |
N3—Cu3 | 1.908 (3) | O24—H24A | 0.810 (19) |
N4—Cu3 | 2.010 (3) | O24—H24B | 0.820 (19) |
N4—H4A | 0.9100 | O25—H25A | 0.817 (19) |
N4—H4B | 0.9100 | O25—H25B | 0.826 (19) |
N5—O5 | 1.392 (3) | ||
N1—C1—O2 | 123.5 (3) | O4—Cu2—O15 | 86.17 (10) |
N1—C1—C2 | 115.0 (3) | N2—Cu2—O15 | 94.35 (12) |
O2—C1—C2 | 121.5 (3) | N3—Cu3—O5 | 90.80 (10) |
N2—C2—C1 | 109.7 (3) | N3—Cu3—O6 | 168.64 (12) |
N2—C2—H2C | 109.7 | O5—Cu3—O6 | 85.53 (9) |
C1—C2—H2C | 109.7 | N3—Cu3—N4 | 82.62 (12) |
N2—C2—H2D | 109.7 | O5—Cu3—N4 | 171.72 (13) |
C1—C2—H2D | 109.7 | O6—Cu3—N4 | 99.97 (11) |
H2C—C2—H2D | 108.2 | N3—Cu3—O19 | 97.77 (10) |
N3—C3—O4 | 124.0 (3) | O5—Cu3—O19 | 97.72 (10) |
N3—C3—C4 | 115.6 (3) | O6—Cu3—O19 | 93.38 (10) |
O4—C3—C4 | 120.4 (3) | N4—Cu3—O19 | 88.20 (13) |
N4—C4—C3 | 110.2 (3) | N5—Cu4—O7 | 91.47 (10) |
N4—C4—H4C | 109.6 | N5—Cu4—O8 | 162.00 (11) |
C3—C4—H4C | 109.6 | O7—Cu4—O8 | 84.51 (9) |
N4—C4—H4D | 109.6 | N5—Cu4—N6 | 83.87 (11) |
C3—C4—H4D | 109.6 | O7—Cu4—N6 | 173.92 (11) |
H4C—C4—H4D | 108.1 | O8—Cu4—N6 | 98.74 (10) |
N5—C5—O6 | 123.9 (3) | N5—Cu4—O20 | 101.33 (10) |
N5—C5—C6 | 116.3 (3) | O7—Cu4—O20 | 99.21 (10) |
O6—C5—C6 | 119.8 (3) | O8—Cu4—O20 | 96.64 (9) |
N6—C6—C5 | 110.8 (3) | N6—Cu4—O20 | 85.56 (11) |
N6—C6—H6C | 109.5 | N7—Cu5—O9 | 89.41 (10) |
C5—C6—H6C | 109.5 | N7—Cu5—O10 | 170.18 (10) |
N6—C6—H6D | 109.5 | O9—Cu5—O10 | 85.63 (9) |
C5—C6—H6D | 109.5 | N7—Cu5—N8 | 83.25 (11) |
H6C—C6—H6D | 108.1 | O9—Cu5—N8 | 169.11 (11) |
N7—C7—O8 | 123.2 (3) | O10—Cu5—N8 | 100.38 (10) |
N7—C7—C8 | 116.1 (3) | N7—Cu5—O24 | 95.87 (10) |
O8—C7—C8 | 120.7 (3) | O9—Cu5—O24 | 87.88 (9) |
N8—C8—C7 | 110.6 (2) | O10—Cu5—O24 | 92.41 (9) |
N8—C8—H8C | 109.5 | N8—Cu5—O24 | 100.83 (10) |
C7—C8—H8C | 109.5 | O13—Ho1—O12 | 56.5 (4) |
N8—C8—H8D | 109.5 | O13—Ho1—O11 | 152.9 (5) |
C7—C8—H8D | 109.5 | O12—Ho1—O11 | 150.1 (3) |
H8C—C8—H8D | 108.1 | O13B—Ho1—O11 | 148.4 (3) |
O10—C9—N9 | 124.0 (3) | O13—Ho1—O3 | 96.3 (8) |
O10—C9—C10 | 120.0 (3) | O12—Ho1—O3 | 86.1 (3) |
N9—C9—C10 | 116.1 (3) | O13B—Ho1—O3 | 94.1 (6) |
N10—C10—C9 | 110.9 (3) | O11—Ho1—O3 | 91.94 (8) |
N10—C10—H10C | 109.5 | O13B—Ho1—O12B | 53.9 (3) |
C9—C10—H10C | 109.5 | O11—Ho1—O12B | 156.3 (3) |
N10—C10—H10D | 109.5 | O3—Ho1—O12B | 93.6 (3) |
C9—C10—H10D | 109.5 | O13—Ho1—O7 | 102.0 (6) |
H10C—C10—H10D | 108.1 | O12—Ho1—O7 | 79.5 (4) |
O12—C11—O14 | 120.4 (12) | O13B—Ho1—O7 | 106.6 (5) |
O12—C11—O13 | 117.9 (14) | O11—Ho1—O7 | 85.22 (8) |
