Unprecedented three-dimensional hydrogen-bonded hex topological chiral lanthanide–organic frameworks built from an achiral ligand

Qin, T.; Feng, Z.; Yang, J.; Shen, X.; Zhu, D.

doi:10.1107/S205322961801313X

Unprecedented three-dimensional hydrogen-bonded hex topological chiral lanthanide–organic frameworks built from an achiral ligand

T. Qin, Z. Feng, J. Yang, X. Shen and D. Zhu

The design and preparation of chiral metal–organic frameworks (CMOFs) from achiral ligands are a big challenge. Using 3-nitro-4-(pyridin-4-yl)benzoic acid (HL) as a new linker, a total of eight chiral lanthanide–organic frameworks (LOFs), namely poly[diaquatris[μ₂-3-nitro-4-(pyridin-4-yl)benzoato-κ²O:O′]lanthanide(III)], L- and D-[Ln(C₁₂H₇N₂O₄)₃(H₂O)₂]_n [(1), Ln = Eu; (2), Ln = Gd; (3), Ln = Dy; (4), Ln = Tb], were hydrothermally synthesized without chiral reagents and determined by X-ray crystallography. Crystal structure analyses show that L-(1)–(4) crystallize in the hexagonal P6₅ space group and are isomorphous and isostructural, while the enantiomers D-(1)–(4) crystallize in the hexagonal P6₁ space group. All Ln^III ions are octacoordinated by six carboxyl O atoms of six 3-nitro-4-(pyridin-4-yl)benzoate ligands and two water molecules in a dodecahedral geometry. A one-dimensional neutral helical [Ln₂(CO₂)₃]_n chain is observed in (1)–(4) as a chiral origin. These helical chains are further interconnected via directional hydrogen-bonding interactions between pyridyl groups and water molecules to construct a three-dimensional (3D) homochiral network with hex topology. The present CMOF structure is the first chiral 3D hydrogen-bonded hex-net and shows good water stability. Solid-state circular dichroism (CD) signals revealed that (1)–(4) crystallized through spontaneous resolution. Furthermore, (1) and (4) display a strong red and green photoluminescence at room temperature, respectively, but their intensities reduce to almost half at 200 °C. Notably, upon excitation under visible light (463 nm), a circularly polarized luminescence (CPL) of (1) in the solid state is observed for the first time, with a g_lum value of 2.61 × 10⁻².

Keywords: hex topology; chiral lanthanide–organic frameworks; crystal structure; hydrogen-bonding-induced spontaneous resolution; circular dichroism; circularly polarized luminescence; CMOF.

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Supporting information

	Crystallographic Information File (CIF) https://doi.org/10.1107/S205322961801313X/lf3080sup1.cif Contains datablocks 1502111, 1502112, 1502113, 1502114, 1502115, 1502116, 1502117, 1502118, global
	Structure factor file (CIF format) https://doi.org/10.1107/S205322961801313X/lf30801502111sup2.hkl Contains datablock 1502111
	Structure factor file (CIF format) https://doi.org/10.1107/S205322961801313X/lf30801502112sup3.hkl Contains datablock 1502112
	Structure factor file (CIF format) https://doi.org/10.1107/S205322961801313X/lf30801502113sup4.hkl Contains datablock 1502113
	Structure factor file (CIF format) https://doi.org/10.1107/S205322961801313X/lf30801502114sup5.hkl Contains datablock 1502114
	Structure factor file (CIF format) https://doi.org/10.1107/S205322961801313X/lf30801502115sup6.hkl Contains datablock 1502115
	Structure factor file (CIF format) https://doi.org/10.1107/S205322961801313X/lf30801502116sup7.hkl Contains datablock 1502116
	Structure factor file (CIF format) https://doi.org/10.1107/S205322961801313X/lf30801502117sup8.hkl Contains datablock 1502117
	Structure factor file (CIF format) https://doi.org/10.1107/S205322961801313X/lf30801502118sup9.hkl Contains datablock 1502118
	Portable Document Format (PDF) file https://doi.org/10.1107/S205322961801313X/lf3080sup10.pdf Additional scheme, spectra, figures and tables

CCDC references: 1502118; 1502117; 1502116; 1502115; 1502114; 1502113; 1502112; 1502111

Computing details top

For all structures, data collection: APEX2 (Bruker, 2005); cell refinement: SAINT (Bruker, 2005); data reduction: SAINT (Bruker, 2005); program(s) used to solve structure: SHELXS97 (Sheldrick, 2008); program(s) used to refine structure: SHELXL97 (Sheldrick, 2008); molecular graphics: SHELXTL (Sheldrick, 2008); software used to prepare material for publication: SHELXTL (Sheldrick, 2008).

Poly[diaquatris[µ₂-3-nitro-4-(pyridin-4-yl)benzoato-κ²O:O']europium(III)] (1502111) top

Crystal data top

[Eu(C₁₂H₇N₂O₄)₃(H₂O)₂]	D_x = 1.648 Mg m⁻³
M_r = 917.58	Mo Kα radiation, λ = 0.71073 Å
Hexagonal, P6₅	Cell parameters from 9989 reflections
Hall symbol: P 65	θ = 2.7–27.0°
a = 15.1172 (10) Å	µ = 1.77 mm⁻¹
c = 28.034 (4) Å	T = 296 K
V = 5548.3 (9) Å³	Rodlike, colorless
Z = 6	0.18 × 0.14 × 0.12 mm
F(000) = 2748

Data collection top

Bruker APEXII CCD diffractometer	6971 independent reflections
Radiation source: fine-focus sealed tube	6247 reflections with I > 2σ(I)
Graphite monochromator	R_int = 0.052
ω scans	θ_max = 26.0°, θ_min = 1.6°
Absorption correction: multi-scan (SADABS; Sheldrick, 2003)	h = −18→18
T_min = 0.742, T_max = 0.808	k = −17→18
41150 measured reflections	l = −34→32

Refinement top

Refinement on F²	Secondary atom site location: difference Fourier map
Least-squares matrix: full	Hydrogen site location: inferred from neighbouring sites
R[F² > 2σ(F²)] = 0.034	H atoms treated by a mixture of independent and constrained refinement
wR(F²) = 0.085	w = 1/[σ²(F_o²) + (0.0473P)² + 1.6277P] where P = (F_o² + 2F_c²)/3
S = 1.06	(Δ/σ)_max = 0.004
6971 reflections	Δρ_max = 0.71 e Å⁻³
585 parameters	Δρ_min = −0.49 e Å⁻³
161 restraints	Absolute structure: Flack (1983), 3261 Friedel pairs
Primary atom site location: structure-invariant direct methods	Absolute structure parameter: −0.008 (14)

Special details top

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

Refinement. 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 > 2sigma(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.

Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å²) top

	x	y	z	U_iso*/U_eq	Occ. (<1)
Eu1	0.932658 (6)	−0.024569 (7)	−0.119546 (7)	0.03134 (2)
O1W	0.76673 (12)	−0.08428 (13)	−0.15811 (8)	0.0829 (7)
H1WA	0.7669 (6)	−0.0309 (3)	−0.1686 (4)	0.100*
H1WB	0.7226 (4)	−0.1108 (7)	−0.1357 (2)	0.100*
O1	1.16382 (17)	0.3560 (2)	−0.20627 (8)	0.1029 (11)
O2W	0.82400 (15)	0.04452 (17)	−0.08281 (8)	0.0942 (9)
H2WA	0.8412 (6)	0.0561 (7)	−0.05352 (15)	0.113*
H2WB	0.7614 (3)	0.0034 (6)	−0.0873 (4)	0.113*
O2	1.32331 (17)	0.45243 (19)	−0.21108 (8)	0.0974 (10)
O3	1.02274 (13)	0.12206 (11)	−0.07384 (6)	0.0553 (6)
O4	1.10653 (11)	0.16071 (12)	−0.00594 (6)	0.0532 (5)
O5	1.2877 (4)	−0.2515 (4)	−0.1196 (3)	0.0687 (18)	0.280 (2)
O6	1.3190 (4)	−0.1000 (4)	−0.1343 (2)	0.0526 (18)	0.280 (2)
O5A	1.3214 (2)	−0.1765 (3)	−0.14493 (13)	0.1102 (12)	0.720 (2)
O6A	1.3121 (3)	−0.0524 (4)	−0.15502 (18)	0.1757 (19)	0.720 (2)
O7	1.02527 (11)	−0.06951 (12)	−0.06835 (6)	0.0519 (5)
O8	1.04109 (11)	−0.05522 (11)	0.01056 (7)	0.0538 (5)
O9	0.81170 (11)	−0.16239 (11)	−0.06869 (5)	0.0498 (5)
O10	0.84145 (11)	−0.07061 (10)	−0.00242 (6)	0.0453 (5)
O11	0.6407 (2)	−0.53055 (19)	−0.05160 (13)	0.1364 (14)
O12	0.5476 (2)	−0.60708 (17)	0.00504 (14)	0.1423 (13)
N1	1.59008 (18)	0.74456 (18)	−0.14855 (11)	0.0798 (10)
N2	1.24684 (16)	0.39844 (16)	−0.18877 (7)	0.0579 (8)
N4	1.2792 (6)	−0.1884 (6)	−0.1115 (4)	0.0744 (14)	0.280 (2)
N4A	1.2896 (3)	−0.1370 (4)	−0.1328 (2)	0.124 (2)	0.720 (2)
N5	0.3495 (2)	−0.6658 (2)	0.13255 (13)	0.1047 (13)
N6	0.60364 (19)	−0.53100 (17)	−0.01517 (11)	0.0816 (10)
C1	1.6026 (2)	0.6677 (2)	−0.13413 (12)	0.0750 (12)
H1A	1.6691	0.6802	−0.1310	0.090*
C2	1.52522 (18)	0.5722 (2)	−0.12358 (13)	0.0694 (10)
H2A	1.5390	0.5219	−0.1133	0.083*
C3	1.42517 (18)	0.55139 (18)	−0.12855 (10)	0.0593 (9)
C4	1.4097 (2)	0.6291 (2)	−0.14358 (13)	0.0738 (11)
H4A	1.3441	0.6185	−0.1477	0.089*
C5	1.4943 (2)	0.7235 (2)	−0.15241 (15)	0.0921 (14)
H5A	1.4830	0.7761	−0.1617	0.110*
C6	1.33872 (17)	0.45017 (16)	−0.11167 (9)	0.0508 (8)
C7	1.25286 (17)	0.38324 (17)	−0.13751 (8)	0.0469 (7)
C8	1.17586 (15)	0.29519 (15)	−0.11816 (9)	0.0437 (6)
H8A	1.1199	0.2513	−0.1367	0.052*
C9	1.18153 (16)	0.27143 (16)	−0.07055 (8)	0.0432 (7)
C10	1.26698 (19)	0.33762 (19)	−0.04489 (9)	0.0570 (9)
H10A	1.2726	0.3219	−0.0134	0.068*
C11	1.3426 (2)	0.4243 (2)	−0.06383 (11)	0.0638 (10)
H11A	1.3982	0.4677	−0.0450	0.077*
C12	1.09846 (16)	0.17843 (14)	−0.04850 (8)	0.0415 (7)
C13	1.53321 (13)	−0.18146 (17)	−0.03167 (10)	0.118 (2)	0.542 (2)
H13A	1.5487	−0.2271	−0.0168	0.141*	0.542 (2)
C14	1.43497 (14)	−0.19612 (19)	−0.02874 (11)	0.0687 (14)	0.542 (2)
H14A	1.3847	−0.2516	−0.0119	0.082*	0.542 (2)
C15	1.41186 (17)	−0.1279 (2)	−0.05093 (12)	0.0621 (13)	0.542 (2)
C16	1.4870 (2)	−0.0451 (2)	−0.07605 (14)	0.0756 (17)	0.542 (2)
H16A	1.4715	0.0006	−0.0909	0.091*	0.542 (2)
C17	1.5852 (2)	−0.0304 (2)	−0.07898 (14)	0.081 (2)	0.542 (2)
H17A	1.6355	0.0250	−0.0958	0.097*	0.542 (2)
N3	1.60833 (15)	−0.09860 (19)	−0.05679 (11)	0.0935 (19)	0.542 (2)
C13A	1.4119 (3)	−0.3178 (4)	0.0005 (2)	0.220 (4)	0.458 (2)
H13B	1.3955	−0.3773	0.0171	0.264*	0.458 (2)
C14A	1.3410 (4)	−0.2853 (5)	−0.0033 (3)	0.167 (4)	0.458 (2)
H14B	1.2771	−0.3230	0.0109	0.200*	0.458 (2)
C15A	1.3656 (6)	−0.1963 (6)	−0.0281 (3)	0.119 (3)	0.458 (2)
C16A	1.4611 (7)	−0.1399 (5)	−0.0492 (3)	0.142 (3)	0.458 (2)
H16B	1.4776	−0.0804	−0.0659	0.171*	0.458 (2)
C17A	1.5321 (5)	−0.1725 (5)	−0.0455 (3)	0.1476 (18)	0.458 (2)
H17B	1.5960	−0.1348	−0.0596	0.177*	0.458 (2)
N3A	1.5075 (4)	−0.2614 (5)	−0.0206 (2)	0.162 (4)	0.458 (2)
C18	1.30429 (18)	−0.1440 (2)	−0.04119 (14)	0.0944 (10)
C19	1.26147 (19)	−0.1261 (2)	−0.07948 (12)	0.0859 (10)
C20	1.18536 (16)	−0.1051 (2)	−0.07567 (10)	0.0603 (8)
H20A	1.1597	−0.0915	−0.1031	0.072*
C21	1.14433 (14)	−0.10332 (15)	−0.03192 (8)	0.0382 (6)
C22	1.18003 (17)	−0.12712 (17)	0.00911 (10)	0.0567 (8)
H22A	1.1517	−0.1285	0.0387	0.068*
C23	1.2584 (2)	−0.1487 (2)	0.00494 (15)	0.0945 (11)
H23A	1.2820	−0.1665	0.0319	0.113*
C24	1.06310 (14)	−0.07403 (14)	−0.02981 (8)	0.0367 (6)
C25	0.3308 (4)	−0.6232 (3)	0.09850 (18)	0.134 (2)
H25A	0.2635	−0.6424	0.0914	0.161*
C26	0.4079 (3)	−0.5493 (3)	0.07193 (14)	0.1161 (18)
H26A	0.3901	−0.5190	0.0478	0.139*
C27	0.5063 (2)	−0.5173 (2)	0.07796 (14)	0.0839 (12)
C28	0.5261 (4)	−0.5596 (4)	0.1137 (2)	0.172 (2)
H28A	0.5931	−0.5403	0.1215	0.207*
C29	0.4402 (4)	−0.6384 (4)	0.1417 (3)	0.171 (2)
H29A	0.4544	−0.6688	0.1671	0.205*
C30	0.5902 (2)	−0.42723 (19)	0.05158 (13)	0.0716 (10)
C31	0.6234 (2)	−0.3310 (2)	0.06961 (11)	0.0688 (10)
H31A	0.5982	−0.3255	0.0990	0.083*
C32	0.69165 (16)	−0.24275 (17)	0.04674 (10)	0.0537 (8)
H32A	0.7124	−0.1796	0.0608	0.064*
C33	0.72976 (14)	−0.24869 (15)	0.00205 (8)	0.0384 (6)
C34	0.69942 (16)	−0.34420 (16)	−0.01643 (9)	0.0455 (7)
H34A	0.7249	−0.3497	−0.0458	0.055*
C35	0.6326 (2)	−0.43080 (18)	0.00760 (12)	0.0618 (9)
C36	0.80057 (14)	−0.15317 (15)	−0.02513 (9)	0.0415 (6)

Atomic displacement parameters (Å²) top

	U¹¹	U²²	U³³	U¹²	U¹³	U²³
Eu1	0.03049 (3)	0.03462 (3)	0.02463 (4)	0.01307 (3)	−0.00029 (4)	0.00281 (4)
O1W	0.0443 (8)	0.0737 (9)	0.1192 (15)	0.0208 (7)	−0.0037 (9)	0.0446 (10)
O1	0.0822 (13)	0.1248 (17)	0.0524 (12)	0.0149 (11)	−0.0094 (11)	0.0174 (12)
O2W	0.1045 (12)	0.1069 (12)	0.0816 (15)	0.0608 (9)	0.0120 (12)	0.0041 (12)
O2	0.0828 (13)	0.1103 (15)	0.0513 (12)	0.0124 (12)	0.0154 (11)	0.0302 (11)
O3	0.0798 (9)	0.0357 (7)	0.0380 (9)	0.0195 (6)	0.0107 (7)	−0.0019 (6)
O4	0.0542 (7)	0.0658 (8)	0.0418 (9)	0.0317 (6)	0.0121 (7)	0.0170 (7)
O5	0.070 (2)	0.086 (2)	0.072 (3)	0.0554 (15)	−0.011 (3)	−0.022 (3)
O6	0.050 (2)	0.046 (2)	0.058 (3)	0.0214 (16)	−0.005 (2)	0.008 (2)
O5A	0.1046 (14)	0.1641 (19)	0.089 (2)	0.0875 (12)	0.0037 (14)	−0.0539 (15)
O6A	0.233 (2)	0.228 (3)	0.121 (3)	0.1557 (19)	0.094 (2)	0.015 (2)
O7	0.0589 (6)	0.0684 (7)	0.0410 (9)	0.0414 (5)	−0.0060 (7)	0.0048 (7)
O8	0.0786 (6)	0.0769 (6)	0.0353 (9)	0.0610 (4)	0.0050 (6)	−0.0024 (6)
O9	0.0575 (7)	0.0541 (7)	0.0271 (7)	0.0199 (6)	0.0084 (7)	0.0068 (6)
O10	0.0415 (7)	0.0354 (6)	0.0454 (9)	0.0092 (5)	−0.0024 (7)	0.0049 (6)
O11	0.198 (2)	0.0828 (13)	0.123 (2)	0.0658 (13)	−0.012 (2)	−0.0329 (14)
O12	0.167 (2)	0.0544 (11)	0.183 (3)	0.0381 (11)	0.0547 (19)	0.0026 (15)
N1	0.0568 (12)	0.0570 (13)	0.098 (2)	0.0077 (10)	0.0083 (13)	0.0121 (13)
N2	0.0624 (11)	0.0565 (10)	0.0364 (11)	0.0159 (8)	0.0031 (9)	0.0121 (9)
N4	0.0738 (18)	0.0748 (18)	0.074 (2)	0.0365 (12)	−0.0019 (16)	−0.0026 (16)
N4A	0.092 (2)	0.121 (3)	0.152 (4)	0.0469 (19)	0.061 (2)	−0.001 (3)
N5	0.1114 (18)	0.0785 (13)	0.118 (2)	0.0426 (12)	0.0326 (18)	0.0358 (17)
N6	0.0824 (13)	0.0537 (11)	0.105 (2)	0.0310 (9)	−0.0031 (14)	0.0045 (13)
C1	0.0416 (12)	0.0762 (17)	0.082 (2)	0.0108 (12)	−0.0040 (13)	0.0006 (16)
C2	0.0522 (11)	0.0602 (13)	0.087 (2)	0.0213 (9)	−0.0078 (15)	0.0138 (14)
C3	0.0454 (11)	0.0480 (12)	0.0607 (17)	0.0056 (9)	−0.0022 (12)	0.0108 (12)
C4	0.0491 (12)	0.0625 (13)	0.107 (3)	0.0260 (9)	0.0047 (14)	0.0195 (14)
C5	0.0630 (15)	0.0615 (15)	0.141 (3)	0.0230 (12)	0.0220 (18)	0.0354 (18)
C6	0.0520 (11)	0.0396 (10)	0.0465 (14)	0.0122 (8)	−0.0030 (11)	−0.0012 (10)
C7	0.0534 (10)	0.0465 (10)	0.0352 (11)	0.0209 (8)	0.0024 (9)	0.0097 (9)
C8	0.0479 (9)	0.0411 (9)	0.0329 (10)	0.0152 (7)	−0.0006 (11)	0.0006 (10)
C9	0.0502 (10)	0.0391 (9)	0.0330 (11)	0.0168 (7)	0.0080 (9)	0.0018 (9)
C10	0.0673 (13)	0.0608 (12)	0.0294 (12)	0.0218 (10)	−0.0043 (11)	0.0031 (10)
C11	0.0588 (13)	0.0530 (13)	0.0536 (15)	0.0084 (11)	−0.0166 (12)	−0.0020 (12)
C12	0.0566 (10)	0.0340 (8)	0.0351 (11)	0.0237 (7)	0.0058 (9)	0.0027 (8)
C13	0.112 (3)	0.137 (3)	0.117 (4)	0.072 (2)	−0.011 (3)	−0.007 (3)
C14	0.0551 (14)	0.0898 (18)	0.094 (3)	0.0610 (11)	−0.0026 (19)	0.006 (2)
C15	0.0442 (14)	0.093 (2)	0.068 (3)	0.0486 (12)	0.0100 (16)	−0.0199 (18)
C16	0.0493 (17)	0.114 (3)	0.076 (3)	0.0502 (15)	−0.008 (2)	−0.041 (2)
C17	0.051 (2)	0.099 (3)	0.089 (4)	0.036 (2)	−0.001 (3)	−0.027 (3)
N3	0.089 (2)	0.100 (2)	0.098 (4)	0.0528 (18)	−0.004 (3)	−0.036 (2)
C13A	0.221 (5)	0.224 (5)	0.207 (5)	0.106 (3)	−0.016 (4)	−0.011 (4)
C14A	0.161 (5)	0.181 (5)	0.201 (8)	0.118 (3)	−0.012 (6)	−0.072 (5)
C15A	0.123 (3)	0.128 (4)	0.122 (4)	0.076 (2)	−0.015 (3)	−0.032 (3)
C16A	0.127 (3)	0.194 (5)	0.144 (7)	0.110 (3)	0.006 (4)	−0.041 (5)
C17A	0.144 (2)	0.153 (2)	0.149 (3)	0.0765 (14)	0.002 (2)	−0.005 (2)
N3A	0.177 (5)	0.192 (6)	0.134 (6)	0.104 (4)	−0.053 (5)	−0.023 (5)
C18	0.0735 (10)	0.1351 (14)	0.108 (2)	0.0773 (8)	−0.0307 (14)	−0.0658 (14)
C19	0.0523 (11)	0.1267 (16)	0.0858 (18)	0.0501 (10)	−0.0080 (12)	−0.0525 (14)
C20	0.0456 (9)	0.0876 (13)	0.0513 (15)	0.0360 (8)	−0.0018 (10)	−0.0193 (12)
C21	0.0361 (7)	0.0467 (9)	0.0352 (11)	0.0232 (6)	−0.0011 (8)	−0.0032 (8)
C22	0.0645 (10)	0.0674 (10)	0.0564 (15)	0.0467 (7)	−0.0106 (11)	−0.0030 (11)
C23	0.0932 (11)	0.1165 (14)	0.117 (2)	0.0849 (8)	−0.0458 (14)	−0.0309 (15)
C24	0.0430 (8)	0.0379 (8)	0.0350 (11)	0.0244 (6)	−0.0028 (8)	0.0001 (8)
C25	0.099 (3)	0.103 (3)	0.132 (4)	−0.001 (2)	0.019 (3)	0.036 (3)
C26	0.082 (2)	0.102 (3)	0.085 (2)	−0.013 (2)	0.0329 (19)	0.021 (2)
C27	0.0829 (17)	0.0589 (13)	0.100 (2)	0.0280 (12)	0.0264 (17)	0.0336 (15)
C28	0.115 (3)	0.184 (3)	0.191 (4)	0.055 (2)	0.050 (3)	0.130 (3)
C29	0.164 (3)	0.167 (3)	0.170 (4)	0.074 (2)	−0.003 (3)	0.054 (3)
C30	0.0690 (13)	0.0476 (11)	0.0836 (19)	0.0182 (9)	0.0265 (15)	0.0268 (14)
C31	0.0649 (14)	0.0700 (15)	0.0568 (16)	0.0227 (11)	0.0248 (13)	0.0143 (13)
C32	0.0519 (10)	0.0441 (10)	0.0532 (13)	0.0150 (8)	0.0160 (12)	0.0120 (12)
C33	0.0309 (8)	0.0353 (8)	0.0451 (12)	0.0137 (6)	0.0002 (8)	0.0095 (8)
C34	0.0474 (10)	0.0425 (9)	0.0468 (14)	0.0228 (7)	0.0016 (9)	0.0049 (9)
C35	0.0615 (13)	0.0372 (10)	0.0785 (19)	0.0187 (9)	−0.0035 (13)	0.0106 (12)
C36	0.0347 (8)	0.0444 (9)	0.0452 (12)	0.0198 (6)	0.0028 (8)	0.0096 (9)

Geometric parameters (Å, º) top

Eu1—O3	2.3218 (15)	C9—C12	1.473 (3)
Eu1—O7	2.3308 (19)	C10—C11	1.344 (3)
Eu1—O10ⁱ	2.3447 (14)	C10—H10A	0.9300
Eu1—O8ⁱ	2.3876 (19)	C11—H11A	0.9300
Eu1—O4ⁱ	2.4053 (15)	C13—C14	1.3900
Eu1—O9	2.4305 (14)	C13—N3	1.3900
Eu1—O1W	2.4518 (19)	C13—H13A	0.9300
Eu1—O2W	2.562 (3)	C14—C15	1.3900
Eu1—H1WA	2.817 (9)	C14—H14A	0.9300
Eu1—H1WB	2.802 (6)	C15—C16	1.3900
O1W—H1WA	0.857 (6)	C15—C18	1.544 (4)
O1W—H1WB	0.857 (5)	C16—C17	1.3900
O1—N2	1.193 (3)	C16—H16A	0.9300
O2W—H2WA	0.853 (5)	C17—N3	1.3900
O2W—H2WB	0.843 (4)	C17—H17A	0.9300
O2—N2	1.204 (3)	C13A—C14A	1.3900
O3—C12	1.251 (2)	C13A—N3A	1.3900
O4—C12	1.242 (3)	C13A—H13B	0.9300
O4—Eu1ⁱⁱ	2.4053 (15)	C14A—C15A	1.3900
O5—N4	1.049 (13)	C14A—H14B	0.9300
O6—N4	1.324 (11)	C15A—C16A	1.3900
O6—C19	1.713 (7)	C15A—C18	1.534 (7)
O5A—N4A	0.995 (7)	C16A—C17A	1.3900
O6A—N4A	1.304 (8)	C16A—H16B	0.9300
O7—C24	1.240 (3)	C17A—N3A	1.3900
O8—C24	1.252 (3)	C17A—H17B	0.9300
O8—Eu1ⁱⁱ	2.3876 (19)	C18—C19	1.349 (5)
O9—C36	1.250 (3)	C18—C23	1.452 (5)
O10—C36	1.254 (3)	C19—C20	1.342 (5)
O10—Eu1ⁱⁱ	2.3446 (14)	C20—C21	1.381 (4)
O11—N6	1.163 (5)	C20—H20A	0.9300
O12—N6	1.178 (4)	C21—C22	1.392 (4)
N1—C5	1.322 (4)	C21—C24	1.501 (3)
N1—C1	1.329 (5)	C22—C23	1.383 (5)
N2—C7	1.465 (3)	C22—H22A	0.9300
N4—C19	1.422 (11)	C23—H23A	0.9300
N4A—C19	1.586 (7)	C25—C26	1.363 (5)
N5—C29	1.245 (7)	C25—H25A	0.9300
N5—C25	1.259 (6)	C26—C27	1.325 (5)
N6—C35	1.493 (4)	C26—H26A	0.9300
C1—C2	1.361 (3)	C27—C28	1.302 (7)
C1—H1A	0.9300	C27—C30	1.511 (4)
C2—C3	1.389 (4)	C28—C29	1.473 (7)
C2—H2A	0.9300	C28—H28A	0.9300
C3—C4	1.373 (5)	C29—H29A	0.9300
C3—C6	1.508 (3)	C30—C31	1.376 (4)
C4—C5	1.381 (4)	C30—C35	1.403 (5)
C4—H4A	0.9300	C31—C32	1.371 (3)
C5—H5A	0.9300	C31—H31A	0.9300
C6—C7	1.386 (3)	C32—C33	1.400 (4)
C6—C11	1.406 (4)	C32—H32A	0.9300
C7—C8	1.368 (3)	C33—C34	1.379 (3)
C8—C9	1.396 (3)	C33—C36	1.505 (3)
C8—H8A	0.9300	C34—C35	1.366 (3)
C9—C10	1.377 (3)	C34—H34A	0.9300

