Supporting information
Crystallographic Information File (CIF) https://doi.org/10.1107/S0108270113031806/fn3156sup1.cif | |
Structure factor file (CIF format) https://doi.org/10.1107/S0108270113031806/fn3156Isup2.hkl | |
Structure factor file (CIF format) https://doi.org/10.1107/S0108270113031806/fn3156IIsup3.hkl | |
Structure factor file (CIF format) https://doi.org/10.1107/S0108270113031806/fn3156IIIsup4.hkl |
CCDC references: 930447; 930448; 930449
Lanthanide chemistry has been a thriving area of research due to the unique properties of lanthanide ions, such as high coordination numbers, subtle differences in reactivity seen along the series, luminescence and magnetism (Bünzil, 2006; Bünzil & Piguet, 2005; Cahill et al., 2007; Sorace et al., 2011). The structural variety seen among lanthanide coordination compounds depends on the ligands and the synthetic method employed. The use of ligands with multiple binding sites may give rise to clusters as well as to coordination polymers. Due to their high coordination numbers and their marked preference for hard donors, carboxylic acids serve as good building blocks in the construction of multi-dimensional lanthanide coordination polymers. By introducing other ligands into the synthesis, the dimensionality and properties of such compounds can be varied. Previously, there have been many reports of polymeric lanthanide (Ln) complexes with oda2- (odaH2 is oxydiacetic acid), including heterometallic coordination polymers (Baggio et al., 1998; Kremer et al., 2008; Mao et al., 1997; Rizzi et al., 2002; Wang et al., 2007). Our previous work with the Ln–Mn–oda2- system resulted in a cubic architecture reminiscent of Prussian blue (Prasad et al., 2007). In order to study the effect of strongly coordinating SO42- dianions (towards lanthanides) on the polymeric structures, hydrothermal reactions were performed with Ln2O3 [Ln = Pr for (I), Nd for (II) and Sm for (III)], ZnSO4 and odaH2. The crystals formed have the following formulae: [Pr2(oda)(SO4)2(H2O)2].0.5H2O for (I), and [Ln2(oda)2(SO4)(H2O)2].1.32H2O [Ln = Nd for (II) and Sm for (III)]. In these compounds, the SO42- dianion acts as a versatile bridging ligand along with oda2- to form three-dimensional networks. The SO42- dianions have entirely different coordination modes in (I) and (II)/(III) and one of the bridging modes has been only rarely observed to date.
Reagent-grade chemicals were purchased from Merck (ZnSO4.7H2O) or Alfa Aesar (lanthanide oxides and oxydiacetic acid) and were used without further purification.
For the preparation of (I), a mixture of Pr2O3 (0.044 g, 0.133 mmol), ZnSO4.7H2O (0.110 g, 0.383 mmol), oxydiacetic acid (0.100 g, 0.746 mmol) and water (10 ml) was sealed in a glass tube and heated at 433 K. After 1 d, pale-green crystals of (I) had formed in the hot solution (yield 0.010 g, 0.015 mmol, 6%). IR (KBr disk, ν, cm-1): 3391, 1586, 1493, 1443, 1373, 1321, 1213, 1130 and 1045.
Compound (II) was prepared by a similar method to that used for (I). Using Nd2O3 (0.044 g, 0.131 mmol), pale-violet crystals of (II) formed in the hot solution (yield 0.030 g, 0.021 mmol, 8%). IR (KBr disk, ν, cm-1): 3366, 1587, 1480, 1435, 1316, 1240, 1132 and 1028.
Compound (III) was also prepared by a similar method to that used for (I). Using Sm2O3 (0.044 g, 0.126 mmol), pale-yellow [Colourless in CIF - please clarify] crystals of (III) formed in the hot solution (yield 0.025 g, 0.017 mmol, 7%). IR (KBr disk, ν, cm-1): 3346, 1586, 1480, 1435, 1315, 1240, 1132 and 1028.
Crystal data, data collection and structure refinement details are summarized in Table 1. The H atoms of the oda2- ligand were placed in geometrically calculated positions and refined using a riding model, with C—H = 0.97 Å and Uiso(H) = 1.2Ueq(C). The positions of the water H atoms were determined from difference Fourier maps and refined using a riding model, with Uiso(H) = 1.5Ueq(O). The large displacement parameters of some of the solvent water molecules indicated fractional site-occupation factors which were therefore refined. Accordingly, the site occupancy of the solvent water molecule in (I) is 0.5, and the disordered water molecule on the inversion centre in (II) and (III) has a site occupancy of 0.32.
Compound (I) has a three-dimensional network structure, in which the O atoms of the SO42- dianions and oda2- ligands act as the bridging nodes. In the asymmetric unit there are two Pr3+ cations, one oda2- ligand and two SO42- dianions, and two coordinated water molecules and half a solvent water molecule. The two Pr3+ cations have different coordination environments. Atom Pr1 is ten-coordinated and is in a highly distorted bicapped square antiprismatic geometry, while Pr2 is nine-coordinated with a distorted tricapped trigonal prismatic geometry. As shown in Fig. 1, the Pr1 coordination consists of five O atoms from two symmetry-related oda2- ligands [O1, O1ii, O2ii, O3 and O4; symmetry code: (ii) -x + 1, -y + 1, ??? [Please complete]], four O atoms from SO42- dianions [O6, O7, O8iii and O14iv; symmetry codes: (iii) -x, -y + 1, -z + 2; (iv) x - 1, y, z] and one water molecule (O10). The Pr2 coordination consists of three O atoms from two symmetry-related oda2- ligands [O4, O5 and O5v; symmetry code: (v) -x + 1, -y, -z + 2], five O atoms from two SO42- dianions [O9vi, O11, O11iv, O12 and O13i; symmetry codes: (i) x + 1, y, z; (vi) -x + 1, -y + 1, -z + 2] and one coordinated water molecule (O15). The oda2- ligand bridges four Pr3+ cations by using all five of its donor sites to form nine bonds, the carboxylate O atoms being used twice. Each of the two SO42- dianions provides four bonds, two chelating and two bridging. Compound (I) has a highly connected three-dimensional network structure formed by the coordination of the Pr3+ cations with both oda2- and SO42- dianions. The highly compact three-dimensional network that results is depicted in Fig. 2.
Compounds (II) and (III) form isostructural three-dimensional networks. However, both the structure and the stoichiometry are entirely different from that of (I). The asymmetric unit consists of two lanthanide cations, two oda2- ligands and one SO42- dianion, and two coordinated water molecules and 1.32 solvent water molecules. The two Nd3+ (Sm3+) atoms are nine-coordinated, with distorted tricapped trigonal prismatic geometries, but have different coordination environments (Figs. 3 and 4). Atom Nd1 (Sm1) is coordinated to six O atoms from three symmetry-related oda2- ligands [O1, O3, O4, O7, O9iii and O10iii; symmetry code: (iii) x - 1, y, z], one O atom from an SO42- dianion (O14iii) and two coordinated water molecules (O15 and O16). The coordination environment of Nd2 (Sm2) consists of six O atoms from three symmetry-related oda2- ligands [O2iv, O4i, O5i, O6, O8 and O9; symmetry codes: (i) -x + 1, -y + 2, -z + 2; (iv) x + 1/2, -y + 3/2, z + 1/2] and three O atoms from two symmetry-related SO42- dianions [O11, O11ii and O12; symmetry code: (ii) -x + 2, -y + 2, -z + 2]. The asymmetric unit is assembled into a tetranuclear cluster with the formula [Ln4(oda)4(SO4)2(H2O)4] [Ln = Nd for (II) and Sm for (III)] (Fig. 5a) and ultimately into a three-dimensional network, a projection of which is shown in Fig. 5(b). In this network, the tetranuclear clusters are crosslinked to form four-membered rings.
Structural analysis has shown that SO42- dianions play a very important and direct role in the control of structures. In the present compounds, there are three different types of SO42- dianion coordination, as shown in Fig. 6. In (I), the two SO42- dianions are coordinated to Pr3+ in different ways, one in mode A and the other in mode B, while in (II) and (III) the SO42- dianions are coordinated in mode C. A search of the Cambridge Structural Database (CSD, Version 5.34; Allen, 2002) was performed to check how common these modes are and it was found that modes A and C are observed frequently, but mode B (Akkari et al., 2006; Ding et al., 2012; Ouellette et al., 2011; Yuan et al., 2004) has been only rarely observed to date. Compounds (I), (II) and (III) are the first complexes containing lanthanide cations, oda2- ligands and SO42- dianions, and even with other metals there is only a single structure reported (Graziani et al., 1983). The driving factor for the formation of such versatile structures might be the early coordination of SO42- to Ln3+, which hinders the formation of the tris-chelate [Ln(oda)3]3-, which is the basic building block in the previously reported coordination compounds (Kremer et al., 2008). Another important fact to note is the role of ZnSO4, which acts as the SO42- dianion source. Reactions using other SO42- salts did not yield any of the present compounds, indicating the importance of ZnSO4 in the synthesis. Compound (I) has a higher SO42- content and an entirely different structure compared with (II) and (III), which are isomorphous. This is in contrast with the other Ln–oda complexes reported, which are usually isostructural for almost the entire lanthanide series, further indicating the pivotal role played by SO42- dianions in the present structures. The SO42- dianion in these compounds tends to reach saturation as a donor, binding to four or five metal atoms at the same time, leading to very rarely observed coordination modes.
For related literature, see: Akkari et al. (2006); Allen (2002); Bünzil (2006); Bünzil & Piguet (2005); Baggio et al. (1998); Cahill et al. (2007); Ding et al. (2012); Graziani et al. (1983); Kremer et al. (2008); Mao et al. (1997); Ouellette et al. (2011); Prasad et al. (2007); Rizzi et al. (2002); Sorace et al. (2011); Wang et al. (2007); Yuan et al. (2004).
For all compounds, data collection: SMART APEX (Bruker, 2007); cell refinement: SMART APEX (Bruker, 2007); data reduction: SAINT-Plus (Bruker, 2007); program(s) used to solve structure: SHELXS97 (Sheldrick, 2008); program(s) used to refine structure: SHELXL97 (Sheldrick, 2008); molecular graphics: DIAMOND (Brandenburg, 1999); software used to prepare material for publication: WinGX (Farrugia, 2012).