O14—C11—O13 | 121.7 (13) | O3—Ho1—O7 | 144.68 (8) |
O12—C11—Ho1 | 59.0 (8) | O12B—Ho1—O7 | 77.0 (3) |
O14—C11—Ho1 | 179.1 (14) | O13—Ho1—O9 | 81.6 (7) |
O13—C11—Ho1 | 58.9 (12) | O12—Ho1—O9 | 121.8 (3) |
C11—O12—Ho1 | 93.5 (9) | O13B—Ho1—O9 | 80.2 (5) |
C11—O13—Ho1 | 92.0 (13) | O11—Ho1—O9 | 76.01 (8) |
H23A—O23—H23B | 137.8 | O3—Ho1—O9 | 141.82 (7) |
O14B—C11B—O12B | 124.9 (10) | O12B—Ho1—O9 | 112.0 (3) |
O14B—C11B—O13B | 122.2 (10) | O7—Ho1—O9 | 71.34 (7) |
O12B—C11B—O13B | 112.9 (10) | O13—Ho1—O1 | 76.1 (4) |
O14B—C11B—Ho1 | 178.2 (8) | O12—Ho1—O1 | 124.9 (4) |
O12B—C11B—Ho1 | 56.8 (6) | O13B—Ho1—O1 | 70.4 (3) |
O13B—C11B—Ho1 | 56.1 (9) | O11—Ho1—O1 | 82.19 (9) |
C11B—O12B—Ho1 | 96.8 (7) | O3—Ho1—O1 | 71.84 (7) |
C11B—O13B—Ho1 | 96.4 (9) | O12B—Ho1—O1 | 121.4 (3) |
C1—N1—O1 | 116.0 (3) | O7—Ho1—O1 | 141.85 (8) |
C1—N1—Cu2 | 119.6 (2) | O9—Ho1—O1 | 70.69 (7) |
O1—N1—Cu2 | 124.2 (2) | O13—Ho1—O5 | 125.9 (5) |
C2—N2—Cu2 | 111.84 (19) | O12—Ho1—O5 | 69.8 (3) |
C2—N2—H2A | 109.2 | O13B—Ho1—O5 | 130.1 (4) |
Cu2—N2—H2A | 109.2 | O11—Ho1—O5 | 81.21 (9) |
C2—N2—H2B | 109.2 | O3—Ho1—O5 | 72.17 (7) |
Cu2—N2—H2B | 109.2 | O12B—Ho1—O5 | 78.7 (3) |
H2A—N2—H2B | 107.9 | O7—Ho1—O5 | 72.61 (7) |
C3—N3—O3 | 115.4 (3) | O9—Ho1—O5 | 138.51 (7) |
C3—N3—Cu3 | 118.6 (2) | O1—Ho1—O5 | 139.56 (7) |
O3—N3—Cu3 | 125.27 (18) | O13—Ho1—C11 | 29.1 (3) |
C4—N4—Cu3 | 110.7 (2) | O12—Ho1—C11 | 27.5 (3) |
C4—N4—H4A | 109.5 | O11—Ho1—C11 | 175.1 (4) |
Cu3—N4—H4A | 109.5 | O3—Ho1—C11 | 91.9 (4) |
C4—N4—H4B | 109.5 | O7—Ho1—C11 | 89.9 (4) |
Cu3—N4—H4B | 109.5 | O9—Ho1—C11 | 102.7 (4) |
H4A—N4—H4B | 108.1 | O1—Ho1—C11 | 101.9 (4) |
C5—N5—O5 | 116.0 (2) | O5—Ho1—C11 | 97.1 (3) |
C5—N5—Cu4 | 117.0 (2) | O13B—Ho1—C11B | 27.5 (2) |
O5—N5—Cu4 | 126.14 (19) | O11—Ho1—C11B | 172.5 (3) |
C6—N6—Cu4 | 109.22 (19) | O3—Ho1—C11B | 94.7 (3) |
C6—N6—H6A | 109.8 | O12B—Ho1—C11B | 26.4 (3) |
Cu4—N6—H6A | 109.8 | O7—Ho1—C11B | 91.3 (3) |
C6—N6—H6B | 109.8 | O9—Ho1—C11B | 96.6 (3) |
Cu4—N6—H6B | 109.8 | O1—Ho1—C11B | 96.6 (3) |
H6A—N6—H6B | 108.3 | O5—Ho1—C11B | 104.1 (3) |
C7—N7—O7 | 115.5 (2) | N1—O1—Cu1 | 107.69 (18) |
C7—N7—Cu5 | 119.1 (2) | N1—O1—Ho1 | 123.14 (18) |
O7—N7—Cu5 | 125.31 (18) | Cu1—O1—Ho1 | 125.76 (10) |
C8—N8—Cu5 | 110.78 (19) | C1—O2—Cu1 | 107.06 (18) |
C8—N8—H8A | 109.5 | N3—O3—Cu2 | 107.65 (16) |
Cu5—N8—H8A | 109.5 | N3—O3—Ho1 | 124.14 (16) |
C8—N8—H8B | 109.5 | Cu2—O3—Ho1 | 128.11 (11) |
Cu5—N8—H8B | 109.5 | C3—O4—Cu2 | 106.88 (19) |