O3—Eu1—O7	77.73 (6)	C6—C11—H11A	119.5
O3—Eu1—O10ⁱ	155.89 (7)	O4—C12—O3	123.61 (17)
O7—Eu1—O10ⁱ	87.28 (6)	O4—C12—C9	118.69 (18)
O3—Eu1—O8ⁱ	81.30 (6)	O3—C12—C9	117.7 (2)
O7—Eu1—O8ⁱ	74.75 (6)	C14—C13—N3	120.0
O10ⁱ—Eu1—O8ⁱ	76.55 (6)	C14—C13—H13A	120.0
O3—Eu1—O4ⁱ	77.72 (6)	N3—C13—H13A	120.0
O7—Eu1—O4ⁱ	143.77 (6)	C13—C14—C15	120.0
O10ⁱ—Eu1—O4ⁱ	105.42 (5)	C13—C14—H14A	120.0
O8ⁱ—Eu1—O4ⁱ	75.54 (6)	C15—C14—H14A	120.0
O3—Eu1—O9	108.99 (5)	C16—C15—C14	120.0
O7—Eu1—O9	72.12 (5)	C16—C15—C18	123.57 (19)
O10ⁱ—Eu1—O9	83.62 (6)	C14—C15—C18	116.1 (2)
O8ⁱ—Eu1—O9	141.93 (6)	C15—C16—C17	120.0
O4ⁱ—Eu1—O9	141.80 (7)	C15—C16—H16A	120.0
O3—Eu1—O1W	126.76 (7)	C17—C16—H16A	120.0
O7—Eu1—O1W	144.81 (5)	N3—C17—C16	120.0
O10ⁱ—Eu1—O1W	75.60 (7)	N3—C17—H17A	120.0
O8ⁱ—Eu1—O1W	128.35 (7)	C16—C17—H17A	120.0
O4ⁱ—Eu1—O1W	71.25 (7)	C17—N3—C13	120.0
O9—Eu1—O1W	75.55 (6)	C14A—C13A—N3A	120.0
O3—Eu1—O2W	65.08 (7)	C14A—C13A—H13B	120.0
O7—Eu1—O2W	118.18 (7)	N3A—C13A—H13B	120.0
O10ⁱ—Eu1—O2W	139.01 (6)	C13A—C14A—C15A	120.0
O8ⁱ—Eu1—O2W	138.18 (5)	C13A—C14A—H14B	120.0
O4ⁱ—Eu1—O2W	73.65 (7)	C15A—C14A—H14B	120.0
O9—Eu1—O2W	75.69 (7)	C14A—C15A—C16A	120.0
O1W—Eu1—O2W	65.22 (7)	C14A—C15A—C18	132.9 (5)
O3—Eu1—H1WA	112.89 (15)	C16A—C15A—C18	107.0 (5)
O7—Eu1—H1WA	160.76 (13)	C15A—C16A—C17A	120.0
O10ⁱ—Eu1—H1WA	87.13 (17)	C15A—C16A—H16B	120.0
O8ⁱ—Eu1—H1WA	121.6 (2)	C17A—C16A—H16B	120.0
O4ⁱ—Eu1—H1WA	55.40 (12)	N3A—C17A—C16A	120.0
O9—Eu1—H1WA	88.96 (15)	N3A—C17A—H17B	120.0
O1W—Eu1—H1WA	16.96 (9)	C16A—C17A—H17B	120.0
O2W—Eu1—H1WA	58.0 (2)	C17A—N3A—C13A	120.0
O3—Eu1—H1WB	121.4 (2)	C19—C18—C23	117.0 (3)
O7—Eu1—H1WB	132.08 (17)	C19—C18—C15A	140.2 (5)
O10ⁱ—Eu1—H1WB	82.7 (2)	C23—C18—C15A	99.1 (4)
O8ⁱ—Eu1—H1WB	145.28 (13)	C19—C18—C15	113.7 (3)
O4ⁱ—Eu1—H1WB	83.75 (19)	C23—C18—C15	127.2 (3)
O9—Eu1—H1WB	60.26 (16)	C15A—C18—C15	42.5 (3)
O1W—Eu1—H1WB	17.15 (12)	C20—C19—C18	122.6 (3)
O2W—Eu1—H1WB	56.4 (2)	C20—C19—N4	132.4 (5)
H1WA—Eu1—H1WB	28.8 (2)	C18—C19—N4	95.9 (5)
Eu1—O1W—H1WA	106.4 (5)	C20—C19—N4A	113.9 (3)
Eu1—O1W—H1WB	105.3 (5)	C18—C19—N4A	123.3 (4)
H1WA—O1W—H1WB	109.1 (10)	N4—C19—N4A	35.5 (5)
Eu1—O2W—H2WA	106.2 (8)	C20—C19—O6	114.5 (4)
Eu1—O2W—H2WB	110.6 (7)	C18—C19—O6	121.4 (3)
H2WA—O2W—H2WB	114.1 (8)	N4—C19—O6	48.9 (4)
C12—O3—Eu1	149.73 (19)	N4A—C19—O6	17.3 (2)
C12—O4—Eu1ⁱⁱ	128.35 (12)	C19—C20—C21	121.5 (3)
N4—O6—C19	54.0 (5)	C19—C20—H20A	119.3
C24—O7—Eu1	155.95 (18)	C21—C20—H20A	119.3
C24—O8—Eu1ⁱⁱ	140.28 (17)	C20—C21—C22	119.5 (2)
C36—O9—Eu1	124.27 (12)	C20—C21—C24	118.9 (2)
C36—O10—Eu1ⁱⁱ	147.53 (17)	C22—C21—C24	121.6 (2)
C5—N1—C1	115.5 (2)	C23—C22—C21	118.7 (3)
O1—N2—O2	123.1 (2)	C23—C22—H22A	120.7
O1—N2—C7	116.7 (2)	C21—C22—H22A	120.7
O2—N2—C7	120.1 (2)	C22—C23—C18	120.5 (3)
O5—N4—O6	127.9 (10)	C22—C23—H23A	119.7
O5—N4—C19	152.7 (10)	C18—C23—H23A	119.7
O6—N4—C19	77.1 (6)	O7—C24—O8	126.4 (2)
O5A—N4A—O6A	117.3 (6)	O7—C24—C21	116.7 (2)
O5A—N4A—C19	128.2 (6)	O8—C24—C21	116.9 (2)
O6A—N4A—C19	107.5 (5)	N5—C25—C26	121.0 (5)
C29—N5—C25	118.5 (4)	N5—C25—H25A	119.5
O11—N6—O12	122.5 (3)	C26—C25—H25A	119.5
O11—N6—C35	118.2 (2)	C27—C26—C25	124.9 (5)
O12—N6—C35	119.2 (3)	C27—C26—H26A	117.5
N1—C1—C2	124.8 (3)	C25—C26—H26A	117.5
N1—C1—H1A	117.6	C28—C27—C26	114.3 (4)
C2—C1—H1A	117.6	C28—C27—C30	121.6 (3)
C1—C2—C3	118.6 (3)	C26—C27—C30	123.3 (4)
C1—C2—H2A	120.7	C27—C28—C29	118.7 (5)
C3—C2—H2A	120.7	C27—C28—H28A	120.6
C4—C3—C2	117.9 (2)	C29—C28—H28A	120.6
C4—C3—C6	122.2 (3)	N5—C29—C28	122.6 (6)
C2—C3—C6	119.4 (3)	N5—C29—H29A	118.7
C3—C4—C5	118.2 (3)	C28—C29—H29A	118.7
C3—C4—H4A	120.9	C31—C30—C35	115.5 (2)
C5—C4—H4A	120.9	C31—C30—C27	118.1 (3)
N1—C5—C4	124.8 (4)	C35—C30—C27	126.1 (3)
N1—C5—H5A	117.6	C32—C31—C30	123.8 (3)
C4—C5—H5A	117.6	C32—C31—H31A	118.1
C7—C6—C11	116.69 (19)	C30—C31—H31A	118.1
C7—C6—C3	126.7 (2)	C31—C32—C33	119.3 (2)
C11—C6—C3	116.5 (2)	C31—C32—H32A	120.3
C8—C7—C6	122.3 (2)	C33—C32—H32A	120.3
C8—C7—N2	116.88 (19)	C34—C33—C32	118.11 (19)
C6—C7—N2	120.48 (18)	C34—C33—C36	121.3 (2)
C7—C8—C9	119.85 (19)	C32—C33—C36	120.6 (2)
C7—C8—H8A	120.1	C35—C34—C33	121.2 (2)
C9—C8—H8A	120.1	C35—C34—H34A	119.4
C10—C9—C8	117.96 (18)	C33—C34—H34A	119.4
C10—C9—C12	121.1 (2)	C34—C35—C30	122.0 (2)
C8—C9—C12	120.93 (18)	C34—C35—N6	117.6 (3)
C11—C10—C9	122.2 (2)	C30—C35—N6	120.4 (2)
C11—C10—H10A	118.9	O9—C36—O10	125.44 (18)
C9—C10—H10A	118.9	O9—C36—C33	117.29 (18)
C10—C11—C6	121.0 (2)	O10—C36—C33	117.2 (2)
C10—C11—H11A	119.5

O7—Eu1—O3—C12	25.2 (3)	C23—C18—C19—C20	5.4 (4)
O10ⁱ—Eu1—O3—C12	−27.6 (4)	C15A—C18—C19—C20	157.9 (5)
O8ⁱ—Eu1—O3—C12	−51.0 (3)	C15—C18—C19—C20	−159.1 (3)
O4ⁱ—Eu1—O3—C12	−128.0 (3)	C23—C18—C19—N4	−145.1 (4)
O9—Eu1—O3—C12	91.2 (3)	C15A—C18—C19—N4	7.4 (7)
O1W—Eu1—O3—C12	177.0 (3)	C15—C18—C19—N4	50.4 (4)
O2W—Eu1—O3—C12	154.5 (3)	C23—C18—C19—N4A	−169.3 (3)
O3—Eu1—O7—C24	41.0 (3)	C15A—C18—C19—N4A	−16.8 (7)
O10ⁱ—Eu1—O7—C24	−158.0 (3)	C15—C18—C19—N4A	26.2 (4)
O8ⁱ—Eu1—O7—C24	125.2 (3)	C23—C18—C19—O6	170.3 (3)
O4ⁱ—Eu1—O7—C24	89.3 (3)	C15A—C18—C19—O6	−37.2 (7)
O9—Eu1—O7—C24	−73.8 (3)	C15—C18—C19—O6	5.8 (4)
O1W—Eu1—O7—C24	−98.0 (3)	O5—N4—C19—C20	−114.8 (17)
O2W—Eu1—O7—C24	−11.7 (3)	O6—N4—C19—C20	86.9 (6)
O3—Eu1—O9—C36	0.8 (2)	O5—N4—C19—C18	31.0 (17)
O7—Eu1—O9—C36	70.5 (2)	O6—N4—C19—C18	−127.3 (4)
O10ⁱ—Eu1—O9—C36	159.7 (2)	O5—N4—C19—N4A	175 (2)
O8ⁱ—Eu1—O9—C36	101.2 (2)	O6—N4—C19—N4A	16.6 (4)
O4ⁱ—Eu1—O9—C36	−93.4 (2)	O5—N4—C19—O6	158 (2)
O1W—Eu1—O9—C36	−123.6 (2)	O5A—N4A—C19—C20	−154.2 (4)
O2W—Eu1—O9—C36	−55.9 (2)	O6A—N4A—C19—C20	56.6 (4)
C19—O6—N4—O5	−167.6 (13)	O5A—N4A—C19—C18	20.8 (6)
C5—N1—C1—C2	0.1 (5)	O6A—N4A—C19—C18	−128.4 (4)
N1—C1—C2—C3	0.8 (5)	O5A—N4A—C19—N4	−23.7 (7)
C1—C2—C3—C4	−0.5 (5)	O6A—N4A—C19—N4	−172.9 (8)
C1—C2—C3—C6	−172.9 (3)	O5A—N4A—C19—O6	110.1 (12)
C2—C3—C4—C5	−0.6 (5)	O6A—N4A—C19—O6	−39.1 (10)
C6—C3—C4—C5	171.6 (3)	N4—O6—C19—C20	−125.9 (6)
C1—N1—C5—C4	−1.4 (6)	N4—O6—C19—C18	68.0 (6)
C3—C4—C5—N1	1.7 (6)	N4—O6—C19—N4A	−33.8 (11)
C4—C3—C6—C7	58.8 (4)	C18—C19—C20—C21	−1.7 (4)
C2—C3—C6—C7	−129.1 (3)	N4—C19—C20—C21	136.7 (6)
C4—C3—C6—C11	−116.8 (3)	N4A—C19—C20—C21	173.4 (3)
C2—C3—C6—C11	55.3 (4)	O6—C19—C20—C21	−167.6 (3)
C11—C6—C7—C8	−1.1 (4)	C19—C20—C21—C22	−2.2 (3)
C3—C6—C7—C8	−176.7 (3)	C19—C20—C21—C24	176.8 (2)
C11—C6—C7—N2	−173.8 (3)	C20—C21—C22—C23	2.1 (3)
C3—C6—C7—N2	10.6 (5)	C24—C21—C22—C23	−176.94 (19)
O1—N2—C7—C8	25.5 (4)	C21—C22—C23—C18	1.6 (4)
O2—N2—C7—C8	−155.1 (3)	C19—C18—C23—C22	−5.3 (4)
O1—N2—C7—C6	−161.4 (3)	C15A—C18—C23—C22	−167.9 (4)
O2—N2—C7—C6	17.9 (4)	C15—C18—C23—C22	156.8 (3)
C6—C7—C8—C9	1.2 (4)	Eu1—O7—C24—O8	14.6 (4)
N2—C7—C8—C9	174.2 (3)	Eu1—O7—C24—C21	−164.3 (2)
C7—C8—C9—C10	−1.4 (4)	Eu1ⁱⁱ—O8—C24—O7	−26.0 (3)
C7—C8—C9—C12	178.4 (3)	Eu1ⁱⁱ—O8—C24—C21	152.95 (14)
C8—C9—C10—C11	1.6 (5)	C20—C21—C24—O7	11.7 (2)
C12—C9—C10—C11	−178.3 (3)	C22—C21—C24—O7	−169.26 (17)
C9—C10—C11—C6	−1.6 (5)	C20—C21—C24—O8	−167.39 (17)
C7—C6—C11—C10	1.2 (5)	C22—C21—C24—O8	11.7 (3)
C3—C6—C11—C10	177.3 (3)	C29—N5—C25—C26	0.4 (8)
Eu1ⁱⁱ—O4—C12—O3	−14.8 (4)	N5—C25—C26—C27	1.7 (8)
Eu1ⁱⁱ—O4—C12—C9	164.31 (18)	C25—C26—C27—C28	−3.0 (7)
Eu1—O3—C12—O4	−79.0 (4)	C25—C26—C27—C30	−172.9 (4)
Eu1—O3—C12—C9	101.8 (3)	C26—C27—C28—C29	2.3 (7)
C10—C9—C12—O4	0.3 (4)	C30—C27—C28—C29	172.3 (5)
C8—C9—C12—O4	−179.6 (3)	C25—N5—C29—C28	−1.0 (9)
C10—C9—C12—O3	179.5 (3)	C27—C28—C29—N5	−0.4 (10)
C8—C9—C12—O3	−0.4 (4)	C28—C27—C30—C31	−85.1 (6)
N3—C13—C14—C15	0.0	C26—C27—C30—C31	84.0 (5)
C13—C14—C15—C16	0.0	C28—C27—C30—C35	100.7 (5)
C13—C14—C15—C18	−173.7 (2)	C26—C27—C30—C35	−90.2 (5)
C14—C15—C16—C17	0.0	C35—C30—C31—C32	1.4 (5)
C18—C15—C16—C17	173.2 (3)	C27—C30—C31—C32	−173.4 (3)
C15—C16—C17—N3	0.0	C30—C31—C32—C33	1.0 (5)
C16—C17—N3—C13	0.0	C31—C32—C33—C34	−2.3 (4)
C14—C13—N3—C17	0.0	C31—C32—C33—C36	176.8 (3)
N3A—C13A—C14A—C15A	0.0	C32—C33—C34—C35	1.2 (4)
C13A—C14A—C15A—C16A	0.0	C36—C33—C34—C35	−177.9 (2)
C13A—C14A—C15A—C18	175.8 (7)	C33—C34—C35—C30	1.2 (5)
C14A—C15A—C16A—C17A	0.0	C33—C34—C35—N6	179.8 (3)
C18—C15A—C16A—C17A	−176.8 (5)	C31—C30—C35—C34	−2.5 (5)
C15A—C16A—C17A—N3A	0.0	C27—C30—C35—C34	171.9 (3)
C16A—C17A—N3A—C13A	0.0	C31—C30—C35—N6	179.0 (3)
C14A—C13A—N3A—C17A	0.0	C27—C30—C35—N6	−6.6 (5)
C14A—C15A—C18—C19	−108.3 (6)	O11—N6—C35—C34	1.5 (5)
C16A—C15A—C18—C19	67.9 (6)	O12—N6—C35—C34	178.7 (3)
C14A—C15A—C18—C23	47.1 (5)	O11—N6—C35—C30	−179.9 (4)
C16A—C15A—C18—C23	−136.7 (3)	O12—N6—C35—C30	−2.7 (5)
C14A—C15A—C18—C15	−175.9 (8)	Eu1—O9—C36—O10	7.9 (4)
C16A—C15A—C18—C15	0.3 (4)	Eu1—O9—C36—C33	−174.04 (15)
C16—C15—C18—C19	44.1 (3)	Eu1ⁱⁱ—O10—C36—O9	−97.3 (3)
C14—C15—C18—C19	−142.5 (2)	Eu1ⁱⁱ—O10—C36—C33	84.6 (3)
C16—C15—C18—C23	−118.5 (3)	C34—C33—C36—O9	16.4 (4)
C14—C15—C18—C23	54.9 (4)	C32—C33—C36—O9	−162.7 (2)
C16—C15—C18—C15A	−176.2 (5)	C34—C33—C36—O10	−165.4 (2)
C14—C15—C18—C15A	−2.7 (5)	C32—C33—C36—O10	15.5 (3)

Symmetry codes: (i) x−y, x−1, z−1/6; (ii) y+1, −x+y+1, z+1/6.

Hydrogen-bond geometry (Å, º) top

D—H···A	D—H	H···A	D···A	D—H···A
O1W—H1WA···N5ⁱⁱⁱ	0.86	2.17	2.885 (4)	141
O1W—H1WB···N1^iv	0.86	2.13	2.644 (3)	118
O2W—H2WA···O1Wⁱⁱ	0.85	2.16	2.965 (3)	156
O2W—H2WB···N3^v	0.84	2.21	2.965 (4)	149
C4—H4A···O12^vi	0.93	2.54	3.448 (5)	167
C16—H16A···O2^v	0.93	2.47	3.061 (5)	121
C31—H31A···O6A^vii	0.93	2.28	3.058 (6)	141

Symmetry codes: (ii) y+1, −x+y+1, z+1/6; (iii) −y, x−y−1, z−1/3; (iv) x−1, y−1, z; (v) x−1, y, z; (vi) x−y, x, z−1/6; (vii) −x+y+2, −x+1, z+1/3.

Poly[diaquatris[µ₂-3-nitro-4-(pyridin-4-yl)benzoato-κ²O:O']europium(III)] (1502112) top

Crystal data top

[Eu(C₁₂H₇N₂O₄)₃(H₂O)₂]	D_x = 1.686 Mg m⁻³
M_r = 917.58	Mo Kα radiation, λ = 0.71073 Å
Hexagonal, P6₁	Cell parameters from 9898 reflections
Hall symbol: P 61	θ = 2.7–22.7°
a = 14.981 (9) Å	µ = 1.82 mm⁻¹
c = 27.897 (17) Å	T = 296 K
V = 5422 (6) Å³	Rodlike, colorless
Z = 6	0.18 × 0.14 × 0.11 mm
F(000) = 2748

Data collection top

Bruker APEXII CCD diffractometer	6882 independent reflections
Radiation source: fine-focus sealed tube	6066 reflections with I > 2σ(I)
Graphite monochromator	R_int = 0.054
ω scans	θ_max = 26.0°, θ_min = 1.6°
Absorption correction: multi-scan (SADABS; Sheldrick, 2003)	h = −18→18
T_min = 0.745, T_max = 0.819	k = −18→18
40512 measured reflections	l = −33→34

Refinement top

Refinement on F²	Secondary atom site location: difference Fourier map
Least-squares matrix: full	Hydrogen site location: inferred from neighbouring sites
R[F² > 2σ(F²)] = 0.043	H atoms treated by a mixture of independent and constrained refinement
wR(F²) = 0.109	w = 1/[σ²(F_o²) + (0.0632P)² + 5.468P] where P = (F_o² + 2F_c²)/3
S = 1.04	(Δ/σ)_max = 0.002
6882 reflections	Δρ_max = 1.09 e Å⁻³
585 parameters	Δρ_min = −0.62 e Å⁻³
226 restraints	Absolute structure: Flack (1983), 3257 Friedel pairs
Primary atom site location: structure-invariant direct methods	Absolute structure parameter: 0.013 (18)