[Pr2(C4H4O5)(SO4)2(H2O)2]·0.5H2O | Z = 2 |
Mr = 651.05 | F(000) = 614 |
Triclinic, P1 | Dx = 3.145 Mg m−3 |
Hall symbol: -P 1 | Mo Kα radiation, λ = 0.71073 Å |
a = 6.618 (2) Å | Cell parameters from 6036 reflections |
b = 8.527 (3) Å | θ = 2.6–28.1° |
c = 13.111 (4) Å | µ = 7.40 mm−1 |
α = 86.340 (5)° | T = 298 K |
β = 89.487 (5)° | Needle, pale green |
γ = 68.617 (5)° | 0.60 × 0.10 × 0.08 mm |
V = 687.4 (4) Å3 |
Bruker SMART APEX CCD area-detector diffractometer | 3119 independent reflections |
Radiation source: sealed tube | 3020 reflections with I > 2σ(I) |
Graphite monochromator | Rint = 0.019 |
ϕ and ω scans | θmax = 28.2°, θmin = 1.6° |
Absorption correction: multi-scan (SADABS; Sheldrick, 1996) | h = −8→8 |
Tmin = 0.316, Tmax = 0.553 | k = −10→11 |
7509 measured reflections | l = −17→17 |
Refinement on F2 | Primary atom site location: structure-invariant direct methods |
Least-squares matrix: full | Secondary atom site location: difference Fourier map |
R[F2 > 2σ(F2)] = 0.021 | Hydrogen site location: inferred from neighbouring sites |
wR(F2) = 0.050 | H-atom parameters constrained |
S = 1.14 | w = 1/[σ2(Fo2) + (0.0214P)2 + 1.2502P] where P = (Fo2 + 2Fc2)/3 |
3119 reflections | (Δ/σ)max = 0.003 |
217 parameters | Δρmax = 0.76 e Å−3 |
0 restraints | Δρmin = −1.03 e Å−3 |
[Pr2(C4H4O5)(SO4)2(H2O)2]·0.5H2O | γ = 68.617 (5)° |
Mr = 651.05 | V = 687.4 (4) Å3 |
Triclinic, P1 | Z = 2 |
a = 6.618 (2) Å | Mo Kα radiation |
b = 8.527 (3) Å | µ = 7.40 mm−1 |
c = 13.111 (4) Å | T = 298 K |
α = 86.340 (5)° | 0.60 × 0.10 × 0.08 mm |
β = 89.487 (5)° |
Bruker SMART APEX CCD area-detector diffractometer | 3119 independent reflections |
Absorption correction: multi-scan (SADABS; Sheldrick, 1996) | 3020 reflections with I > 2σ(I) |
Tmin = 0.316, Tmax = 0.553 | Rint = 0.019 |
7509 measured reflections |
R[F2 > 2σ(F2)] = 0.021 | 0 restraints |
wR(F2) = 0.050 | H-atom parameters constrained |
S = 1.14 | Δρmax = 0.76 e Å−3 |
3119 reflections | Δρmin = −1.03 e Å−3 |
217 parameters |
Geometry. All e.s.d.'s (except the e.s.d. in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell e.s.d.'s are taken into account individually in the estimation of e.s.d.'s in distances, angles and torsion angles; correlations between e.s.d.'s in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell e.s.d.'s is used for estimating e.s.d.'s involving l.s. planes. |
Refinement. Refinement of F2 against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F2, conventional R-factors R are based on F, with F set to zero for negative F2. The threshold expression of F2 > σ(F2) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F2 are statistically about twice as large as those based on F, and R-factors based on ALL data will be even larger. |
x | y | z | Uiso*/Ueq | Occ. (<1) | |
Pr1 | 0.38812 (3) | 0.47758 (2) | 0.663048 (12) | 0.00975 (6) | |
Pr2 | 0.26110 (3) | 0.25533 (2) | 1.005609 (12) | 0.00847 (6) | |
S1 | 0.79216 (13) | 0.56048 (10) | 0.73700 (6) | 0.01177 (16) | |
S2 | −0.21987 (12) | 0.30505 (10) | 1.08640 (6) | 0.00974 (15) | |
C1 | 0.7432 (5) | 0.2345 (4) | 0.4939 (3) | 0.0163 (7) | |
C2 | 0.7278 (8) | 0.0917 (5) | 0.5610 (3) | 0.0293 (10) | |
H2A | 0.6454 | 0.0364 | 0.5267 | 0.035* | |
H2B | 0.8717 | 0.0093 | 0.5770 | 0.035* | |
C3 | 0.6373 (7) | 0.0305 (5) | 0.7295 (3) | 0.0254 (9) | |
H3A | 0.7882 | −0.0337 | 0.7474 | 0.030* | |
H3B | 0.5727 | −0.0462 | 0.7056 | 0.030* | |
C4 | 0.5190 (5) | 0.1142 (4) | 0.8207 (2) | 0.0122 (6) | |
O1 | 0.6705 (4) | 0.3802 (3) | 0.52743 (19) | 0.0209 (5) | |
O2 | 0.8178 (4) | 0.2112 (3) | 0.40645 (19) | 0.0224 (6) | |
O3 | 0.6226 (4) | 0.1582 (3) | 0.65198 (18) | 0.0203 (5) | |
O4 | 0.4085 (4) | 0.2691 (3) | 0.81568 (18) | 0.0136 (5) | |
O5 | 0.5324 (4) | 0.0231 (3) | 0.90248 (18) | 0.0143 (5) | |
O6 | 0.7400 (4) | 0.4089 (3) | 0.7645 (2) | 0.0194 (5) | |
O7 | 0.6332 (4) | 0.6569 (3) | 0.65608 (18) | 0.0172 (5) | |
O8 | 1.0134 (4) | 0.5124 (4) | 0.6998 (2) | 0.0255 (6) | |
O9 | 0.7664 (4) | 0.6622 (3) | 0.82478 (19) | 0.0191 (5) | |
O10 | 0.2188 (5) | 0.3368 (4) | 0.5404 (2) | 0.0288 (6) | |
H10A | 0.2312 | 0.3385 | 0.4727 | 0.043* | |
H10B | 0.1801 | 0.2693 | 0.5640 | 0.043* | |
O11 | −0.1514 (4) | 0.4377 (3) | 1.03282 (18) | 0.0138 (5) | |
O12 | −0.0202 (4) | 0.1508 (3) | 1.09050 (19) | 0.0145 (5) | |
O13 | −0.3887 (4) | 0.2799 (3) | 1.02581 (19) | 0.0171 (5) | |
O14 | −0.2943 (4) | 0.3515 (3) | 1.18773 (19) | 0.0190 (5) | |
O15 | 0.0571 (4) | 0.1639 (3) | 0.87499 (19) | 0.0194 (5) | |
H15A | −0.0400 | 0.2344 | 0.8386 | 0.029* | |
H15B | 0.0521 | 0.0627 | 0.8948 | 0.029* | |
O1W | 1.1591 (15) | 0.0947 (11) | 0.6575 (6) | 0.061 (2) | 0.50 |
H1A | 1.0584 | 0.0993 | 0.6899 | 0.092* | 0.50 |
H1B | 1.1925 | 0.0129 | 0.6219 | 0.092* | 0.50 |
U11 | U22 | U33 | U12 | U13 | U23 | |
Pr1 | 0.01011 (10) | 0.01046 (9) | 0.00872 (9) | −0.00378 (7) | 0.00145 (6) | −0.00098 (6) |
Pr2 | 0.00855 (9) | 0.00876 (9) | 0.00814 (9) | −0.00313 (7) | 0.00141 (6) | −0.00112 (6) |
S1 | 0.0105 (4) | 0.0152 (4) | 0.0106 (4) | −0.0056 (3) | 0.0016 (3) | −0.0032 (3) |
S2 | 0.0089 (4) | 0.0108 (4) | 0.0105 (4) | −0.0046 (3) | 0.0019 (3) | −0.0018 (3) |
C1 | 0.0123 (16) | 0.0165 (17) | 0.0150 (17) | 0.0002 (13) | 0.0016 (13) | 0.0015 (13) |
C2 | 0.050 (3) | 0.0170 (18) | 0.0143 (18) | −0.0038 (18) | 0.0186 (17) | −0.0031 (15) |
C3 | 0.040 (2) | 0.0141 (17) | 0.0147 (18) | −0.0017 (16) | 0.0101 (16) | 0.0021 (14) |
C4 | 0.0130 (15) | 0.0127 (15) | 0.0110 (15) | −0.0053 (12) | 0.0022 (12) | 0.0017 (12) |
O1 | 0.0282 (14) | 0.0141 (12) | 0.0172 (13) | −0.0042 (11) | 0.0069 (10) | −0.0011 (10) |
O2 | 0.0259 (14) | 0.0205 (13) | 0.0133 (12) | −0.0001 (11) | 0.0066 (10) | 0.0023 (10) |
O3 | 0.0323 (14) | 0.0113 (11) | 0.0102 (12) | −0.0002 (10) | 0.0108 (10) | 0.0006 (9) |
O4 | 0.0164 (12) | 0.0104 (11) | 0.0126 (11) | −0.0035 (9) | 0.0043 (9) | −0.0002 (9) |
O5 | 0.0168 (12) | 0.0115 (11) | 0.0106 (11) | −0.0006 (9) | 0.0037 (9) | 0.0003 (9) |
O6 | 0.0172 (13) | 0.0166 (12) | 0.0259 (14) | −0.0084 (10) | −0.0054 (10) | 0.0027 (10) |
O7 | 0.0199 (12) | 0.0207 (13) | 0.0121 (12) | −0.0089 (10) | −0.0019 (9) | 0.0010 (10) |
O8 | 0.0141 (13) | 0.0353 (16) | 0.0306 (15) | −0.0115 (12) | 0.0083 (11) | −0.0127 (13) |
O9 | 0.0210 (13) | 0.0250 (13) | 0.0134 (12) | −0.0099 (11) | 0.0011 (10) | −0.0068 (10) |
O10 | 0.0386 (17) | 0.0413 (17) | 0.0157 (13) | −0.0244 (14) | 0.0055 (12) | −0.0088 (12) |
O11 | 0.0128 (11) | 0.0098 (11) | 0.0193 (12) | −0.0053 (9) | 0.0020 (9) | 0.0009 (9) |
O12 | 0.0120 (11) | 0.0111 (11) | 0.0192 (12) | −0.0032 (9) | 0.0019 (9) | 0.0009 (9) |
O13 | 0.0139 (12) | 0.0236 (13) | 0.0171 (12) | −0.0105 (10) | 0.0010 (9) | −0.0040 (10) |
O14 | 0.0188 (13) | 0.0265 (14) | 0.0138 (12) | −0.0098 (11) | 0.0048 (10) | −0.0084 (10) |
O15 | 0.0224 (13) | 0.0170 (12) | 0.0203 (13) | −0.0092 (10) | −0.0054 (10) | 0.0021 (10) |
O1W | 0.096 (7) | 0.061 (5) | 0.049 (5) | −0.052 (5) | 0.030 (5) | −0.020 (4) |
Pr1—O8i | 2.435 (3) | S2—O12 | 1.485 (2) |
Pr1—O14ii | 2.453 (2) | S2—O11 | 1.499 (2) |
Pr1—O1 | 2.518 (3) | C1—O2 | 1.243 (4) |
Pr1—O6 | 2.549 (3) | C1—O1 | 1.265 (4) |
Pr1—O10 | 2.558 (3) | C1—C2 | 1.490 (5) |
Pr1—O4 | 2.561 (2) | C1—Pr1iii | 2.975 (3) |
Pr1—O7 | 2.601 (2) | C2—O3 | 1.418 (4) |
Pr1—O2iii | 2.609 (3) | C2—H2A | 0.9700 |
Pr1—O3 | 2.610 (3) | C2—H2B | 0.9700 |
Pr1—O1iii | 2.673 (3) | C3—O3 | 1.418 (4) |
Pr1—C1iii | 2.975 (3) | C3—C4 | 1.495 (5) |
Pr1—S1 | 3.1782 (12) | C3—H3A | 0.9700 |
Pr2—O9iv | 2.360 (2) | C3—H3B | 0.9700 |
Pr2—O13v | 2.420 (2) | C4—O4 | 1.252 (4) |
Pr2—O11ii | 2.466 (2) | C4—O5 | 1.267 (4) |
Pr2—O5vi | 2.501 (2) | O1—Pr1iii | 2.673 (3) |
Pr2—O15 | 2.518 (3) | O2—Pr1iii | 2.609 (3) |
Pr2—O12 | 2.558 (2) | O5—Pr2vi | 2.501 (2) |
Pr2—O5 | 2.584 (2) | O8—Pr1v | 2.435 (3) |
Pr2—O11 | 2.637 (2) | O9—Pr2iv | 2.360 (2) |
Pr2—O4 | 2.677 (2) | O10—H10A | 0.8909 |
Pr2—C4 | 3.007 (3) | O10—H10B | 0.7587 |
Pr2—S2 | 3.2319 (13) | O11—Pr2ii | 2.466 (2) |
S1—O9 | 1.457 (3) | O13—Pr2i | 2.420 (2) |
S1—O8 | 1.458 (3) | O14—Pr1ii | 2.453 (2) |