H8A—N8—H8B | 108.1 | N5—O5—Cu3 | 107.34 (17) |
C9—N9—O9 | 115.8 (2) | N5—O5—Ho1 | 121.38 (17) |
C9—N9—Cu1 | 118.3 (2) | Cu3—O5—Ho1 | 123.44 (10) |
O9—N9—Cu1 | 125.40 (19) | C5—O6—Cu3 | 106.62 (19) |
C10—N10—Cu1 | 110.2 (2) | N7—O7—Cu4 | 107.95 (16) |
C10—N10—H10A | 109.6 | N7—O7—Ho1 | 124.58 (17) |
Cu1—N10—H10A | 109.6 | Cu4—O7—Ho1 | 125.63 (10) |
C10—N10—H10B | 109.6 | C7—O8—Cu4 | 107.32 (18) |
Cu1—N10—H10B | 109.6 | N9—O9—Cu5 | 107.61 (16) |
H10A—N10—H10B | 108.1 | N9—O9—Ho1 | 125.18 (16) |
O17—N11—O16 | 120.7 (4) | Cu5—O9—Ho1 | 126.63 (10) |
O17—N11—O15 | 121.9 (3) | C9—O10—Cu5 | 107.02 (19) |
O16—N11—O15 | 117.4 (3) | Ho1—O11—H11A | 122 (3) |
N9—Cu1—O1 | 89.22 (10) | Ho1—O11—H11B | 122 (3) |
N9—Cu1—O2 | 171.80 (11) | H11A—O11—H11B | 114 (5) |
O1—Cu1—O2 | 85.31 (9) | N11—O15—Cu2 | 124.4 (2) |
N9—Cu1—N10 | 83.88 (11) | Cu1—O18—H18A | 93 (4) |
O1—Cu1—N10 | 165.90 (12) | Cu1—O18—H18B | 93 (4) |
O2—Cu1—N10 | 100.11 (11) | H18A—O18—H18B | 114 (5) |
N9—Cu1—O18 | 92.05 (10) | Cu3—O19—H19A | 104 (3) |
O1—Cu1—O18 | 95.36 (10) | Cu3—O19—H19B | 118 (3) |
O2—Cu1—O18 | 94.54 (9) | H19A—O19—H19B | 108 (5) |
N10—Cu1—O18 | 97.16 (11) | Cu4—O20—H20A | 105 (4) |
N1—Cu2—O3 | 90.61 (10) | Cu4—O20—H20B | 137 (4) |
N1—Cu2—O4 | 168.51 (11) | H20A—O20—H20B | 116 (5) |
O3—Cu2—O4 | 85.63 (9) | H21A—O21—H21B | 99 (6) |
N1—Cu2—N2 | 82.56 (12) | H22A—O22—H22B | 100 (6) |
O3—Cu2—N2 | 173.12 (11) | Cu5—O24—H24A | 112 (3) |
O4—Cu2—N2 | 100.93 (11) | Cu5—O24—H24B | 104 (3) |
N1—Cu2—O15 | 104.57 (11) | H24A—O24—H24B | 106 (5) |
O3—Cu2—O15 | 88.10 (10) | H25A—O25—H25B | 105 (5) |
N1—C1—C2—N2 | 8.4 (4) | C9—N9—Cu1—N10 | 7.6 (2) |
O2—C1—C2—N2 | −169.9 (3) | O9—N9—Cu1—N10 | 178.8 (2) |
N3—C3—C4—N4 | −2.7 (4) | C9—N9—Cu1—O18 | 104.6 (2) |
O4—C3—C4—N4 | 177.8 (3) | O9—N9—Cu1—O18 | −84.2 (2) |
N5—C5—C6—N6 | 1.1 (4) | C1—N1—Cu2—O3 | 173.7 (2) |
O6—C5—C6—N6 | −178.8 (3) | O1—N1—Cu2—O3 | −12.2 (2) |
N7—C7—C8—N8 | −3.6 (4) | C1—N1—Cu2—O4 | 103.0 (5) |
O8—C7—C8—N8 | 177.4 (3) | O1—N1—Cu2—O4 | −82.9 (6) |
O10—C9—C10—N10 | −174.3 (3) | C1—N1—Cu2—N2 | −5.5 (3) |
N9—C9—C10—N10 | 6.7 (4) | O1—N1—Cu2—N2 | 168.6 (3) |
O14—C11—O12—Ho1 | 179.1 (16) | C1—N1—Cu2—O15 | −98.1 (2) |
O13—C11—O12—Ho1 | −2.4 (19) | O1—N1—Cu2—O15 | 76.0 (2) |
O12—C11—O13—Ho1 | 2.4 (19) | C1—N1—O1—Cu1 | −6.7 (3) |
O14—C11—O13—Ho1 | −179.2 (16) | Cu2—N1—O1—Cu1 | 178.98 (15) |
O14B—C11B—O12B—Ho1 | 179.6 (12) | C1—N1—O1—Ho1 | −166.9 (2) |
O13B—C11B—O12B—Ho1 | −1.4 (14) | Cu2—N1—O1—Ho1 | 18.8 (3) |