Special details top

Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å²) top

	x	y	z	U_iso*/U_eq	Occ. (<1)
Eu1	0.068100 (7)	0.039417 (9)	0.061399 (9)	0.03439 (3)
O1W	0.23517 (17)	0.15975 (17)	0.03587 (11)	0.1118 (9)
H1WA	0.2464 (5)	0.2208 (3)	0.0432 (3)	0.134*
H1WB	0.2798 (3)	0.1504 (4)	0.0512 (3)	0.134*
O1	−0.15956 (18)	0.1954 (3)	−0.02690 (11)	0.1061 (12)
O2W	0.1955 (2)	0.2266 (3)	0.09662 (15)	0.2374 (17)
H2WA	0.2284 (3)	0.2196 (4)	0.1213 (2)	0.285*
H2WB	0.1615 (3)	0.2539 (3)	0.1084 (2)	0.285*
O2	−0.32124 (18)	0.1220 (2)	−0.03283 (10)	0.0982 (11)
O3	−0.01025 (11)	0.11131 (12)	0.10642 (7)	0.0441 (5)
O4	−0.09772 (14)	0.06089 (15)	0.17419 (7)	0.0556 (7)
O5	−0.3318 (6)	−0.3618 (5)	0.0303 (3)	0.162 (3)	0.638 (3)
O5A	−0.2800 (7)	−0.4163 (8)	0.0347 (4)	0.125 (4)	0.362 (3)
O6	−0.3223 (4)	−0.4994 (4)	0.03588 (18)	0.119 (2)	0.638 (3)
O6A	−0.2808 (6)	−0.5471 (5)	0.0657 (3)	0.094 (3)	0.362 (3)
O7	−0.02990 (14)	−0.09543 (14)	0.11264 (7)	0.0517 (7)
O8	−0.04203 (16)	−0.09721 (13)	0.19182 (8)	0.0554 (7)
O9	0.18790 (12)	0.01810 (14)	0.11234 (6)	0.0494 (6)
O10	0.16008 (11)	0.08849 (12)	0.17663 (7)	0.0438 (5)
O11	0.3709 (2)	−0.1695 (2)	0.13239 (14)	0.1215 (13)
O12	0.4499 (3)	−0.1602 (2)	0.19528 (19)	0.1643 (15)
N1	−0.5913 (2)	0.1452 (3)	0.02874 (18)	0.1115 (16)
N2	−0.24529 (16)	0.14989 (18)	−0.00883 (9)	0.0575 (8)
N4	−0.3132 (3)	−0.4228 (3)	0.04943 (17)	0.0679 (16)	0.638 (3)
N4A	−0.2802 (5)	−0.4660 (5)	0.0687 (3)	0.059 (2)	0.362 (3)
N5	0.6525 (2)	−0.0132 (2)	0.31720 (16)	0.1047 (14)
N6	0.40178 (19)	−0.1346 (2)	0.17049 (16)	0.0944 (13)
C1	−0.6047 (2)	0.0540 (3)	0.04667 (19)	0.0974 (17)
H1A	−0.6710	−0.0002	0.0524	0.117*
C2	−0.5239 (2)	0.0420 (2)	0.05604 (17)	0.0789 (13)
H2A	−0.5351	−0.0213	0.0672	0.095*
C3	−0.42372 (19)	0.1216 (2)	0.04952 (13)	0.0602 (10)
C4	−0.4097 (2)	0.2155 (2)	0.03331 (18)	0.0859 (15)
H4A	−0.3443	0.2727	0.0301	0.103*
C5	−0.4962 (3)	0.2202 (3)	0.0223 (2)	0.1034 (16)
H5A	−0.4869	0.2814	0.0093	0.124*
C6	−0.33795 (17)	0.10967 (19)	0.06804 (12)	0.0532 (9)
C7	−0.24966 (18)	0.13058 (19)	0.04172 (10)	0.0449 (8)
C8	−0.16983 (17)	0.12322 (17)	0.06143 (12)	0.0446 (7)
H8A	−0.1132	0.1366	0.0426	0.053*
C9	−0.17256 (19)	0.09609 (17)	0.10908 (9)	0.0408 (7)
C10	−0.2594 (2)	0.0751 (2)	0.13506 (12)	0.0563 (9)
H10A	−0.2640	0.0543	0.1668	0.068*
C11	−0.3383 (2)	0.0838 (2)	0.11609 (12)	0.0628 (10)
H11A	−0.3935	0.0723	0.1355	0.075*
C12	−0.0877 (2)	0.08733 (18)	0.13153 (10)	0.0436 (8)
N3	−0.5927 (3)	−0.7224 (3)	0.13885 (19)	0.190 (4)	0.538 (3)
C13	−0.5066 (4)	−0.7198 (4)	0.1590 (2)	0.181 (4)	0.538 (3)
H13A	−0.5136	−0.7765	0.1759	0.217*	0.538 (3)
C14	−0.4100 (3)	−0.6325 (5)	0.1539 (3)	0.157 (4)	0.538 (3)
H14A	−0.3524	−0.6307	0.1674	0.189*	0.538 (3)
C15	−0.3995 (4)	−0.5477 (4)	0.1287 (3)	0.086 (3)	0.538 (3)
C16	−0.4856 (5)	−0.5503 (3)	0.1086 (2)	0.121 (3)	0.538 (3)
H16A	−0.4786	−0.4936	0.0917	0.145*	0.538 (3)
C17	−0.5822 (4)	−0.6376 (4)	0.1136 (2)	0.1558 (17)	0.538 (3)
H17A	−0.6398	−0.6393	0.1002	0.187*	0.538 (3)
N3A	−0.4697 (3)	−0.7936 (3)	0.17497 (17)	0.122 (4)	0.462 (3)
C13A	−0.3768 (4)	−0.7396 (3)	0.1994 (2)	0.160 (3)	0.462 (3)
H13B	−0.3550	−0.7744	0.2196	0.192*	0.462 (3)
C14A	−0.3163 (4)	−0.6335 (3)	0.1937 (3)	0.119 (5)	0.462 (3)
H14B	−0.2541	−0.5974	0.2100	0.142*	0.462 (3)
C15A	−0.3487 (5)	−0.5815 (3)	0.1635 (3)	0.081 (3)	0.462 (3)
C16A	−0.4417 (6)	−0.6355 (3)	0.1391 (2)	0.100 (4)	0.462 (3)
H16B	−0.4634	−0.6007	0.1189	0.120*	0.462 (3)
C17A	−0.5022 (4)	−0.7416 (3)	0.1448 (2)	0.116 (4)	0.462 (3)
H17B	−0.5644	−0.7777	0.1285	0.139*	0.462 (3)
C18	−0.2971 (3)	−0.4552 (3)	0.14479 (18)	0.0972 (12)
C19	−0.2621 (3)	−0.3907 (3)	0.10428 (19)	0.1023 (13)
C20	−0.1871 (2)	−0.2936 (2)	0.10700 (13)	0.0665 (11)
H20A	−0.1628	−0.2548	0.0791	0.080*
C21	−0.14460 (18)	−0.24929 (17)	0.15031 (11)	0.0414 (8)
C22	−0.1784 (2)	−0.3078 (2)	0.19117 (13)	0.0635 (11)
H22A	−0.1520	−0.2778	0.2208	0.076*
C23	−0.2517 (3)	−0.4111 (2)	0.18836 (16)	0.0902 (15)
H23A	−0.2707	−0.4515	0.2159	0.108*
C24	−0.06567 (18)	−0.13818 (17)	0.15161 (10)	0.0404 (8)
C25	0.6744 (3)	0.0407 (4)	0.2805 (2)	0.1202 (18)
H25A	0.7421	0.0829	0.2705	0.144*
C26	0.5919 (3)	0.0339 (3)	0.2553 (2)	0.1054 (15)
H26A	0.6096	0.0763	0.2285	0.127*
C27	0.4947 (3)	−0.0213 (3)	0.26302 (18)	0.0989 (13)
C28	0.4711 (4)	−0.0737 (5)	0.3040 (3)	0.181 (3)
H28A	0.4030	−0.1135	0.3139	0.218*
C29	0.5588 (5)	−0.0663 (5)	0.3339 (3)	0.181 (3)
H29A	0.5462	−0.0989	0.3635	0.218*
C30	0.4113 (2)	−0.0140 (2)	0.23626 (15)	0.0824 (11)
C31	0.3778 (2)	0.0505 (2)	0.25388 (15)	0.0747 (11)
H31A	0.4027	0.0832	0.2832	0.090*
C32	0.3082 (2)	0.0673 (2)	0.22892 (12)	0.0601 (9)
H32A	0.2853	0.1097	0.2416	0.072*
C33	0.27234 (16)	0.01999 (17)	0.18441 (10)	0.0382 (7)
C34	0.30356 (17)	−0.04498 (19)	0.16650 (11)	0.0472 (8)
H34A	0.2789	−0.0774	0.1371	0.057*
C35	0.3722 (2)	−0.0619 (2)	0.19252 (15)	0.0679 (11)
C36	0.20126 (16)	0.04359 (16)	0.15554 (10)	0.0388 (7)

Atomic displacement parameters (Å²) top

	U¹¹	U²²	U³³	U¹²	U¹³	U²³
Eu1	0.03727 (3)	0.04887 (4)	0.02326 (4)	0.02622 (3)	0.00064 (5)	0.00303 (4)
O1W	0.0913 (11)	0.1114 (12)	0.1376 (16)	0.0543 (8)	−0.0083 (11)	0.0360 (12)
O1	0.0799 (12)	0.159 (2)	0.0748 (18)	0.0564 (11)	0.0108 (14)	0.0254 (16)
O2W	0.242 (2)	0.231 (2)	0.242 (2)	0.1208 (13)	−0.0089 (19)	−0.0023 (19)
O2	0.0864 (12)	0.1471 (18)	0.0633 (16)	0.0599 (11)	−0.0248 (11)	0.0067 (14)
O3	0.0578 (6)	0.0604 (7)	0.0359 (10)	0.0459 (5)	−0.0030 (7)	−0.0056 (7)
O4	0.0521 (9)	0.0589 (9)	0.0434 (11)	0.0185 (7)	−0.0103 (8)	0.0080 (9)
O5	0.204 (5)	0.128 (4)	0.130 (5)	0.065 (3)	−0.048 (4)	−0.017 (4)
O5A	0.103 (5)	0.150 (6)	0.097 (6)	0.044 (4)	−0.001 (4)	−0.016 (5)
O6	0.127 (3)	0.105 (3)	0.080 (3)	0.024 (2)	0.008 (2)	−0.049 (2)
O6A	0.106 (4)	0.065 (3)	0.053 (3)	0.001 (3)	0.023 (3)	−0.027 (3)
O7	0.0650 (10)	0.0415 (8)	0.0354 (11)	0.0167 (7)	0.0071 (8)	0.0128 (7)
O8	0.0773 (12)	0.0278 (7)	0.0395 (11)	0.0102 (8)	−0.0056 (9)	−0.0035 (7)
O9	0.0582 (7)	0.0878 (9)	0.0228 (9)	0.0519 (5)	−0.0098 (7)	−0.0025 (7)
O10	0.0436 (6)	0.0510 (7)	0.0474 (11)	0.0316 (5)	0.0025 (7)	0.0073 (7)
O11	0.1570 (18)	0.1265 (16)	0.114 (3)	0.0954 (12)	0.0089 (19)	−0.0120 (17)
O12	0.1916 (17)	0.1541 (15)	0.218 (3)	0.1398 (10)	−0.057 (2)	−0.0452 (19)
N1	0.0506 (12)	0.1002 (18)	0.186 (4)	0.0393 (11)	−0.0172 (18)	0.024 (2)
N2	0.0584 (9)	0.0808 (11)	0.0451 (14)	0.0436 (8)	−0.0089 (10)	0.0113 (11)
N4	0.054 (2)	0.067 (2)	0.061 (3)	0.0137 (16)	−0.0072 (19)	−0.018 (2)
N4A	0.059 (3)	0.050 (3)	0.046 (3)	0.0116 (19)	−0.005 (3)	−0.009 (2)
N5	0.1012 (16)	0.1037 (16)	0.128 (3)	0.0654 (11)	−0.0289 (19)	−0.001 (2)
N6	0.0757 (10)	0.0760 (11)	0.161 (3)	0.0602 (7)	−0.0286 (16)	−0.0097 (16)
C1	0.0443 (14)	0.105 (2)	0.135 (4)	0.0316 (13)	0.0171 (19)	0.035 (2)
C2	0.0608 (12)	0.0783 (14)	0.111 (3)	0.0447 (9)	0.0062 (18)	0.0300 (18)
C3	0.0490 (10)	0.0607 (12)	0.080 (2)	0.0342 (8)	0.0044 (13)	0.0142 (14)
C4	0.0494 (13)	0.0638 (15)	0.144 (4)	0.0283 (11)	−0.0092 (18)	0.0269 (18)
C5	0.0779 (18)	0.0694 (17)	0.161 (4)	0.0352 (13)	−0.028 (2)	0.024 (2)
C6	0.0484 (9)	0.0686 (11)	0.0599 (19)	0.0423 (7)	0.0066 (12)	0.0049 (13)
C7	0.0496 (10)	0.0593 (11)	0.0356 (14)	0.0346 (8)	0.0014 (10)	0.0066 (10)
C8	0.0472 (9)	0.0453 (10)	0.0449 (14)	0.0259 (7)	−0.0041 (13)	0.0014 (12)
C9	0.0609 (11)	0.0416 (9)	0.0260 (12)	0.0303 (7)	−0.0005 (10)	−0.0030 (9)
C10	0.0650 (12)	0.0772 (13)	0.0422 (16)	0.0473 (9)	0.0101 (12)	0.0084 (12)
C11	0.0571 (12)	0.0909 (16)	0.0513 (18)	0.0452 (10)	0.0200 (12)	0.0175 (14)
C12	0.0627 (12)	0.0384 (10)	0.0309 (13)	0.0262 (8)	−0.0035 (11)	−0.0007 (9)
N3	0.167 (5)	0.166 (5)	0.189 (6)	0.047 (4)	0.017 (5)	−0.021 (5)
C13	0.173 (5)	0.161 (4)	0.182 (5)	0.063 (4)	0.021 (4)	−0.018 (4)
C14	0.151 (5)	0.136 (5)	0.161 (6)	0.054 (4)	0.000 (5)	−0.018 (5)
C15	0.058 (3)	0.061 (3)	0.092 (5)	−0.005 (3)	0.003 (3)	−0.017 (3)
C16	0.108 (3)	0.124 (3)	0.117 (4)	0.048 (2)	0.013 (3)	−0.033 (3)
C17	0.152 (2)	0.157 (2)	0.154 (2)	0.0743 (14)	0.003 (2)	−0.004 (2)
N3A	0.119 (5)	0.110 (5)	0.109 (5)	0.036 (4)	0.035 (4)	−0.007 (4)
C13A	0.161 (4)	0.157 (4)	0.162 (5)	0.080 (3)	0.006 (4)	0.002 (4)
C14A	0.164 (7)	0.038 (3)	0.146 (9)	0.045 (3)	0.049 (7)	0.022 (4)
C15A	0.072 (4)	0.056 (3)	0.081 (4)	0.007 (3)	0.021 (3)	−0.026 (3)
C16A	0.087 (5)	0.055 (4)	0.079 (5)	−0.024 (3)	0.004 (4)	−0.018 (4)
C17A	0.142 (6)	0.059 (4)	0.126 (7)	0.035 (3)	0.016 (5)	−0.015 (4)
C18	0.0972 (17)	0.0783 (15)	0.0976 (19)	0.0298 (11)	0.0227 (15)	−0.0241 (14)
C19	0.0911 (17)	0.1028 (17)	0.0935 (19)	0.0337 (12)	0.0173 (15)	−0.0244 (15)
C20	0.0451 (14)	0.0656 (16)	0.0599 (18)	0.0061 (12)	0.0033 (13)	−0.0333 (14)
C21	0.0404 (10)	0.0345 (10)	0.0455 (15)	0.0158 (7)	0.0038 (11)	−0.0020 (10)
C22	0.0741 (17)	0.0342 (12)	0.071 (2)	0.0183 (11)	0.0157 (16)	0.0142 (13)
C23	0.091 (2)	0.0405 (14)	0.119 (3)	0.0176 (14)	0.0589 (19)	0.0268 (17)
C24	0.0495 (11)	0.0297 (10)	0.0352 (13)	0.0147 (7)	−0.0049 (10)	−0.0019 (9)
C25	0.113 (2)	0.140 (2)	0.131 (3)	0.0798 (15)	−0.030 (2)	−0.011 (2)
C26	0.0900 (15)	0.143 (2)	0.113 (3)	0.0809 (12)	−0.0384 (18)	−0.027 (2)
C27	0.1059 (15)	0.0909 (16)	0.123 (3)	0.0665 (11)	−0.0554 (17)	0.0000 (18)
C28	0.132 (3)	0.190 (4)	0.202 (5)	0.065 (2)	−0.063 (3)	0.076 (3)
C29	0.186 (3)	0.179 (3)	0.199 (4)	0.106 (2)	−0.022 (3)	0.049 (3)
C30	0.0862 (13)	0.0796 (14)	0.097 (2)	0.0531 (10)	−0.0551 (14)	−0.0093 (16)
C31	0.0855 (14)	0.0759 (14)	0.081 (2)	0.0540 (10)	−0.0377 (15)	−0.0097 (15)
C32	0.0671 (11)	0.0721 (12)	0.0528 (16)	0.0435 (9)	−0.0302 (13)	−0.0178 (14)
C33	0.0365 (9)	0.0420 (9)	0.0408 (14)	0.0232 (7)	−0.0074 (10)	0.0033 (9)
C34	0.0395 (9)	0.0567 (11)	0.0520 (17)	0.0291 (8)	−0.0065 (11)	−0.0017 (11)
C35	0.0721 (12)	0.0590 (11)	0.094 (3)	0.0491 (8)	−0.0181 (15)	0.0017 (14)
C36	0.0355 (9)	0.0368 (9)	0.0485 (15)	0.0214 (6)	−0.0106 (10)	0.0007 (10)

Geometric parameters (Å, º) top

Eu1—O7	2.305 (2)	C6—C7	1.404 (4)
Eu1—O3	2.319 (2)	C7—C8	1.370 (4)
Eu1—O10ⁱ	2.329 (2)	C8—C9	1.385 (4)
Eu1—O1W	2.347 (3)	C9—C10	1.381 (4)
Eu1—O4ⁱ	2.377 (2)	C9—C12	1.481 (4)
Eu1—O8ⁱ	2.378 (2)	C10—C11	1.359 (5)
Eu1—O9	2.432 (2)	N3—C13	1.3900
Eu1—O2W	2.668 (4)	N3—C17	1.3900
O1—N2	1.222 (3)	C13—C14	1.3900
O2—N2	1.201 (3)	C14—C15	1.3900
O3—C12	1.245 (3)	C15—C16	1.3900
O4—C12	1.240 (3)	C15—C18	1.533 (6)
O4—Eu1ⁱⁱ	2.377 (2)	C16—C17	1.3900
O5—N4	1.206 (10)	N3A—C13A	1.3900
O5A—N4A	1.205 (14)	N3A—C17A	1.3900
O6—N4	1.149 (8)	C13A—C14A	1.3900
O6A—N4A	1.213 (12)	C14A—C15A	1.3900
O7—C24	1.239 (3)	C15A—C16A	1.3900
O8—C24	1.242 (3)	C15A—C18	1.728 (6)
O8—Eu1ⁱⁱ	2.378 (2)	C16A—C17A	1.3900
O9—C36	1.250 (3)	C18—C23	1.388 (6)
O10—C36	1.263 (4)	C18—C19	1.407 (7)
O10—Eu1ⁱⁱ	2.329 (2)	C19—C20	1.322 (5)
O11—N6	1.173 (6)	C20—C21	1.372 (4)
O12—N6	1.193 (6)	C21—C22	1.371 (4)
N1—C5	1.313 (4)	C21—C24	1.484 (3)
N1—C1	1.372 (6)	C22—C23	1.381 (4)
N2—C7	1.434 (4)	C25—C26	1.380 (7)
N4—C19	1.671 (7)	C26—C27	1.283 (5)
N4A—C19	1.423 (9)	C27—C28	1.331 (8)
N5—C25	1.243 (7)	C27—C30	1.505 (6)
N5—C29	1.305 (8)	C28—C29	1.513 (10)
N6—C35	1.497 (5)	C30—C31	1.384 (6)
C1—C2	1.336 (6)	C30—C35	1.388 (5)
C2—C3	1.384 (3)	C31—C32	1.377 (5)
C3—C4	1.389 (5)	C32—C33	1.397 (4)
C3—C6	1.477 (5)	C33—C34	1.368 (4)
C4—C5	1.366 (6)	C33—C36	1.511 (4)
C6—C11	1.395 (5)	C34—C35	1.382 (5)

O7—Eu1—O3	79.79 (8)	C11—C10—C9	122.6 (3)
O7—Eu1—O10ⁱ	90.56 (8)	C10—C11—C6	121.2 (3)
O3—Eu1—O10ⁱ	160.49 (5)	O4—C12—O3	125.4 (3)
O7—Eu1—O1W	145.94 (9)	O4—C12—C9	117.5 (3)
O3—Eu1—O1W	113.61 (8)	O3—C12—C9	117.0 (2)
O10ⁱ—Eu1—O1W	83.76 (9)	C13—N3—C17	120.0
O7—Eu1—O4ⁱ	143.33 (7)	C14—C13—N3	120.0
O3—Eu1—O4ⁱ	76.70 (8)	C13—C14—C15	120.0
O10ⁱ—Eu1—O4ⁱ	102.61 (8)	C16—C15—C14	120.0
O1W—Eu1—O4ⁱ	70.29 (9)	C16—C15—C18	129.7 (5)
O7—Eu1—O8ⁱ	73.99 (8)	C14—C15—C18	106.4 (5)
O3—Eu1—O8ⁱ	83.62 (7)	C17—C16—C15	120.0
O10ⁱ—Eu1—O8ⁱ	77.40 (7)	C16—C17—N3	120.0
O1W—Eu1—O8ⁱ	136.18 (10)	C13A—N3A—C17A	120.0
O4ⁱ—Eu1—O8ⁱ	75.76 (8)	C14A—C13A—N3A	120.0
O7—Eu1—O9	73.20 (7)	C15A—C14A—C13A	120.0
O3—Eu1—O9	108.82 (8)	C14A—C15A—C16A	120.0
O10ⁱ—Eu1—O9	84.11 (7)	C14A—C15A—C18	134.9 (4)
O1W—Eu1—O9	72.82 (9)	C16A—C15A—C18	105.0 (4)
O4ⁱ—Eu1—O9	141.41 (6)	C17A—C16A—C15A	120.0
O8ⁱ—Eu1—O9	141.92 (7)	C16A—C17A—N3A	120.0
O7—Eu1—O2W	120.00 (11)	C23—C18—C19	116.8 (3)
O3—Eu1—O2W	64.82 (9)	C23—C18—C15	135.8 (5)
O10ⁱ—Eu1—O2W	134.19 (10)	C19—C18—C15	104.3 (5)
O1W—Eu1—O2W	51.46 (11)	C23—C18—C15A	95.8 (4)
O4ⁱ—Eu1—O2W	73.78 (11)	C19—C18—C15A	143.5 (5)
O8ⁱ—Eu1—O2W	140.12 (11)	C15—C18—C15A	53.2 (4)
O9—Eu1—O2W	74.68 (10)	C20—C19—C18	122.0 (4)
C12—O3—Eu1	141.81 (16)	C20—C19—N4A	129.2 (5)
C12—O4—Eu1ⁱⁱ	128.77 (19)	C18—C19—N4A	99.1 (5)
C24—O7—Eu1	156.66 (17)	C20—C19—N4	112.6 (4)
C24—O8—Eu1ⁱⁱ	140.09 (18)	C18—C19—N4	125.3 (3)
C36—O9—Eu1	122.64 (19)	N4A—C19—N4	41.8 (4)
C36—O10—Eu1ⁱⁱ	145.40 (14)	C19—C20—C21	121.1 (4)
C5—N1—C1	117.2 (4)	C22—C21—C20	119.3 (2)
O2—N2—O1	120.8 (3)	C22—C21—C24	121.9 (3)
O2—N2—C7	122.6 (2)	C20—C21—C24	118.8 (3)
O1—N2—C7	116.6 (2)	C21—C22—C23	120.1 (3)
O6—N4—O5	130.9 (6)	C22—C23—C18	120.6 (4)
O6—N4—C19	113.4 (5)	O7—C24—O8	126.4 (2)
O5—N4—C19	115.7 (5)	O7—C24—C21	117.0 (2)
O5A—N4A—O6A	124.1 (9)	O8—C24—C21	116.5 (2)
O5A—N4A—C19	96.8 (8)	N5—C25—C26	115.8 (4)
O6A—N4A—C19	138.2 (8)	C27—C26—C25	130.5 (5)
C25—N5—C29	122.9 (6)	C26—C27—C28	113.9 (5)
O11—N6—O12	123.3 (4)	C26—C27—C30	125.9 (4)
O11—N6—C35	120.2 (4)	C28—C27—C30	118.9 (4)
O12—N6—C35	116.2 (4)	C27—C28—C29	117.7 (5)
C2—C1—N1	121.0 (3)	N5—C29—C28	118.6 (7)
C1—C2—C3	121.5 (3)	C31—C30—C35	117.8 (3)
C2—C3—C4	117.7 (3)	C31—C30—C27	118.6 (3)
C2—C3—C6	118.9 (3)	C35—C30—C27	123.3 (4)
C4—C3—C6	122.5 (2)	C32—C31—C30	121.3 (4)
C5—C4—C3	117.2 (3)	C31—C32—C33	119.4 (3)
N1—C5—C4	125.2 (4)	C34—C33—C32	120.3 (3)
C11—C6—C7	115.9 (3)	C34—C33—C36	120.2 (2)
C11—C6—C3	119.2 (3)	C32—C33—C36	119.5 (3)
C7—C6—C3	124.7 (3)	C33—C34—C35	119.3 (3)
C8—C7—C6	122.3 (3)	C34—C35—C30	121.8 (3)
C8—C7—N2	117.2 (3)	C34—C35—N6	115.8 (3)
C6—C7—N2	120.1 (3)	C30—C35—N6	122.4 (3)
C7—C8—C9	120.7 (3)	O9—C36—O10	124.5 (3)
C10—C9—C8	117.2 (3)	O9—C36—C33	117.8 (3)
C10—C9—C12	120.7 (3)	O10—C36—C33	117.7 (2)
C8—C9—C12	122.1 (2)

O7—Eu1—O3—C12	−24.0 (3)	C14A—C15A—C18—C19	116.6 (8)
O10ⁱ—Eu1—O3—C12	37.4 (4)	C16A—C15A—C18—C19	−60.7 (8)
O1W—Eu1—O3—C12	−171.2 (3)	C14A—C15A—C18—C15	177.1 (7)
O4ⁱ—Eu1—O3—C12	127.6 (3)	C16A—C15A—C18—C15	−0.2 (5)
O8ⁱ—Eu1—O3—C12	50.8 (3)	C23—C18—C19—C20	2.2 (8)
O9—Eu1—O3—C12	−92.2 (3)	C15—C18—C19—C20	165.5 (6)
O2W—Eu1—O3—C12	−154.3 (3)	C15A—C18—C19—C20	−148.5 (7)
O3—Eu1—O7—C24	−48.0 (6)	C23—C18—C19—N4A	150.9 (5)
O10ⁱ—Eu1—O7—C24	149.0 (6)	C15—C18—C19—N4A	−45.7 (6)
O1W—Eu1—O7—C24	69.4 (6)	C15A—C18—C19—N4A	0.2 (10)
O4ⁱ—Eu1—O7—C24	−98.7 (5)	C23—C18—C19—N4	−173.3 (5)
O8ⁱ—Eu1—O7—C24	−134.3 (6)	C15—C18—C19—N4	−10.0 (8)
O9—Eu1—O7—C24	65.3 (6)	C15A—C18—C19—N4	35.9 (11)
O2W—Eu1—O7—C24	4.9 (6)	O5A—N4A—C19—C20	−54.4 (10)
O7—Eu1—O9—C36	−72.69 (16)	O6A—N4A—C19—C20	114.1 (10)
O3—Eu1—O9—C36	−0.06 (16)	O5A—N4A—C19—C18	160.3 (7)
O10ⁱ—Eu1—O9—C36	−165.06 (16)	O6A—N4A—C19—C18	−31.2 (11)
O1W—Eu1—O9—C36	109.67 (17)	O5A—N4A—C19—N4	25.9 (6)
O4ⁱ—Eu1—O9—C36	92.08 (18)	O6A—N4A—C19—N4	−165.6 (12)
O8ⁱ—Eu1—O9—C36	−104.22 (18)	O6—N4—C19—C20	132.8 (5)
O2W—Eu1—O9—C36	55.93 (17)	O5—N4—C19—C20	−45.4 (7)
C5—N1—C1—C2	−1.5 (8)	O6—N4—C19—C18	−51.3 (8)
N1—C1—C2—C3	2.0 (8)	O5—N4—C19—C18	130.5 (7)
C1—C2—C3—C4	0.7 (7)	O6—N4—C19—N4A	8.6 (5)
C1—C2—C3—C6	169.8 (4)	O5—N4—C19—N4A	−169.6 (7)
C2—C3—C4—C5	−3.8 (6)	C18—C19—C20—C21	−4.4 (8)
C6—C3—C4—C5	−172.4 (4)	N4A—C19—C20—C21	−142.9 (7)
C1—N1—C5—C4	−1.9 (8)	N4—C19—C20—C21	171.7 (4)
C3—C4—C5—N1	4.6 (8)	C19—C20—C21—C22	2.0 (6)
C2—C3—C6—C11	−53.7 (5)	C19—C20—C21—C24	−175.9 (4)
C4—C3—C6—C11	114.9 (4)	C20—C21—C22—C23	2.4 (6)
C2—C3—C6—C7	131.8 (4)	C24—C21—C22—C23	−179.7 (4)
C4—C3—C6—C7	−59.7 (5)	C21—C22—C23—C18	−4.5 (7)
C11—C6—C7—C8	1.9 (4)	C19—C18—C23—C22	2.2 (8)
C3—C6—C7—C8	176.6 (3)	C15—C18—C23—C22	−154.2 (7)
C11—C6—C7—N2	175.1 (3)	C15A—C18—C23—C22	165.2 (5)
C3—C6—C7—N2	−10.2 (4)	Eu1—O7—C24—O8	−4.6 (8)
O2—N2—C7—C8	152.2 (3)	Eu1—O7—C24—C21	175.4 (4)
O1—N2—C7—C8	−26.8 (4)	Eu1ⁱⁱ—O8—C24—O7	23.5 (6)
O2—N2—C7—C6	−21.3 (5)	Eu1ⁱⁱ—O8—C24—C21	−156.4 (2)
O1—N2—C7—C6	159.7 (3)	C22—C21—C24—O7	170.4 (3)
C6—C7—C8—C9	−1.1 (4)	C20—C21—C24—O7	−11.8 (5)
N2—C7—C8—C9	−174.5 (2)	C22—C21—C24—O8	−9.7 (5)
C7—C8—C9—C10	1.2 (4)	C20—C21—C24—O8	168.2 (3)
C7—C8—C9—C12	180.0 (2)	C29—N5—C25—C26	−5.8 (9)
C8—C9—C10—C11	−2.4 (4)	N5—C25—C26—C27	−1.9 (9)
C12—C9—C10—C11	178.9 (3)	C25—C26—C27—C28	6.2 (9)
C9—C10—C11—C6	3.3 (5)	C25—C26—C27—C30	172.8 (5)
C7—C6—C11—C10	−2.9 (4)	C26—C27—C28—C29	−3.3 (9)
C3—C6—C11—C10	−177.9 (3)	C30—C27—C28—C29	−170.9 (5)
Eu1ⁱⁱ—O4—C12—O3	9.9 (4)	C25—N5—C29—C28	8.0 (10)
Eu1ⁱⁱ—O4—C12—C9	−166.96 (16)	C27—C28—C29—N5	−3.1 (10)
Eu1—O3—C12—O4	81.4 (3)	C26—C27—C30—C31	−91.6 (6)
Eu1—O3—C12—C9	−101.7 (3)	C28—C27—C30—C31	74.4 (5)
C10—C9—C12—O4	−0.1 (4)	C26—C27—C30—C35	82.7 (6)
C8—C9—C12—O4	−178.8 (2)	C28—C27—C30—C35	−111.3 (6)
C10—C9—C12—O3	−177.3 (2)	C35—C30—C31—C32	−0.2 (4)
C8—C9—C12—O3	4.1 (3)	C27—C30—C31—C32	174.4 (3)
C17—N3—C13—C14	0.0	C30—C31—C32—C33	−1.4 (4)
N3—C13—C14—C15	0.0	C31—C32—C33—C34	2.1 (4)
C13—C14—C15—C16	0.0	C31—C32—C33—C36	−176.1 (2)
C13—C14—C15—C18	159.9 (5)	C32—C33—C34—C35	−1.1 (4)
C14—C15—C16—C17	0.0	C36—C33—C34—C35	177.1 (2)
C18—C15—C16—C17	−154.7 (6)	C33—C34—C35—C30	−0.6 (4)
C15—C16—C17—N3	0.0	C33—C34—C35—N6	179.6 (2)
C13—N3—C17—C16	0.0	C31—C30—C35—C34	1.3 (4)
C17A—N3A—C13A—C14A	0.0	C27—C30—C35—C34	−173.1 (3)
N3A—C13A—C14A—C15A	0.0	C31—C30—C35—N6	−179.0 (3)
C13A—C14A—C15A—C16A	0.0	C27—C30—C35—N6	6.7 (5)
C13A—C14A—C15A—C18	−177.0 (5)	O11—N6—C35—C34	3.5 (4)
C14A—C15A—C16A—C17A	0.0	O12—N6—C35—C34	−170.5 (3)
C18—C15A—C16A—C17A	177.8 (4)	O11—N6—C35—C30	−176.3 (3)
C15A—C16A—C17A—N3A	0.0	O12—N6—C35—C30	9.8 (4)
C13A—N3A—C17A—C16A	0.0	Eu1—O9—C36—O10	−4.7 (3)
C16—C15—C18—C23	104.7 (8)	Eu1—O9—C36—C33	175.94 (12)
C14—C15—C18—C23	−52.6 (8)	Eu1ⁱⁱ—O10—C36—O9	101.4 (3)
C16—C15—C18—C19	−53.7 (7)	Eu1ⁱⁱ—O10—C36—C33	−79.2 (3)
C14—C15—C18—C19	149.0 (4)	C34—C33—C36—O9	−12.9 (3)
C16—C15—C18—C15A	158.6 (7)	C32—C33—C36—O9	165.3 (2)
C14—C15—C18—C15A	1.3 (4)	C34—C33—C36—O10	167.63 (19)
C14A—C15A—C18—C23	−37.3 (6)	C32—C33—C36—O10	−14.2 (3)
C16A—C15A—C18—C23	145.3 (4)

Symmetry codes: (i) y, −x+y, z−1/6; (ii) x−y, x, z+1/6.