S1—O6 | 1.478 (3) | O15—H15A | 0.8299 |
S1—O7 | 1.479 (3) | O15—H15B | 0.8976 |
S2—O14 | 1.442 (3) | O1W—H1A | 0.7775 |
S2—O13 | 1.462 (2) | O1W—H1B | 0.8256 |
O8i—Pr1—O14ii | 74.82 (9) | O15—Pr2—O4 | 66.87 (8) |
O8i—Pr1—O1 | 141.45 (9) | O12—Pr2—O4 | 135.51 (7) |
O14ii—Pr1—O1 | 142.39 (9) | O5—Pr2—O4 | 49.31 (7) |
O8i—Pr1—O6 | 136.99 (9) | O11—Pr2—O4 | 116.15 (7) |
O14ii—Pr1—O6 | 73.67 (9) | O9iv—Pr2—C4 | 152.11 (9) |
O1—Pr1—O6 | 77.86 (9) | O13v—Pr2—C4 | 73.43 (9) |
O8i—Pr1—O10 | 65.56 (9) | O11ii—Pr2—C4 | 102.29 (8) |
O14ii—Pr1—O10 | 140.38 (9) | O5vi—Pr2—C4 | 86.53 (8) |
O1—Pr1—O10 | 76.58 (9) | O15—Pr2—C4 | 65.42 (9) |
O6—Pr1—O10 | 138.92 (9) | O12—Pr2—C4 | 125.18 (8) |
O8i—Pr1—O4 | 74.53 (9) | O5—Pr2—C4 | 24.76 (8) |
O14ii—Pr1—O4 | 74.59 (8) | O11—Pr2—C4 | 133.25 (8) |
O1—Pr1—O4 | 117.28 (8) | O4—Pr2—C4 | 24.59 (8) |
O6—Pr1—O4 | 69.40 (8) | O9iv—Pr2—S2 | 71.41 (6) |
O10—Pr1—O4 | 94.90 (9) | O13v—Pr2—S2 | 151.23 (6) |
O8i—Pr1—O7 | 138.79 (9) | O11ii—Pr2—S2 | 90.66 (6) |
O14ii—Pr1—O7 | 73.89 (8) | O5vi—Pr2—S2 | 98.99 (6) |
O1—Pr1—O7 | 69.64 (8) | O15—Pr2—S2 | 69.99 (7) |
O6—Pr1—O7 | 54.38 (8) | O12—Pr2—S2 | 26.60 (5) |
O10—Pr1—O7 | 138.90 (8) | O5—Pr2—S2 | 131.41 (6) |
O4—Pr1—O7 | 120.95 (8) | O11—Pr2—S2 | 27.25 (5) |
O8i—Pr1—O2iii | 78.57 (10) | O4—Pr2—S2 | 130.82 (5) |
O14ii—Pr1—O2iii | 73.35 (9) | C4—Pr2—S2 | 135.34 (7) |
O1—Pr1—O2iii | 100.13 (8) | O9—S1—O8 | 109.82 (16) |
O6—Pr1—O2iii | 118.49 (9) | O9—S1—O6 | 110.54 (16) |
O10—Pr1—O2iii | 97.36 (10) | O8—S1—O6 | 110.44 (16) |
O4—Pr1—O2iii | 142.41 (8) | O9—S1—O7 | 109.51 (15) |
O7—Pr1—O2iii | 67.24 (9) | O8—S1—O7 | 110.95 (16) |
O8i—Pr1—O3 | 109.98 (9) | O6—S1—O7 | 105.51 (14) |
O14ii—Pr1—O3 | 129.82 (8) | O9—S1—Pr1 | 118.47 (11) |
O1—Pr1—O3 | 59.02 (8) | O8—S1—Pr1 | 131.70 (12) |
O6—Pr1—O3 | 71.04 (8) | O6—S1—Pr1 | 51.97 (10) |
O10—Pr1—O3 | 68.31 (10) | O7—S1—Pr1 | 54.02 (10) |
O4—Pr1—O3 | 60.24 (7) | O14—S2—O13 | 111.15 (15) |
O7—Pr1—O3 | 110.55 (9) | O14—S2—O12 | 111.04 (15) |
O2iii—Pr1—O3 | 156.26 (8) | O13—S2—O12 | 110.18 (15) |
O8i—Pr1—O1iii | 98.61 (9) | O14—S2—O11 | 110.58 (15) |
O14ii—Pr1—O1iii | 121.56 (9) | O13—S2—O11 | 109.51 (14) |
O1—Pr1—O1iii | 57.55 (10) | O12—S2—O11 | 104.16 (14) |
O6—Pr1—O1iii | 122.74 (8) | O14—S2—Pr2 | 124.33 (11) |
O10—Pr1—O1iii | 66.12 (9) | O13—S2—Pr2 | 124.50 (11) |
O4—Pr1—O1iii | 160.81 (8) | O12—S2—Pr2 | 50.48 (9) |
O7—Pr1—O1iii | 76.13 (8) | O11—S2—Pr2 | 53.69 (9) |
O2iii—Pr1—O1iii | 48.90 (8) | O2—C1—O1 | 121.4 (3) |
O3—Pr1—O1iii | 107.36 (8) | O2—C1—C2 | 120.7 (3) |
O8i—Pr1—C1iii | 92.71 (10) | O1—C1—C2 | 117.8 (3) |
O14ii—Pr1—C1iii | 96.41 (9) | O2—C1—Pr1iii | 60.98 (18) |
O1—Pr1—C1iii | 76.55 (9) | O1—C1—Pr1iii | 63.94 (18) |
O6—Pr1—C1iii | 119.19 (9) | C2—C1—Pr1iii | 158.5 (3) |
O10—Pr1—C1iii | 85.08 (10) | O3—C2—C1 | 107.9 (3) |
O4—Pr1—C1iii | 165.83 (8) | O3—C2—H2A | 110.1 |
O7—Pr1—C1iii | 65.11 (9) | C1—C2—H2A | 110.1 |
O2iii—Pr1—C1iii | 24.62 (8) | O3—C2—H2B | 110.1 |
O3—Pr1—C1iii | 131.83 (8) | C1—C2—H2B | 110.1 |
O1iii—Pr1—C1iii | 25.15 (8) | H2A—C2—H2B | 108.4 |
O8i—Pr1—S1 | 144.16 (7) | O3—C3—C4 | 108.0 (3) |
O14ii—Pr1—S1 | 69.36 (6) | O3—C3—H3A | 110.1 |
O1—Pr1—S1 | 74.04 (7) | C4—C3—H3A | 110.1 |
O6—Pr1—S1 | 27.17 (6) | O3—C3—H3B | 110.1 |
O10—Pr1—S1 | 150.26 (7) | C4—C3—H3B | 110.1 |
O4—Pr1—S1 | 94.41 (6) | H3A—C3—H3B | 108.4 |
O7—Pr1—S1 | 27.39 (6) | O4—C4—O5 | 121.3 (3) |
O2iii—Pr1—S1 | 92.25 (7) | O4—C4—C3 | 120.8 (3) |
O3—Pr1—S1 | 92.33 (7) | O5—C4—C3 | 117.9 (3) |
O1iii—Pr1—S1 | 101.00 (6) | O4—C4—Pr2 | 62.82 (17) |
C1iii—Pr1—S1 | 92.50 (7) | O5—C4—Pr2 | 58.63 (16) |
O9iv—Pr2—O13v | 80.10 (9) | C3—C4—Pr2 | 174.2 (2) |
O9iv—Pr2—O11ii | 81.83 (9) | C1—O1—Pr1 | 125.9 (2) |
O13v—Pr2—O11ii | 81.20 (8) | C1—O1—Pr1iii | 90.9 (2) |
O9iv—Pr2—O5vi | 80.13 (8) | Pr1—O1—Pr1iii | 122.45 (10) |
O13v—Pr2—O5vi | 79.60 (9) | C1—O2—Pr1iii | 94.4 (2) |
O11ii—Pr2—O5vi | 155.58 (8) | C2—O3—C3 | 112.6 (3) |
O9iv—Pr2—O15 | 140.95 (9) | C2—O3—Pr1 | 122.4 (2) |
O13v—Pr2—O15 | 138.74 (8) | C3—O3—Pr1 | 124.6 (2) |
O11ii—Pr2—O15 | 104.20 (8) | C4—O4—Pr1 | 125.8 (2) |
O5vi—Pr2—O15 | 100.18 (8) | C4—O4—Pr2 | 92.59 (19) |
O9iv—Pr2—O12 | 74.10 (8) | Pr1—O4—Pr2 | 141.60 (9) |
O13v—Pr2—O12 | 145.18 (8) | C4—O5—Pr2vi | 144.7 (2) |
O11ii—Pr2—O12 | 117.02 (8) | C4—O5—Pr2 | 96.62 (19) |
O5vi—Pr2—O12 | 73.32 (8) | Pr2vi—O5—Pr2 | 118.06 (9) |
O15—Pr2—O12 | 68.83 (8) | S1—O6—Pr1 | 100.86 (12) |
O9iv—Pr2—O5 | 136.68 (8) | S1—O7—Pr1 | 98.59 (12) |
O13v—Pr2—O5 | 73.50 (8) | S1—O8—Pr1v | 167.29 (17) |
O11ii—Pr2—O5 | 125.81 (8) | S1—O9—Pr2iv | 161.89 (17) |
O5vi—Pr2—O5 | 61.94 (9) | Pr1—O10—H10A | 126.4 |
O15—Pr2—O5 | 70.49 (8) | Pr1—O10—H10B | 116.4 |
O12—Pr2—O5 | 110.77 (8) | H10A—O10—H10B | 115.2 |
O9iv—Pr2—O11 | 73.55 (8) | S2—O11—Pr2ii | 143.41 (14) |
O13v—Pr2—O11 | 138.34 (8) | S2—O11—Pr2 | 99.06 (11) |
O11ii—Pr2—O11 | 63.76 (9) | Pr2ii—O11—Pr2 | 116.24 (9) |
O5vi—Pr2—O11 | 125.34 (7) | S2—O12—Pr2 | 102.92 (12) |
O15—Pr2—O11 | 74.98 (8) | S2—O13—Pr2i | 152.72 (15) |
O12—Pr2—O11 | 53.84 (7) | S2—O14—Pr1ii | 158.40 (17) |
O5—Pr2—O11 | 145.46 (8) | Pr2—O15—H15A | 121.0 |
O9iv—Pr2—O4 | 149.81 (8) | Pr2—O15—H15B | 110.3 |
O13v—Pr2—O4 | 74.63 (8) | H15A—O15—H15B | 121.7 |
O11ii—Pr2—O4 | 78.25 (7) | H1A—O1W—H1B | 109.7 |
O5vi—Pr2—O4 | 110.68 (7) | ||
O2—C1—C2—O3 | −175.7 (3) | O9—S1—O7—Pr1 | −111.57 (13) |
O1—C1—C2—O3 | 1.6 (5) | O8—S1—O7—Pr1 | 127.04 (14) |
Pr1iii—C1—C2—O3 | −87.5 (7) | O6—S1—O7—Pr1 | 7.41 (15) |
O3—C3—C4—O4 | 8.1 (5) | O9—S1—O8—Pr1v | −11.2 (9) |
O3—C3—C4—O5 | −172.7 (3) | O6—S1—O8—Pr1v | −133.4 (9) |
O2—C1—O1—Pr1 | 153.8 (3) | O7—S1—O8—Pr1v | 110.0 (9) |
C2—C1—O1—Pr1 | −23.6 (5) | Pr1—S1—O8—Pr1v | 169.9 (8) |
Pr1iii—C1—O1—Pr1 | 132.4 (2) | O8—S1—O9—Pr2iv | −100.3 (5) |
O2—C1—O1—Pr1iii | 21.4 (3) | O6—S1—O9—Pr2iv | 21.8 (6) |
C2—C1—O1—Pr1iii | −155.9 (3) | O7—S1—O9—Pr2iv | 137.7 (5) |
O1—C1—O2—Pr1iii | −22.0 (4) | Pr1—S1—O9—Pr2iv | 78.8 (5) |
C2—C1—O2—Pr1iii | 155.3 (3) | O14—S2—O11—Pr2ii | −46.8 (3) |
C1—C2—O3—C3 | −168.3 (3) | O13—S2—O11—Pr2ii | 76.0 (3) |
C1—C2—O3—Pr1 | 19.1 (5) | O12—S2—O11—Pr2ii | −166.2 (2) |
C4—C3—O3—C2 | −179.2 (3) | Pr2—S2—O11—Pr2ii | −165.0 (3) |
C4—C3—O3—Pr1 | −6.7 (5) | O14—S2—O11—Pr2 | 118.15 (13) |
O5—C4—O4—Pr1 | 174.4 (2) | O13—S2—O11—Pr2 | −119.04 (13) |
C3—C4—O4—Pr1 | −6.4 (5) | O12—S2—O11—Pr2 | −1.21 (14) |
Pr2—C4—O4—Pr1 | 178.7 (2) | O14—S2—O12—Pr2 | −117.78 (14) |
O5—C4—O4—Pr2 | −4.4 (3) | O13—S2—O12—Pr2 | 118.63 (13) |
C3—C4—O4—Pr2 | 174.8 (3) | O11—S2—O12—Pr2 | 1.27 (15) |
O4—C4—O5—Pr2vi | −164.6 (2) | O14—S2—O13—Pr2i | −7.7 (4) |
C3—C4—O5—Pr2vi | 16.2 (6) | O12—S2—O13—Pr2i | 115.8 (3) |
Pr2—C4—O5—Pr2vi | −169.2 (4) | O11—S2—O13—Pr2i | −130.2 (3) |
O4—C4—O5—Pr2 | 4.6 (3) | Pr2—S2—O13—Pr2i | 171.1 (3) |
C3—C4—O5—Pr2 | −174.6 (3) | O13—S2—O14—Pr1ii | −120.8 (4) |
O9—S1—O6—Pr1 | 110.68 (14) | O12—S2—O14—Pr1ii | 116.2 (4) |
O8—S1—O6—Pr1 | −127.58 (14) | O11—S2—O14—Pr1ii | 1.1 (5) |
O7—S1—O6—Pr1 | −7.62 (15) | Pr2—S2—O14—Pr1ii | 60.4 (5) |
Symmetry codes: (i) x−1, y, z; (ii) −x, −y+1, −z+2; (iii) −x+1, −y+1, −z+1; (iv) −x+1, −y+1, −z+2; (v) x+1, y, z; (vi) −x+1, −y, −z+2. |
[Nd2(C4H4O5)2(SO4)(H2O)2]·1.32H2O | F(000) = 1348.8 |
Mr = 708.51 | Dx = 2.624 Mg m−3 |
Monoclinic, P21/n | Mo Kα radiation, λ = 0.71073 Å |
Hall symbol: -P 2yn | Cell parameters from 6880 reflections |
a = 10.542 (3) Å | θ = 2.3–28.2° |
b = 16.520 (5) Å | µ = 5.93 mm−1 |
c = 10.885 (4) Å | T = 298 K |
β = 108.921 (5)° | Block, pale violet |
V = 1793.4 (10) Å3 | 0.40 × 0.20 × 0.18 mm |
Z = 4 |
Bruker SMART APEX CCD area-detector diffractometer | 4230 independent reflections |
Radiation source: sealed tube | 4132 reflections with I > 2σ(I) |
Graphite monochromator | Rint = 0.022 |
ϕ and ω scans | θmax = 28.3°, θmin = 2.4° |
Absorption correction: multi-scan (SADABS; Sheldrick, 1996) | h = −13→13 |
Tmin = 0.197, Tmax = 0.344 | k = −21→21 |
19838 measured reflections | l = −14→13 |
Refinement on F2 | Primary atom site location: structure-invariant direct methods |
Least-squares matrix: full | Secondary atom site location: difference Fourier map |