O14B—C11B—O13B—Ho1 | −179.5 (12) | N1—C1—O2—Cu1 | 2.0 (4) |
O12B—C11B—O13B—Ho1 | 1.4 (14) | C2—C1—O2—Cu1 | −179.9 (2) |
O2—C1—N1—O1 | 3.3 (4) | C3—N3—O3—Cu2 | 4.8 (3) |
C2—C1—N1—O1 | −174.9 (2) | Cu3—N3—O3—Cu2 | −165.17 (16) |
O2—C1—N1—Cu2 | 177.9 (2) | C3—N3—O3—Ho1 | −171.8 (2) |
C2—C1—N1—Cu2 | −0.3 (4) | Cu3—N3—O3—Ho1 | 18.3 (3) |
C1—C2—N2—Cu2 | −12.2 (3) | N3—C3—O4—Cu2 | −4.1 (4) |
O4—C3—N3—O3 | −0.4 (5) | C4—C3—O4—Cu2 | 175.3 (2) |
C4—C3—N3—O3 | −179.8 (3) | C5—N5—O5—Cu3 | −6.4 (3) |
O4—C3—N3—Cu3 | 170.2 (2) | Cu4—N5—O5—Cu3 | 162.64 (16) |
C4—C3—N3—Cu3 | −9.2 (4) | C5—N5—O5—Ho1 | −156.4 (2) |
C3—C4—N4—Cu3 | 12.1 (4) | Cu4—N5—O5—Ho1 | 12.6 (3) |
O6—C5—N5—O5 | 1.8 (5) | N5—C5—O6—Cu3 | 3.7 (4) |
C6—C5—N5—O5 | −178.0 (3) | C6—C5—O6—Cu3 | −176.4 (2) |
O6—C5—N5—Cu4 | −168.2 (2) | C7—N7—O7—Cu4 | 9.1 (3) |
C6—C5—N5—Cu4 | 11.9 (4) | Cu5—N7—O7—Cu4 | −171.06 (15) |
C5—C6—N6—Cu4 | −12.2 (3) | C7—N7—O7—Ho1 | 174.4 (2) |
O8—C7—N7—O7 | −0.8 (4) | Cu5—N7—O7—Ho1 | −5.8 (3) |
C8—C7—N7—O7 | −179.8 (3) | N7—C7—O8—Cu4 | −8.0 (4) |
O8—C7—N7—Cu5 | 179.4 (2) | C8—C7—O8—Cu4 | 171.0 (2) |
C8—C7—N7—Cu5 | 0.4 (4) | C9—N9—O9—Cu5 | 0.9 (3) |
C7—C8—N8—Cu5 | 4.8 (3) | Cu1—N9—O9—Cu5 | −170.52 (14) |
O10—C9—N9—O9 | −1.0 (4) | C9—N9—O9—Ho1 | 172.60 (19) |
C10—C9—N9—O9 | 177.9 (2) | Cu1—N9—O9—Ho1 | 1.2 (3) |
O10—C9—N9—Cu1 | 171.0 (2) | N9—C9—O10—Cu5 | 0.6 (3) |
C10—C9—N9—Cu1 | −10.0 (3) | C10—C9—O10—Cu5 | −178.3 (2) |
C9—C10—N10—Cu1 | −0.8 (3) | O17—N11—O15—Cu2 | 132.2 (3) |
C9—N9—Cu1—O1 | −160.1 (2) | O16—N11—O15—Cu2 | −50.0 (5) |
O9—N9—Cu1—O1 | 11.1 (2) |
D—H···A | D—H | H···A | D···A | D—H···A |
O23—H23A···O16i | 0.88 | 1.87 | 2.747 (11) | 173 |
O23—H23B···O14 | 0.83 | 1.98 | 2.509 (13) | 121 |
N2—H2A···O13i | 0.91 | 2.17 | 3.00 (3) | 150 |
N2—H2A···O13Bi | 0.91 | 2.05 | 2.90 (2) | 155 |
N2—H2B···O16 | 0.91 | 2.26 | 3.078 (5) | 149 |
N4—H4A···O21 | 0.91 | 2.07 | 2.914 (5) | 154 |
N4—H4B···O23ii | 0.91 | 1.98 | 2.726 (10) | 138 |
N6—H6A···O16iii | 0.91 | 2.25 | 3.060 (5) | 149 |
N6—H6B···N5iv | 0.91 | 2.52 | 3.267 (4) | 139 |
N6—H6B···O5iv | 0.91 | 2.46 | 3.359 (4) | 171 |
N8—H8A···O7v | 0.91 | 2.49 | 3.285 (4) | 146 |
N8—H8A···O20v | 0.91 | 2.41 | 3.017 (4) | 124 |
N8—H8B···O22vi | 0.91 | 2.17 | 3.048 (5) | 163 |
N10—H10A···O17vii | 0.91 | 2.23 | 3.024 (4) | 145 |
N10—H10B···O11viii | 0.91 | 2.39 | 3.183 (4) | 146 |
O11—H11A···O25 | 0.82 (2) | 1.86 (2) | 2.660 (4) | 165 (5) |
O11—H11B···O24 | 0.81 (2) | 2.00 (2) | 2.801 (4) | 166 (5) |