Poly[diaquatris[µ₂-3-nitro-4-(pyridin-4-yl)benzoato-κ²O:O']gadolinium(III)] (1502113) top

Crystal data top

[Gd(C₁₂H₇N₂O₄)₃(H₂O)₂]	D_x = 1.692 Mg m⁻³
M_r = 922.87	Mo Kα radiation, λ = 0.71073 Å
Hexagonal, P6₅	Cell parameters from 9953 reflections
Hall symbol: P 65	θ = 2.7–27.0°
a = 14.9855 (8) Å	µ = 1.91 mm⁻¹
c = 27.949 (3) Å	T = 296 K
V = 5435.5 (7) Å³	Rodlike, colorless
Z = 6	0.17 × 0.14 × 0.12 mm
F(000) = 2754

Data collection top

Bruker APEXII CCD diffractometer	6882 independent reflections
Radiation source: fine-focus sealed tube	5967 reflections with I > 2σ(I)
Graphite monochromator	R_int = 0.053
ω scans	θ_max = 26.0°, θ_min = 1.6°
Absorption correction: multi-scan (SADABS; Sheldrick, 2003)	h = −18→18
T_min = 0.733, T_max = 0.795	k = −16→18
40707 measured reflections	l = −34→33

Refinement top

Refinement on F²	Secondary atom site location: difference Fourier map
Least-squares matrix: full	Hydrogen site location: inferred from neighbouring sites
R[F² > 2σ(F²)] = 0.046	H atoms treated by a mixture of independent and constrained refinement
wR(F²) = 0.128	w = 1/[σ²(F_o²) + (0.0803P)² + 2.5694P] where P = (F_o² + 2F_c²)/3
S = 1.09	(Δ/σ)_max = 0.007
6882 reflections	Δρ_max = 1.75 e Å⁻³
579 parameters	Δρ_min = −0.86 e Å⁻³
220 restraints	Absolute structure: Flack (1983), 3245 Friedel pairs
Primary atom site location: structure-invariant direct methods	Absolute structure parameter: 0.00 (2)

Special details top

Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å²) top

	x	y	z	U_iso*/U_eq	Occ. (<1)
Gd1	0.040102 (7)	−0.028087 (7)	0.181986 (9)	0.03709 (3)
O1W	0.1623 (3)	−0.0715 (2)	0.20742 (13)	0.1912 (6)
H1WA	0.2228 (3)	−0.0193 (4)	0.2058 (3)	0.229*
H1WB	0.1586 (6)	−0.1208 (3)	0.1910 (2)	0.229*
O1	0.1949 (2)	0.3567 (2)	0.27096 (12)	0.1164 (10)
O2W	0.2239 (3)	0.03791 (19)	0.14059 (11)	0.1912 (6)
H2WA	0.2274 (7)	0.0782 (3)	0.11473 (16)	0.229*
H2WB	0.2138 (3)	−0.0196 (2)	0.1259 (2)	0.229*
O2	0.1224 (2)	0.44475 (18)	0.27673 (9)	0.1022 (9)
O3	0.11424 (13)	0.12171 (11)	0.13725 (6)	0.0464 (6)
O4	0.06234 (13)	0.15995 (14)	0.06977 (7)	0.0570 (6)
O5	−0.4987 (4)	−0.1775 (4)	0.20613 (19)	0.142 (2)	0.722 (3)
O5A	−0.5496 (5)	−0.2730 (6)	0.1778 (3)	0.080 (2)	0.278 (3)
O6	−0.3647 (5)	−0.0325 (7)	0.2121 (3)	0.231 (4)	0.722 (3)
O6A	−0.4190 (11)	−0.1429 (11)	0.2065 (5)	0.139 (5)	0.278 (3)
O7	−0.09520 (12)	−0.06419 (13)	0.13139 (7)	0.0541 (6)
O8	−0.09544 (13)	−0.05415 (16)	0.05171 (8)	0.0597 (7)
O9	0.01913 (14)	−0.16740 (12)	0.13049 (6)	0.0551 (6)
O10	0.08975 (13)	−0.06888 (11)	0.06643 (7)	0.0477 (6)
O11	−0.1713 (3)	−0.5386 (2)	0.10879 (14)	0.1236 (15)
O12	−0.1548 (3)	−0.6097 (3)	0.05015 (18)	0.1599 (13)
N1	0.1440 (2)	0.7383 (2)	0.21466 (17)	0.1187 (15)
N2	0.15007 (19)	0.39778 (17)	0.25261 (10)	0.0634 (8)
N4	−0.4241 (3)	−0.1097 (3)	0.1919 (2)	0.0945 (16)	0.722 (3)
N4A	−0.4650 (5)	−0.1935 (6)	0.1730 (3)	0.052 (2)	0.278 (3)
N5	−0.0132 (3)	−0.6646 (2)	−0.07648 (16)	0.1090 (15)
N6	−0.1354 (2)	−0.53544 (18)	0.07231 (15)	0.0956 (12)
C1	0.2212 (3)	0.7177 (3)	0.2214 (2)	0.1138 (18)
H1A	0.2825	0.7690	0.2346	0.137*
C2	0.2142 (3)	0.6248 (3)	0.20991 (18)	0.0922 (15)
H2A	0.2709	0.6157	0.2128	0.111*
C3	0.1218 (2)	0.54684 (18)	0.19416 (14)	0.0671 (11)
C4	0.0407 (2)	0.5657 (2)	0.18827 (18)	0.0900 (14)
H4A	−0.0230	0.5135	0.1777	0.108*
C5	0.0540 (3)	0.6575 (2)	0.1977 (2)	0.0998 (15)
H5A	−0.0011	0.6683	0.1924	0.120*
C6	0.11050 (19)	0.44781 (16)	0.17655 (13)	0.0576 (9)
C7	0.13044 (19)	0.38139 (18)	0.20214 (10)	0.0475 (8)
C8	0.12446 (18)	0.29407 (17)	0.18264 (11)	0.0469 (7)
H8A	0.1393	0.2519	0.2015	0.056*
C9	0.09604 (19)	0.26827 (18)	0.13445 (9)	0.0445 (8)
C10	0.0743 (2)	0.33397 (19)	0.10926 (11)	0.0574 (9)
H10A	0.0513	0.3165	0.0779	0.069*
C11	0.0844 (2)	0.42294 (19)	0.12722 (13)	0.0675 (10)
H11A	0.0743	0.4673	0.1076	0.081*
C12	0.08928 (16)	0.17657 (17)	0.11325 (9)	0.0412 (7)
N3	−0.7262 (2)	−0.1352 (3)	0.10304 (19)	0.176 (3)	0.505 (3)
C13	−0.7260 (3)	−0.2206 (4)	0.0839 (3)	0.174 (3)	0.505 (3)
H13A	−0.7840	−0.2710	0.0680	0.209*	0.505 (3)
C14	−0.6392 (4)	−0.2308 (5)	0.0883 (3)	0.142 (3)	0.505 (3)
H14A	−0.6390	−0.2880	0.0755	0.170*	0.505 (3)
C15	−0.5525 (3)	−0.1555 (5)	0.1120 (3)	0.079 (2)	0.505 (3)
C16	−0.5527 (3)	−0.0700 (5)	0.1312 (3)	0.099 (2)	0.505 (3)
H16A	−0.4947	−0.0197	0.1470	0.118*	0.505 (3)
C17	−0.6395 (3)	−0.0599 (4)	0.1267 (3)	0.232 (5)	0.505 (3)
H17A	−0.6397	−0.0027	0.1395	0.278*	0.505 (3)
N3A	−0.7937 (3)	−0.3206 (3)	0.06936 (16)	0.129 (3)	0.495 (3)
C13A	−0.7395 (3)	−0.3589 (4)	0.04454 (19)	0.142 (4)	0.495 (3)
H13B	−0.7742	−0.4146	0.0239	0.171*	0.495 (3)
C14A	−0.6336 (3)	−0.3138 (5)	0.0505 (2)	0.111 (3)	0.495 (3)
H14B	−0.5974	−0.3394	0.0339	0.133*	0.495 (3)
C15A	−0.5818 (3)	−0.2306 (5)	0.0813 (3)	0.079 (2)	0.495 (3)
C16A	−0.6359 (3)	−0.1924 (5)	0.1062 (3)	0.129 (3)	0.495 (3)
H16B	−0.6013	−0.1367	0.1268	0.154*	0.495 (3)
C17A	−0.7419 (3)	−0.2374 (4)	0.1002 (2)	0.114 (3)	0.495 (3)
H17B	−0.7781	−0.2118	0.1168	0.137*	0.495 (3)
C18	−0.4549 (3)	−0.1561 (3)	0.09897 (19)	0.0989 (11)
C19	−0.3963 (3)	−0.1347 (3)	0.1367 (2)	0.1100 (14)
C20	−0.29374 (19)	−0.1059 (2)	0.13587 (12)	0.0714 (10)
H20A	−0.2554	−0.0884	0.1640	0.086*
C21	−0.24945 (16)	−0.10365 (17)	0.09305 (10)	0.0435 (7)
C22	−0.30642 (19)	−0.1300 (2)	0.05204 (13)	0.0633 (11)
H22A	−0.2758	−0.1275	0.0227	0.076*
C23	−0.4104 (2)	−0.1606 (3)	0.05439 (15)	0.0901 (14)
H23A	−0.4510	−0.1840	0.0270	0.108*
C24	−0.13814 (16)	−0.07188 (18)	0.09198 (10)	0.0460 (8)
C25	0.0356 (4)	−0.6354 (3)	−0.0379 (2)	0.132 (2)
H25A	0.0738	−0.6646	−0.0269	0.159*
C26	0.0315 (4)	−0.5595 (3)	−0.0121 (2)	0.1244 (18)
H26A	0.0719	−0.5383	0.0154	0.149*
C27	−0.0190 (3)	−0.5141 (3)	−0.02023 (17)	0.1039 (14)
C28	−0.0721 (4)	−0.5468 (4)	−0.0603 (3)	0.165 (2)
H28A	−0.1162	−0.5221	−0.0680	0.198*
C29	−0.0663 (5)	−0.6210 (5)	−0.0942 (3)	0.177 (3)
H29A	−0.0962	−0.6356	−0.1245	0.213*
C30	−0.0117 (2)	−0.4243 (2)	0.00694 (15)	0.0906 (13)
C31	0.0520 (3)	−0.3247 (3)	−0.01220 (15)	0.0899 (14)
H31A	0.0821	−0.3171	−0.0421	0.108*
C32	0.0694 (2)	−0.2388 (2)	0.01333 (12)	0.0663 (10)
H32A	0.1126	−0.1733	0.0011	0.080*
C33	0.02133 (18)	−0.25119 (17)	0.05824 (10)	0.0456 (8)
C34	−0.0439 (2)	−0.34661 (19)	0.07592 (12)	0.0571 (9)
H34A	−0.0763	−0.3544	0.1053	0.069*
C35	−0.0614 (2)	−0.4318 (2)	0.04955 (16)	0.0785 (13)
C36	0.04448 (17)	−0.15522 (17)	0.08727 (10)	0.0463 (8)

Atomic displacement parameters (Å²) top

	U¹¹	U²²	U³³	U¹²	U¹³	U²³
Gd1	0.05397 (4)	0.03601 (3)	0.02465 (4)	0.02501 (3)	−0.00267 (5)	−0.00176 (4)
O1W	0.1905 (7)	0.1899 (7)	0.1962 (8)	0.0974 (5)	−0.0001 (7)	−0.0050 (7)
O1	0.1328 (13)	0.1212 (12)	0.1081 (16)	0.0731 (9)	−0.0072 (13)	−0.0079 (13)
O2W	0.1905 (7)	0.1899 (7)	0.1962 (8)	0.0974 (5)	−0.0001 (7)	−0.0050 (7)
O2	0.1614 (15)	0.1188 (11)	0.0634 (15)	0.0978 (9)	−0.0166 (13)	−0.0368 (10)
O3	0.0631 (8)	0.0328 (6)	0.0362 (9)	0.0186 (5)	−0.0020 (7)	−0.0001 (6)
O4	0.0579 (7)	0.0774 (9)	0.0437 (10)	0.0397 (6)	−0.0068 (7)	−0.0119 (8)
O5	0.126 (3)	0.179 (3)	0.114 (3)	0.072 (2)	0.043 (2)	0.070 (2)
O5A	0.071 (3)	0.108 (3)	0.059 (4)	0.043 (2)	−0.001 (3)	0.033 (3)
O6	0.173 (4)	0.388 (8)	0.127 (5)	0.137 (4)	0.014 (4)	−0.076 (4)
O6A	0.143 (6)	0.147 (6)	0.124 (7)	0.070 (4)	−0.003 (5)	0.012 (5)
O7	0.0446 (7)	0.0786 (9)	0.0405 (11)	0.0318 (6)	−0.0153 (7)	−0.0085 (8)
O8	0.0348 (7)	0.0870 (12)	0.0416 (11)	0.0185 (7)	0.0032 (7)	−0.0095 (9)
O9	0.1021 (9)	0.0560 (7)	0.0219 (8)	0.0506 (5)	0.0028 (7)	−0.0089 (6)
O10	0.0593 (8)	0.0309 (6)	0.0462 (10)	0.0175 (5)	−0.0044 (8)	0.0013 (7)
O11	0.141 (2)	0.0876 (16)	0.118 (3)	0.0386 (15)	0.000 (2)	0.0006 (18)
O12	0.1641 (17)	0.1421 (16)	0.1620 (19)	0.0680 (11)	0.0278 (15)	−0.0140 (15)
N1	0.1117 (17)	0.0692 (12)	0.190 (4)	0.0566 (10)	−0.021 (2)	−0.0410 (17)
N2	0.0848 (12)	0.0620 (10)	0.0514 (14)	0.0428 (8)	−0.0130 (11)	−0.0173 (10)
N4	0.0815 (16)	0.116 (2)	0.107 (3)	0.0654 (12)	0.024 (2)	0.015 (2)
N4A	0.037 (2)	0.094 (4)	0.028 (4)	0.036 (2)	0.007 (2)	0.013 (3)
N5	0.1039 (19)	0.0835 (16)	0.123 (3)	0.0344 (13)	0.012 (2)	−0.0263 (18)
N6	0.0787 (14)	0.0425 (10)	0.153 (3)	0.0205 (9)	0.0184 (17)	−0.0293 (14)
C1	0.0924 (18)	0.0939 (18)	0.170 (4)	0.0581 (13)	−0.024 (2)	−0.039 (2)
C2	0.0734 (16)	0.0689 (15)	0.140 (4)	0.0398 (11)	−0.025 (2)	−0.0289 (19)
C3	0.0827 (13)	0.0410 (9)	0.087 (2)	0.0381 (8)	−0.0143 (15)	−0.0098 (12)
C4	0.0862 (15)	0.0687 (13)	0.125 (3)	0.0460 (10)	−0.034 (2)	−0.0360 (19)
C5	0.0903 (15)	0.0814 (14)	0.150 (4)	0.0599 (10)	−0.028 (2)	−0.0208 (19)
C6	0.0711 (11)	0.0324 (8)	0.0752 (19)	0.0302 (7)	−0.0137 (14)	−0.0063 (12)
C7	0.0570 (11)	0.0420 (10)	0.0382 (13)	0.0207 (8)	−0.0054 (11)	−0.0070 (10)
C8	0.0590 (10)	0.0418 (9)	0.0346 (12)	0.0213 (7)	0.0001 (12)	−0.0003 (11)
C9	0.0555 (11)	0.0400 (10)	0.0266 (12)	0.0153 (8)	−0.0016 (10)	0.0030 (9)
C10	0.0858 (13)	0.0609 (11)	0.0341 (14)	0.0431 (9)	−0.0102 (11)	0.0011 (11)
C11	0.0970 (13)	0.0568 (10)	0.0655 (19)	0.0510 (8)	−0.0175 (14)	0.0051 (12)
C12	0.0421 (9)	0.0449 (10)	0.0329 (12)	0.0190 (7)	0.0030 (9)	0.0039 (10)
N3	0.137 (3)	0.207 (4)	0.216 (5)	0.110 (3)	0.010 (4)	0.016 (4)
C13	0.114 (4)	0.209 (5)	0.204 (5)	0.085 (4)	−0.014 (4)	0.020 (5)
C14	0.082 (3)	0.188 (4)	0.177 (5)	0.083 (3)	−0.010 (4)	0.012 (4)
C15	0.053 (2)	0.101 (3)	0.096 (5)	0.0488 (17)	0.006 (3)	0.019 (3)
C16	0.089 (2)	0.124 (3)	0.109 (4)	0.0731 (19)	0.049 (3)	0.032 (3)
C17	0.250 (7)	0.236 (7)	0.236 (8)	0.143 (4)	−0.012 (7)	0.006 (7)
N3A	0.113 (4)	0.155 (4)	0.121 (5)	0.069 (3)	−0.016 (4)	0.033 (4)
C13A	0.132 (5)	0.122 (5)	0.167 (7)	0.059 (4)	0.013 (5)	0.021 (5)
C14A	0.086 (4)	0.116 (5)	0.121 (6)	0.043 (3)	−0.010 (4)	0.010 (5)
C15A	0.048 (2)	0.117 (4)	0.070 (4)	0.040 (2)	0.015 (2)	0.035 (3)
C16A	0.110 (4)	0.160 (5)	0.127 (5)	0.075 (3)	0.008 (4)	0.004 (4)
C17A	0.064 (3)	0.137 (5)	0.125 (6)	0.038 (3)	0.018 (4)	0.027 (5)
C18	0.0836 (13)	0.1124 (15)	0.1051 (18)	0.0524 (10)	0.0069 (14)	0.0247 (14)
C19	0.1125 (16)	0.1431 (18)	0.111 (3)	0.0914 (11)	0.0210 (19)	0.0423 (19)
C20	0.0721 (11)	0.1119 (15)	0.0561 (17)	0.0653 (9)	0.0273 (12)	0.0345 (13)
C21	0.0414 (9)	0.0448 (9)	0.0462 (14)	0.0231 (7)	0.0060 (10)	0.0057 (10)
C22	0.0346 (10)	0.0739 (15)	0.071 (2)	0.0195 (10)	−0.0069 (12)	−0.0030 (15)
C23	0.0352 (11)	0.116 (2)	0.103 (3)	0.0253 (12)	−0.0135 (14)	0.032 (2)
C24	0.0332 (9)	0.0546 (11)	0.0438 (14)	0.0173 (8)	0.0003 (10)	−0.0026 (11)
C25	0.180 (3)	0.0852 (18)	0.137 (4)	0.0703 (17)	0.037 (3)	−0.020 (2)
C26	0.186 (3)	0.0764 (16)	0.114 (3)	0.0684 (15)	0.053 (2)	−0.0047 (19)
C27	0.0874 (18)	0.0974 (17)	0.117 (3)	0.0386 (13)	0.0029 (19)	−0.0585 (16)
C28	0.164 (3)	0.182 (3)	0.185 (4)	0.1134 (19)	−0.005 (3)	−0.074 (3)
C29	0.157 (4)	0.163 (4)	0.195 (6)	0.067 (3)	−0.039 (4)	−0.063 (4)
C30	0.0808 (15)	0.0591 (12)	0.124 (3)	0.0289 (10)	0.0216 (17)	−0.0405 (14)
C31	0.0870 (19)	0.0870 (16)	0.085 (2)	0.0358 (14)	−0.0009 (18)	−0.0458 (16)
C32	0.0834 (13)	0.0648 (12)	0.0510 (16)	0.0372 (9)	0.0188 (15)	−0.0069 (13)
C33	0.0545 (11)	0.0415 (9)	0.0389 (13)	0.0225 (7)	0.0027 (10)	−0.0118 (9)
C34	0.0638 (12)	0.0519 (11)	0.0612 (18)	0.0331 (8)	−0.0032 (12)	−0.0142 (11)
C35	0.0622 (15)	0.0489 (13)	0.113 (3)	0.0190 (11)	0.0015 (18)	−0.0231 (16)
C36	0.0472 (9)	0.0458 (9)	0.0508 (14)	0.0270 (7)	−0.0075 (10)	−0.0140 (10)

Geometric parameters (Å, º) top

Gd1—O7	2.3037 (19)	C6—C11	1.431 (5)
Gd1—O10ⁱ	2.3109 (19)	C7—C8	1.378 (4)
Gd1—O3	2.3113 (15)	C8—C9	1.407 (4)
Gd1—O1W	2.339 (4)	C9—C10	1.375 (4)
Gd1—O8ⁱ	2.3620 (18)	C9—C12	1.453 (4)
Gd1—O4ⁱ	2.389 (2)	C10—C11	1.361 (4)
Gd1—O9	2.4233 (18)	N3—C13	1.3900
Gd1—O2W	2.679 (4)	N3—C17	1.3900
O1—N2	1.228 (5)	C13—C14	1.3900
O2—N2	1.189 (4)	C14—C15	1.3900
O3—C12	1.254 (3)	C15—C16	1.3900
O4—C12	1.265 (3)	C15—C18	1.511 (6)
O4—Gd1ⁱⁱ	2.389 (2)	C16—C17	1.3900
O5—N4	1.142 (6)	N3A—C13A	1.3900
O5A—N4A	1.239 (9)	N3A—C17A	1.3900
O6—N4	1.192 (9)	C13A—C14A	1.3900
O6A—N4A	1.183 (16)	C14A—C15A	1.3900
O7—C24	1.251 (3)	C15A—C16A	1.3900
O8—C24	1.256 (3)	C15A—C18	1.727 (5)
O8—Gd1ⁱⁱ	2.3620 (18)	C16A—C17A	1.3900
O9—C36	1.252 (3)	C18—C19	1.305 (7)
O10—C36	1.263 (3)	C18—C23	1.431 (7)
O10—Gd1ⁱⁱ	2.3108 (19)	C19—C20	1.373 (5)
O11—N6	1.143 (6)	C20—C21	1.361 (4)
O12—N6	1.175 (6)	C21—C22	1.364 (4)
N1—C1	1.352 (6)	C21—C24	1.489 (3)
N1—C5	1.370 (4)	C22—C23	1.388 (4)
N2—C7	1.437 (4)	C25—C26	1.373 (8)
N4—C19	1.688 (8)	C26—C27	1.266 (8)
N4A—C19	1.400 (8)	C27—C28	1.318 (8)
N5—C25	1.252 (7)	C27—C30	1.502 (6)
N5—C29	1.351 (10)	C28—C29	1.498 (11)
N6—C35	1.524 (4)	C30—C35	1.379 (6)
C1—C2	1.380 (6)	C30—C31	1.414 (5)
C2—C3	1.363 (4)	C31—C32	1.377 (5)
C3—C4	1.389 (5)	C32—C33	1.413 (4)
C3—C6	1.491 (4)	C33—C34	1.359 (3)
C4—C5	1.313 (5)	C33—C36	1.532 (4)
C6—C7	1.374 (4)	C34—C35	1.381 (5)