R[F2 > 2σ(F2)] = 0.020 | Hydrogen site location: inferred from neighbouring sites |
wR(F2) = 0.046 | H-atom parameters constrained |
S = 1.15 | w = 1/[σ2(Fo2) + (0.018P)2 + 2.2749P] where P = (Fo2 + 2Fc2)/3 |
4230 reflections | (Δ/σ)max = 0.003 |
259 parameters | Δρmax = 0.71 e Å−3 |
0 restraints | Δρmin = −0.42 e Å−3 |
[Nd2(C4H4O5)2(SO4)(H2O)2]·1.32H2O | V = 1793.4 (10) Å3 |
Mr = 708.51 | Z = 4 |
Monoclinic, P21/n | Mo Kα radiation |
a = 10.542 (3) Å | µ = 5.93 mm−1 |
b = 16.520 (5) Å | T = 298 K |
c = 10.885 (4) Å | 0.40 × 0.20 × 0.18 mm |
β = 108.921 (5)° |
Bruker SMART APEX CCD area-detector diffractometer | 4230 independent reflections |
Absorption correction: multi-scan (SADABS; Sheldrick, 1996) | 4132 reflections with I > 2σ(I) |
Tmin = 0.197, Tmax = 0.344 | Rint = 0.022 |
19838 measured reflections |
R[F2 > 2σ(F2)] = 0.020 | 0 restraints |
wR(F2) = 0.046 | H-atom parameters constrained |
S = 1.15 | Δρmax = 0.71 e Å−3 |
4230 reflections | Δρmin = −0.42 e Å−3 |
259 parameters |
Geometry. All e.s.d.'s (except the e.s.d. in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell e.s.d.'s are taken into account individually in the estimation of e.s.d.'s in distances, angles and torsion angles; correlations between e.s.d.'s in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell e.s.d.'s is used for estimating e.s.d.'s involving l.s. planes. |
Refinement. Refinement of F2 against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F2, conventional R-factors R are based on F, with F set to zero for negative F2. The threshold expression of F2 > σ(F2) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F2 are statistically about twice as large as those based on F, and R-factors based on ALL data will be even larger. |
x | y | z | Uiso*/Ueq | Occ. (<1) | |
Nd1 | 0.211726 (14) | 0.831008 (8) | 0.841567 (14) | 0.01832 (5) | |
Nd2 | 0.878731 (14) | 0.906051 (8) | 1.035860 (13) | 0.01736 (5) | |
S1 | 1.19320 (7) | 0.89778 (4) | 1.15487 (6) | 0.02096 (14) | |
C1 | 0.2777 (3) | 0.77853 (17) | 0.5732 (3) | 0.0254 (6) | |
C2 | 0.2404 (3) | 0.86445 (18) | 0.5300 (3) | 0.0266 (6) | |
H2A | 0.3144 | 0.8912 | 0.5120 | 0.032* | |
H2B | 0.1631 | 0.8652 | 0.4518 | 0.032* | |
C3 | 0.1886 (3) | 0.98804 (17) | 0.6143 (3) | 0.0252 (6) | |
H3A | 0.1163 | 0.9980 | 0.5339 | 0.030* | |
H3B | 0.2690 | 1.0142 | 0.6088 | 0.030* | |
C4 | 0.1528 (3) | 1.02177 (16) | 0.7270 (3) | 0.0205 (5) | |
C5 | 0.5468 (3) | 0.89503 (17) | 0.9024 (3) | 0.0258 (6) | |
C6 | 0.5802 (3) | 0.8734 (2) | 0.7817 (3) | 0.0356 (8) | |
H6A | 0.5535 | 0.8180 | 0.7566 | 0.043* | |
H6B | 0.5320 | 0.9087 | 0.7107 | 0.043* | |
C7 | 0.7643 (3) | 0.8582 (3) | 0.7037 (3) | 0.0378 (8) | |
H7A | 0.7360 | 0.8976 | 0.6340 | 0.045* | |
H7B | 0.7255 | 0.8063 | 0.6701 | 0.045* | |
C8 | 0.9143 (3) | 0.85207 (19) | 0.7517 (3) | 0.0251 (6) | |
O1 | 0.2541 (3) | 0.75360 (13) | 0.6716 (2) | 0.0340 (5) | |
O2 | 0.3303 (3) | 0.73772 (13) | 0.5060 (2) | 0.0361 (5) | |
O3 | 0.2103 (2) | 0.90460 (12) | 0.6328 (2) | 0.0286 (5) | |
O4 | 0.1582 (2) | 0.97619 (11) | 0.82212 (18) | 0.0218 (4) | |
O5 | 0.1205 (2) | 1.09411 (12) | 0.7268 (2) | 0.0297 (5) | |
O6 | 0.6417 (2) | 0.91260 (14) | 1.0027 (2) | 0.0326 (5) | |
O7 | 0.4265 (2) | 0.89353 (15) | 0.8941 (3) | 0.0365 (5) | |
O8 | 0.72004 (19) | 0.88212 (14) | 0.80760 (19) | 0.0256 (4) | |
O9 | 0.97639 (19) | 0.86234 (12) | 0.87117 (18) | 0.0223 (4) | |
O10 | 0.9756 (2) | 0.83545 (16) | 0.6743 (2) | 0.0358 (6) | |
O11 | 1.1117 (2) | 0.96942 (12) | 1.0871 (2) | 0.0241 (4) | |
O12 | 1.0914 (2) | 0.84140 (13) | 1.1701 (2) | 0.0317 (5) | |
O13 | 1.2906 (2) | 0.92120 (15) | 1.2754 (2) | 0.0362 (5) | |
O14 | 1.2605 (2) | 0.86208 (15) | 1.0681 (2) | 0.0300 (5) | |
O15 | 0.0930 (3) | 0.70812 (16) | 0.8891 (3) | 0.0543 (7) | |
H15A | 0.0999 | 0.6645 | 0.8504 | 0.081* | |
H15B | 0.0143 | 0.7199 | 0.8498 | 0.081* | |
O16 | 0.3820 (3) | 0.72519 (14) | 0.9313 (2) | 0.0415 (6) | |
H16A | 0.4067 | 0.7062 | 1.0153 | 0.062* | |
H16B | 0.3849 | 0.6850 | 0.8774 | 0.062* | |
O1W | 0.0470 (3) | 0.58536 (18) | 0.7203 (3) | 0.0519 (7) | |
H1A | −0.0342 | 0.5933 | 0.6923 | 0.078* | |
H1B | 0.0669 | 0.5874 | 0.6396 | 0.078* | |
O2W | 0.5000 | 1.0000 | 0.5000 | 0.166 (6) | 0.64 |
H2C | 0.5600 | 1.0123 | 0.5800 | 0.249* | 0.32 |
H2D | 0.5082 | 1.0600 | 0.5200 | 0.249* | 0.32 |
U11 | U22 | U33 | U12 | U13 | U23 | |
Nd1 | 0.02005 (8) | 0.01898 (8) | 0.01601 (8) | 0.00118 (5) | 0.00596 (6) | 0.00065 (5) |
Nd2 | 0.01705 (8) | 0.01954 (8) | 0.01663 (8) | −0.00206 (5) | 0.00705 (6) | −0.00222 (5) |
S1 | 0.0187 (3) | 0.0289 (3) | 0.0150 (3) | 0.0007 (3) | 0.0050 (3) | 0.0018 (3) |
C1 | 0.0312 (15) | 0.0223 (14) | 0.0202 (14) | 0.0055 (12) | 0.0050 (12) | −0.0035 (11) |
C2 | 0.0398 (17) | 0.0251 (14) | 0.0180 (13) | 0.0091 (12) | 0.0138 (12) | 0.0000 (11) |
C3 | 0.0393 (17) | 0.0195 (13) | 0.0219 (14) | 0.0051 (12) | 0.0169 (13) | 0.0026 (11) |
C4 | 0.0207 (13) | 0.0213 (13) | 0.0204 (13) | −0.0006 (10) | 0.0079 (11) | −0.0016 (10) |
C5 | 0.0205 (14) | 0.0234 (14) | 0.0346 (17) | 0.0001 (11) | 0.0105 (12) | 0.0007 (12) |
C6 | 0.0143 (13) | 0.059 (2) | 0.0311 (17) | −0.0030 (14) | 0.0043 (12) | −0.0091 (16) |
C7 | 0.0238 (15) | 0.069 (2) | 0.0194 (15) | 0.0001 (16) | 0.0051 (12) | −0.0084 (15) |
C8 | 0.0220 (14) | 0.0328 (15) | 0.0216 (14) | −0.0017 (12) | 0.0085 (12) | −0.0025 (12) |
O1 | 0.0580 (15) | 0.0213 (10) | 0.0243 (11) | 0.0074 (10) | 0.0155 (11) | 0.0017 (8) |
O2 | 0.0552 (15) | 0.0246 (11) | 0.0340 (12) | 0.0156 (10) | 0.0219 (11) | 0.0005 (9) |
O3 | 0.0515 (14) | 0.0183 (10) | 0.0232 (11) | 0.0082 (9) | 0.0221 (10) | 0.0015 (8) |
O4 | 0.0341 (11) | 0.0168 (9) | 0.0187 (9) | 0.0020 (8) | 0.0144 (8) | 0.0015 (7) |
O5 | 0.0480 (14) | 0.0192 (10) | 0.0273 (11) | 0.0067 (9) | 0.0195 (10) | 0.0018 (8) |
O6 | 0.0222 (11) | 0.0456 (14) | 0.0317 (12) | −0.0024 (9) | 0.0109 (9) | −0.0074 (10) |
O7 | 0.0191 (10) | 0.0426 (13) | 0.0492 (15) | −0.0037 (9) | 0.0131 (10) | −0.0031 (11) |
O8 | 0.0158 (9) | 0.0409 (12) | 0.0202 (10) | −0.0048 (8) | 0.0060 (8) | −0.0056 (9) |
O9 | 0.0193 (9) | 0.0306 (10) | 0.0173 (9) | −0.0015 (8) | 0.0065 (8) | −0.0020 (8) |
O10 | 0.0231 (11) | 0.0647 (17) | 0.0203 (11) | −0.0025 (10) | 0.0077 (9) | −0.0121 (10) |
O11 | 0.0222 (10) | 0.0228 (10) | 0.0255 (10) | −0.0003 (8) | 0.0051 (8) | 0.0040 (8) |
O12 | 0.0261 (11) | 0.0307 (11) | 0.0381 (13) | 0.0014 (9) | 0.0102 (10) | 0.0126 (9) |
O13 | 0.0298 (12) | 0.0555 (15) | 0.0181 (11) | 0.0004 (10) | 0.0008 (9) | −0.0020 (10) |
O14 | 0.0232 (10) | 0.0475 (13) | 0.0193 (10) | 0.0083 (9) | 0.0068 (8) | −0.0027 (9) |
O15 | 0.0575 (18) | 0.0305 (13) | 0.075 (2) | −0.0050 (12) | 0.0222 (16) | 0.0096 (13) |
O16 | 0.0655 (17) | 0.0352 (13) | 0.0199 (11) | 0.0261 (12) | 0.0083 (11) | 0.0031 (9) |
O1W | 0.0309 (13) | 0.073 (2) | 0.0539 (17) | 0.0018 (13) | 0.0158 (13) | −0.0034 (14) |
O2W | 0.153 (12) | 0.219 (16) | 0.107 (9) | −0.095 (11) | 0.017 (9) | −0.003 (10) |
Nd1—O7 | 2.383 (2) | C3—H3A | 0.9700 |
Nd1—O14i | 2.406 (2) | C3—H3B | 0.9700 |
Nd1—O1 | 2.407 (2) | C4—O5 | 1.242 (3) |
Nd1—O4 | 2.457 (2) | C4—O4 | 1.266 (3) |
Nd1—O16 | 2.469 (2) | C4—Nd2iv | 2.958 (3) |
Nd1—O15 | 2.525 (3) | C5—O7 | 1.242 (4) |
Nd1—O10i | 2.565 (2) | C5—O6 | 1.253 (4) |
Nd1—O3 | 2.573 (2) | C5—C6 | 1.510 (4) |
Nd1—O9i | 2.654 (2) | C6—O8 | 1.416 (3) |
Nd1—C8i | 2.986 (3) | C6—H6A | 0.9700 |
Nd2—O6 | 2.408 (2) | C6—H6B | 0.9700 |
Nd2—O2ii | 2.429 (2) | C7—O8 | 1.413 (4) |
Nd2—O9 | 2.448 (2) | C7—C8 | 1.499 (4) |
Nd2—O11iii | 2.474 (2) | C7—H7A | 0.9700 |
Nd2—O12 | 2.486 (2) | C7—H7B | 0.9700 |
Nd2—O8 | 2.536 (2) | C8—O10 | 1.247 (4) |
Nd2—O11 | 2.560 (2) | C8—O9 | 1.263 (3) |
Nd2—O5iv | 2.581 (2) | C8—Nd1v | 2.986 (3) |
Nd2—O4iv | 2.5915 (19) | O2—Nd2vi | 2.429 (2) |
Nd2—C4iv | 2.958 (3) | O4—Nd2iv | 2.5915 (19) |
Nd2—S | 3.1469 (12) | O5—Nd2iv | 2.581 (2) |
S—O13 | 1.432 (2) | O9—Nd1v | 2.654 (2) |
S—O12 | 1.470 (2) | O10—Nd1v | 2.565 (2) |
S—O14 | 1.476 (2) | O11—Nd2iii | 2.474 (2) |
S—O11 | 1.507 (2) | O14—Nd1v | 2.406 (2) |