O18—H18A···O4i | 0.82 (2) | 2.01 (3) | 2.801 (3) | 160 (5) |
O18—H18B···O13 | 0.83 (2) | 2.04 (3) | 2.87 (2) | 173 (5) |
O18—H18B···O13B | 0.83 (2) | 1.84 (3) | 2.671 (18) | 171 (5) |
O19—H19A···O8iv | 0.82 (2) | 1.90 (2) | 2.713 (3) | 174 (5) |
O19—H19B···O18ii | 0.83 (2) | 2.02 (2) | 2.840 (4) | 174 (5) |
O20—H20A···O10v | 0.82 (2) | 1.96 (3) | 2.732 (3) | 156 (5) |
O20—H20B···O14ix | 0.81 (2) | 2.21 (3) | 2.997 (12) | 162 (5) |
O20—H20B···O14Bix | 0.81 (2) | 2.27 (3) | 3.060 (9) | 163 (5) |
O21—H21A···O6x | 0.82 (2) | 2.07 (3) | 2.813 (4) | 151 (6) |
O21—H21B···O22 | 0.83 (2) | 1.87 (3) | 2.638 (5) | 154 (6) |
O22—H22A···O14ix | 0.87 (2) | 1.88 (3) | 2.736 (12) | 170 (7) |
O22—H22A···O14Bix | 0.87 (2) | 1.84 (2) | 2.709 (9) | 173 (7) |
O22—H22B···O12 | 0.86 (2) | 1.74 (3) | 2.600 (16) | 170 (7) |
O22—H22B···O14 | 0.86 (2) | 2.51 (6) | 3.088 (11) | 125 (6) |
O22—H22B···O12B | 0.86 (2) | 1.93 (3) | 2.791 (14) | 173 (7) |
O24—H24A···O2viii | 0.81 (2) | 1.99 (2) | 2.781 (3) | 166 (5) |
O24—H24B···O21vi | 0.82 (2) | 1.94 (2) | 2.759 (4) | 174 (5) |
O25—H25A···O19 | 0.82 (2) | 1.96 (2) | 2.779 (4) | 177 (5) |
O25—H25B···O15 | 0.83 (2) | 1.95 (2) | 2.751 (4) | 165 (5) |
Symmetry codes: (i) −x+2, −y+1, −z+1; (ii) x−1, y, z; (iii) x, y, z−1; (iv) −x+1, −y, −z; (v) −x+2, −y, −z; (vi) x, y−1, z; (vii) x+1, y, z; (viii) −x+2, −y, −z+1; (ix) −x+2, −y+1, −z; (x) −x+1, −y+1, −z. |
CCDC127569 | Complex 1 | Complex 2 | Complex 3 | |
Formula | [EuCu5(GlyHA)5(CO3)(NO3)(H2O)5]·3.5H2O | [GdCu5(GlyHA)5(CO3)(NO3)(H2O)5]·3.5(H2O) | [DyCu5(GlyHA)5(CO3)(NO3)(H2O)5]·3.28(H2O) | [HoCu5(GlyHA)5(CO3)(NO3)(H2O)5]·3.445(H2O) |
M (g mol-1) | 1186.17 | 1190.49 | 1191.77 | 1197.21 |
Crystal system | Triclinic | Triclinic | Triclinic | Triclinic |
Space group | P1 | P1 | P1 | P1 |
a (Å) | 11.163 (5) | 11.2057 (15) | 11.1083 (5) | 11.2027 (9) |
b (Å) | 11.524 (4) | 11.5054 (15) | 11.4991 (5) | 11.4955 (9) |
c (Å) | 13.323 (4) | 13.2983 (10) | 13.2894 (6) | 13.2467 (10) |
α (°) | 93.85 (3) | 94.026 (4) | 93.9235 (16) | 94.001 (3) |
β (°) | 94.79 (3) | 94.942 (3) | 94.7713 (17) | 94.784 (3) |
γ (°) | 107.14 (3) | 107.558 (3) | 107.1470 (17) | 107.518 (3) |
Volume (Å3) | 1624.5 (10) | 1620.2 (3) | 1608.73 (13) | 1613.0 (2) |
Z | 2 | 2 | 2 | 2 |
T (K) | 293 (2) | 150 (2) | 150 (2) | 150 (2) |
Range of data collection | 2.53 °<2θ < 26.03° | 3.091° < 2θ <33.234° | 3.091° <2θ <28.693° | 2.544° <2θ <33.243° |