O7—Gd1—O10ⁱ	90.81 (6)	C11—C10—C9	124.2 (3)
O7—Gd1—O3	80.52 (6)	C10—C11—C6	119.5 (3)
O10ⁱ—Gd1—O3	161.73 (7)	O3—C12—O4	123.7 (3)
O7—Gd1—O1W	147.21 (10)	O3—C12—C9	119.9 (2)
O10ⁱ—Gd1—O1W	84.09 (8)	O4—C12—C9	116.3 (3)
O3—Gd1—O1W	111.80 (8)	C13—N3—C17	120.0
O7—Gd1—O8ⁱ	73.62 (8)	N3—C13—C14	120.0
O10ⁱ—Gd1—O8ⁱ	77.37 (8)	C15—C14—C13	120.0
O3—Gd1—O8ⁱ	84.74 (8)	C14—C15—C16	120.0
O1W—Gd1—O8ⁱ	135.64 (10)	C14—C15—C18	113.2 (4)
O7—Gd1—O4ⁱ	143.39 (7)	C16—C15—C18	123.1 (4)
O10ⁱ—Gd1—O4ⁱ	102.01 (7)	C15—C16—C17	120.0
O3—Gd1—O4ⁱ	76.82 (7)	C16—C17—N3	120.0
O1W—Gd1—O4ⁱ	68.98 (8)	C13A—N3A—C17A	120.0
O8ⁱ—Gd1—O4ⁱ	75.98 (7)	C14A—C13A—N3A	120.0
O7—Gd1—O9	73.34 (7)	C13A—C14A—C15A	120.0
O10ⁱ—Gd1—O9	84.58 (6)	C14A—C15A—C16A	120.0
O3—Gd1—O9	107.92 (6)	C14A—C15A—C18	134.2 (4)
O1W—Gd1—O9	73.94 (9)	C16A—C15A—C18	105.8 (4)
O8ⁱ—Gd1—O9	141.85 (7)	C17A—C16A—C15A	120.0
O4ⁱ—Gd1—O9	141.28 (6)	C16A—C17A—N3A	120.0
O7—Gd1—O2W	116.30 (9)	C19—C18—C23	116.3 (4)
O10ⁱ—Gd1—O2W	137.77 (8)	C19—C18—C15	109.8 (5)
O3—Gd1—O2W	60.11 (9)	C23—C18—C15	133.3 (5)
O1W—Gd1—O2W	55.31 (11)	C19—C18—C15A	141.0 (5)
O8ⁱ—Gd1—O2W	138.94 (9)	C23—C18—C15A	96.3 (4)
O4ⁱ—Gd1—O2W	75.84 (7)	C15—C18—C15A	46.9 (4)
O9—Gd1—O2W	74.23 (7)	C18—C19—C20	125.0 (5)
C12—O3—Gd1	140.34 (14)	C18—C19—N4A	103.8 (4)
C12—O4—Gd1ⁱⁱ	129.2 (2)	C20—C19—N4A	124.4 (5)
C24—O7—Gd1	156.00 (17)	C18—C19—N4	125.6 (4)
C24—O8—Gd1ⁱⁱ	141.20 (16)	C20—C19—N4	107.9 (4)
C36—O9—Gd1	123.25 (15)	N4A—C19—N4	44.9 (4)
C36—O10—Gd1ⁱⁱ	144.66 (17)	C21—C20—C19	118.5 (3)
C1—N1—C5	115.0 (3)	C20—C21—C22	120.3 (2)
O2—N2—O1	120.0 (3)	C20—C21—C24	118.7 (2)
O2—N2—C7	123.7 (3)	C22—C21—C24	121.0 (3)
O1—N2—C7	116.2 (3)	C21—C22—C23	119.5 (3)
O5—N4—O6	128.4 (7)	C22—C23—C18	119.9 (4)
O5—N4—C19	111.2 (5)	O7—C24—O8	125.8 (2)
O6—N4—C19	120.1 (5)	O7—C24—C21	117.0 (2)
O6A—N4A—O5A	121.4 (10)	O8—C24—C21	117.2 (2)
O6A—N4A—C19	99.3 (8)	N5—C25—C26	118.8 (6)
O5A—N4A—C19	139.4 (7)	C27—C26—C25	129.6 (5)
C25—N5—C29	122.0 (5)	C26—C27—C28	111.4 (5)
O11—N6—O12	122.8 (3)	C26—C27—C30	126.6 (4)
O11—N6—C35	120.1 (3)	C28—C27—C30	121.5 (5)
O12—N6—C35	117.0 (4)	C27—C28—C29	124.4 (7)
N1—C1—C2	123.7 (4)	N5—C29—C28	113.2 (7)
C3—C2—C1	118.2 (4)	C35—C30—C31	117.7 (3)
C2—C3—C4	118.7 (3)	C35—C30—C27	124.7 (3)
C2—C3—C6	121.4 (3)	C31—C30—C27	117.6 (4)
C4—C3—C6	119.2 (3)	C32—C31—C30	120.2 (4)
C5—C4—C3	119.9 (3)	C31—C32—C33	119.5 (3)
C4—C5—N1	124.3 (4)	C34—C33—C32	120.8 (3)
C7—C6—C11	116.3 (3)	C34—C33—C36	120.1 (3)
C7—C6—C3	126.3 (3)	C32—C33—C36	119.1 (2)
C11—C6—C3	117.2 (3)	C33—C34—C35	118.9 (3)
C6—C7—C8	123.2 (3)	C30—C35—C34	122.7 (3)
C6—C7—N2	119.2 (3)	C30—C35—N6	122.1 (3)
C8—C7—N2	117.4 (3)	C34—C35—N6	115.1 (3)
C7—C8—C9	120.4 (3)	O9—C36—O10	124.2 (2)
C10—C9—C8	116.2 (3)	O9—C36—C33	117.7 (2)
C10—C9—C12	122.6 (2)	O10—C36—C33	118.1 (2)
C8—C9—C12	121.2 (3)

O7—Gd1—O3—C12	26.5 (3)	C14A—C15A—C18—C23	33.5 (6)
O10ⁱ—Gd1—O3—C12	−36.1 (4)	C16A—C15A—C18—C23	−147.5 (3)
O1W—Gd1—O3—C12	174.8 (3)	C14A—C15A—C18—C15	−179.2 (8)
O8ⁱ—Gd1—O3—C12	−47.7 (3)	C16A—C15A—C18—C15	−0.2 (5)
O4ⁱ—Gd1—O3—C12	−124.6 (3)	C23—C18—C19—C20	7.3 (7)
O9—Gd1—O3—C12	95.4 (3)	C15—C18—C19—C20	−164.4 (5)
O2W—Gd1—O3—C12	154.4 (3)	C15A—C18—C19—C20	150.9 (6)
O10ⁱ—Gd1—O7—C24	−146.7 (5)	C23—C18—C19—N4A	−144.6 (6)
O3—Gd1—O7—C24	49.5 (5)	C15—C18—C19—N4A	43.7 (7)
O1W—Gd1—O7—C24	−66.4 (5)	C15A—C18—C19—N4A	−1.0 (10)
O8ⁱ—Gd1—O7—C24	136.7 (5)	C23—C18—C19—N4	171.6 (4)
O4ⁱ—Gd1—O7—C24	101.7 (5)	C15—C18—C19—N4	−0.1 (6)
O9—Gd1—O7—C24	−62.6 (5)	C15A—C18—C19—N4	−44.8 (10)
O2W—Gd1—O7—C24	−0.3 (5)	O6A—N4A—C19—C18	−154.0 (11)
O7—Gd1—O9—C36	73.1 (2)	O5A—N4A—C19—C18	25.4 (16)
O10ⁱ—Gd1—O9—C36	165.5 (2)	O6A—N4A—C19—C20	53.8 (13)
O3—Gd1—O9—C36	−0.8 (2)	O5A—N4A—C19—C20	−126.8 (13)
O1W—Gd1—O9—C36	−109.1 (2)	O6A—N4A—C19—N4	−27.0 (10)
O8ⁱ—Gd1—O9—C36	104.0 (2)	O5A—N4A—C19—N4	152.5 (17)
O4ⁱ—Gd1—O9—C36	−92.0 (2)	O5—N4—C19—C18	59.3 (7)
O2W—Gd1—O9—C36	−51.4 (2)	O6—N4—C19—C18	−126.0 (8)
C5—N1—C1—C2	3.5 (8)	O5—N4—C19—C20	−134.2 (5)
N1—C1—C2—C3	−5.1 (8)	O6—N4—C19—C20	40.5 (9)
C1—C2—C3—C4	3.0 (7)	O5—N4—C19—N4A	−13.0 (7)
C1—C2—C3—C6	174.0 (4)	O6—N4—C19—N4A	161.7 (10)
C2—C3—C4—C5	0.2 (7)	C18—C19—C20—C21	−3.2 (7)
C6—C3—C4—C5	−170.9 (4)	N4A—C19—C20—C21	143.2 (6)
C3—C4—C5—N1	−1.9 (8)	N4—C19—C20—C21	−169.8 (3)
C1—N1—C5—C4	0.1 (8)	C19—C20—C21—C22	−0.3 (5)
C2—C3—C6—C7	59.3 (5)	C19—C20—C21—C24	179.7 (3)
C4—C3—C6—C7	−129.7 (4)	C20—C21—C22—C23	−0.9 (5)
C2—C3—C6—C11	−115.3 (4)	C24—C21—C22—C23	179.1 (3)
C4—C3—C6—C11	55.6 (4)	C21—C22—C23—C18	5.2 (6)
C11—C6—C7—C8	−1.1 (4)	C19—C18—C23—C22	−8.2 (6)
C3—C6—C7—C8	−175.8 (3)	C15—C18—C23—C22	161.0 (5)
C11—C6—C7—N2	−175.7 (2)	C15A—C18—C23—C22	−166.1 (4)
C3—C6—C7—N2	9.6 (4)	Gd1—O7—C24—O8	2.3 (7)
O2—N2—C7—C6	22.5 (3)	Gd1—O7—C24—C21	−176.9 (3)
O1—N2—C7—C6	−160.2 (2)	Gd1ⁱⁱ—O8—C24—O7	−23.9 (5)
O2—N2—C7—C8	−152.3 (2)	Gd1ⁱⁱ—O8—C24—C21	155.3 (2)
O1—N2—C7—C8	25.0 (3)	C20—C21—C24—O7	10.7 (4)
C6—C7—C8—C9	−0.5 (4)	C22—C21—C24—O7	−169.4 (3)
N2—C7—C8—C9	174.1 (2)	C20—C21—C24—O8	−168.6 (3)
C7—C8—C9—C10	−0.7 (3)	C22—C21—C24—O8	11.4 (4)
C7—C8—C9—C12	−180.0 (2)	C29—N5—C25—C26	2.5 (7)
C8—C9—C10—C11	3.8 (4)	N5—C25—C26—C27	3.1 (8)
C12—C9—C10—C11	−176.8 (3)	C25—C26—C27—C28	−1.5 (7)
C9—C10—C11—C6	−5.7 (4)	C25—C26—C27—C30	−173.5 (4)
C7—C6—C11—C10	4.1 (4)	C26—C27—C28—C29	−5.2 (7)
C3—C6—C11—C10	179.2 (3)	C30—C27—C28—C29	167.3 (5)
Gd1—O3—C12—O4	−84.6 (3)	C25—N5—C29—C28	−7.8 (7)
Gd1—O3—C12—C9	99.0 (2)	C27—C28—C29—N5	9.8 (8)
Gd1ⁱⁱ—O4—C12—O3	−8.5 (3)	C26—C27—C30—C35	−81.8 (6)
Gd1ⁱⁱ—O4—C12—C9	168.03 (15)	C28—C27—C30—C35	107.0 (6)
C10—C9—C12—O3	176.9 (2)	C26—C27—C30—C31	97.2 (6)
C8—C9—C12—O3	−3.8 (3)	C28—C27—C30—C31	−74.1 (5)
C10—C9—C12—O4	0.2 (3)	C35—C30—C31—C32	5.3 (6)
C8—C9—C12—O4	179.5 (2)	C27—C30—C31—C32	−173.8 (4)
C17—N3—C13—C14	0.0	C30—C31—C32—C33	−1.5 (6)
N3—C13—C14—C15	0.0	C31—C32—C33—C34	−1.7 (5)
C13—C14—C15—C16	0.0	C31—C32—C33—C36	177.7 (3)
C13—C14—C15—C18	−159.2 (4)	C32—C33—C34—C35	1.0 (5)
C14—C15—C16—C17	0.0	C36—C33—C34—C35	−178.4 (3)
C18—C15—C16—C17	157.0 (5)	C31—C30—C35—C34	−6.2 (6)
C15—C16—C17—N3	0.0	C27—C30—C35—C34	172.8 (4)
C13—N3—C17—C16	0.0	C31—C30—C35—N6	177.4 (4)
C17A—N3A—C13A—C14A	0.0	C27—C30—C35—N6	−3.6 (6)
N3A—C13A—C14A—C15A	0.0	C33—C34—C35—C30	3.1 (6)
C13A—C14A—C15A—C16A	0.0	C33—C34—C35—N6	179.8 (3)
C13A—C14A—C15A—C18	178.9 (6)	O11—N6—C35—C30	176.2 (4)
C14A—C15A—C16A—C17A	0.0	O12—N6—C35—C30	−5.8 (6)
C18—C15A—C16A—C17A	−179.2 (4)	O11—N6—C35—C34	−0.5 (6)
C15A—C16A—C17A—N3A	0.0	O12—N6—C35—C34	177.5 (4)
C13A—N3A—C17A—C16A	0.0	Gd1—O9—C36—O10	4.9 (4)
C14—C15—C18—C19	−143.1 (4)	Gd1—O9—C36—C33	−176.67 (17)
C16—C15—C18—C19	58.5 (6)	Gd1ⁱⁱ—O10—C36—O9	−102.2 (3)
C14—C15—C18—C23	47.2 (7)	Gd1ⁱⁱ—O10—C36—C33	79.4 (4)
C16—C15—C18—C23	−111.2 (6)	C34—C33—C36—O9	14.2 (4)
C14—C15—C18—C15A	−0.3 (5)	C32—C33—C36—O9	−165.2 (3)
C16—C15—C18—C15A	−158.8 (7)	C34—C33—C36—O10	−167.3 (3)
C14A—C15A—C18—C19	−114.1 (8)	C32—C33—C36—O10	13.3 (4)
C16A—C15A—C18—C19	64.9 (8)

Symmetry codes: (i) y, −x+y, z+1/6; (ii) x−y, x, z−1/6.

Poly[diaquatris[µ₂-3-nitro-4-(pyridin-4-yl)benzoato-κ²O:O']gadolinium(III)] (1502114) top

Crystal data top

[Gd(C₁₂H₇N₂O₄)₃(H₂O)₂]	D_x = 1.695 Mg m⁻³
M_r = 922.87	Mo Kα radiation, λ = 0.71073 Å
Hexagonal, P6₁	Cell parameters from 5480 reflections
Hall symbol: P 61	θ = 2.7–26.9°
a = 14.9709 (18) Å	µ = 1.91 mm⁻¹
c = 27.952 (3) Å	T = 296 K
V = 5425.5 (11) Å³	Rodlike, colorless
Z = 6	0.17 × 0.13 × 0.12 mm
F(000) = 2754

Data collection top

Bruker APEXII CCD diffractometer	6864 independent reflections
Radiation source: fine-focus sealed tube	5722 reflections with I > 2σ(I)
Graphite monochromator	R_int = 0.086
ω scans	θ_max = 26.0°, θ_min = 1.6°
Absorption correction: multi-scan (SADABS; Sheldrick, 2003)	h = −18→16
T_min = 0.742, T_max = 0.795	k = −18→18
40174 measured reflections	l = −34→33

Refinement top

Refinement on F²	Secondary atom site location: difference Fourier map
Least-squares matrix: full	Hydrogen site location: inferred from neighbouring sites
R[F² > 2σ(F²)] = 0.074	H atoms treated by a mixture of independent and constrained refinement
wR(F²) = 0.167	w = 1/[σ²(F_o²) + (0.0537P)² + 56.758P] where P = (F_o² + 2F_c²)/3
S = 1.05	(Δ/σ)_max = 0.003
6864 reflections	Δρ_max = 1.41 e Å⁻³
573 parameters	Δρ_min = −1.94 e Å⁻³
226 restraints	Absolute structure: Flack (1983), 3237 Friedel pairs
Primary atom site location: structure-invariant direct methods	Absolute structure parameter: 0.07 (3)

Special details top

Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å²) top

	x	y	z	U_iso*/U_eq	Occ. (<1)
Gd1	0.068500 (14)	0.037750 (17)	0.061199 (18)	0.03706 (5)
O1W	0.2374 (3)	0.1658 (3)	0.04233 (16)	0.1854 (13)
H1WA	0.2359 (5)	0.2218 (3)	0.0436 (8)	0.223*
H1WB	0.2754 (3)	0.1588 (5)	0.0628 (3)	0.223*
O1	−0.1553 (4)	0.1999 (5)	−0.0292 (2)	0.113 (2)
O2W	0.1899 (3)	0.2192 (3)	0.10031 (14)	0.1854 (13)
H2WA	0.2207 (3)	0.2140 (5)	0.1258 (2)	0.223*
H2WB	0.1456 (3)	0.2339 (4)	0.1131 (3)	0.223*
O2	−0.3197 (4)	0.1191 (5)	−0.03372 (19)	0.106 (2)
O3	−0.00511 (19)	0.1181 (2)	0.10530 (11)	0.0322 (9)
O4	−0.0917 (2)	0.0669 (3)	0.17338 (13)	0.0478 (12)
O5	−0.3400 (9)	−0.3594 (8)	0.0304 (4)	0.122 (4)	0.551 (5)
O5A	−0.2903 (9)	−0.4396 (8)	0.0383 (4)	0.093 (4)	0.449 (5)
O6	−0.3311 (7)	−0.5038 (7)	0.0342 (4)	0.096 (3)	0.551 (5)
O6A	−0.2753 (8)	−0.5542 (8)	0.0679 (4)	0.087 (4)	0.449 (5)
O7	−0.0299 (3)	−0.0930 (2)	0.11225 (13)	0.0471 (12)
O8	−0.0419 (3)	−0.0962 (2)	0.19224 (15)	0.0629 (15)
O9	0.1860 (2)	0.0144 (3)	0.11336 (12)	0.0499 (10)
O10	0.1580 (2)	0.0895 (2)	0.17591 (13)	0.0411 (10)
O11	0.3752 (4)	−0.1676 (4)	0.1329 (2)	0.117 (2)
O12	0.4575 (6)	−0.1564 (6)	0.1978 (3)	0.162 (3)
N1	−0.5970 (6)	0.1392 (6)	0.0301 (4)	0.142 (3)
N2	−0.2443 (3)	0.1492 (3)	−0.00965 (17)	0.0554 (15)
N4	−0.3131 (7)	−0.4112 (6)	0.0451 (3)	0.062 (3)	0.551 (5)
N4A	−0.2772 (10)	−0.4677 (9)	0.0720 (4)	0.075 (4)	0.449 (5)
N5	0.6515 (5)	−0.0100 (5)	0.3235 (3)	0.123 (3)
N6	0.4024 (4)	−0.1345 (4)	0.1737 (3)	0.0889 (17)
C1	−0.6046 (5)	0.0490 (6)	0.0438 (4)	0.112 (3)
H1A	−0.6695	−0.0098	0.0445	0.135*
C2	−0.5226 (4)	0.0409 (5)	0.0562 (4)	0.095 (3)
H2A	−0.5322	−0.0189	0.0711	0.114*
C3	−0.4235 (4)	0.1207 (4)	0.0472 (3)	0.069 (2)
C4	−0.4082 (4)	0.2161 (5)	0.0334 (3)	0.083 (2)
H4A	−0.3447	0.2766	0.0348	0.099*
C5	−0.5013 (6)	0.2117 (6)	0.0165 (4)	0.122 (3)
H5A	−0.4951	0.2617	−0.0052	0.147*
C6	−0.3354 (3)	0.1119 (3)	0.0676 (2)	0.0521 (16)
C7	−0.2478 (4)	0.1336 (4)	0.0409 (2)	0.0453 (16)
C8	−0.1663 (3)	0.1250 (3)	0.0601 (2)	0.0398 (14)
H8A	−0.1114	0.1353	0.0407	0.048*
C9	−0.1674 (4)	0.1008 (3)	0.10866 (18)	0.0392 (16)
C10	−0.2552 (4)	0.0797 (4)	0.1349 (2)	0.0508 (17)
H10A	−0.2601	0.0599	0.1668	0.061*
C11	−0.3346 (4)	0.0877 (5)	0.1145 (2)	0.064 (2)
H11A	−0.3902	0.0760	0.1336	0.077*
C12	−0.0827 (3)	0.0922 (3)	0.13013 (16)	0.0328 (13)
N3	−0.5835 (4)	−0.7263 (5)	0.1455 (3)	0.177 (7)	0.490 (5)
C13	−0.4926 (5)	−0.7225 (6)	0.1596 (4)	0.175 (4)	0.490 (5)
H13A	−0.4951	−0.7784	0.1754	0.210*	0.490 (5)
C14	−0.3980 (4)	−0.6353 (8)	0.1501 (5)	0.104 (5)	0.490 (5)
H14A	−0.3373	−0.6328	0.1595	0.125*	0.490 (5)
C15	−0.3943 (6)	−0.5518 (7)	0.1265 (5)	0.068 (4)	0.490 (5)
C16	−0.4852 (7)	−0.5555 (6)	0.1124 (4)	0.126 (4)	0.490 (5)
H16A	−0.4827	−0.4996	0.0966	0.151*	0.490 (5)
C17	−0.5797 (6)	−0.6428 (6)	0.1219 (4)	0.148 (3)	0.490 (5)
H17A	−0.6405	−0.6452	0.1125	0.177*	0.490 (5)
N3A	−0.4643 (5)	−0.7969 (4)	0.1751 (2)	0.111 (6)	0.510 (5)
C13A	−0.3728 (6)	−0.7419 (5)	0.2005 (3)	0.175 (4)	0.510 (5)
H13B	−0.3507	−0.7764	0.2207	0.210*	0.510 (5)
C14A	−0.3144 (6)	−0.6353 (5)	0.1958 (4)	0.069 (3)	0.510 (5)
H14B	−0.2532	−0.5985	0.2128	0.082*	0.510 (5)
C15A	−0.3474 (7)	−0.5838 (4)	0.1657 (4)	0.069 (4)	0.510 (5)
C16A	−0.4389 (8)	−0.6388 (6)	0.1402 (4)	0.096 (5)	0.510 (5)
H16B	−0.4610	−0.6043	0.1201	0.115*	0.510 (5)
C17A	−0.4974 (7)	−0.7453 (5)	0.1449 (3)	0.091 (5)	0.510 (5)
H17B	−0.5586	−0.7821	0.1279	0.109*	0.510 (5)
C18	−0.2925 (6)	−0.4537 (6)	0.1432 (4)	0.102 (3)
C19	−0.2594 (6)	−0.3912 (7)	0.1042 (3)	0.108 (3)
C20	−0.1884 (4)	−0.2929 (5)	0.1061 (2)	0.073 (2)
H20A	−0.1669	−0.2532	0.0784	0.088*
C21	−0.1460 (3)	−0.2495 (3)	0.1503 (2)	0.0409 (15)
C22	−0.1764 (5)	−0.3066 (4)	0.1909 (3)	0.062 (2)
H22A	−0.1479	−0.2765	0.2202	0.075*
C23	−0.2532 (5)	−0.4146 (4)	0.1883 (3)	0.078 (2)
H23A	−0.2753	−0.4560	0.2154	0.093*
C24	−0.0661 (4)	−0.1371 (3)	0.15239 (19)	0.0447 (17)
C25	0.6812 (7)	0.0430 (7)	0.2842 (4)	0.132 (4)
H25A	0.7500	0.0811	0.2751	0.159*
C26	0.5966 (6)	0.0376 (7)	0.2555 (4)	0.115 (3)
H26A	0.6145	0.0784	0.2281	0.139*
C27	0.4986 (4)	−0.0194 (5)	0.2649 (3)	0.105 (3)
C28	0.4801 (8)	−0.0693 (8)	0.3019 (5)	0.167 (4)
H28A	0.4107	−0.1151	0.3078	0.200*
C29	0.5522 (8)	−0.0674 (8)	0.3384 (5)	0.173 (4)
H29A	0.5323	−0.1010	0.3677	0.207*
C30	0.4154 (4)	−0.0099 (5)	0.2380 (3)	0.083 (2)
C31	0.3822 (5)	0.0565 (4)	0.2548 (3)	0.079 (2)
H31A	0.4097	0.0931	0.2830	0.095*
C32	0.3086 (5)	0.0684 (5)	0.2299 (3)	0.072 (2)
H32A	0.2823	0.1078	0.2428	0.087*
C33	0.2739 (3)	0.0205 (3)	0.18499 (19)	0.0398 (13)
C34	0.3072 (3)	−0.0429 (4)	0.1690 (2)	0.0486 (16)
H34A	0.2823	−0.0768	0.1400	0.058*
C35	0.3769 (4)	−0.0590 (4)	0.1943 (3)	0.071 (2)
C36	0.2022 (3)	0.0431 (3)	0.15579 (19)	0.0362 (13)