C1—O1 | 1.246 (4) | O15—H15A | 0.8494 |
C1—O2 | 1.249 (3) | O15—H15B | 0.8242 |
C1—C2 | 1.507 (4) | O16—H16A | 0.9210 |
C2—O3 | 1.422 (3) | O16—H16B | 0.8936 |
C2—H2A | 0.9700 | O1W—H1A | 0.8202 |
C2—H2B | 0.9700 | O1W—H1B | 0.9675 |
C3—O3 | 1.401 (3) | O2W—H2C | 0.9179 |
C3—C4 | 1.503 (4) | O2W—H2D | 1.0125 |
O7—Nd1—O14i | 77.92 (8) | O9—Nd2—S | 69.61 (5) |
O7—Nd1—O1 | 90.93 (9) | O11iii—Nd2—S | 92.09 (5) |
O14i—Nd1—O1 | 150.46 (8) | O12—Nd2—S | 27.16 (5) |
O7—Nd1—O4 | 76.79 (8) | O8—Nd2—S | 131.97 (5) |
O14i—Nd1—O4 | 81.19 (7) | O11—Nd2—S | 28.31 (5) |
O1—Nd1—O4 | 123.17 (7) | O5iv—Nd2—S | 85.82 (6) |
O7—Nd1—O16 | 72.52 (9) | O4iv—Nd2—S | 97.41 (5) |
O14i—Nd1—O16 | 81.90 (7) | C4iv—Nd2—S | 93.42 (6) |
O1—Nd1—O16 | 68.63 (8) | O13—S—O12 | 113.63 (14) |
O4—Nd1—O16 | 147.40 (8) | O13—S—O14 | 110.06 (14) |
O7—Nd1—O15 | 142.63 (9) | O12—S—O14 | 109.80 (14) |
O14i—Nd1—O15 | 85.25 (9) | O13—S—O11 | 111.21 (14) |
O1—Nd1—O15 | 87.59 (9) | O12—S—O11 | 103.39 (12) |
O4—Nd1—O15 | 133.40 (8) | O14—S—O11 | 108.47 (13) |
O16—Nd1—O15 | 72.23 (10) | O13—S—Nd2 | 135.41 (10) |
O7—Nd1—O10i | 141.80 (8) | O12—S—Nd2 | 50.50 (9) |
O14i—Nd1—O10i | 123.87 (7) | O14—S—Nd2 | 114.52 (9) |
O1—Nd1—O10i | 81.31 (8) | O11—S—Nd2 | 53.65 (8) |
O4—Nd1—O10i | 76.58 (8) | O1—C1—O2 | 125.1 (3) |
O16—Nd1—O10i | 135.64 (9) | O1—C1—C2 | 118.4 (2) |
O15—Nd1—O10i | 74.75 (9) | O2—C1—C2 | 116.5 (3) |
O7—Nd1—O3 | 74.94 (8) | O3—C2—C1 | 107.2 (2) |
O14i—Nd1—O3 | 137.95 (8) | O3—C2—H2A | 110.3 |
O1—Nd1—O3 | 61.42 (7) | C1—C2—H2A | 110.3 |
O4—Nd1—O3 | 61.79 (6) | O3—C2—H2B | 110.3 |
O16—Nd1—O3 | 118.64 (8) | C1—C2—H2B | 110.3 |
O15—Nd1—O3 | 134.39 (9) | H2A—C2—H2B | 108.5 |
O10i—Nd1—O3 | 68.48 (8) | O3—C3—C4 | 108.6 (2) |
O7—Nd1—O9i | 137.64 (7) | O3—C3—H3A | 110.0 |
O14i—Nd1—O9i | 74.43 (7) | C4—C3—H3A | 110.0 |
O1—Nd1—O9i | 127.63 (7) | O3—C3—H3B | 110.0 |
O4—Nd1—O9i | 67.82 (6) | C4—C3—H3B | 110.0 |
O16—Nd1—O9i | 132.71 (8) | H3A—C3—H3B | 108.3 |
O15—Nd1—O9i | 65.60 (8) | O5—C4—O4 | 120.9 (3) |
O10i—Nd1—O9i | 49.48 (7) | O5—C4—C3 | 119.7 (2) |
O3—Nd1—O9i | 106.09 (7) | O4—C4—C3 | 119.4 (2) |
O7—Nd1—C8i | 147.44 (8) | O5—C4—Nd2iv | 60.40 (15) |
O14i—Nd1—C8i | 99.42 (7) | O4—C4—Nd2iv | 60.95 (14) |
O1—Nd1—C8i | 104.30 (8) | C3—C4—Nd2iv | 172.2 (2) |
O4—Nd1—C8i | 70.77 (8) | O7—C5—O6 | 125.2 (3) |
O16—Nd1—C8i | 139.77 (9) | O7—C5—C6 | 117.0 (3) |
O15—Nd1—C8i | 67.86 (9) | O6—C5—C6 | 117.9 (3) |
O10i—Nd1—C8i | 24.49 (7) | O8—C6—C5 | 108.9 (3) |
O3—Nd1—C8i | 87.19 (8) | O8—C6—H6A | 109.9 |
O9i—Nd1—C8i | 25.00 (7) | C5—C6—H6A | 109.9 |
O6—Nd2—O2ii | 82.02 (9) | O8—C6—H6B | 109.9 |
O6—Nd2—O9 | 124.46 (7) | C5—C6—H6B | 109.9 |
O2ii—Nd2—O9 | 74.55 (7) | H6A—C6—H6B | 108.3 |
O6—Nd2—O11iii | 95.96 (7) | O8—C7—C8 | 108.9 (2) |
O2ii—Nd2—O11iii | 141.66 (7) | O8—C7—H7A | 109.9 |
O9—Nd2—O11iii | 75.44 (7) | C8—C7—H7A | 109.9 |
O6—Nd2—O12 | 143.29 (8) | O8—C7—H7B | 109.9 |
O2ii—Nd2—O12 | 76.63 (8) | C8—C7—H7B | 109.9 |
O9—Nd2—O12 | 77.89 (8) | H7A—C7—H7B | 108.3 |
O11iii—Nd2—O12 | 119.21 (7) | O10—C8—O9 | 121.1 (3) |
O6—Nd2—O8 | 62.45 (7) | O10—C8—C7 | 119.8 (3) |
O2ii—Nd2—O8 | 70.93 (8) | O9—C8—C7 | 119.1 (3) |
O9—Nd2—O8 | 62.42 (7) | O10—C8—Nd1v | 58.49 (15) |
O11iii—Nd2—O8 | 74.29 (7) | O9—C8—Nd1v | 62.63 (15) |
O12—Nd2—O8 | 133.75 (7) | C7—C8—Nd1v | 177.0 (2) |
O6—Nd2—O11 | 152.86 (7) | C1—O1—Nd1 | 128.60 (19) |
O2ii—Nd2—O11 | 125.05 (8) | C1—O2—Nd2vi | 124.3 (2) |
O9—Nd2—O11 | 71.25 (7) | C3—O3—C2 | 114.4 (2) |
O11iii—Nd2—O11 | 64.74 (8) | C3—O3—Nd1 | 123.09 (16) |
O12—Nd2—O11 | 55.16 (7) | C2—O3—Nd1 | 122.38 (16) |
O8—Nd2—O11 | 123.97 (6) | C4—O4—Nd1 | 126.80 (17) |
O6—Nd2—O5iv | 79.41 (8) | C4—O4—Nd2iv | 93.76 (16) |
O2ii—Nd2—O5iv | 93.74 (7) | Nd1—O4—Nd2iv | 139.12 (8) |
O9—Nd2—O5iv | 150.15 (7) | C4—O5—Nd2iv | 94.86 (17) |
O11iii—Nd2—O5iv | 123.70 (7) | C5—O6—Nd2 | 128.1 (2) |
O12—Nd2—O5iv | 72.66 (8) | C5—O7—Nd1 | 153.4 (2) |
O8—Nd2—O5iv | 140.12 (7) | C7—O8—C6 | 113.9 (2) |
O11—Nd2—O5iv | 95.23 (7) | C7—O8—Nd2 | 122.93 (17) |
O6—Nd2—O4iv | 72.93 (7) | C6—O8—Nd2 | 121.65 (18) |
O2ii—Nd2—O4iv | 138.43 (7) | C8—O9—Nd2 | 126.36 (18) |
O9—Nd2—O4iv | 146.98 (6) | C8—O9—Nd1v | 92.38 (16) |
O11iii—Nd2—O4iv | 74.86 (7) | Nd2—O9—Nd1v | 141.08 (8) |
O12—Nd2—O4iv | 104.67 (7) | C8—O10—Nd1v | 97.02 (18) |
O8—Nd2—O4iv | 121.50 (7) | S—O11—Nd2iii | 143.22 (12) |
O11—Nd2—O4iv | 83.23 (7) | S—O11—Nd2 | 98.04 (10) |
O5iv—Nd2—O4iv | 49.90 (6) | Nd2iii—O11—Nd2 | 115.26 (8) |
O6—Nd2—C4iv | 73.02 (8) | S—O12—Nd2 | 102.34 (11) |
O2ii—Nd2—C4iv | 115.64 (7) | S—O14—Nd1v | 138.92 (12) |
O9—Nd2—C4iv | 161.96 (7) | Nd1—O15—H15A | 116.9 |
O11iii—Nd2—C4iv | 99.94 (7) | Nd1—O15—H15B | 100.7 |
O12—Nd2—C4iv | 89.74 (8) | H15A—O15—H15B | 100.2 |
O8—Nd2—C4iv | 133.84 (7) | Nd1—O16—H16A | 124.7 |
O11—Nd2—C4iv | 90.94 (7) | Nd1—O16—H16B | 116.2 |
O5iv—Nd2—C4iv | 24.73 (7) | H16A—O16—H16B | 109.8 |
O4iv—Nd2—C4iv | 25.29 (7) | H1A—O1W—H1B | 99.5 |
O6—Nd2—S | 165.23 (6) | H2C—O2W—H2D | 66.1 |
O2ii—Nd2—S | 99.22 (7) | ||
O1—C1—C2—O3 | 12.5 (4) | C6—C5—O7—Nd1 | 52.1 (6) |
O2—C1—C2—O3 | −167.6 (3) | C8—C7—O8—C6 | −167.3 (3) |
O3—C3—C4—O5 | −175.3 (3) | C8—C7—O8—Nd2 | −1.2 (4) |
O3—C3—C4—O4 | 5.9 (4) | C5—C6—O8—C7 | 176.0 (3) |
O7—C5—C6—O8 | 177.2 (3) | C5—C6—O8—Nd2 | 9.7 (4) |
O6—C5—C6—O8 | −3.1 (4) | O10—C8—O9—Nd2 | 174.6 (2) |
O8—C7—C8—O10 | −176.6 (3) | C7—C8—O9—Nd2 | −6.8 (4) |
O8—C7—C8—O9 | 4.8 (5) | Nd1v—C8—O9—Nd2 | 176.0 (2) |
O2—C1—O1—Nd1 | 161.5 (2) | O10—C8—O9—Nd1v | −1.5 (3) |
C2—C1—O1—Nd1 | −18.6 (4) | C7—C8—O9—Nd1v | 177.1 (3) |
O1—C1—O2—Nd2vi | 7.0 (5) | O9—C8—O10—Nd1v | 1.5 (3) |
C2—C1—O2—Nd2vi | −172.9 (2) | C7—C8—O10—Nd1v | −177.1 (3) |
C4—C3—O3—C2 | 177.8 (2) | O13—S—O11—Nd2iii | 73.2 (2) |
C4—C3—O3—Nd1 | −6.1 (3) | O12—S—O11—Nd2iii | −164.55 (19) |
C1—C2—O3—C3 | 173.0 (3) | O14—S—O11—Nd2iii | −48.0 (2) |
C1—C2—O3—Nd1 | −3.1 (3) | Nd2—S—O11—Nd2iii | −155.3 (2) |
O5—C4—O4—Nd1 | 177.8 (2) | O13—S—O11—Nd2 | −131.52 (12) |
C3—C4—O4—Nd1 | −3.4 (4) | O12—S—O11—Nd2 | −9.22 (13) |
Nd2iv—C4—O4—Nd1 | −174.5 (2) | O14—S—O11—Nd2 | 107.31 (12) |
O5—C4—O4—Nd2iv | −7.7 (3) | O13—S—O12—Nd2 | 130.30 (13) |
C3—C4—O4—Nd2iv | 171.1 (2) | O14—S—O12—Nd2 | −105.96 (12) |
O4—C4—O5—Nd2iv | 7.7 (3) | O11—S—O12—Nd2 | 9.63 (13) |
C3—C4—O5—Nd2iv | −171.0 (2) | O13—S—O14—Nd1v | −162.7 (2) |
O7—C5—O6—Nd2 | 174.0 (2) | O12—S—O14—Nd1v | 71.5 (2) |
C6—C5—O6—Nd2 | −5.6 (4) | O11—S—O14—Nd1v | −40.8 (2) |
O6—C5—O7—Nd1 | −127.5 (5) | Nd2—S—O14—Nd1v | 16.8 (2) |
Symmetry codes: (i) x−1, y, z; (ii) x+1/2, −y+3/2, z+1/2; (iii) −x+2, −y+2, −z+2; (iv) −x+1, −y+2, −z+2; (v) x+1, y, z; (vi) x−1/2, −y+3/2, z−1/2. |
[Sm2(C4H4O5)2(SO4)(H2O)2]·1.32H2O | F(000) = 1364.8 |
Mr = 720.75 | Dx = 2.714 Mg m−3 |
Monoclinic, P21/n | Mo Kα radiation, λ = 0.71073 Å |
Hall symbol: -P 2yn | Cell parameters from 6577 reflections |
a = 10.4709 (17) Å | θ = 2.3–28.1° |
b = 16.441 (3) Å | µ = 6.80 mm−1 |
c = 10.8721 (18) Å | T = 298 K |
β = 109.528 (2)° | Block, pale yellow |
V = 1764.0 (5) Å3 | 0.38 × 0.18 × 0.16 mm |
Z = 4 |
Bruker SMART APEX CCD area-detector diffractometer | 4177 independent reflections |
Radiation source: sealed tube | 3978 reflections with I > 2σ(I) |
Graphite monochromator | Rint = 0.029 |
ϕ and ω scans | θmax = 28.1°, θmin = 2.4° |
Absorption correction: multi-scan (SADABS; Sheldrick, 1996) | h = −13→13 |
Tmin = 0.192, Tmax = 0.337 | k = −21→21 |
19764 measured reflections | l = −14→13 |
Refinement on F2 | Primary atom site location: structure-invariant direct methods |
Least-squares matrix: full | Secondary atom site location: difference Fourier map |
R[F2 > 2σ(F2)] = 0.019 | Hydrogen site location: inferred from neighbouring sites |
wR(F2) = 0.047 | H-atom parameters constrained |
S = 1.09 | w = 1/[σ2(Fo2) + (0.0235P)2 + 1.3713P] where P = (Fo2 + 2Fc2)/3 |
4177 reflections | (Δ/σ)max = 0.004 |
259 parameters | Δρmax = 0.55 e Å−3 |
0 restraints | Δρmin = −1.07 e Å−3 |
[Sm2(C4H4O5)2(SO4)(H2O)2]·1.32H2O | V = 1764.0 (5) Å3 |
Mr = 720.75 | Z = 4 |
Monoclinic, P21/n | Mo Kα radiation |
a = 10.4709 (17) Å | µ = 6.80 mm−1 |
b = 16.441 (3) Å | T = 298 K |