ρcalc (g cm-3) | 2.425 | 2.440 | 2.460 | 2.467 |
Absorption coefficient (mm-1) | 5.229 | 5.353 | 5.651 | 5.773 |
F(000) | 1168 | 1170 | 1170 | 1174.9 |
Collected reflections | 6344 | 118155 | 74286 | 50443 |
Reflections unique | 6344 | 12399 | 8274 | 12306 |
Rint | 0.1272 | 0.0560 | 0.0483 | 0.0417 |
Goodness-of-fit on F2 | 1.114 | 1.050 | 1.084 | 1.053 |
R1([I>2σ(I)]a | 0.1230 | 0.0343 | 0.0307 | 0.0334 |
wR2[I>2σ(I)]b | 0.2979 | 0.0681 | 0.0709 | 0.0769 |
Notes: (a) R1 = Σ||Fo| - |Fc||/Σ|Fo|, (b) wR2= {Σ[w(Fo2 - Fc2)2]/Σ[w(Fo2)2]}1/2 |
Cu1—O1 | 1.929 (2) | Cu2—O3 | 1.929 (2) | Cu3—O5 | 1.935 (2) |
Cu1—O2 | 1.949 (2) | Cu2—O4 | 1.939 (2) | Cu3—O6 | 1.952 (2) |
Cu1—N9 | 1.898 (2) | Cu2—N1 | 1.902 (3) | Cu3—N3 | 1.910 (3) |
Cu1—N10 | 2.016 (3) | Cu2—N2 | 1.985 (3) | Cu3—N4 | 2.010 (3) |
Cu1—O18w | 2.470 (3) | Cu2—O15(NO3) | 2.469 (3) | Cu3—O19w | 2.444 (2) |
Cu4—O7 | 1.938 (2) | Cu5—O9 | 1.931 (2) | Gd1—O1 | 2.457 (2) |
Cu4—O8 | 1.953 (2) | Cu5—O10 | 1.939 (2) | Gd1—O3 | 2.381 (2) |
Cu4—N5 | 1.906 (2) | Cu5—N7 | 1.901 (2) | Gd1—O5 | 2.483 (2) |
Cu4—N6 | 2.005 (2) | Cu5—N8 | 2.022 (2) | Gd1—O7 | 2.408 (2) |
Cu4—O20w | 2.401 (3) | Cu5—O24w | 2.449 (2) | Gd1—O9 | 2.414 (2) |
C11—O12 | 1.284 (9) | C11B—O12B | 1.310 (10) | Gd1—O11w | 2.359 (2) |
C11—O13 | 1.307 (10) | C11B—O13B | 1.307 (10) | Gd1—O12 | 2.317 (11) |
C11—O14 | 1.252 (9) | C11B—O14B | 1.253 (9) | Gd1—O13 | 2.288 (17) |
Gd1—O12B | 2.396 (10) | Gd1—O13B | 2.388 (17) |
Cu1—O1 | 1.931 (3) | Cu2—O3 | 1.931 (3) | Cu3—O5 | 1.941 (3) |
Cu1—O2 | 1.949 (3) | Cu2—O4 | 1.939 (3) | Cu3—O6 | 1.954 (3) |
Cu1—N9 | 1.897 (3) | Cu2—N1 | 1.907 (4) | Cu3—N3 | 1.905 (4) |
Cu1—N10 | 2.012 (4) | Cu2—N2 | 1.983 (4) | Cu3—N4 | 2.017 (4) |
Cu1—O18w | 2.476 (3) | Cu2—O15(NO3) | 2.464 (3) | Cu3—O19w | 2.430 (3) |
Cu4—O7 | 1.936 (3) | Cu5—O9 | 1.932 (3) | Dy1—O1 | 2.453 (3) |
Cu4—O8 | 1.956 (3) | Cu5—O10 | 1.941 (3) | Dy1—O3 | 2.382 (3) |
Cu4—N5 | 1.904 (3) | Cu5—N7 | 1.899 (3) | Dy1—O5 | 2.469 (3) |
Cu4—N6 | 2.005 (3) | Cu5—N8 | 2.021 (3) | Dy1—O7 | 2.412 (3) |
Cu4—O20w | 2.400 (3) | Cu5—O24w | 2.440 (3) | Dy1—O9 | 2.410 (3) |
C11—O12 | 1.275 (16) | C11B—O12B | 1.295 (9) | Dy1—O11w | 2.357 (3) |
C11—O13 | 1.318 (16) | C11B—O13B | 1.326 (8) | Dy1—O12 | 2.27 (2) |
C11—O14 | 1.256 (15) | C11B—O14B | 1.251 (8) | Dy1—O13 | 2.31 (3) |
Dy1—O12B | 2.380 (8) | Dy1—O13B | 2.347 (12) |
Cu1—O1 | 1.930 (2) | Cu2—O3 | 1.926 (2) | Cu3—O5 | 1.939 (2) |
Cu1—O2 | 1.948 (2) | Cu2—O4 | 1.940 (2) | Cu3—O6 | 1.949 (2) |