Atomic displacement parameters (Å²) top

	U¹¹	U²²	U³³	U¹²	U¹³	U²³
Gd1	0.04588 (6)	0.05846 (8)	0.02227 (8)	0.03764 (5)	0.00015 (11)	0.00098 (9)
O1W	0.1844 (17)	0.1834 (17)	0.1893 (19)	0.0926 (11)	−0.0070 (15)	0.0036 (15)
O1	0.077 (2)	0.169 (4)	0.077 (4)	0.051 (2)	0.013 (3)	0.018 (3)
O2W	0.1844 (17)	0.1834 (17)	0.1893 (19)	0.0926 (11)	−0.0070 (15)	0.0036 (15)
O2	0.076 (3)	0.146 (4)	0.066 (3)	0.034 (3)	−0.030 (2)	0.006 (3)
O3	0.0382 (11)	0.0370 (11)	0.0331 (17)	0.0275 (8)	0.0051 (12)	0.0073 (11)
O4	0.0381 (15)	0.0522 (17)	0.040 (2)	0.0128 (13)	0.0010 (15)	0.0058 (16)
O5	0.145 (6)	0.105 (5)	0.107 (6)	0.057 (4)	−0.036 (5)	0.006 (5)
O5A	0.105 (6)	0.074 (5)	0.084 (6)	0.033 (4)	−0.012 (5)	0.020 (5)
O6	0.095 (5)	0.088 (4)	0.083 (5)	0.030 (3)	0.017 (4)	−0.034 (4)
O6A	0.106 (5)	0.076 (4)	0.069 (6)	0.037 (4)	0.011 (5)	−0.020 (4)
O7	0.0736 (19)	0.0253 (12)	0.0373 (19)	0.0210 (12)	−0.0048 (16)	0.0081 (12)
O8	0.094 (2)	0.0210 (14)	0.050 (2)	0.0112 (15)	−0.0288 (19)	0.0020 (14)
O9	0.0638 (12)	0.1031 (17)	0.0159 (16)	0.0667 (10)	−0.0135 (12)	−0.0056 (13)
O10	0.0471 (12)	0.0459 (12)	0.046 (2)	0.0347 (9)	−0.0027 (13)	0.0023 (13)
O11	0.162 (3)	0.138 (3)	0.099 (4)	0.111 (2)	0.018 (3)	0.002 (3)
O12	0.176 (3)	0.164 (3)	0.188 (4)	0.116 (2)	−0.045 (3)	−0.020 (3)
N1	0.109 (4)	0.141 (5)	0.183 (7)	0.067 (3)	−0.021 (4)	0.024 (5)
N2	0.0560 (18)	0.072 (2)	0.049 (3)	0.0402 (14)	−0.0153 (18)	0.008 (2)
N4	0.076 (4)	0.042 (3)	0.067 (5)	0.030 (3)	−0.042 (4)	−0.037 (3)
N4A	0.087 (6)	0.067 (5)	0.046 (6)	0.019 (4)	0.013 (5)	−0.016 (4)
N5	0.134 (3)	0.114 (3)	0.155 (6)	0.087 (2)	−0.030 (4)	−0.003 (4)
N6	0.0875 (19)	0.090 (2)	0.127 (4)	0.0725 (13)	−0.025 (2)	−0.005 (2)
C1	0.057 (3)	0.108 (4)	0.165 (7)	0.036 (3)	−0.001 (4)	0.042 (4)
C2	0.043 (2)	0.101 (3)	0.150 (7)	0.0435 (19)	0.023 (4)	0.052 (4)
C3	0.049 (2)	0.049 (2)	0.113 (6)	0.0275 (17)	−0.006 (3)	0.023 (3)
C4	0.057 (2)	0.076 (3)	0.130 (5)	0.0445 (18)	−0.019 (3)	0.017 (3)
C5	0.107 (4)	0.105 (4)	0.152 (6)	0.051 (3)	−0.027 (4)	0.048 (4)
C6	0.0466 (16)	0.065 (2)	0.066 (4)	0.0442 (12)	0.012 (2)	0.015 (2)
C7	0.046 (2)	0.047 (2)	0.042 (3)	0.0228 (17)	0.010 (2)	0.013 (2)
C8	0.0243 (16)	0.0368 (19)	0.048 (3)	0.0072 (14)	−0.001 (2)	0.005 (2)
C9	0.038 (2)	0.026 (2)	0.030 (2)	−0.0021 (17)	0.004 (2)	−0.0045 (18)
C10	0.053 (2)	0.064 (3)	0.041 (3)	0.0336 (17)	0.020 (2)	0.006 (2)
C11	0.056 (2)	0.099 (3)	0.053 (3)	0.0510 (19)	0.020 (2)	0.001 (3)
C12	0.0476 (19)	0.0298 (17)	0.022 (2)	0.0205 (13)	0.0105 (18)	0.0040 (16)
N3	0.152 (8)	0.171 (8)	0.197 (10)	0.073 (5)	0.000 (7)	0.004 (8)
C13	0.175 (5)	0.173 (5)	0.179 (5)	0.088 (3)	0.008 (4)	−0.003 (4)
C14	0.110 (7)	0.096 (6)	0.119 (8)	0.061 (4)	−0.012 (6)	0.021 (6)
C15	0.049 (5)	0.049 (5)	0.074 (7)	0.001 (4)	−0.003 (5)	−0.011 (5)
C16	0.121 (6)	0.132 (6)	0.134 (6)	0.071 (4)	0.024 (5)	−0.014 (5)
C17	0.145 (4)	0.149 (4)	0.146 (4)	0.071 (3)	0.004 (4)	0.004 (4)
N3A	0.138 (9)	0.092 (7)	0.104 (10)	0.058 (6)	0.031 (8)	−0.004 (7)
C13A	0.175 (5)	0.173 (5)	0.179 (5)	0.088 (3)	0.008 (4)	−0.003 (4)
C14A	0.076 (4)	0.059 (4)	0.072 (5)	0.034 (3)	0.000 (4)	0.001 (3)
C15A	0.068 (6)	0.060 (5)	0.077 (9)	0.029 (4)	0.003 (6)	−0.026 (6)
C16A	0.088 (7)	0.086 (7)	0.084 (7)	0.021 (5)	−0.009 (6)	0.019 (6)
C17A	0.118 (7)	0.038 (4)	0.110 (8)	0.034 (4)	0.011 (6)	−0.020 (5)
C18	0.099 (3)	0.082 (3)	0.109 (4)	0.034 (2)	0.021 (3)	−0.025 (3)
C19	0.095 (3)	0.113 (4)	0.098 (4)	0.039 (2)	0.023 (3)	−0.032 (3)
C20	0.050 (3)	0.078 (3)	0.070 (4)	0.017 (2)	0.011 (3)	−0.046 (3)
C21	0.037 (2)	0.0279 (19)	0.051 (3)	0.0114 (15)	0.011 (2)	0.003 (2)
C22	0.068 (3)	0.027 (2)	0.076 (4)	0.012 (2)	−0.001 (3)	0.014 (2)
C23	0.089 (3)	0.031 (2)	0.111 (5)	0.028 (2)	0.047 (3)	0.023 (3)
C24	0.059 (3)	0.025 (2)	0.036 (3)	0.0098 (17)	0.004 (2)	0.0017 (19)
C25	0.135 (4)	0.144 (4)	0.157 (7)	0.099 (3)	−0.031 (5)	−0.043 (5)
C26	0.109 (3)	0.130 (4)	0.123 (4)	0.072 (2)	−0.021 (3)	−0.026 (3)
C27	0.123 (4)	0.087 (3)	0.124 (6)	0.066 (2)	−0.041 (4)	0.005 (4)
C28	0.157 (6)	0.162 (5)	0.171 (7)	0.072 (4)	−0.051 (5)	0.053 (5)
C29	0.168 (6)	0.177 (6)	0.194 (8)	0.102 (4)	−0.034 (5)	0.058 (5)
C30	0.083 (3)	0.081 (3)	0.100 (5)	0.051 (2)	−0.052 (3)	−0.025 (3)
C31	0.101 (3)	0.072 (3)	0.081 (4)	0.056 (2)	−0.051 (3)	−0.019 (3)
C32	0.082 (3)	0.076 (3)	0.057 (4)	0.038 (2)	−0.035 (3)	−0.018 (3)
C33	0.0450 (16)	0.0425 (17)	0.047 (3)	0.0331 (12)	−0.0283 (18)	−0.0103 (18)
C34	0.0427 (19)	0.047 (2)	0.065 (4)	0.0294 (14)	−0.019 (2)	−0.011 (2)
C35	0.081 (2)	0.060 (2)	0.104 (5)	0.0592 (14)	−0.044 (3)	−0.023 (3)
C36	0.0393 (17)	0.0385 (16)	0.042 (3)	0.0278 (12)	−0.0085 (19)	0.0052 (18)

Geometric parameters (Å, º) top

Gd1—O7	2.270 (3)	C6—C7	1.396 (7)
Gd1—O10ⁱ	2.288 (3)	C7—C8	1.396 (8)
Gd1—O1W	2.346 (3)	C8—C9	1.404 (8)
Gd1—O3	2.347 (3)	C9—C10	1.397 (7)
Gd1—O8ⁱ	2.361 (3)	C9—C12	1.466 (8)
Gd1—O4ⁱ	2.374 (4)	C10—C11	1.376 (9)
Gd1—O9	2.440 (4)	N3—C13	1.3900
Gd1—O2W	2.635 (4)	N3—C17	1.3900
O1—N2	1.280 (6)	C13—C14	1.3900
O2—N2	1.192 (6)	C14—C15	1.3900
O3—C12	1.237 (5)	C15—C16	1.3900
O4—C12	1.254 (6)	C15—C18	1.568 (10)
O4—Gd1ⁱⁱ	2.375 (4)	C16—C17	1.3900
O5—N4	1.116 (17)	N3A—C13A	1.3900
O5A—N4A	1.089 (18)	N3A—C17A	1.3900
O6—N4	1.309 (14)	C13A—C14A	1.3900
O6A—N4A	1.314 (19)	C14A—C15A	1.3900
O7—C24	1.277 (6)	C15A—C16A	1.3900
O8—C24	1.235 (6)	C15A—C18	1.805 (11)
O8—Gd1ⁱⁱ	2.361 (3)	C16A—C17A	1.3900
O9—C36	1.243 (6)	C18—C19	1.360 (13)
O10—C36	1.304 (6)	C18—C23	1.389 (12)
O10—Gd1ⁱⁱ	2.288 (3)	C19—C20	1.316 (9)
O11—N6	1.229 (9)	C20—C21	1.394 (8)
O12—N6	1.231 (11)	C21—C22	1.354 (8)
N1—C5	1.349 (10)	C21—C24	1.501 (6)
N1—C1	1.351 (14)	C22—C23	1.443 (7)
N2—C7	1.430 (7)	C25—C26	1.468 (15)
N4—C19	1.794 (13)	C26—C27	1.304 (10)
N4A—C19	1.374 (16)	C27—C28	1.222 (14)
N5—C25	1.295 (14)	C27—C30	1.521 (9)
N5—C29	1.358 (13)	C28—C29	1.475 (18)
N6—C35	1.478 (9)	C30—C35	1.393 (10)
C1—C2	1.339 (11)	C30—C31	1.397 (11)
C2—C3	1.386 (7)	C31—C32	1.390 (11)
C3—C4	1.383 (9)	C32—C33	1.410 (8)
C3—C6	1.503 (8)	C33—C34	1.349 (8)
C4—C5	1.441 (12)	C33—C36	1.515 (7)
C6—C11	1.364 (9)	C34—C35	1.379 (9)

O7—Gd1—O10ⁱ	93.18 (13)	C11—C10—C9	121.2 (5)
O7—Gd1—O1W	144.66 (15)	C6—C11—C10	123.0 (5)
O10ⁱ—Gd1—O1W	87.63 (14)	O3—C12—O4	125.4 (5)
O7—Gd1—O3	80.98 (12)	O3—C12—C9	117.4 (4)
O10ⁱ—Gd1—O3	162.28 (9)	O4—C12—C9	117.0 (4)
O1W—Gd1—O3	106.84 (12)	C13—N3—C17	120.0
O7—Gd1—O8ⁱ	73.97 (14)	C14—C13—N3	120.0
O10ⁱ—Gd1—O8ⁱ	78.07 (13)	C15—C14—C13	120.0
O1W—Gd1—O8ⁱ	140.08 (15)	C14—C15—C16	120.0
O3—Gd1—O8ⁱ	84.23 (13)	C14—C15—C18	106.5 (8)
O7—Gd1—O4ⁱ	144.19 (13)	C16—C15—C18	126.6 (7)
O10ⁱ—Gd1—O4ⁱ	100.35 (13)	C17—C16—C15	120.0
O1W—Gd1—O4ⁱ	69.52 (14)	C16—C17—N3	120.0
O3—Gd1—O4ⁱ	76.11 (11)	C13A—N3A—C17A	120.0
O8ⁱ—Gd1—O4ⁱ	76.64 (15)	N3A—C13A—C14A	120.0
O7—Gd1—O9	72.80 (12)	C13A—C14A—C15A	120.0
O10ⁱ—Gd1—O9	85.43 (11)	C14A—C15A—C16A	120.0
O1W—Gd1—O9	72.05 (13)	C14A—C15A—C18	135.5 (6)
O3—Gd1—O9	108.45 (12)	C16A—C15A—C18	104.1 (6)
O8ⁱ—Gd1—O9	141.78 (14)	C15A—C16A—C17A	120.0
O4ⁱ—Gd1—O9	140.79 (11)	C16A—C17A—N3A	120.0
O7—Gd1—O2W	116.35 (12)	C19—C18—C23	120.3 (7)
O10ⁱ—Gd1—O2W	135.74 (12)	C19—C18—C15	104.8 (8)
O1W—Gd1—O2W	49.04 (13)	C23—C18—C15	132.3 (8)
O3—Gd1—O2W	60.78 (11)	C19—C18—C15A	146.5 (8)
O8ⁱ—Gd1—O2W	139.24 (16)	C23—C18—C15A	90.5 (7)
O4ⁱ—Gd1—O2W	75.21 (14)	C15—C18—C15A	52.3 (6)
O9—Gd1—O2W	74.04 (13)	C20—C19—C18	123.3 (8)
C12—O3—Gd1	137.8 (3)	C20—C19—N4A	132.1 (9)
C12—O4—Gd1ⁱⁱ	130.5 (3)	C18—C19—N4A	95.7 (9)
C24—O7—Gd1	157.4 (3)	C20—C19—N4	105.6 (7)
C24—O8—Gd1ⁱⁱ	140.0 (3)	C18—C19—N4	130.1 (6)
C36—O9—Gd1	123.4 (3)	N4A—C19—N4	51.3 (8)
C36—O10—Gd1ⁱⁱ	144.1 (3)	C19—C20—C21	118.9 (7)
C5—N1—C1	114.1 (9)	C22—C21—C20	121.2 (4)
O2—N2—O1	119.4 (5)	C22—C21—C24	120.2 (5)
O2—N2—C7	123.1 (4)	C20—C21—C24	118.6 (5)
O1—N2—C7	117.5 (4)	C21—C22—C23	119.5 (6)
O5—N4—O6	134.0 (11)	C18—C23—C22	116.8 (7)
O5—N4—C19	120.6 (10)	O8—C24—O7	126.3 (4)
O6—N4—C19	103.3 (8)	O8—C24—C21	117.5 (4)
O5A—N4A—O6A	113.7 (13)	O7—C24—C21	116.2 (4)
O5A—N4A—C19	104.0 (14)	N5—C25—C26	114.1 (8)
O6A—N4A—C19	142.0 (13)	C27—C26—C25	125.6 (10)
C25—N5—C29	125.4 (10)	C28—C27—C26	114.1 (9)
O11—N6—O12	122.1 (8)	C28—C27—C30	122.0 (8)
O11—N6—C35	120.7 (7)	C26—C27—C30	123.0 (8)
O12—N6—C35	117.0 (7)	C27—C28—C29	129.3 (10)
C2—C1—N1	122.8 (6)	N5—C29—C28	111.0 (11)
C1—C2—C3	120.5 (7)	C35—C30—C31	118.1 (6)
C4—C3—C2	119.7 (6)	C35—C30—C27	121.8 (7)
C4—C3—C6	119.9 (4)	C31—C30—C27	119.9 (6)
C2—C3—C6	117.5 (6)	C32—C31—C30	120.7 (6)
C3—C4—C5	112.7 (5)	C31—C32—C33	119.7 (7)
N1—C5—C4	123.9 (9)	C34—C33—C32	118.8 (5)
C11—C6—C7	116.3 (5)	C34—C33—C36	122.1 (5)
C11—C6—C3	120.9 (5)	C32—C33—C36	119.2 (5)
C7—C6—C3	122.7 (6)	C33—C34—C35	122.1 (6)
C8—C7—C6	122.5 (5)	C34—C35—C30	120.4 (6)
C8—C7—N2	115.5 (5)	C34—C35—N6	116.2 (6)
C6—C7—N2	121.2 (5)	C30—C35—N6	123.3 (6)
C7—C8—C9	119.7 (5)	O9—C36—O10	122.1 (5)
C10—C9—C8	117.1 (5)	O9—C36—C33	118.3 (5)
C10—C9—C12	121.5 (5)	O10—C36—C33	119.5 (4)
C8—C9—C12	121.3 (4)

O7—Gd1—O3—C12	−23.1 (4)	C14A—C15A—C18—C23	−42.8 (10)
O10ⁱ—Gd1—O3—C12	48.7 (7)	C16A—C15A—C18—C23	145.2 (6)
O1W—Gd1—O3—C12	−167.6 (4)	C14A—C15A—C18—C15	169.6 (11)
O8ⁱ—Gd1—O3—C12	51.6 (5)	C16A—C15A—C18—C15	−2.5 (7)
O4ⁱ—Gd1—O3—C12	129.2 (5)	C23—C18—C19—C20	1.5 (17)
O9—Gd1—O3—C12	−91.4 (4)	C15—C18—C19—C20	165.5 (10)
O2W—Gd1—O3—C12	−150.2 (5)	C15A—C18—C19—C20	−152.9 (12)
O10ⁱ—Gd1—O7—C24	145.6 (11)	C23—C18—C19—N4A	152.1 (11)
O1W—Gd1—O7—C24	55.3 (12)	C15—C18—C19—N4A	−43.9 (11)
O3—Gd1—O7—C24	−51.2 (11)	C15A—C18—C19—N4A	−2.3 (19)
O8ⁱ—Gd1—O7—C24	−137.7 (11)	C23—C18—C19—N4	−165.4 (9)
O4ⁱ—Gd1—O7—C24	−101.7 (11)	C15—C18—C19—N4	−1.4 (15)
O9—Gd1—O7—C24	61.4 (11)	C15A—C18—C19—N4	40 (2)
O2W—Gd1—O7—C24	−0.2 (11)	O5A—N4A—C19—C20	−60.3 (19)
O7—Gd1—O9—C36	−74.8 (3)	O6A—N4A—C19—C20	112.3 (18)
O10ⁱ—Gd1—O9—C36	−169.6 (3)	O5A—N4A—C19—C18	153.2 (12)
O1W—Gd1—O9—C36	101.4 (3)	O6A—N4A—C19—C18	−34 (2)
O3—Gd1—O9—C36	−0.9 (3)	O5A—N4A—C19—N4	14.7 (9)
O8ⁱ—Gd1—O9—C36	−105.5 (3)	O6A—N4A—C19—N4	−173 (2)
O4ⁱ—Gd1—O9—C36	89.6 (3)	O5—N4—C19—C20	−50.4 (12)
O2W—Gd1—O9—C36	50.1 (3)	O6—N4—C19—C20	143.6 (9)
C5—N1—C1—C2	18.7 (16)	O5—N4—C19—C18	118.3 (13)
N1—C1—C2—C3	−12.3 (16)	O6—N4—C19—C18	−47.7 (14)
C1—C2—C3—C4	11.9 (14)	O5—N4—C19—N4A	177.7 (13)
C1—C2—C3—C6	172.5 (9)	O6—N4—C19—N4A	11.7 (9)
C2—C3—C4—C5	−17.5 (12)	C18—C19—C20—C21	−1.3 (15)
C6—C3—C4—C5	−177.6 (8)	N4A—C19—C20—C21	−140.2 (13)
C1—N1—C5—C4	−26.6 (16)	N4—C19—C20—C21	168.3 (7)
C3—C4—C5—N1	26.4 (14)	C19—C20—C21—C22	0.2 (11)
C4—C3—C6—C11	111.1 (8)	C19—C20—C21—C24	−179.2 (8)
C2—C3—C6—C11	−49.4 (9)	C20—C21—C22—C23	0.6 (10)
C4—C3—C6—C7	−64.9 (9)	C24—C21—C22—C23	−179.9 (6)
C2—C3—C6—C7	134.5 (7)	C19—C18—C23—C22	−0.5 (14)
C11—C6—C7—C8	3.9 (7)	C15—C18—C23—C22	−159.4 (11)
C3—C6—C7—C8	−179.9 (5)	C15A—C18—C23—C22	165.7 (7)
C11—C6—C7—N2	173.4 (5)	C21—C22—C23—C18	−0.5 (11)
C3—C6—C7—N2	−10.4 (8)	Gd1ⁱⁱ—O8—C24—O7	22.5 (12)
O2—N2—C7—C8	149.6 (6)	Gd1ⁱⁱ—O8—C24—C21	−157.3 (5)
O1—N2—C7—C8	−31.8 (8)	Gd1—O7—C24—O8	−0.7 (16)
O2—N2—C7—C6	−20.5 (9)	Gd1—O7—C24—C21	179.2 (7)
O1—N2—C7—C6	158.1 (6)	C22—C21—C24—O8	−11.0 (9)
C6—C7—C8—C9	−4.6 (7)	C20—C21—C24—O8	168.4 (6)
N2—C7—C8—C9	−174.6 (4)	C22—C21—C24—O7	169.1 (6)
C7—C8—C9—C10	4.1 (7)	C20—C21—C24—O7	−11.4 (9)
C7—C8—C9—C12	−179.4 (4)	C29—N5—C25—C26	0.5 (16)
C8—C9—C10—C11	−3.3 (7)	N5—C25—C26—C27	−4.5 (16)
C12—C9—C10—C11	−179.8 (5)	C25—C26—C27—C28	1.6 (16)
C7—C6—C11—C10	−3.0 (8)	C25—C26—C27—C30	170.7 (9)
C3—C6—C11—C10	−179.3 (5)	C26—C27—C28—C29	6 (2)
C9—C10—C11—C6	2.9 (9)	C30—C27—C28—C29	−163.7 (12)
Gd1—O3—C12—O4	82.7 (6)	C25—N5—C29—C28	4.9 (17)
Gd1—O3—C12—C9	−103.4 (5)	C27—C28—C29—N5	−9 (2)
Gd1ⁱⁱ—O4—C12—O3	5.2 (7)	C28—C27—C30—C35	−108.7 (11)
Gd1ⁱⁱ—O4—C12—C9	−168.8 (3)	C26—C27—C30—C35	83.0 (10)
C10—C9—C12—O3	−175.8 (4)	C28—C27—C30—C31	77.0 (11)
C8—C9—C12—O3	7.9 (6)	C26—C27—C30—C31	−91.2 (11)
C10—C9—C12—O4	−1.4 (6)	C35—C30—C31—C32	3.6 (8)
C8—C9—C12—O4	−177.7 (4)	C27—C30—C31—C32	178.0 (6)
C17—N3—C13—C14	0.0	C30—C31—C32—C33	−5.9 (8)
N3—C13—C14—C15	0.0	C31—C32—C33—C34	5.3 (7)
C13—C14—C15—C16	0.0	C31—C32—C33—C36	−173.6 (5)
C13—C14—C15—C18	152.6 (7)	C32—C33—C34—C35	−2.6 (7)
C14—C15—C16—C17	0.0	C36—C33—C34—C35	176.3 (4)
C18—C15—C16—C17	−146.7 (9)	C33—C34—C35—C30	0.4 (8)
C15—C16—C17—N3	0.0	C33—C34—C35—N6	177.0 (4)
C13—N3—C17—C16	0.0	C31—C30—C35—C34	−0.8 (8)
C17A—N3A—C13A—C14A	0.0	C27—C30—C35—C34	−175.1 (5)
N3A—C13A—C14A—C15A	0.0	C31—C30—C35—N6	−177.2 (5)
C13A—C14A—C15A—C16A	0.0	C27—C30—C35—N6	8.5 (8)
C13A—C14A—C15A—C18	−171.1 (9)	O11—N6—C35—C34	11.1 (8)
C14A—C15A—C16A—C17A	0.0	O12—N6—C35—C34	−173.9 (6)
C18—C15A—C16A—C17A	173.6 (6)	O11—N6—C35—C30	−172.4 (5)
C15A—C16A—C17A—N3A	0.0	O12—N6—C35—C30	2.6 (8)
C13A—N3A—C17A—C16A	0.0	Gd1—O9—C36—O10	−0.8 (5)
C14—C15—C18—C19	145.6 (7)	Gd1—O9—C36—C33	177.8 (2)
C16—C15—C18—C19	−64.1 (11)	Gd1ⁱⁱ—O10—C36—O9	104.2 (6)
C14—C15—C18—C23	−53.2 (13)	Gd1ⁱⁱ—O10—C36—C33	−74.3 (5)
C16—C15—C18—C23	97.1 (14)	C34—C33—C36—O9	−10.7 (6)
C14—C15—C18—C15A	−6.9 (6)	C32—C33—C36—O9	168.2 (4)
C16—C15—C18—C15A	143.4 (10)	C34—C33—C36—O10	167.9 (4)
C14A—C15A—C18—C19	115.3 (15)	C32—C33—C36—O10	−13.2 (6)
C16A—C15A—C18—C19	−56.7 (17)

Symmetry codes: (i) y, −x+y, z−1/6; (ii) x−y, x, z+1/6.