c = 10.8721 (18) Å | 0.38 × 0.18 × 0.16 mm |
β = 109.528 (2)° |
Bruker SMART APEX CCD area-detector diffractometer | 4177 independent reflections |
Absorption correction: multi-scan (SADABS; Sheldrick, 1996) | 3978 reflections with I > 2σ(I) |
Tmin = 0.192, Tmax = 0.337 | Rint = 0.029 |
19764 measured reflections |
R[F2 > 2σ(F2)] = 0.019 | 0 restraints |
wR(F2) = 0.047 | H-atom parameters constrained |
S = 1.09 | Δρmax = 0.55 e Å−3 |
4177 reflections | Δρmin = −1.07 e Å−3 |
259 parameters |
Geometry. All e.s.d.'s (except the e.s.d. in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell e.s.d.'s are taken into account individually in the estimation of e.s.d.'s in distances, angles and torsion angles; correlations between e.s.d.'s in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell e.s.d.'s is used for estimating e.s.d.'s involving l.s. planes. |
Refinement. Refinement of F2 against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F2, conventional R-factors R are based on F, with F set to zero for negative F2. The threshold expression of F2 > σ(F2) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F2 are statistically about twice as large as those based on F, and R-factors based on ALL data will be even larger. |
x | y | z | Uiso*/Ueq | Occ. (<1) | |
Sm1 | 0.208765 (13) | 0.831653 (8) | 0.841267 (12) | 0.01657 (5) | |
Sm2 | 0.876426 (13) | 0.906940 (8) | 1.032500 (12) | 0.01542 (5) | |
S1 | 1.19114 (6) | 0.89549 (4) | 1.15395 (6) | 0.01881 (13) | |
C1 | 0.2693 (3) | 0.77705 (16) | 0.5744 (3) | 0.0210 (5) | |
C2 | 0.2343 (3) | 0.86410 (17) | 0.5311 (3) | 0.0230 (6) | |
H2A | 0.3097 | 0.8899 | 0.5135 | 0.028* | |
H2B | 0.1559 | 0.8657 | 0.4521 | 0.028* | |
C3 | 0.1879 (3) | 0.98916 (16) | 0.6172 (3) | 0.0225 (5) | |
H3A | 0.1158 | 1.0007 | 0.5359 | 0.027* | |
H3B | 0.2705 | 1.0144 | 0.6141 | 0.027* | |
C4 | 0.1519 (3) | 1.02248 (16) | 0.7304 (3) | 0.0189 (5) | |
C5 | 0.5436 (3) | 0.89659 (17) | 0.9012 (3) | 0.0246 (6) | |
C6 | 0.5749 (3) | 0.8745 (2) | 0.7796 (3) | 0.0331 (7) | |
H6A | 0.5487 | 0.8186 | 0.7554 | 0.040* | |
H6B | 0.5245 | 0.9095 | 0.7080 | 0.040* | |
C7 | 0.7595 (3) | 0.8605 (2) | 0.7016 (3) | 0.0353 (7) | |
H7A | 0.7320 | 0.9006 | 0.6323 | 0.042* | |
H7B | 0.7188 | 0.8088 | 0.6667 | 0.042* | |
C8 | 0.9110 (3) | 0.85280 (18) | 0.7513 (3) | 0.0221 (5) | |
O1 | 0.2453 (2) | 0.75324 (12) | 0.6733 (2) | 0.0301 (5) | |
O2 | 0.3200 (2) | 0.73454 (12) | 0.5070 (2) | 0.0311 (5) | |
O3 | 0.2061 (2) | 0.90490 (11) | 0.6341 (2) | 0.0281 (5) | |
O4 | 0.1550 (2) | 0.97602 (11) | 0.82424 (18) | 0.0202 (4) | |
O5 | 0.1214 (2) | 1.09591 (11) | 0.7318 (2) | 0.0271 (5) | |
O6 | 0.6406 (2) | 0.91571 (13) | 1.0010 (2) | 0.0296 (5) | |
O7 | 0.4230 (2) | 0.89445 (14) | 0.8944 (2) | 0.0341 (5) | |
O8 | 0.71622 (18) | 0.88431 (13) | 0.80509 (19) | 0.0236 (4) | |
O9 | 0.97360 (18) | 0.86166 (12) | 0.87167 (17) | 0.0199 (4) | |
O10 | 0.9725 (2) | 0.83665 (15) | 0.6740 (2) | 0.0334 (5) | |
O11 | 1.11123 (19) | 0.96923 (11) | 1.08828 (19) | 0.0222 (4) | |
O12 | 1.0863 (2) | 0.83910 (12) | 1.1647 (2) | 0.0280 (5) | |
O13 | 1.2900 (2) | 0.91652 (14) | 1.2774 (2) | 0.0333 (5) | |
O14 | 1.2588 (2) | 0.86067 (14) | 1.06651 (19) | 0.0273 (4) | |
O15 | 0.0936 (3) | 0.70877 (15) | 0.8857 (3) | 0.0471 (6) | |
H15A | 0.1096 | 0.6646 | 0.8513 | 0.071* | |
H15B | 0.0020 | 0.7153 | 0.8393 | 0.071* | |
O16 | 0.3804 (3) | 0.72700 (13) | 0.9299 (2) | 0.0375 (6) | |
H16A | 0.4171 | 0.7105 | 1.0047 | 0.056* | |
H16B | 0.3757 | 0.6866 | 0.8842 | 0.056* | |
O1W | 0.0443 (3) | 0.58554 (16) | 0.7161 (3) | 0.0472 (7) | |
H1A | −0.0302 | 0.5955 | 0.6667 | 0.071* | |
H1B | 0.0963 | 0.5759 | 0.6685 | 0.071* | |
O2W | 0.5000 | 1.0000 | 0.5000 | 0.155 (5) | 0.64 |
H2C | 0.5594 | 1.0236 | 0.5630 | 0.233* | 0.32 |
H2D | 0.4200 | 1.0000 | 0.4800 | 0.233* | 0.32 |
U11 | U22 | U33 | U12 | U13 | U23 | |
Sm1 | 0.01847 (7) | 0.01733 (8) | 0.01420 (7) | 0.00124 (5) | 0.00585 (5) | 0.00032 (5) |
Sm2 | 0.01568 (7) | 0.01718 (7) | 0.01473 (7) | −0.00193 (4) | 0.00686 (5) | −0.00185 (4) |
S1 | 0.0167 (3) | 0.0262 (3) | 0.0134 (3) | 0.0002 (2) | 0.0048 (2) | 0.0012 (2) |
C1 | 0.0240 (13) | 0.0210 (13) | 0.0166 (12) | 0.0032 (10) | 0.0050 (10) | −0.0026 (10) |
C2 | 0.0335 (15) | 0.0212 (13) | 0.0172 (13) | 0.0066 (11) | 0.0125 (11) | −0.0002 (10) |
C3 | 0.0347 (15) | 0.0158 (12) | 0.0208 (13) | 0.0032 (11) | 0.0145 (12) | 0.0011 (10) |
C4 | 0.0204 (12) | 0.0192 (12) | 0.0183 (12) | −0.0012 (10) | 0.0081 (10) | −0.0014 (10) |
C5 | 0.0191 (13) | 0.0231 (14) | 0.0318 (16) | −0.0004 (10) | 0.0088 (12) | 0.0019 (11) |
C6 | 0.0136 (13) | 0.054 (2) | 0.0299 (16) | −0.0030 (12) | 0.0043 (11) | −0.0087 (14) |
C7 | 0.0217 (14) | 0.063 (2) | 0.0201 (15) | 0.0007 (14) | 0.0059 (12) | −0.0085 (15) |
C8 | 0.0190 (13) | 0.0292 (14) | 0.0181 (13) | −0.0012 (11) | 0.0062 (10) | −0.0035 (11) |
O1 | 0.0500 (13) | 0.0211 (10) | 0.0207 (10) | 0.0077 (9) | 0.0138 (10) | 0.0023 (8) |
O2 | 0.0431 (13) | 0.0235 (11) | 0.0320 (12) | 0.0111 (9) | 0.0196 (10) | −0.0024 (9) |
O3 | 0.0533 (14) | 0.0158 (9) | 0.0228 (11) | 0.0073 (8) | 0.0229 (10) | 0.0012 (7) |
O4 | 0.0300 (10) | 0.0172 (9) | 0.0172 (9) | 0.0018 (7) | 0.0127 (8) | 0.0003 (7) |
O5 | 0.0448 (13) | 0.0173 (10) | 0.0243 (11) | 0.0061 (8) | 0.0184 (10) | 0.0015 (8) |
O6 | 0.0199 (10) | 0.0406 (12) | 0.0285 (11) | −0.0018 (8) | 0.0082 (9) | −0.0067 (9) |
O7 | 0.0189 (10) | 0.0401 (12) | 0.0463 (14) | −0.0026 (9) | 0.0151 (10) | −0.0023 (10) |
O8 | 0.0153 (9) | 0.0351 (11) | 0.0202 (10) | −0.0040 (8) | 0.0054 (7) | −0.0057 (8) |
O9 | 0.0189 (9) | 0.0268 (10) | 0.0142 (9) | −0.0014 (7) | 0.0060 (7) | −0.0035 (7) |
O10 | 0.0244 (11) | 0.0589 (15) | 0.0177 (10) | −0.0018 (10) | 0.0080 (9) | −0.0122 (9) |
O11 | 0.0209 (9) | 0.0223 (9) | 0.0224 (10) | −0.0005 (7) | 0.0058 (8) | 0.0017 (8) |
O12 | 0.0225 (10) | 0.0287 (11) | 0.0337 (12) | 0.0007 (8) | 0.0106 (9) | 0.0121 (9) |
O13 | 0.0260 (11) | 0.0512 (14) | 0.0179 (10) | −0.0004 (9) | 0.0008 (8) | −0.0041 (9) |
O14 | 0.0226 (10) | 0.0421 (12) | 0.0186 (10) | 0.0054 (9) | 0.0086 (8) | −0.0014 (9) |
O15 | 0.0524 (16) | 0.0264 (12) | 0.0642 (18) | −0.0046 (11) | 0.0219 (14) | 0.0079 (12) |
O16 | 0.0574 (15) | 0.0315 (12) | 0.0184 (10) | 0.0224 (11) | 0.0060 (10) | 0.0028 (9) |
O1W | 0.0297 (12) | 0.0652 (18) | 0.0491 (16) | 0.0045 (11) | 0.0162 (12) | −0.0019 (13) |
O2W | 0.134 (10) | 0.186 (13) | 0.116 (9) | −0.081 (10) | 0.004 (8) | 0.007 (9) |
Sm1—O7 | 2.359 (2) | C3—H3A | 0.9700 |
Sm1—O1 | 2.369 (2) | C3—H3B | 0.9700 |
Sm1—O14i | 2.375 (2) | C4—O5 | 1.250 (3) |
Sm1—O4 | 2.4320 (18) | C4—O4 | 1.266 (3) |
Sm1—O16 | 2.441 (2) | C4—Sm2iv | 2.931 (3) |
Sm1—O15 | 2.482 (2) | C5—O7 | 1.241 (3) |
Sm1—O10i | 2.535 (2) | C5—O6 | 1.254 (4) |
Sm1—O3 | 2.546 (2) | C5—C6 | 1.509 (4) |
Sm1—O9i | 2.6382 (19) | C6—O8 | 1.421 (3) |
Sm1—C8i | 2.960 (3) | C6—H6A | 0.9700 |
Sm2—O6 | 2.382 (2) | C6—H6B | 0.9700 |
Sm2—O2ii | 2.393 (2) | C7—O8 | 1.402 (3) |
Sm2—O9 | 2.4159 (18) | C7—C8 | 1.500 (4) |
Sm2—O11iii | 2.4494 (19) | C7—H7A | 0.9700 |
Sm2—O12 | 2.455 (2) | C7—H7B | 0.9700 |
Sm2—O8 | 2.5085 (19) | C8—O10 | 1.247 (3) |
Sm2—O11 | 2.5425 (19) | C8—O9 | 1.261 (3) |
Sm2—O5iv | 2.555 (2) | C8—Sm1v | 2.960 (3) |
Sm2—O4iv | 2.5653 (18) | O2—Sm2vi | 2.393 (2) |
Sm2—C4iv | 2.931 (3) | O4—Sm2iv | 2.5653 (18) |
Sm2—S | 3.1192 (8) | O5—Sm2iv | 2.555 (2) |
S—O13 | 1.437 (2) | O9—Sm1v | 2.6382 (18) |
S—O12 | 1.471 (2) | O10—Sm1v | 2.535 (2) |
S—O14 | 1.478 (2) | O11—Sm2iii | 2.4495 (19) |
S—O11 | 1.510 (2) | O14—Sm1v | 2.375 (2) |
C1—O1 | 1.246 (3) | O15—H15A | 0.8591 |
C1—O2 | 1.252 (3) | O15—H15B | 0.9287 |
C1—C2 | 1.513 (4) | O16—H16A | 0.8206 |
C2—O3 | 1.419 (3) | O16—H16B | 0.8212 |
C2—H2A | 0.9700 | O1W—H1A | 0.8022 |
C2—H2B | 0.9700 | O1W—H1B | 0.8819 |
C3—O3 | 1.402 (3) | O2W—H2C | 0.8496 |
C3—C4 | 1.505 (3) | O2W—H2D | 0.7920 |
O7—Sm1—O1 | 92.39 (8) | O9—Sm2—S | 69.32 (5) |
O7—Sm1—O14i | 78.20 (8) | O11iii—Sm2—S | 92.27 (5) |
O1—Sm1—O14i | 150.16 (7) | O12—Sm2—S | 27.43 (5) |
O7—Sm1—O4 | 76.60 (7) | O8—Sm2—S | 132.23 (4) |