Cu1—N9 | 1.897 (2) | Cu2—N1 | 1.898 (3) | Cu3—N3 | 1.908 (3) |
Cu1—N10 | 2.013 (3) | Cu2–N2 | 1.987 (3) | Cu3—N4 | 2.010 (3) |
Cu1—O18w | 2.471 (3) | Cu2—O15(NO3) | 2.463 (3) | Cu3—O19w | 2.437 (3) |
Cu4—O7 | 1.937 (2) | Cu5—O9 | 1.931 (2) | Ho1—O1 | 2.446 (2) |
Cu4—O8 | 1.949 (2) | Cu5—O10 | 1.941 (2) | Ho1—O3 | 2.374 (2) |
Cu4—N5 | 1.903 (3) | Cu5—N7 | 1.902 (3) | Ho1—O5 | 2.475 (2) |
Cu4—N6 | 2.008 (3) | Cu5—N8 | 2.019 (3) | Ho1—O7 | 2.404 (2) |
Cu4—O20w | 2.405 (3) | Cu5—O24w | 2.443 (3) | Ho1—O9 | 2.407 (2) |
C11—O12 | 1.239 (11) | C11B—O12B | 1.262 (10) | Ho1—O11w | 2.358 (2) |
C11—O13 | 1.305 (13) | C11B—O13B | 1.309 (10) | Ho1—O12 | 2.304 (16) |
C11—O14 | 1.283 (12) | C11B—O14B | 1.261 (9) | Ho1—O13 | 2.30 (3) |
Ho1—O12B | 2.374 (12) | Ho1—O13B | 2.35 (2) |
O1—Cu1—O2 | 85.28 (9) | O3—Cu2—O4 | 85.63 (9) | O5—Cu3—O6 | 85.44 (9) |
N9—Cu1—O1 | 89.32 (9) | N1—Cu2—O3 | 90.48 (9) | N3—Cu3—O5 | 90.98 (10) |
O2—Cu1—N10 | 100.27 (10) | O4—Cu2—N2 | 100.83 (10) | O6—Cu3—N4 | 99.85 (11)- |
N9–Cu1—N10 | 83.70 (10) | N1—Cu2—N2 | 82.87 (11) | N3—Cu3—N4 | 82.70 (12) |
O7—Cu4—O8 | 84.56 (8) | O9—Cu5—O10 | 85.57 (8) | O3—Gd1—O1 | 71.71 (7) |
N5—Cu4—O7 | 91.39 (9) | N7—Cu5—O9 | 89.59 (9) | O3—Gd1—O5 | 72.08 (7) |
O8—Cu4—N6 | 98.79 (9) | O10—Cu5—N8 | 100.42 (9) | O7—Gd1—O5 | 72.87 (7) |
N5—Cu4—N6 | 83.88 (10) | N7—Cu5—N8 | 83.14 (10) | O7—Gd1—O9 | 71.27 (6) |
O13—Gd1—O12 | 56.4 (3) | O13B–Gd1–O12B | 54.1 (3) | O9—Gd1—O1 | 70.62 (7) |
O1—Cu1—O2 | 85.19 (12) | O3—Cu2—O4 | 85.41 (12) | O5–Cu3—O6 | 85.39 (12) |
O1—Cu1—N9 | 89.39 (13) | O3—Cu2—N1 | 90.66 (13) | O5—Cu3—N3 | 90.67 (13) |
O2—Cu1—N10 | 100.37 (13) | O4—Cu2—N2 | 101.00 (14) | O6—Cu3—N4 | 100.11 (14) |
N9—Cu1—N10 | 83.73 (14) | N1—Cu2—N2 | 82.65 (15) | N3—Cu3—N4 | 82.79 (15) |
O7—Cu4—O8 | 84.56 (11) | O9—Cu5—O10 | 85.47 (11) | O1—Dy1—O3 | 71.77 (9) |
O7—Cu4—N5 | 91.62 (13) | O9—Cu5—N7 | 89.53 (12) | O3—Dy1—O5 | 71.92 (9) |
O8—Cu4—N6 | 98.55 (13) | O10—Cu5—N8 | 100.49 (13) | O5—Dy1—O7 | 72.60 (9) |
N5—Cu4—N6 | 83.78 (14) | N7—Cu5—N8 | 83.23 (14) | O7—Dy1—O9 | 71.21 (9) |
O12—Dy1—O13 | 57.1 (6) | O12B–Dy1—O13B | 54.7 (2) | O9—Dy1—O1 | 70.83 (9) |
O1—Cu1—O2 | 85.31 (9) | O3—Cu2—O4 | 85.63 (9) | O5—Cu3—O6 | 85.53 (9) |
O1—Cu1—N9 | 89.22 (10) | O3—Cu2—N1 | 90.61 (10) | O5—Cu3—N3 | 90.80 (10) |
O2—Cu1—N10 | 100.11 (11) | O4–Cu2—N2 | 100.93 (11) | O6—Cu3—N4 | 99.97 (11) |
N9—Cu1—N10 | 83.88 (11) | N1—Cu2—N2 | 82.56 (12) | N3—Cu3—N4 | 82.62 (12) |