Poly[diaquatris[µ₂-3-nitro-4-(pyridin-4-yl)benzoato-κ²O:O']dysprosium(III)] (1502115) top

Crystal data top

[Dy(C₁₂H₇N₂O₄)₃(H₂O)₂]	D_x = 1.722 Mg m⁻³
M_r = 928.12	Mo Kα radiation, λ = 0.71073 Å
Hexagonal, P6₅	Cell parameters from 8195 reflections
Hall symbol: P 65	θ = 2.2–27.0°
a = 14.905 (4) Å	µ = 2.17 mm⁻¹
c = 27.912 (15) Å	T = 296 K
V = 5370 (3) Å³	Rodlike, colorless
Z = 6	0.17 × 0.14 × 0.11 mm
F(000) = 2766

Data collection top

Bruker APEXII CCD diffractometer	6872 independent reflections
Radiation source: fine-focus sealed tube	5684 reflections with I > 2σ(I)
Graphite monochromator	R_int = 0.083
ω scans	θ_max = 26.0°, θ_min = 1.6°
Absorption correction: multi-scan (SADABS; Sheldrick, 2003)	h = −17→18
T_min = 0.703, T_max = 0.788	k = −18→17
38985 measured reflections	l = −33→34

Refinement top

Refinement on F²	Secondary atom site location: difference Fourier map
Least-squares matrix: full	Hydrogen site location: inferred from neighbouring sites
R[F² > 2σ(F²)] = 0.052	H atoms treated by a mixture of independent and constrained refinement
wR(F²) = 0.135	w = 1/[σ²(F_o²) + (0.080P)² + 3.0141P] where P = (F_o² + 2F_c²)/3
S = 1.07	(Δ/σ)_max = 0.008
6872 reflections	Δρ_max = 2.46 e Å⁻³
579 parameters	Δρ_min = −1.48 e Å⁻³
241 restraints	Absolute structure: Flack (1983), 3287 Friedel pairs
Primary atom site location: structure-invariant direct methods	Absolute structure parameter: −0.02 (2)

Special details top

Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å²) top

	x	y	z	U_iso*/U_eq	Occ. (<1)
Dy1	0.040796 (8)	−0.026714 (8)	0.182051 (10)	0.03063 (3)
O1W	0.1768 (3)	−0.0572 (2)	0.19802 (13)	0.1811 (16)
H1WA	0.2337 (4)	−0.0057 (4)	0.2076 (3)	0.217*
H1WB	0.1621 (4)	−0.1100 (2)	0.21439 (18)	0.217*
O1	0.1957 (3)	0.3583 (2)	0.27148 (12)	0.1049 (12)
O2W	0.2162 (3)	0.04443 (19)	0.13363 (11)	0.1811 (16)
H2WA	0.2118 (4)	0.0863 (3)	0.11304 (14)	0.217*
H2WB	0.2087 (3)	−0.0085 (2)	0.1163 (2)	0.217*
O2	0.1231 (2)	0.4484 (2)	0.27568 (10)	0.0956 (11)
O3	0.11712 (13)	0.12341 (12)	0.13800 (7)	0.0342 (6)
O4	0.06233 (14)	0.15843 (15)	0.07047 (7)	0.0430 (6)
O5	−0.5038 (4)	−0.1803 (4)	0.2041 (2)	0.117 (2)	0.654 (3)
O5A	−0.5455 (5)	−0.2584 (6)	0.1801 (3)	0.083 (3)	0.346 (3)
O6	−0.3725 (5)	−0.0318 (5)	0.2100 (2)	0.130 (3)	0.654 (3)
O6A	−0.4084 (9)	−0.1113 (9)	0.2108 (5)	0.131 (3)	0.346 (3)
O7	−0.09342 (14)	−0.06121 (16)	0.13222 (8)	0.0468 (7)
O8	−0.09267 (16)	−0.05358 (18)	0.05242 (9)	0.0558 (9)
O9	0.02117 (15)	−0.16224 (13)	0.12945 (7)	0.0451 (7)
O10	0.09495 (14)	−0.06383 (13)	0.06445 (7)	0.0406 (7)
O11	−0.1724 (3)	−0.5352 (3)	0.11048 (15)	0.1249 (18)
O12	−0.1543 (3)	−0.6077 (3)	0.05096 (18)	0.1439 (13)
N1	0.1451 (3)	0.7434 (2)	0.21148 (16)	0.0906 (15)
N2	0.1511 (2)	0.39955 (19)	0.25254 (10)	0.0532 (9)
N4	−0.4287 (3)	−0.1108 (4)	0.1879 (3)	0.0819 (19)	0.654 (3)
N4A	−0.4626 (7)	−0.1892 (7)	0.1722 (4)	0.073 (2)	0.346 (3)
N5	−0.0180 (3)	−0.6653 (3)	−0.07722 (15)	0.0874 (13)
N6	−0.1350 (3)	−0.5324 (2)	0.07284 (16)	0.0851 (14)
C1	0.2280 (3)	0.7243 (3)	0.2183 (2)	0.0919 (18)
H1A	0.2912	0.7765	0.2299	0.110*
C2	0.2156 (3)	0.6295 (2)	0.20773 (17)	0.0718 (15)
H2A	0.2718	0.6189	0.2106	0.086*
C3	0.1198 (2)	0.5476 (2)	0.19266 (14)	0.0530 (11)
C4	0.0413 (3)	0.5696 (2)	0.18742 (18)	0.0722 (13)
H4A	−0.0238	0.5175	0.1778	0.087*
C5	0.0569 (3)	0.6647 (3)	0.1960 (2)	0.0917 (19)
H5A	0.0019	0.6763	0.1906	0.110*
C6	0.1093 (2)	0.44906 (19)	0.17515 (12)	0.0428 (9)
C7	0.1308 (2)	0.3825 (2)	0.20175 (11)	0.0394 (9)
C8	0.1240 (2)	0.29521 (19)	0.18274 (12)	0.0393 (8)
H8A	0.1373	0.2522	0.2020	0.047*
C9	0.0972 (2)	0.2694 (2)	0.13466 (10)	0.0363 (9)
C10	0.0747 (2)	0.3345 (2)	0.10889 (11)	0.0494 (10)
H10A	0.0524	0.3170	0.0774	0.059*
C11	0.0836 (2)	0.4243 (2)	0.12738 (13)	0.0556 (11)
H11A	0.0723	0.4682	0.1078	0.067*
C12	0.0912 (2)	0.1770 (2)	0.11368 (10)	0.0355 (9)
N3	−0.7414 (2)	−0.1539 (3)	0.09696 (16)	0.139 (4)	0.446 (3)
C13	−0.7392 (3)	−0.2399 (3)	0.0793 (2)	0.085 (2)	0.446 (3)
H13A	−0.7972	−0.2927	0.0642	0.102*	0.446 (3)
C14	−0.6502 (4)	−0.2471 (4)	0.0843 (3)	0.0734 (14)	0.446 (3)
H14A	−0.6487	−0.3047	0.0726	0.088*	0.446 (3)
C15	−0.5635 (3)	−0.1682 (4)	0.1070 (2)	0.0564 (9)	0.446 (3)
C16	−0.5657 (3)	−0.0822 (4)	0.1246 (2)	0.060 (2)	0.446 (3)
H16A	−0.5077	−0.0294	0.1397	0.072*	0.446 (3)
C17	−0.6547 (3)	−0.0750 (3)	0.1196 (2)	0.092 (3)	0.446 (3)
H17A	−0.6562	−0.0174	0.1314	0.110*	0.446 (3)
N3A	−0.7882 (3)	−0.3008 (4)	0.07785 (19)	0.166 (3)	0.554 (3)
C13A	−0.7404 (4)	−0.3466 (5)	0.0532 (2)	0.175 (4)	0.554 (3)
H13B	−0.7799	−0.4060	0.0351	0.210*	0.554 (3)
C14A	−0.6335 (4)	−0.3035 (6)	0.0555 (3)	0.134 (4)	0.554 (3)
H14B	−0.6015	−0.3341	0.0390	0.160*	0.554 (3)
C15A	−0.5744 (3)	−0.2146 (6)	0.0826 (3)	0.072 (2)	0.554 (3)
C16A	−0.6222 (4)	−0.1689 (5)	0.1073 (3)	0.150 (2)	0.554 (3)
H16B	−0.5826	−0.1095	0.1253	0.180*	0.554 (3)
C17A	−0.7291 (4)	−0.2120 (5)	0.1049 (2)	0.154 (2)	0.554 (3)
H17B	−0.7611	−0.1814	0.1214	0.185*	0.554 (3)
C18	−0.4567 (2)	−0.1587 (3)	0.0961 (2)	0.0934 (16)
C19	−0.3958 (3)	−0.1315 (3)	0.13671 (17)	0.0871 (13)
C20	−0.2961 (2)	−0.1048 (3)	0.13530 (13)	0.0571 (11)
H20A	−0.2577	−0.0868	0.1635	0.068*
C21	−0.25007 (18)	−0.1038 (2)	0.09308 (11)	0.0357 (9)
C22	−0.3059 (2)	−0.1320 (3)	0.05197 (13)	0.0537 (12)
H22A	−0.2751	−0.1322	0.0230	0.064*
C23	−0.4111 (3)	−0.1610 (3)	0.05387 (17)	0.0703 (15)
H23A	−0.4505	−0.1821	0.0260	0.084*
C24	−0.1362 (2)	−0.0699 (2)	0.09297 (11)	0.0426 (10)
C25	0.0354 (4)	−0.6338 (3)	−0.0371 (2)	0.106 (2)
H25A	0.0732	−0.6637	−0.0258	0.128*
C26	0.0329 (4)	−0.5564 (3)	−0.0129 (2)	0.1006 (17)
H26A	0.0783	−0.5294	0.0129	0.121*
C27	−0.0240 (3)	−0.5147 (3)	−0.02084 (17)	0.0826 (15)
C28	−0.0800 (4)	−0.5481 (4)	−0.0601 (3)	0.141 (2)
H28A	−0.1230	−0.5223	−0.0689	0.169*
C29	−0.0742 (5)	−0.6279 (5)	−0.0906 (3)	0.146 (3)
H29A	−0.1113	−0.6498	−0.1191	0.176*
C30	−0.0129 (3)	−0.4229 (3)	0.00530 (16)	0.0718 (14)
C31	0.0511 (3)	−0.3251 (3)	−0.01276 (15)	0.0699 (14)
H31A	0.0836	−0.3186	−0.0420	0.084*
C32	0.0688 (2)	−0.2363 (2)	0.01098 (14)	0.0587 (11)
H32A	0.1099	−0.1714	−0.0028	0.070*
C33	0.0224 (2)	−0.2460 (2)	0.05738 (11)	0.0377 (9)
C34	−0.0429 (2)	−0.3426 (2)	0.07422 (13)	0.0464 (10)
H34A	−0.0765	−0.3501	0.1033	0.056*
C35	−0.0607 (3)	−0.4301 (3)	0.04936 (16)	0.0644 (13)
C36	0.0466 (2)	−0.1504 (2)	0.08667 (13)	0.0454 (10)

Atomic displacement parameters (Å²) top

	U¹¹	U²²	U³³	U¹²	U¹³	U²³
Dy1	0.04360 (4)	0.03075 (4)	0.01963 (4)	0.02016 (3)	−0.00247 (6)	−0.00138 (5)
O1W	0.1805 (19)	0.1672 (19)	0.208 (3)	0.0963 (13)	0.012 (2)	−0.018 (2)
O1	0.1466 (18)	0.1135 (15)	0.0776 (19)	0.0823 (11)	−0.0271 (16)	−0.0214 (15)
O2W	0.1805 (19)	0.1672 (19)	0.208 (3)	0.0963 (13)	0.012 (2)	−0.018 (2)
O2	0.1419 (17)	0.1265 (15)	0.0518 (17)	0.0921 (11)	0.0005 (14)	−0.0257 (13)
O3	0.0418 (8)	0.0277 (7)	0.0300 (10)	0.0151 (5)	−0.0057 (8)	0.0001 (7)
O4	0.0470 (8)	0.0547 (9)	0.0311 (10)	0.0284 (6)	−0.0092 (8)	−0.0088 (8)
O5	0.114 (3)	0.125 (3)	0.109 (3)	0.0582 (18)	0.018 (2)	0.014 (2)
O5A	0.062 (3)	0.116 (4)	0.073 (4)	0.046 (2)	0.010 (4)	0.046 (4)
O6	0.116 (3)	0.166 (4)	0.092 (4)	0.059 (3)	0.017 (3)	−0.024 (3)
O6A	0.132 (4)	0.134 (4)	0.129 (4)	0.068 (2)	0.000 (3)	0.000 (3)
O7	0.0364 (8)	0.0726 (11)	0.0296 (12)	0.0258 (7)	−0.0099 (8)	−0.0089 (9)
O8	0.0467 (10)	0.0813 (14)	0.0289 (11)	0.0241 (9)	0.0082 (9)	−0.0068 (10)
O9	0.0870 (11)	0.0426 (8)	0.0122 (9)	0.0372 (7)	0.0020 (8)	−0.0075 (7)
O10	0.0496 (9)	0.0304 (8)	0.0374 (11)	0.0167 (6)	−0.0058 (9)	−0.0016 (8)
O11	0.170 (3)	0.098 (2)	0.100 (3)	0.0617 (18)	0.018 (2)	0.009 (2)
O12	0.1452 (16)	0.1322 (16)	0.1479 (19)	0.0645 (11)	0.0257 (15)	−0.0134 (15)
N1	0.0963 (17)	0.0573 (13)	0.133 (3)	0.0496 (11)	−0.005 (2)	−0.0199 (17)
N2	0.0683 (12)	0.0582 (11)	0.0418 (15)	0.0380 (9)	−0.0100 (12)	−0.0185 (11)
N4	0.0588 (19)	0.100 (3)	0.095 (4)	0.0457 (16)	0.018 (3)	0.020 (3)
N4A	0.068 (3)	0.083 (3)	0.063 (4)	0.033 (2)	0.002 (3)	0.002 (3)
N5	0.0868 (17)	0.0811 (16)	0.092 (2)	0.0405 (12)	0.0053 (17)	−0.0201 (17)
N6	0.0736 (17)	0.0393 (12)	0.136 (3)	0.0233 (11)	0.0021 (19)	−0.0243 (16)
C1	0.080 (2)	0.0647 (18)	0.138 (4)	0.0411 (14)	0.000 (2)	−0.014 (2)
C2	0.0608 (16)	0.0474 (14)	0.115 (4)	0.0331 (11)	−0.006 (2)	−0.0120 (18)
C3	0.0651 (14)	0.0413 (11)	0.062 (2)	0.0339 (9)	−0.0149 (15)	−0.0133 (13)
C4	0.0754 (16)	0.0540 (13)	0.098 (3)	0.0407 (11)	−0.029 (2)	−0.024 (2)
C5	0.0636 (16)	0.0702 (17)	0.153 (5)	0.0423 (12)	−0.027 (2)	−0.029 (2)
C6	0.0547 (13)	0.0307 (10)	0.0429 (18)	0.0212 (8)	−0.0013 (13)	−0.0014 (12)
C7	0.0474 (13)	0.0325 (12)	0.0311 (14)	0.0146 (9)	−0.0099 (12)	−0.0082 (11)
C8	0.0513 (11)	0.0413 (11)	0.0246 (13)	0.0227 (8)	0.0003 (14)	0.0025 (13)
C9	0.0452 (13)	0.0351 (11)	0.0216 (13)	0.0148 (9)	−0.0014 (11)	0.0049 (11)
C10	0.0791 (16)	0.0560 (13)	0.0213 (15)	0.0400 (10)	−0.0094 (13)	−0.0014 (12)
C11	0.0845 (15)	0.0521 (12)	0.0469 (19)	0.0467 (9)	−0.0179 (15)	0.0000 (13)
C12	0.0427 (12)	0.0346 (11)	0.0241 (14)	0.0156 (9)	−0.0027 (11)	0.0035 (11)
N3	0.117 (4)	0.163 (5)	0.171 (7)	0.096 (3)	0.015 (5)	0.022 (5)
C13	0.070 (3)	0.086 (3)	0.084 (3)	0.027 (2)	−0.013 (3)	−0.003 (3)
C14	0.0691 (18)	0.0740 (18)	0.076 (2)	0.0353 (11)	−0.0001 (16)	0.0012 (16)
C15	0.0544 (11)	0.0592 (11)	0.0570 (12)	0.0294 (7)	0.0005 (10)	0.0001 (10)
C16	0.058 (2)	0.078 (3)	0.058 (3)	0.0447 (19)	0.019 (3)	0.014 (3)
C17	0.097 (4)	0.103 (4)	0.086 (4)	0.057 (3)	0.002 (4)	0.007 (4)
N3A	0.149 (4)	0.179 (4)	0.176 (5)	0.086 (3)	−0.014 (4)	0.036 (4)
C13A	0.156 (5)	0.182 (5)	0.179 (5)	0.078 (4)	−0.014 (4)	0.029 (5)
C14A	0.113 (5)	0.146 (5)	0.150 (7)	0.070 (3)	−0.003 (5)	0.024 (5)
C15A	0.055 (2)	0.093 (3)	0.069 (3)	0.0379 (18)	0.009 (2)	0.019 (3)
C16A	0.140 (3)	0.175 (3)	0.148 (3)	0.089 (3)	0.003 (3)	0.008 (3)
C17A	0.146 (3)	0.169 (3)	0.150 (3)	0.0806 (19)	0.003 (2)	0.006 (2)
C18	0.0534 (14)	0.123 (2)	0.111 (3)	0.0500 (13)	0.009 (2)	0.054 (2)
C19	0.0863 (14)	0.137 (2)	0.079 (2)	0.0868 (11)	0.0435 (17)	0.0527 (19)
C20	0.0642 (14)	0.0839 (17)	0.0351 (17)	0.0461 (11)	0.0053 (14)	0.0132 (14)
C21	0.0316 (10)	0.0402 (12)	0.0364 (15)	0.0187 (8)	0.0017 (11)	0.0029 (11)
C22	0.0290 (13)	0.0684 (18)	0.050 (2)	0.0140 (12)	−0.0009 (14)	−0.0047 (16)
C23	0.0380 (15)	0.081 (2)	0.084 (3)	0.0233 (13)	−0.0083 (18)	−0.003 (2)
C24	0.0368 (12)	0.0511 (14)	0.0329 (16)	0.0167 (10)	0.0009 (12)	0.0012 (13)
C25	0.154 (3)	0.0651 (19)	0.105 (3)	0.0579 (17)	0.016 (3)	−0.014 (2)
C26	0.127 (2)	0.0821 (19)	0.097 (3)	0.0559 (15)	0.020 (2)	−0.012 (2)
C27	0.0692 (19)	0.0765 (18)	0.089 (2)	0.0268 (14)	0.0012 (19)	−0.0492 (17)
C28	0.135 (3)	0.152 (3)	0.170 (5)	0.0971 (19)	−0.023 (3)	−0.077 (3)
C29	0.129 (4)	0.128 (4)	0.161 (5)	0.048 (3)	−0.041 (4)	−0.064 (3)
C30	0.0714 (17)	0.0556 (14)	0.089 (3)	0.0325 (12)	0.0004 (19)	−0.0312 (16)
C31	0.076 (2)	0.0681 (17)	0.058 (2)	0.0304 (14)	0.0010 (18)	−0.0326 (16)
C32	0.0778 (14)	0.0633 (13)	0.0481 (19)	0.0452 (10)	0.0121 (16)	−0.0086 (15)
C33	0.0487 (12)	0.0383 (11)	0.0273 (14)	0.0227 (9)	0.0059 (11)	−0.0108 (11)
C34	0.0477 (13)	0.0433 (13)	0.050 (2)	0.0243 (10)	0.0009 (13)	−0.0027 (13)
C35	0.0652 (17)	0.0498 (15)	0.078 (3)	0.0288 (12)	−0.0003 (18)	−0.0184 (16)
C36	0.0391 (12)	0.0307 (11)	0.068 (2)	0.0185 (8)	−0.0050 (13)	−0.0117 (13)

Geometric parameters (Å, º) top

Dy1—O10ⁱ	2.261 (2)	C6—C7	1.399 (5)
Dy1—O7	2.274 (2)	C7—C8	1.360 (5)
Dy1—O3	2.2950 (18)	C8—C9	1.398 (4)
Dy1—O8ⁱ	2.321 (2)	C9—C10	1.377 (5)
Dy1—O1W	2.332 (5)	C9—C12	1.458 (4)
Dy1—O4ⁱ	2.362 (2)	C10—C11	1.377 (5)
Dy1—O9	2.394 (2)	N3—C13	1.3900
Dy1—O2W	2.648 (4)	N3—C17	1.3900
O1—N2	1.228 (5)	C13—C14	1.3900
O2—N2	1.193 (5)	C14—C15	1.3900
O3—C12	1.248 (4)	C15—C16	1.3900
O4—C12	1.264 (3)	C15—C18	1.555 (5)
O4—Dy1ⁱⁱ	2.362 (2)	C16—C17	1.3900
O5—N4	1.170 (7)	N3A—C13A	1.3900
O5A—N4A	1.168 (10)	N3A—C17A	1.3900
O6—N4	1.217 (8)	C13A—C14A	1.3900
O6A—N4A	1.490 (16)	C14A—C15A	1.3900
O7—C24	1.241 (4)	C15A—C16A	1.3900
O8—C24	1.266 (4)	C15A—C18	1.565 (6)
O8—Dy1ⁱⁱ	2.321 (2)	C16A—C17A	1.3900
O9—C36	1.239 (4)	C18—C23	1.370 (7)
O10—C36	1.280 (3)	C18—C19	1.380 (6)
O10—Dy1ⁱⁱ	2.261 (2)	C19—C20	1.332 (5)
O11—N6	1.180 (6)	C20—C21	1.360 (5)
O12—N6	1.181 (6)	C21—C22	1.355 (5)
N1—C5	1.323 (5)	C21—C24	1.509 (4)
N1—C1	1.413 (7)	C22—C23	1.404 (5)
N2—C7	1.445 (4)	C25—C26	1.352 (8)
N4—C19	1.591 (8)	C26—C27	1.298 (8)
N4A—C19	1.362 (10)	C27—C28	1.316 (8)
N5—C29	1.272 (10)	C27—C30	1.485 (6)
N5—C25	1.318 (7)	C28—C29	1.499 (11)
N6—C35	1.514 (5)	C30—C31	1.377 (5)
C1—C2	1.362 (6)	C30—C35	1.398 (6)
C2—C3	1.401 (4)	C31—C32	1.383 (5)
C3—C4	1.372 (6)	C32—C33	1.441 (5)
C3—C6	1.480 (5)	C33—C34	1.356 (4)
C4—C5	1.339 (6)	C33—C36	1.522 (4)
C6—C11	1.386 (5)	C34—C35	1.381 (5)

O10ⁱ—Dy1—O7	91.59 (7)	C9—C10—C11	123.4 (3)
O10ⁱ—Dy1—O3	164.40 (7)	C10—C11—C6	119.9 (3)
O7—Dy1—O3	81.02 (7)	O3—C12—O4	124.0 (3)
O10ⁱ—Dy1—O8ⁱ	78.35 (9)	O3—C12—C9	119.6 (2)
O7—Dy1—O8ⁱ	73.59 (9)	O4—C12—C9	116.3 (3)
O3—Dy1—O8ⁱ	86.35 (9)	C13—N3—C17	120.0
O10ⁱ—Dy1—O1W	90.17 (8)	C14—C13—N3	120.0
O7—Dy1—O1W	145.60 (11)	C13—C14—C15	120.0
O3—Dy1—O1W	103.71 (9)	C16—C15—C14	120.0
O8ⁱ—Dy1—O1W	140.07 (11)	C16—C15—C18	118.7 (3)
O10ⁱ—Dy1—O4ⁱ	101.65 (8)	C14—C15—C18	117.7 (3)
O7—Dy1—O4ⁱ	143.27 (8)	C17—C16—C15	120.0
O3—Dy1—O4ⁱ	77.25 (8)	C16—C17—N3	120.0
O8ⁱ—Dy1—O4ⁱ	75.79 (8)	C13A—N3A—C17A	120.0
O1W—Dy1—O4ⁱ	69.25 (9)	C14A—C13A—N3A	120.0
O10ⁱ—Dy1—O9	84.08 (8)	C15A—C14A—C13A	120.0
O7—Dy1—O9	73.24 (9)	C14A—C15A—C16A	120.0
O3—Dy1—O9	106.62 (7)	C14A—C15A—C18	130.2 (5)
O8ⁱ—Dy1—O9	141.76 (9)	C16A—C15A—C18	109.4 (5)
O1W—Dy1—O9	72.79 (10)	C17A—C16A—C15A	120.0
O4ⁱ—Dy1—O9	141.57 (7)	C16A—C17A—N3A	120.0
O10ⁱ—Dy1—O2W	140.43 (9)	C23—C18—C19	116.9 (4)
O7—Dy1—O2W	111.04 (10)	C23—C18—C15	131.6 (5)
O3—Dy1—O2W	55.06 (9)	C19—C18—C15	111.1 (5)
O8ⁱ—Dy1—O2W	138.03 (10)	C23—C18—C15A	102.5 (5)
O1W—Dy1—O2W	52.78 (11)	C19—C18—C15A	138.8 (5)
O4ⁱ—Dy1—O2W	79.65 (8)	C15—C18—C15A	34.5 (4)
O9—Dy1—O2W	72.82 (8)	C20—C19—N4A	124.3 (6)
C12—O3—Dy1	138.95 (16)	C20—C19—C18	122.4 (4)
C12—O4—Dy1ⁱⁱ	130.5 (2)	N4A—C19—C18	104.2 (5)
C24—O7—Dy1	155.7 (2)	C20—C19—N4	112.0 (4)
C24—O8—Dy1ⁱⁱ	141.93 (19)	N4A—C19—N4	43.1 (5)
C36—O9—Dy1	124.82 (18)	C18—C19—N4	125.0 (4)
C36—O10—Dy1ⁱⁱ	141.6 (2)	C19—C20—C21	120.7 (3)
C5—N1—C1	116.5 (4)	C22—C21—C20	120.1 (3)
O2—N2—O1	121.0 (3)	C22—C21—C24	121.0 (3)
O2—N2—C7	122.2 (3)	C20—C21—C24	118.8 (3)
O1—N2—C7	116.8 (3)	C21—C22—C23	118.8 (4)
O5—N4—O6	123.6 (7)	C18—C23—C22	121.1 (4)
O5—N4—C19	115.2 (5)	O7—C24—O8	125.6 (3)
O6—N4—C19	120.8 (5)	O7—C24—C21	117.8 (3)
O5A—N4A—C19	144.2 (10)	O8—C24—C21	116.6 (3)
O5A—N4A—O6A	118.3 (10)	N5—C25—C26	117.3 (6)
C19—N4A—O6A	95.4 (7)	C27—C26—C25	128.9 (5)
C29—N5—C25	120.4 (5)	C26—C27—C28	113.8 (5)
O12—N6—O11	122.7 (4)	C26—C27—C30	124.1 (4)
O12—N6—C35	116.2 (4)	C28—C27—C30	121.0 (5)
O11—N6—C35	121.1 (4)	C27—C28—C29	119.7 (7)
C2—C1—N1	120.1 (3)	N5—C29—C28	119.6 (6)
C1—C2—C3	121.3 (4)	C31—C30—C35	117.4 (4)
C4—C3—C2	116.3 (3)	C31—C30—C27	119.6 (4)
C4—C3—C6	121.5 (3)	C35—C30—C27	122.9 (3)
C2—C3—C6	121.3 (3)	C30—C31—C32	122.5 (4)
C5—C4—C3	121.2 (3)	C31—C32—C33	118.8 (3)
N1—C5—C4	124.5 (4)	C34—C33—C32	118.2 (3)
C11—C6—C7	116.9 (3)	C34—C33—C36	121.1 (3)
C11—C6—C3	117.4 (3)	C32—C33—C36	120.7 (2)
C7—C6—C3	125.5 (3)	C33—C34—C35	121.7 (3)
C8—C7—C6	122.5 (3)	C34—C35—C30	121.3 (3)
C8—C7—N2	117.4 (3)	C34—C35—N6	115.6 (4)
C6—C7—N2	119.8 (3)	C30—C35—N6	123.1 (3)
C7—C8—C9	120.8 (3)	O9—C36—O10	126.1 (3)
C10—C9—C8	116.4 (3)	O9—C36—C33	118.1 (2)
C10—C9—C12	122.3 (3)	O10—C36—C33	115.7 (3)
C8—C9—C12	121.3 (3)