O1—Sm1—O4 | 124.42 (6) | O11—Sm2—S | 28.69 (4) |
O14i—Sm1—O4 | 81.27 (7) | O5iv—Sm2—S | 85.44 (5) |
O7—Sm1—O16 | 72.40 (8) | O4iv—Sm2—S | 96.90 (5) |
O1—Sm1—O16 | 68.51 (7) | C4iv—Sm2—S | 93.13 (5) |
O14i—Sm1—O16 | 81.65 (7) | O13—S—O12 | 113.66 (14) |
O4—Sm1—O16 | 147.02 (8) | O13—S—O14 | 110.10 (13) |
O7—Sm1—O15 | 142.45 (9) | O12—S—O14 | 109.74 (13) |
O1—Sm1—O15 | 85.49 (9) | O13—S—O11 | 111.15 (13) |
O14i—Sm1—O15 | 85.22 (9) | O12—S—O11 | 103.50 (11) |
O4—Sm1—O15 | 133.95 (8) | O14—S—O11 | 108.41 (12) |
O16—Sm1—O15 | 71.99 (9) | O13—S—Sm2 | 135.26 (10) |
O7—Sm1—O10i | 141.41 (8) | O12—S—Sm2 | 50.28 (8) |
O1—Sm1—O10i | 80.50 (7) | O14—S—Sm2 | 114.64 (9) |
O14i—Sm1—O10i | 124.00 (7) | O11—S—Sm2 | 53.94 (7) |
O4—Sm1—O10i | 76.60 (7) | O1—C1—O2 | 125.2 (3) |
O16—Sm1—O10i | 135.98 (8) | O1—C1—C2 | 117.9 (2) |
O15—Sm1—O10i | 75.21 (9) | O2—C1—C2 | 116.9 (2) |
O7—Sm1—O3 | 74.82 (8) | O3—C2—C1 | 107.1 (2) |
O1—Sm1—O3 | 62.11 (7) | O3—C2—H2A | 110.3 |
O14i—Sm1—O3 | 138.63 (7) | C1—C2—H2A | 110.3 |
O4—Sm1—O3 | 62.43 (6) | O3—C2—H2B | 110.3 |
O16—Sm1—O3 | 118.15 (7) | C1—C2—H2B | 110.3 |
O15—Sm1—O3 | 134.03 (8) | H2A—C2—H2B | 108.5 |
O10i—Sm1—O3 | 68.32 (8) | O3—C3—C4 | 108.2 (2) |
O7—Sm1—O9i | 137.59 (7) | O3—C3—H3A | 110.1 |
O1—Sm1—O9i | 126.61 (7) | C4—C3—H3A | 110.1 |
O14i—Sm1—O9i | 74.14 (6) | O3—C3—H3B | 110.1 |
O4—Sm1—O9i | 67.99 (6) | C4—C3—H3B | 110.1 |
O16—Sm1—O9i | 132.60 (7) | H3A—C3—H3B | 108.4 |
O15—Sm1—O9i | 65.99 (8) | O5—C4—O4 | 120.7 (2) |
O10i—Sm1—O9i | 49.90 (6) | O5—C4—C3 | 119.8 (2) |
O3—Sm1—O9i | 106.72 (6) | O4—C4—C3 | 119.5 (2) |
O7—Sm1—C8i | 147.13 (8) | O5—C4—Sm2iv | 60.36 (14) |
O1—Sm1—C8i | 103.47 (8) | O4—C4—Sm2iv | 60.87 (13) |
O14i—Sm1—C8i | 99.32 (7) | C3—C4—Sm2iv | 171.69 (19) |
O4—Sm1—C8i | 70.66 (7) | O7—C5—O6 | 124.9 (3) |
O16—Sm1—C8i | 140.19 (8) | O7—C5—C6 | 117.2 (3) |
O15—Sm1—C8i | 68.47 (9) | O6—C5—C6 | 118.0 (2) |
O10i—Sm1—C8i | 24.70 (7) | O8—C6—C5 | 108.6 (2) |
O3—Sm1—C8i | 87.33 (8) | O8—C6—H6A | 110.0 |
O9i—Sm1—C8i | 25.19 (7) | C5—C6—H6A | 110.0 |
O6—Sm2—O2ii | 80.68 (8) | O8—C6—H6B | 110.0 |
O6—Sm2—O9 | 125.60 (7) | C5—C6—H6B | 110.0 |
O2ii—Sm2—O9 | 76.36 (7) | H6A—C6—H6B | 108.3 |
O6—Sm2—O11iii | 96.35 (7) | O8—C7—C8 | 108.7 (2) |
O2ii—Sm2—O11iii | 143.23 (7) | O8—C7—H7A | 109.9 |
O9—Sm2—O11iii | 75.98 (6) | C8—C7—H7A | 109.9 |
O6—Sm2—O12 | 142.56 (7) | O8—C7—H7B | 109.9 |
O2ii—Sm2—O12 | 76.37 (8) | C8—C7—H7B | 109.9 |
O9—Sm2—O12 | 76.84 (7) | H7A—C7—H7B | 108.3 |
O11iii—Sm2—O12 | 119.61 (6) | O10—C8—O9 | 121.2 (3) |
O6—Sm2—O8 | 63.11 (7) | O10—C8—C7 | 119.8 (3) |
O2ii—Sm2—O8 | 71.56 (7) | O9—C8—C7 | 119.0 (2) |
O9—Sm2—O8 | 62.97 (6) | O10—C8—Sm1v | 58.21 (15) |
O11iii—Sm2—O8 | 74.49 (7) | O9—C8—Sm1v | 62.98 (14) |
O12—Sm2—O8 | 133.03 (7) | C7—C8—Sm1v | 177.5 (2) |
O6—Sm2—O11 | 152.07 (7) | C1—O1—Sm1 | 128.71 (18) |
O2ii—Sm2—O11 | 126.93 (7) | C1—O2—Sm2vi | 127.71 (19) |
O9—Sm2—O11 | 71.89 (6) | C3—O3—C2 | 114.8 (2) |
O11iii—Sm2—O11 | 64.72 (7) | C3—O3—Sm1 | 122.95 (16) |
O12—Sm2—O11 | 55.82 (6) | C2—O3—Sm1 | 122.08 (15) |
O8—Sm2—O11 | 124.72 (6) | C4—O4—Sm1 | 126.39 (16) |
O6—Sm2—O5iv | 78.83 (7) | C4—O4—Sm2iv | 93.59 (15) |
O2ii—Sm2—O5iv | 91.00 (7) | Sm1—O4—Sm2iv | 139.40 (8) |
O9—Sm2—O5iv | 148.81 (7) | C4—O5—Sm2iv | 94.48 (16) |
O11iii—Sm2—O5iv | 124.64 (6) | C5—O6—Sm2 | 127.59 (19) |
O12—Sm2—O5iv | 72.47 (7) | C5—O7—Sm1 | 153.2 (2) |
O8—Sm2—O5iv | 139.86 (7) | C7—O8—C6 | 114.0 (2) |
O11—Sm2—O5iv | 94.85 (7) | C7—O8—Sm2 | 122.90 (16) |
O6—Sm2—O4iv | 72.80 (7) | C6—O8—Sm2 | 121.25 (17) |
O2ii—Sm2—O4iv | 136.27 (6) | C8—O9—Sm2 | 126.01 (17) |
O9—Sm2—O4iv | 147.27 (6) | C8—O9—Sm1v | 91.82 (15) |
O11iii—Sm2—O4iv | 75.08 (6) | Sm2—O9—Sm1v | 141.71 (8) |
O12—Sm2—O4iv | 104.89 (7) | C8—O10—Sm1v | 97.08 (17) |
O8—Sm2—O4iv | 122.04 (6) | S—O11—Sm2iii | 143.19 (11) |
O11—Sm2—O4iv | 82.14 (6) | S—O11—Sm2 | 97.37 (9) |
O5iv—Sm2—O4iv | 50.56 (6) | Sm2iii—O11—Sm2 | 115.28 (7) |
O6—Sm2—C4iv | 72.40 (7) | S—O12—Sm2 | 102.30 (10) |
O2ii—Sm2—C4iv | 113.14 (7) | S—O14—Sm1v | 138.86 (12) |
O9—Sm2—C4iv | 161.70 (7) | Sm1—O15—H15A | 115.1 |
O11iii—Sm2—C4iv | 100.45 (7) | Sm1—O15—H15B | 106.3 |
O12—Sm2—C4iv | 89.94 (7) | H15A—O15—H15B | 100.2 |
O8—Sm2—C4iv | 134.01 (7) | Sm1—O16—H16A | 131.6 |
O11—Sm2—C4iv | 90.27 (7) | Sm1—O16—H16B | 116.4 |
O5iv—Sm2—C4iv | 25.16 (6) | H16A—O16—H16B | 104.2 |
O4iv—Sm2—C4iv | 25.54 (6) | H1A—O1W—H1B | 107.2 |
O6—Sm2—S | 164.26 (6) | H2C—O2W—H2D | 130.1 |
O2ii—Sm2—S | 100.10 (6) | ||
O1—C1—C2—O3 | 12.2 (4) | C6—C5—O7—Sm1 | 49.6 (6) |
O2—C1—C2—O3 | −168.0 (3) | C8—C7—O8—C6 | −165.4 (3) |
O3—C3—C4—O5 | −175.0 (3) | C8—C7—O8—Sm2 | −0.6 (4) |
O3—C3—C4—O4 | 6.2 (4) | C5—C6—O8—C7 | 176.1 (3) |
O7—C5—C6—O8 | 177.3 (3) | C5—C6—O8—Sm2 | 11.0 (4) |
O6—C5—C6—O8 | −2.6 (4) | O10—C8—O9—Sm2 | 173.0 (2) |
O8—C7—C8—O10 | −175.9 (3) | C7—C8—O9—Sm2 | −8.1 (4) |
O8—C7—C8—O9 | 5.2 (4) | Sm1v—C8—O9—Sm2 | 173.7 (2) |
O2—C1—O1—Sm1 | 161.3 (2) | O10—C8—O9—Sm1v | −0.7 (3) |
C2—C1—O1—Sm1 | −18.9 (4) | C7—C8—O9—Sm1v | 178.2 (3) |
O1—C1—O2—Sm2vi | 4.0 (4) | O9—C8—O10—Sm1v | 0.7 (3) |
C2—C1—O2—Sm2vi | −175.76 (19) | C7—C8—O10—Sm1v | −178.2 (3) |
C4—C3—O3—C2 | 177.1 (2) | O13—S—O11—Sm2iii | 75.6 (2) |
C4—C3—O3—Sm1 | −7.9 (3) | O12—S—O11—Sm2iii | −162.00 (18) |
C1—C2—O3—C3 | 172.5 (2) | O14—S—O11—Sm2iii | −45.5 (2) |
C1—C2—O3—Sm1 | −2.5 (3) | Sm2—S—O11—Sm2iii | −153.0 (2) |
O5—C4—O4—Sm1 | 179.28 (19) | O13—S—O11—Sm2 | −131.33 (11) |
C3—C4—O4—Sm1 | −1.9 (3) | O12—S—O11—Sm2 | −8.96 (12) |
Sm2iv—C4—O4—Sm1 | −172.4 (2) | O14—S—O11—Sm2 | 107.53 (11) |
O5—C4—O4—Sm2iv | −8.3 (3) | O13—S—O12—Sm2 | 130.10 (12) |
C3—C4—O4—Sm2iv | 170.5 (2) | O14—S—O12—Sm2 | −106.13 (11) |
O4—C4—O5—Sm2iv | 8.3 (3) | O11—S—O12—Sm2 | 9.42 (13) |
C3—C4—O5—Sm2iv | −170.4 (2) | O13—S—O14—Sm1v | −164.25 (18) |
O7—C5—O6—Sm2 | 172.2 (2) | O12—S—O14—Sm1v | 69.9 (2) |
C6—C5—O6—Sm2 | −7.9 (4) | O11—S—O14—Sm1v | −42.5 (2) |
O6—C5—O7—Sm1 | −130.4 (4) | Sm2—S—O14—Sm1v | 15.5 (2) |
Symmetry codes: (i) x−1, y, z; (ii) x+1/2, −y+3/2, z+1/2; (iii) −x+2, −y+2, −z+2; (iv) −x+1, −y+2, −z+2; (v) x+1, y, z; (vi) x−1/2, −y+3/2, z−1/2. |
Experimental details
(I) | (II) | (III) | |
Crystal data | |||
Chemical formula | [Pr2(C4H4O5)(SO4)2(H2O)2]·0.5H2O | [Nd2(C4H4O5)2(SO4)(H2O)2]·1.32H2O | [Sm2(C4H4O5)2(SO4)(H2O)2]·1.32H2O |
Mr | 651.05 | 708.51 | 720.75 |
Crystal system, space group | Triclinic, P1 | Monoclinic, P21/n | Monoclinic, P21/n |
Temperature (K) | 298 | 298 | 298 |
a, b, c (Å) | 6.618 (2), 8.527 (3), 13.111 (4) | 10.542 (3), 16.520 (5), 10.885 (4) | 10.4709 (17), 16.441 (3), 10.8721 (18) |
α, β, γ (°) | 86.340 (5), 89.487 (5), 68.617 (5) | 90, 108.921 (5), 90 | 90, 109.528 (2), 90 |
V (Å3) | 687.4 (4) | 1793.4 (10) | 1764.0 (5) |
Z | 2 | 4 | 4 |
Radiation type | Mo Kα | Mo Kα | Mo Kα |
µ (mm−1) | 7.40 | 5.93 | 6.80 |
Crystal size (mm) | 0.60 × 0.10 × 0.08 | 0.40 × 0.20 × 0.18 | 0.38 × 0.18 × 0.16 |
Data collection | |||
Diffractometer | Bruker SMART APEX CCD area-detector diffractometer | Bruker SMART APEX CCD area-detector diffractometer | Bruker SMART APEX CCD area-detector diffractometer |
Absorption correction | Multi-scan (SADABS; Sheldrick, 1996) | Multi-scan (SADABS; Sheldrick, 1996) | Multi-scan (SADABS; Sheldrick, 1996) |
Tmin, Tmax | 0.316, 0.553 | 0.197, 0.344 | 0.192, 0.337 |
No. of measured, independent and observed [I > 2σ(I)] reflections | 7509, 3119, 3020 | 19838, 4230, 4132 | 19764, 4177, 3978 |
Rint | 0.019 | 0.022 | 0.029 |
(sin θ/λ)max (Å−1) | 0.665 | 0.666 | 0.663 |
Refinement | |||
R[F2 > 2σ(F2)], wR(F2), S | 0.021, 0.050, 1.14 | 0.020, 0.046, 1.15 | 0.019, 0.047, 1.09 |
No. of reflections | 3119 | 4230 | 4177 |
No. of parameters | 217 | 259 | 259 |
H-atom treatment | H-atom parameters constrained | H-atom parameters constrained | H-atom parameters constrained |
Δρmax, Δρmin (e Å−3) | 0.76, −1.03 | 0.71, −0.42 | 0.55, −1.07 |
Computer programs: SMART APEX (Bruker, 2007), SAINT-Plus (Bruker, 2007), SHELXS97 (Sheldrick, 2008), SHELXL97 (Sheldrick, 2008), DIAMOND (Brandenburg, 1999), WinGX (Farrugia, 2012).