O7—Cu4—O8 | 84.51 (9) | O9—Cu5—O10 | 85.63 (9) | O1—Ho1—O3 | 71.84 (7) |
O7—Cu4—N5 | 91.47 (10) | O9—Cu5—N7 | 89.41 (10) | O3—Ho1—O5 | 72.17 (7) |
O8—Cu4—N6 | 98.74 (10) | O10—Cu5—N8 | 100.38 (10) | O5—Ho1—O7 | 72.61 (7) |
N5—Cu4—N6 | 83.87 (11) | N7—Cu5—N8 | 83.25 (11) | O7—Ho1—O9 | 71.34 (7) |
O12—Ho1—O13 | 56.5 (4) | O12B—Ho1—O13B | 53.9 (3) | O9—Ho1—O1 | 70.69 (7) |
CCDC127569 | Complex 1 | Complex 2 | Complex 3 | |
EuCu5 | GdCu5 | DyCu5 | HoCu5 | |
Range of Ln···Cu separations (Å) | 3.890 (2)–3.911 (3) | 3.8699 (5)–3.9097 (5) | 3.8715 (5)–3.9016 (6) | 3.8670 (5)–3.9021 (5) |
Range of Cu···Cu separations (Å) | 4.575 (3)–4.589 (3) | 4.5677 (7)–4.5846 (7) | 4.5645 (7)–4.5797 (8) | 4.5583 (7)–4.5808 (7) |
Range of Ln—Oequat (Å) | 2.406 (11)–2.493 (11) | 2.381 (2)–2.484 (2) | 2.382 (3)–2.469 (3) | 2.374 (2)–2.475 (2) |
Range of Ln—Ocarbonate (Å) | 2.369 (13)–2.392 (15) | 2.288 (17)–2.396 (10) | 2.27 (2)–2.380 (8) | 2.30 (3)–2.374 (12) |
Range of Cu—Oequat (Å) | 1.901 (11)–1.972 (10) | 1.929 (2)–1.953 (2) | 1.931 (3)–1.956 (4) | 1.929 (2)–1.953 (2) |
Range of Cu—Nequat (Å) | 1.886 (14)–2.022 (13) | 1.898 (2)–2.022 (2) | 1.898 (3)–2.022 (3) | 1.898 (2)–2.022 (2) |
Range of τ values (Addison et al., 1984) for pentacoordinate CuII ions | 0.00–0.20 | 0.01–0.20 | 0.01–0.20 | 0.02–0.20 |
LnIII coordination number | 8 | 8 | 8 | 8 |
Average deviation of non-hydrogen atoms from Cu5 plane (Å) | 0.179 | 0.188 | 0.183 | 0.186 |
Largest deviation among non-hydrogen atoms from Cu5 plane (Å) | 0.605 | 0.606 | 0.602 | 0.597 |
Deviation of LnIII ion from Cu5 plane (Å) | 0.351 | 0.337 | 0.354 | 0.330 |
Complex 1 | Complex 2 | Complex 3 | |
OP-8 | 31.930 | 31.846 | 31.915 |
HPY-8 | 22.627 | 22.698 | 22.560 |
HBPY-8 | 16.081 | 16.114 | 16.307 |
CU-8 | 12.990 | 12.970 | 12.794 |
SAPR-8 | 3.769 | 3.759 | 3.770 |
TDD-8 | 1.805 | 1.743 | 1.763 |
JGBF-8 | 12.037 | 12.418 | 12.302 |
JETBPY-8 | 27.751 | 27.478 | 27.602 |
Funding information
AWA thanks Drexel University for support under the Collaborative Research Agreement between the Drexel University College of Arts & Sciences and the Pisarzhevskii Institute of Physical Chemistry. The X-ray diffractometer was funded by the National Science Foundation, Division of Chemistry (grant No. 1625543 to MZ). AVP thanks the Foundation Volkswagen Stiftung (project No. 90343) and the Fulbright Foundation for a Research Fellowship.
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