Pr1—O8i | 2.435 (3) | Pr2—O9iv | 2.360 (2) |
Pr1—O14ii | 2.453 (2) | Pr2—O13v | 2.420 (2) |
Pr1—O1 | 2.518 (3) | Pr2—O11ii | 2.466 (2) |
Pr1—O6 | 2.549 (3) | Pr2—O5vi | 2.501 (2) |
Pr1—O10 | 2.558 (3) | Pr2—O15 | 2.518 (3) |
Pr1—O4 | 2.561 (2) | Pr2—O12 | 2.558 (2) |
Pr1—O7 | 2.601 (2) | Pr2—O5 | 2.584 (2) |
Pr1—O2iii | 2.609 (3) | Pr2—O11 | 2.637 (2) |
Pr1—O3 | 2.610 (3) | Pr2—O4 | 2.677 (2) |
Pr1—O1iii | 2.673 (3) | ||
O8i—Pr1—O14ii | 74.82 (9) | O4—Pr1—O1iii | 160.81 (8) |
O8i—Pr1—O1 | 141.45 (9) | O7—Pr1—O1iii | 76.13 (8) |
O14ii—Pr1—O1 | 142.39 (9) | O2iii—Pr1—O1iii | 48.90 (8) |
O8i—Pr1—O6 | 136.99 (9) | O3—Pr1—O1iii | 107.36 (8) |
O14ii—Pr1—O6 | 73.67 (9) | O9iv—Pr2—O13v | 80.10 (9) |
O1—Pr1—O6 | 77.86 (9) | O9iv—Pr2—O11ii | 81.83 (9) |
O8i—Pr1—O10 | 65.56 (9) | O13v—Pr2—O11ii | 81.20 (8) |
O14ii—Pr1—O10 | 140.38 (9) | O9iv—Pr2—O5vi | 80.13 (8) |
O1—Pr1—O10 | 76.58 (9) | O13v—Pr2—O5vi | 79.60 (9) |
O6—Pr1—O10 | 138.92 (9) | O11ii—Pr2—O5vi | 155.58 (8) |
O8i—Pr1—O4 | 74.53 (9) | O9iv—Pr2—O15 | 140.95 (9) |
O14ii—Pr1—O4 | 74.59 (8) | O13v—Pr2—O15 | 138.74 (8) |
O1—Pr1—O4 | 117.28 (8) | O11ii—Pr2—O15 | 104.20 (8) |
O6—Pr1—O4 | 69.40 (8) | O5vi—Pr2—O15 | 100.18 (8) |
O10—Pr1—O4 | 94.90 (9) | O9iv—Pr2—O12 | 74.10 (8) |
O8i—Pr1—O7 | 138.79 (9) | O13v—Pr2—O12 | 145.18 (8) |
O14ii—Pr1—O7 | 73.89 (8) | O11ii—Pr2—O12 | 117.02 (8) |
O1—Pr1—O7 | 69.64 (8) | O5vi—Pr2—O12 | 73.32 (8) |
O6—Pr1—O7 | 54.38 (8) | O15—Pr2—O12 | 68.83 (8) |
O10—Pr1—O7 | 138.90 (8) | O9iv—Pr2—O5 | 136.68 (8) |
O4—Pr1—O7 | 120.95 (8) | O13v—Pr2—O5 | 73.50 (8) |
O8i—Pr1—O2iii | 78.57 (10) | O11ii—Pr2—O5 | 125.81 (8) |
O14ii—Pr1—O2iii | 73.35 (9) | O5vi—Pr2—O5 | 61.94 (9) |
O1—Pr1—O2iii | 100.13 (8) | O15—Pr2—O5 | 70.49 (8) |
O6—Pr1—O2iii | 118.49 (9) | O12—Pr2—O5 | 110.77 (8) |
O10—Pr1—O2iii | 97.36 (10) | O9iv—Pr2—O11 | 73.55 (8) |
O4—Pr1—O2iii | 142.41 (8) | O13v—Pr2—O11 | 138.34 (8) |
O7—Pr1—O2iii | 67.24 (9) | O11ii—Pr2—O11 | 63.76 (9) |
O8i—Pr1—O3 | 109.98 (9) | O5vi—Pr2—O11 | 125.34 (7) |
O14ii—Pr1—O3 | 129.82 (8) | O15—Pr2—O11 | 74.98 (8) |
O1—Pr1—O3 | 59.02 (8) | O12—Pr2—O11 | 53.84 (7) |
O6—Pr1—O3 | 71.04 (8) | O5—Pr2—O11 | 145.46 (8) |
O10—Pr1—O3 | 68.31 (10) | O9iv—Pr2—O4 | 149.81 (8) |
O4—Pr1—O3 | 60.24 (7) | O13v—Pr2—O4 | 74.63 (8) |
O7—Pr1—O3 | 110.55 (9) | O11ii—Pr2—O4 | 78.25 (7) |
O2iii—Pr1—O3 | 156.26 (8) | O5vi—Pr2—O4 | 110.68 (7) |
O8i—Pr1—O1iii | 98.61 (9) | O15—Pr2—O4 | 66.87 (8) |
O14ii—Pr1—O1iii | 121.56 (9) | O12—Pr2—O4 | 135.51 (7) |
O1—Pr1—O1iii | 57.55 (10) | O5—Pr2—O4 | 49.31 (7) |
O6—Pr1—O1iii | 122.74 (8) | O11—Pr2—O4 | 116.15 (7) |
O10—Pr1—O1iii | 66.12 (9) |
Symmetry codes: (i) x−1, y, z; (ii) −x, −y+1, −z+2; (iii) −x+1, −y+1, −z+1; (iv) −x+1, −y+1, −z+2; (v) x+1, y, z; (vi) −x+1, −y, −z+2. |
Nd1—O7 | 2.383 (2) | Nd2—O6 | 2.408 (2) |
Nd1—O14i | 2.406 (2) | Nd2—O2ii | 2.429 (2) |
Nd1—O1 | 2.407 (2) | Nd2—O9 | 2.448 (2) |
Nd1—O4 | 2.457 (2) | Nd2—O11iii | 2.474 (2) |
Nd1—O16 | 2.469 (2) | Nd2—O12 | 2.486 (2) |
Nd1—O15 | 2.525 (3) | Nd2—O8 | 2.536 (2) |
Nd1—O10i | 2.565 (2) | Nd2—O11 | 2.560 (2) |
Nd1—O3 | 2.573 (2) | Nd2—O5iv | 2.581 (2) |
Nd1—O9i | 2.654 (2) | Nd2—O4iv | 2.5915 (19) |
O7—Nd1—O14i | 77.92 (8) | O6—Nd2—O2ii | 82.02 (9) |
O7—Nd1—O1 | 90.93 (9) | O6—Nd2—O9 | 124.46 (7) |
O14i—Nd1—O1 | 150.46 (8) | O2ii—Nd2—O9 | 74.55 (7) |
O7—Nd1—O4 | 76.79 (8) | O6—Nd2—O11iii | 95.96 (7) |
O14i—Nd1—O4 | 81.19 (7) | O2ii—Nd2—O11iii | 141.66 (7) |
O1—Nd1—O4 | 123.17 (7) | O9—Nd2—O11iii | 75.44 (7) |
O7—Nd1—O16 | 72.52 (9) | O6—Nd2—O12 | 143.29 (8) |
O14i—Nd1—O16 | 81.90 (7) | O2ii—Nd2—O12 | 76.63 (8) |
O1—Nd1—O16 | 68.63 (8) | O9—Nd2—O12 | 77.89 (8) |
O4—Nd1—O16 | 147.40 (8) | O11iii—Nd2—O12 | 119.21 (7) |
O7—Nd1—O15 | 142.63 (9) | O6—Nd2—O8 | 62.45 (7) |
O14i—Nd1—O15 | 85.25 (9) | O2ii—Nd2—O8 | 70.93 (8) |
O1—Nd1—O15 | 87.59 (9) | O9—Nd2—O8 | 62.42 (7) |
O4—Nd1—O15 | 133.40 (8) | O11iii—Nd2—O8 | 74.29 (7) |
O16—Nd1—O15 | 72.23 (10) | O12—Nd2—O8 | 133.75 (7) |
O7—Nd1—O10i | 141.80 (8) | O6—Nd2—O11 | 152.86 (7) |
O14i—Nd1—O10i | 123.87 (7) | O2ii—Nd2—O11 | 125.05 (8) |
O1—Nd1—O10i | 81.31 (8) | O9—Nd2—O11 | 71.25 (7) |
O4—Nd1—O10i | 76.58 (8) | O11iii—Nd2—O11 | 64.74 (8) |
O16—Nd1—O10i | 135.64 (9) | O12—Nd2—O11 | 55.16 (7) |
O15—Nd1—O10i | 74.75 (9) | O8—Nd2—O11 | 123.97 (6) |
O7—Nd1—O3 | 74.94 (8) | O6—Nd2—O5iv | 79.41 (8) |
O14i—Nd1—O3 | 137.95 (8) | O2ii—Nd2—O5iv | 93.74 (7) |
O1—Nd1—O3 | 61.42 (7) | O9—Nd2—O5iv | 150.15 (7) |
O4—Nd1—O3 | 61.79 (6) | O11iii—Nd2—O5iv | 123.70 (7) |
O16—Nd1—O3 | 118.64 (8) | O12—Nd2—O5iv | 72.66 (8) |
O15—Nd1—O3 | 134.39 (9) | O8—Nd2—O5iv | 140.12 (7) |
O10i—Nd1—O3 | 68.48 (8) | O11—Nd2—O5iv | 95.23 (7) |
O7—Nd1—O9i | 137.64 (7) | O6—Nd2—O4iv | 72.93 (7) |
O14i—Nd1—O9i | 74.43 (7) | O2ii—Nd2—O4iv | 138.43 (7) |
O1—Nd1—O9i | 127.63 (7) | O9—Nd2—O4iv | 146.98 (6) |
O4—Nd1—O9i | 67.82 (6) | O11iii—Nd2—O4iv | 74.86 (7) |
O16—Nd1—O9i | 132.71 (8) | O12—Nd2—O4iv | 104.67 (7) |
O15—Nd1—O9i | 65.60 (8) | O8—Nd2—O4iv | 121.50 (7) |
O10i—Nd1—O9i | 49.48 (7) | O11—Nd2—O4iv | 83.23 (7) |
O3—Nd1—O9i | 106.09 (7) | O5iv—Nd2—O4iv | 49.90 (6) |
Symmetry codes: (i) x−1, y, z; (ii) x+1/2, −y+3/2, z+1/2; (iii) −x+2, −y+2, −z+2; (iv) −x+1, −y+2, −z+2. |
Sm1—O7 | 2.359 (2) | Sm2—O6 | 2.382 (2) |
Sm1—O1 | 2.369 (2) | Sm2—O2ii | 2.393 (2) |
Sm1—O14i | 2.375 (2) | Sm2—O9 | 2.4159 (18) |
Sm1—O4 | 2.4320 (18) | Sm2—O11iii | 2.4494 (19) |
Sm1—O16 | 2.441 (2) | Sm2—O12 | 2.455 (2) |
Sm1—O15 | 2.482 (2) | Sm2—O8 | 2.5085 (19) |
Sm1—O10i | 2.535 (2) | Sm2—O11 | 2.5425 (19) |
Sm1—O3 | 2.546 (2) | Sm2—O5iv | 2.555 (2) |
Sm1—O9i | 2.6382 (19) | Sm2—O4iv | 2.5653 (18) |
Sm1—C8i | 2.960 (3) | ||
O7—Sm1—O1 | 92.39 (8) | O6—Sm2—O2ii | 80.68 (8) |
O7—Sm1—O14i | 78.20 (8) | O6—Sm2—O9 | 125.60 (7) |
O1—Sm1—O14i | 150.16 (7) | O2ii—Sm2—O9 | 76.36 (7) |
O7—Sm1—O4 | 76.60 (7) | O6—Sm2—O11iii | 96.35 (7) |
O1—Sm1—O4 | 124.42 (6) | O2ii—Sm2—O11iii | 143.23 (7) |
O14i—Sm1—O4 | 81.27 (7) | O9—Sm2—O11iii | 75.98 (6) |
O7—Sm1—O16 | 72.40 (8) | O6—Sm2—O12 | 142.56 (7) |
O1—Sm1—O16 | 68.51 (7) | O2ii—Sm2—O12 | 76.37 (8) |
O14i—Sm1—O16 | 81.65 (7) | O9—Sm2—O12 | 76.84 (7) |
O4—Sm1—O16 | 147.02 (8) | O11iii—Sm2—O12 | 119.61 (6) |
O7—Sm1—O15 | 142.45 (9) | O6—Sm2—O8 | 63.11 (7) |
O1—Sm1—O15 | 85.49 (9) | O2ii—Sm2—O8 | 71.56 (7) |
O14i—Sm1—O15 | 85.22 (9) | O9—Sm2—O8 | 62.97 (6) |
O4—Sm1—O15 | 133.95 (8) | O11iii—Sm2—O8 | 74.49 (7) |
O16—Sm1—O15 | 71.99 (9) | O12—Sm2—O8 | 133.03 (7) |
O7—Sm1—O10i | 141.41 (8) | O6—Sm2—O11 | 152.07 (7) |
O1—Sm1—O10i | 80.50 (7) | O2ii—Sm2—O11 | 126.93 (7) |
O14i—Sm1—O10i | 124.00 (7) | O9—Sm2—O11 | 71.89 (6) |
O4—Sm1—O10i | 76.60 (7) | O11iii—Sm2—O11 | 64.72 (7) |
O16—Sm1—O10i | 135.98 (8) | O12—Sm2—O11 | 55.82 (6) |
O15—Sm1—O10i | 75.21 (9) | O8—Sm2—O11 | 124.72 (6) |
O7—Sm1—O3 | 74.82 (8) | O6—Sm2—O5iv | 78.83 (7) |
O1—Sm1—O3 | 62.11 (7) | O2ii—Sm2—O5iv | 91.00 (7) |
O14i—Sm1—O3 | 138.63 (7) | O9—Sm2—O5iv | 148.81 (7) |
O4—Sm1—O3 | 62.43 (6) | O11iii—Sm2—O5iv | 124.64 (6) |
O16—Sm1—O3 | 118.15 (7) | O12—Sm2—O5iv | 72.47 (7) |
O15—Sm1—O3 | 134.03 (8) | O8—Sm2—O5iv | 139.86 (7) |
O10i—Sm1—O3 | 68.32 (8) | O11—Sm2—O5iv | 94.85 (7) |
O7—Sm1—O9i | 137.59 (7) | O6—Sm2—O4iv | 72.80 (7) |
O1—Sm1—O9i | 126.61 (7) | O2ii—Sm2—O4iv | 136.27 (6) |
O14i—Sm1—O9i | 74.14 (6) | O9—Sm2—O4iv | 147.27 (6) |
O4—Sm1—O9i | 67.99 (6) | O11iii—Sm2—O4iv | 75.08 (6) |
O16—Sm1—O9i | 132.60 (7) | O12—Sm2—O4iv | 104.89 (7) |
O15—Sm1—O9i | 65.99 (8) | O8—Sm2—O4iv | 122.04 (6) |
O10i—Sm1—O9i | 49.90 (6) | O11—Sm2—O4iv | 82.14 (6) |
O3—Sm1—O9i | 106.72 (6) | O5iv—Sm2—O4iv | 50.56 (6) |
Symmetry codes: (i) x−1, y, z; (ii) x+1/2, −y+3/2, z+1/2; (iii) −x+2, −y+2, −z+2; (iv) −x+1, −y+2, −z+2. |
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