O10ⁱ—Dy1—O3—C12	−37.9 (4)	C14A—C15A—C18—C19	−119.9 (8)
O7—Dy1—O3—C12	24.7 (3)	C16A—C15A—C18—C19	52.7 (8)
O8ⁱ—Dy1—O3—C12	−49.3 (3)	C14A—C15A—C18—C15	−165.7 (10)
O1W—Dy1—O3—C12	169.9 (3)	C16A—C15A—C18—C15	6.8 (6)
O4ⁱ—Dy1—O3—C12	−125.5 (3)	O5A—N4A—C19—C20	−134.8 (18)
O9—Dy1—O3—C12	94.1 (3)	O6A—N4A—C19—C20	64.6 (11)
O2W—Dy1—O3—C12	148.3 (3)	O5A—N4A—C19—C18	12 (2)
O10ⁱ—Dy1—O7—C24	−141.9 (5)	O6A—N4A—C19—C18	−148.1 (8)
O3—Dy1—O7—C24	51.9 (5)	O5A—N4A—C19—N4	139 (2)
O8ⁱ—Dy1—O7—C24	140.8 (6)	O6A—N4A—C19—N4	−21.6 (7)
O1W—Dy1—O7—C24	−49.2 (6)	C23—C18—C19—C20	2.3 (7)
O4ⁱ—Dy1—O7—C24	106.1 (6)	C15—C18—C19—C20	−170.6 (4)
O9—Dy1—O7—C24	−58.6 (5)	C15A—C18—C19—C20	163.5 (7)
O2W—Dy1—O7—C24	4.9 (6)	C23—C18—C19—N4A	−145.7 (7)
O10ⁱ—Dy1—O9—C36	167.1 (3)	C15—C18—C19—N4A	41.3 (7)
O7—Dy1—O9—C36	73.7 (3)	C15A—C18—C19—N4A	15.5 (11)
O3—Dy1—O9—C36	−1.3 (3)	C23—C18—C19—N4	172.2 (4)
O8ⁱ—Dy1—O9—C36	104.5 (3)	C15—C18—C19—N4	−0.7 (6)
O1W—Dy1—O9—C36	−100.8 (3)	C15A—C18—C19—N4	−26.6 (10)
O4ⁱ—Dy1—O9—C36	−91.6 (3)	O5—N4—C19—C20	−130.7 (6)
O2W—Dy1—O9—C36	−45.4 (3)	O6—N4—C19—C20	42.2 (9)
C5—N1—C1—C2	1.7 (8)	O5—N4—C19—N4A	−13.4 (9)
N1—C1—C2—C3	−3.6 (8)	O6—N4—C19—N4A	159.4 (11)
C1—C2—C3—C4	2.4 (7)	O5—N4—C19—C18	58.5 (8)
C1—C2—C3—C6	171.9 (4)	O6—N4—C19—C18	−128.6 (7)
C2—C3—C4—C5	0.6 (7)	N4A—C19—C20—C21	141.4 (7)
C6—C3—C4—C5	−168.8 (4)	C18—C19—C20—C21	−0.2 (7)
C1—N1—C5—C4	1.4 (8)	N4—C19—C20—C21	−171.3 (4)
C3—C4—C5—N1	−2.6 (9)	C19—C20—C21—C22	−1.3 (6)
C4—C3—C6—C11	54.9 (5)	C19—C20—C21—C24	178.1 (4)
C2—C3—C6—C11	−113.9 (4)	C20—C21—C22—C23	0.6 (5)
C4—C3—C6—C7	−130.2 (4)	C24—C21—C22—C23	−178.7 (3)
C2—C3—C6—C7	60.9 (5)	C19—C18—C23—C22	−3.0 (7)
C11—C6—C7—C8	−2.1 (4)	C15—C18—C23—C22	168.2 (5)
C3—C6—C7—C8	−177.0 (3)	C15A—C18—C23—C22	−170.4 (5)
C11—C6—C7—N2	−175.6 (3)	C21—C22—C23—C18	1.6 (6)
C3—C6—C7—N2	9.5 (4)	Dy1—O7—C24—O8	0.5 (8)
O2—N2—C7—C8	−152.6 (3)	Dy1—O7—C24—C21	179.7 (4)
O1—N2—C7—C8	25.0 (4)	Dy1ⁱⁱ—O8—C24—O7	−27.0 (6)
O2—N2—C7—C6	21.3 (4)	Dy1ⁱⁱ—O8—C24—C21	153.8 (3)
O1—N2—C7—C6	−161.1 (3)	C22—C21—C24—O7	−168.6 (3)
C6—C7—C8—C9	1.6 (4)	C20—C21—C24—O7	12.0 (5)
N2—C7—C8—C9	175.3 (2)	C22—C21—C24—O8	10.7 (5)
C7—C8—C9—C10	−2.4 (4)	C20—C21—C24—O8	−168.6 (3)
C7—C8—C9—C12	179.0 (3)	C29—N5—C25—C26	−4.2 (7)
C8—C9—C10—C11	3.9 (4)	N5—C25—C26—C27	8.2 (8)
C12—C9—C10—C11	−177.5 (3)	C25—C26—C27—C28	−6.0 (8)
C9—C10—C11—C6	−4.6 (5)	C25—C26—C27—C30	−173.9 (5)
C7—C6—C11—C10	3.4 (4)	C26—C27—C28—C29	0.4 (7)
C3—C6—C11—C10	178.8 (3)	C30—C27—C28—C29	168.8 (4)
Dy1—O3—C12—O4	−82.3 (4)	C25—N5—C29—C28	−0.5 (8)
Dy1—O3—C12—C9	100.1 (3)	C27—C28—C29—N5	2.6 (8)
Dy1ⁱⁱ—O4—C12—O3	−10.1 (4)	C26—C27—C30—C31	91.6 (6)
Dy1ⁱⁱ—O4—C12—C9	167.59 (16)	C28—C27—C30—C31	−75.5 (6)
C10—C9—C12—O3	176.6 (3)	C26—C27—C30—C35	−84.9 (6)
C8—C9—C12—O3	−4.9 (4)	C28—C27—C30—C35	107.9 (6)
C10—C9—C12—O4	−1.2 (4)	C35—C30—C31—C32	0.0 (7)
C8—C9—C12—O4	177.3 (2)	C27—C30—C31—C32	−176.7 (4)
C17—N3—C13—C14	0.0	C30—C31—C32—C33	2.9 (6)
N3—C13—C14—C15	0.0	C31—C32—C33—C34	−4.7 (5)
C13—C14—C15—C16	0.0	C31—C32—C33—C36	175.0 (4)
C13—C14—C15—C18	−158.5 (4)	C32—C33—C34—C35	3.7 (5)
C14—C15—C16—C17	0.0	C36—C33—C34—C35	−176.0 (4)
C18—C15—C16—C17	158.2 (4)	C33—C34—C35—C30	−0.8 (6)
C15—C16—C17—N3	0.0	C33—C34—C35—N6	179.6 (4)
C13—N3—C17—C16	0.0	C31—C30—C35—C34	−1.2 (7)
C17A—N3A—C13A—C14A	0.0	C27—C30—C35—C34	175.4 (4)
N3A—C13A—C14A—C15A	0.0	C31—C30—C35—N6	178.4 (4)
C13A—C14A—C15A—C16A	0.0	C27—C30—C35—N6	−5.0 (7)
C13A—C14A—C15A—C18	171.9 (7)	O12—N6—C35—C34	176.9 (5)
C14A—C15A—C16A—C17A	0.0	O11—N6—C35—C34	−1.7 (7)
C18—C15A—C16A—C17A	−173.4 (5)	O12—N6—C35—C30	−2.7 (7)
C15A—C16A—C17A—N3A	0.0	O11—N6—C35—C30	178.7 (5)
C13A—N3A—C17A—C16A	0.0	Dy1—O9—C36—O10	6.2 (5)
C16—C15—C18—C23	−112.4 (6)	Dy1—O9—C36—C33	−176.1 (2)
C14—C15—C18—C23	46.3 (7)	Dy1ⁱⁱ—O10—C36—O9	−98.3 (4)
C16—C15—C18—C19	59.2 (5)	Dy1ⁱⁱ—O10—C36—C33	83.9 (4)
C14—C15—C18—C19	−142.0 (4)	C34—C33—C36—O9	13.1 (5)
C16—C15—C18—C15A	−151.3 (8)	C32—C33—C36—O9	−166.6 (3)
C14—C15—C18—C15A	7.5 (7)	C34—C33—C36—O10	−168.9 (3)
C14A—C15A—C18—C23	43.0 (7)	C32—C33—C36—O10	11.4 (5)
C16A—C15A—C18—C23	−144.4 (4)

Symmetry codes: (i) y, −x+y, z+1/6; (ii) x−y, x, z−1/6.

Poly[diaquatris[µ₂-3-nitro-4-(pyridin-4-yl)benzoato-κ²O:O']dysprosium(III)] (1502116) top

Crystal data top

[Dy(C₁₂H₇N₂O₄)₃(H₂O)₂]	D_x = 1.719 Mg m⁻³
M_r = 928.12	Mo Kα radiation, λ = 0.71073 Å
Hexagonal, P6₁	Cell parameters from 8153 reflections
Hall symbol: P 61	θ = 2.7–25.1°
a = 14.9066 (18) Å	µ = 2.17 mm⁻¹
c = 27.948 (3) Å	T = 296 K
V = 5378.1 (11) Å³	Rodlike, colorless
Z = 6	0.17 × 0.13 × 0.11 mm
F(000) = 2766

Data collection top

Bruker APEXII CCD diffractometer	6126 independent reflections
Radiation source: fine-focus sealed tube	5654 reflections with I > 2σ(I)
Graphite monochromator	R_int = 0.058
ω scans	θ_max = 25.0°, θ_min = 1.6°
Absorption correction: multi-scan (SADABS; Sheldrick, 2003)	h = −16→17
T_min = 0.721, T_max = 0.788	k = −17→16
38354 measured reflections	l = −31→33

Refinement top

Refinement on F²	Secondary atom site location: difference Fourier map
Least-squares matrix: full	Hydrogen site location: inferred from neighbouring sites
R[F² > 2σ(F²)] = 0.040	H atoms treated by a mixture of independent and constrained refinement
wR(F²) = 0.110	w = 1/[σ²(F_o²) + (0.0665P)² + 9.5469P] where P = (F_o² + 2F_c²)/3
S = 1.05	(Δ/σ)_max = 0.012
6126 reflections	Δρ_max = 2.41 e Å⁻³
567 parameters	Δρ_min = −1.72 e Å⁻³
156 restraints	Absolute structure: Flack (1983), 2882 Friedel pairs
Primary atom site location: structure-invariant direct methods	Absolute structure parameter: −0.023 (17)

Special details top

Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å²) top

	x	y	z	U_iso*/U_eq	Occ. (<1)
Dy1	−0.067140 (8)	−0.027479 (9)	0.116275 (10)	0.02431 (3)
O1	0.1630 (3)	0.3566 (3)	0.20616 (12)	0.1007 (16)
O1W	−0.2353 (4)	−0.0602 (4)	0.13226 (17)	0.1533 (15)
H1WA	−0.2556	−0.0256	0.1487	0.184*
H1WB	−0.2824	−0.1235	0.1332	0.184*
O2	0.3275 (2)	0.4499 (3)	0.20848 (12)	0.0850 (14)
O2W	−0.1777 (3)	0.0435 (3)	0.06371 (15)	0.1533 (15)
H2WA	−0.2125	−0.0013	0.0421	0.184*
H2WB	−0.1360	0.1048	0.0576	0.184*
O3	0.00477 (14)	0.12270 (14)	0.07262 (8)	0.0312 (6)
O4	0.09488 (15)	0.15662 (17)	0.00489 (8)	0.0395 (7)
O5	0.3240 (3)	−0.1892 (4)	0.1347 (2)	0.1083 (19)	0.683 (3)
O5A	0.2807 (6)	−0.2670 (7)	0.1118 (4)	0.082 (3)	0.317 (3)
O6	0.3360 (5)	−0.0402 (5)	0.1443 (2)	0.115 (2)	0.683 (3)
O6A	0.2868 (10)	−0.1270 (11)	0.1444 (5)	0.111 (5)	0.317 (3)
O7	0.03302 (14)	−0.06082 (16)	0.06583 (9)	0.0389 (6)
O8	0.03780 (17)	−0.05592 (17)	−0.01427 (10)	0.0464 (7)
O9	−0.18345 (16)	−0.16179 (16)	0.06323 (8)	0.0390 (7)
O10	−0.15914 (15)	−0.06503 (14)	−0.00136 (8)	0.0344 (7)
O11	−0.3612 (3)	−0.5351 (3)	0.04513 (15)	0.0978 (15)
O12	−0.4547 (3)	−0.6092 (3)	−0.01403 (19)	0.1207 (13)
N1	0.5989 (3)	0.7448 (3)	0.14488 (17)	0.0751 (15)
N2	0.2485 (2)	0.3998 (2)	0.18623 (11)	0.0454 (10)
N4	0.3182 (3)	−0.1126 (4)	0.1229 (2)	0.0639 (16)	0.683 (3)
N4A	0.2848 (6)	−0.1777 (6)	0.1099 (4)	0.043 (3)	0.317 (3)
N5	−0.6478 (3)	−0.6674 (3)	−0.14369 (19)	0.0847 (15)
N6	−0.3972 (3)	−0.5321 (2)	0.00730 (18)	0.0727 (15)
C1	0.6094 (3)	0.6675 (3)	0.12911 (19)	0.0668 (16)
H1A	0.6762	0.6801	0.1237	0.080*
C2	0.5288 (3)	0.5696 (3)	0.12004 (19)	0.0576 (13)
H2A	0.5419	0.5176	0.1104	0.069*
C3	0.4277 (2)	0.5490 (3)	0.12538 (15)	0.0463 (12)
C4	0.4133 (3)	0.6300 (3)	0.14074 (19)	0.0628 (15)
H4A	0.3467	0.6193	0.1447	0.075*
C5	0.4980 (3)	0.7260 (3)	0.1500 (2)	0.0769 (19)
H5A	0.4875	0.7797	0.1598	0.092*
C6	0.3391 (2)	0.4497 (2)	0.10891 (13)	0.0381 (10)
C7	0.2519 (2)	0.3827 (2)	0.13633 (13)	0.0350 (9)
C8	0.1709 (2)	0.2948 (2)	0.11710 (13)	0.0344 (9)
H8A	0.1143	0.2522	0.1362	0.041*
C9	0.1722 (2)	0.2680 (2)	0.06872 (11)	0.0315 (9)
C10	0.2584 (2)	0.3333 (3)	0.04269 (13)	0.0436 (12)
H10A	0.2627	0.3173	0.0109	0.052*
C11	0.3388 (3)	0.4219 (3)	0.06213 (15)	0.0478 (12)
H11A	0.3950	0.4646	0.0428	0.057*
C12	0.0853 (2)	0.1748 (2)	0.04773 (11)	0.0285 (8)
N3	0.57965 (19)	−0.1698 (2)	0.02880 (15)	0.122 (3)	0.590 (4)
C13	0.4886 (2)	−0.2519 (3)	0.0108 (2)	0.100 (3)	0.590 (4)
H13A	0.4898	−0.3068	−0.0044	0.120*	0.590 (4)
C14	0.3958 (2)	−0.2519 (3)	0.0154 (2)	0.085 (3)	0.590 (4)
H14A	0.3349	−0.3068	0.0034	0.102*	0.590 (4)
C15	0.3940 (2)	−0.1698 (4)	0.0381 (2)	0.0584 (19)	0.590 (4)
C16	0.4850 (3)	−0.0878 (4)	0.0562 (2)	0.066 (2)	0.590 (4)
H16A	0.4838	−0.0329	0.0714	0.080*	0.590 (4)
C17	0.5778 (3)	−0.0878 (3)	0.0515 (2)	0.105 (4)	0.590 (4)
H17A	0.6388	−0.0329	0.0636	0.126*	0.590 (4)
N3A	0.4826 (4)	−0.3091 (4)	0.0072 (2)	0.113 (4)	0.410 (4)
C13A	0.3897 (4)	−0.3517 (6)	−0.0179 (3)	0.126 (5)	0.410 (4)
H13B	0.3694	−0.4100	−0.0369	0.151*	0.410 (4)
C14A	0.3272 (5)	−0.3073 (7)	−0.0146 (3)	0.093 (4)	0.410 (4)
H14B	0.2651	−0.3358	−0.0314	0.112*	0.410 (4)
C15A	0.3576 (6)	−0.2203 (7)	0.0139 (4)	0.061 (2)	0.410 (4)
C16A	0.4504 (7)	−0.1777 (6)	0.0390 (4)	0.100 (4)	0.410 (4)
H16B	0.4707	−0.1194	0.0580	0.120*	0.410 (4)
C17A	0.5129 (5)	−0.2221 (5)	0.0357 (3)	0.097 (4)	0.410 (4)
H17B	0.5750	−0.1936	0.0525	0.117*	0.410 (4)
C18	0.2982 (2)	−0.1597 (3)	0.0304 (2)	0.0813 (15)
C19	0.2637 (3)	−0.1329 (4)	0.06973 (18)	0.0864 (15)
C20	0.1915 (3)	−0.1034 (3)	0.06980 (15)	0.0531 (12)
H20A	0.1734	−0.0828	0.0979	0.064*
C21	0.1454 (2)	−0.1049 (2)	0.02647 (12)	0.0310 (9)
C22	0.1734 (2)	−0.1341 (2)	−0.01437 (13)	0.0416 (10)
H22A	0.1408	−0.1368	−0.0431	0.050*
C23	0.2515 (3)	−0.1599 (3)	−0.01292 (18)	0.0618 (13)
H23A	0.2725	−0.1774	−0.0410	0.074*
C24	0.0650 (2)	−0.0718 (2)	0.02669 (12)	0.0324 (9)
C25	−0.6672 (4)	−0.6322 (4)	−0.1057 (2)	0.101 (2)
H25A	−0.7358	−0.6590	−0.0963	0.122*
C26	−0.5908 (4)	−0.5568 (4)	−0.0786 (2)	0.097 (2)
H26A	−0.6107	−0.5327	−0.0522	0.117*
C27	−0.4931 (3)	−0.5164 (3)	−0.08672 (17)	0.0664 (14)
C28	−0.4705 (4)	−0.5536 (4)	−0.1240 (3)	0.115 (2)
H28A	−0.4016	−0.5322	−0.1308	0.138*
C29	−0.5543 (5)	−0.6309 (5)	−0.1561 (3)	0.126 (2)
H29A	−0.5378	−0.6515	−0.1846	0.151*
C30	−0.4093 (3)	−0.4249 (3)	−0.05919 (17)	0.0614 (14)
C31	−0.3743 (3)	−0.3263 (3)	−0.07787 (16)	0.0600 (14)
H31A	−0.3981	−0.3197	−0.1077	0.072*
C32	−0.3057 (2)	−0.2384 (3)	−0.05348 (15)	0.0482 (11)
H32A	−0.2836	−0.1733	−0.0666	0.058*
C33	−0.2691 (2)	−0.2481 (2)	−0.00826 (12)	0.0322 (9)
C34	−0.2992 (2)	−0.3432 (2)	0.00963 (13)	0.0386 (10)
H34A	−0.2735	−0.3498	0.0389	0.046*
C35	−0.3694 (3)	−0.4325 (3)	−0.01602 (17)	0.0515 (13)
C36	−0.1954 (2)	−0.1490 (2)	0.02090 (14)	0.0381 (10)

Atomic displacement parameters (Å²) top

	U¹¹	U²²	U³³	U¹²	U¹³	U²³
Dy1	0.02531 (4)	0.02246 (4)	0.01965 (5)	0.00780 (4)	0.00029 (6)	−0.00134 (5)
O1	0.0703 (19)	0.131 (3)	0.0529 (19)	0.0147 (18)	0.0057 (16)	−0.0331 (19)
O1W	0.1418 (18)	0.145 (2)	0.173 (3)	0.0716 (14)	−0.010 (2)	−0.026 (2)
O2	0.0706 (18)	0.100 (2)	0.0540 (19)	0.0193 (16)	−0.0140 (16)	−0.0268 (17)
O2W	0.1418 (18)	0.145 (2)	0.173 (3)	0.0716 (14)	−0.010 (2)	−0.026 (2)
O3	0.0337 (8)	0.0255 (8)	0.0274 (12)	0.0094 (6)	0.0033 (8)	−0.0017 (8)
O4	0.0383 (9)	0.0539 (10)	0.0270 (11)	0.0236 (7)	−0.0021 (9)	−0.0122 (9)
O5	0.088 (2)	0.158 (3)	0.099 (3)	0.0773 (18)	0.003 (2)	0.072 (2)
O5A	0.077 (3)	0.111 (4)	0.081 (6)	0.064 (3)	0.014 (4)	0.039 (4)
O6	0.130 (3)	0.153 (4)	0.084 (4)	0.086 (2)	−0.033 (3)	−0.011 (3)
O6A	0.096 (6)	0.125 (7)	0.097 (7)	0.045 (4)	−0.006 (6)	0.014 (6)
O7	0.0458 (8)	0.0610 (9)	0.0272 (12)	0.0398 (6)	0.0041 (8)	−0.0080 (9)
O8	0.0692 (9)	0.0658 (9)	0.0307 (13)	0.0535 (6)	−0.0126 (10)	−0.0059 (9)
O9	0.0407 (10)	0.0397 (10)	0.0159 (10)	0.0046 (8)	−0.0106 (9)	−0.0080 (9)
O10	0.0341 (9)	0.0198 (8)	0.0384 (13)	0.0054 (7)	0.0078 (9)	0.0000 (8)
O11	0.143 (3)	0.0664 (16)	0.077 (3)	0.0469 (15)	−0.013 (2)	−0.0008 (17)
O12	0.1250 (17)	0.1065 (16)	0.129 (2)	0.0567 (11)	−0.0254 (16)	0.0081 (15)
N1	0.0445 (17)	0.0382 (16)	0.120 (4)	0.0037 (13)	−0.005 (2)	−0.0165 (19)
N2	0.0480 (13)	0.0431 (13)	0.0346 (16)	0.0148 (10)	−0.0096 (12)	−0.0111 (12)
N4	0.0460 (16)	0.087 (2)	0.072 (3)	0.0431 (14)	0.012 (2)	0.023 (3)
N4A	0.065 (3)	0.049 (3)	0.032 (5)	0.039 (2)	0.003 (4)	0.009 (3)
N5	0.0740 (19)	0.0592 (17)	0.115 (3)	0.0291 (14)	−0.042 (2)	−0.031 (2)
N6	0.0567 (16)	0.0254 (12)	0.127 (4)	0.0135 (11)	−0.024 (2)	−0.0179 (17)
C1	0.0360 (15)	0.065 (2)	0.089 (4)	0.0177 (14)	−0.0039 (19)	−0.018 (2)
C2	0.0498 (16)	0.0431 (16)	0.071 (3)	0.0166 (12)	0.001 (2)	−0.0044 (19)
C3	0.0363 (13)	0.0423 (15)	0.052 (2)	0.0131 (11)	−0.0019 (15)	−0.0065 (16)
C4	0.0330 (14)	0.0480 (17)	0.105 (4)	0.0187 (12)	−0.0050 (19)	−0.014 (2)
C5	0.0504 (19)	0.0431 (18)	0.130 (5)	0.0182 (14)	−0.002 (2)	−0.012 (2)
C6	0.0323 (12)	0.0256 (12)	0.045 (2)	0.0064 (10)	0.0023 (14)	−0.0007 (13)
C7	0.0331 (12)	0.0348 (12)	0.0378 (18)	0.0173 (9)	−0.0043 (12)	−0.0059 (12)
C8	0.0412 (12)	0.0326 (12)	0.0236 (14)	0.0141 (9)	0.0039 (15)	0.0048 (13)
C9	0.0428 (13)	0.0307 (12)	0.0181 (15)	0.0162 (9)	0.0017 (12)	−0.0005 (11)
C10	0.0356 (15)	0.0489 (17)	0.0260 (17)	0.0057 (13)	0.0058 (13)	0.0014 (15)
C11	0.0364 (15)	0.0394 (17)	0.045 (2)	0.0021 (13)	0.0192 (15)	0.0053 (16)
C12	0.0333 (11)	0.0294 (11)	0.0265 (16)	0.0184 (8)	−0.0005 (11)	0.0028 (11)
N3	0.084 (3)	0.150 (5)	0.153 (7)	0.074 (3)	0.003 (5)	0.019 (5)
C13	0.109 (3)	0.094 (3)	0.130 (6)	0.077 (2)	0.036 (4)	−0.024 (3)
C14	0.086 (3)	0.080 (3)	0.127 (7)	0.0686 (19)	−0.002 (4)	0.004 (4)
C15	0.0377 (18)	0.084 (3)	0.075 (4)	0.0462 (15)	−0.005 (3)	0.021 (3)
C16	0.045 (2)	0.101 (3)	0.064 (4)	0.045 (2)	0.011 (3)	0.040 (3)
C17	0.085 (4)	0.136 (6)	0.096 (6)	0.057 (3)	0.013 (4)	0.015 (5)
N3A	0.123 (6)	0.125 (6)	0.113 (7)	0.079 (4)	0.022 (5)	0.017 (6)
C13A	0.123 (6)	0.133 (7)	0.148 (9)	0.083 (4)	0.034 (6)	0.014 (7)
C14A	0.094 (5)	0.098 (5)	0.103 (8)	0.059 (4)	0.023 (6)	0.016 (6)
C15A	0.066 (3)	0.068 (3)	0.058 (4)	0.042 (2)	−0.008 (3)	0.021 (3)
C16A	0.075 (4)	0.143 (6)	0.100 (8)	0.068 (4)	−0.003 (5)	0.013 (6)
C17A	0.096 (5)	0.126 (6)	0.090 (7)	0.070 (4)	0.009 (6)	0.021 (6)
C18	0.0521 (13)	0.111 (2)	0.109 (3)	0.0616 (11)	0.039 (2)	0.059 (2)
C19	0.0523 (16)	0.149 (3)	0.071 (3)	0.0603 (15)	0.0182 (17)	0.069 (2)
C20	0.0464 (14)	0.0825 (19)	0.037 (2)	0.0369 (12)	0.0052 (14)	0.0169 (16)
C21	0.0275 (11)	0.0273 (11)	0.0361 (17)	0.0123 (8)	−0.0002 (12)	0.0074 (12)
C22	0.0453 (12)	0.0533 (13)	0.0420 (19)	0.0365 (9)	−0.0051 (13)	−0.0147 (13)
C23	0.0522 (14)	0.0722 (17)	0.081 (3)	0.0464 (11)	0.0168 (18)	0.0098 (19)
C24	0.0319 (11)	0.0356 (12)	0.0317 (17)	0.0183 (9)	−0.0029 (12)	−0.0026 (12)
C25	0.088 (3)	0.046 (2)	0.123 (5)	−0.001 (2)	−0.040 (3)	−0.001 (3)
C26	0.087 (3)	0.059 (3)	0.085 (4)	−0.010 (3)	−0.035 (3)	−0.001 (3)
C27	0.0733 (19)	0.0506 (16)	0.078 (3)	0.0327 (13)	−0.0479 (19)	−0.0341 (18)
C28	0.083 (3)	0.126 (3)	0.127 (4)	0.045 (2)	−0.035 (3)	−0.074 (3)
C29	0.128 (3)	0.117 (3)	0.136 (4)	0.064 (2)	−0.005 (3)	−0.040 (3)
C30	0.0476 (16)	0.0420 (15)	0.084 (3)	0.0142 (12)	−0.0273 (19)	−0.0293 (18)
C31	0.0693 (19)	0.0552 (17)	0.052 (2)	0.0286 (14)	−0.0311 (18)	−0.0315 (16)
C32	0.0423 (15)	0.0416 (15)	0.044 (2)	0.0085 (12)	−0.0092 (17)	−0.0007 (17)
C33	0.0348 (12)	0.0317 (12)	0.0246 (16)	0.0125 (9)	−0.0115 (12)	−0.0062 (12)
C34	0.0321 (13)	0.0362 (14)	0.041 (2)	0.0120 (10)	−0.0051 (13)	−0.0037 (13)
C35	0.0469 (16)	0.0334 (14)	0.069 (3)	0.0161 (12)	−0.0133 (18)	−0.0103 (16)
C36	0.0255 (12)	0.0335 (13)	0.047 (2)	0.0088 (10)	−0.0046 (13)	−0.0106 (14)

Geometric parameters (Å, º) top

Dy1—O10ⁱ	2.2587 (19)	C6—C7	1.406 (4)
Dy1—O7	2.282 (2)	C7—C8	1.372 (4)
Dy1—O3	2.2912 (19)	C8—C9	1.413 (5)
Dy1—O8ⁱ	2.320 (3)	C9—C10	1.370 (4)
Dy1—O1W	2.345 (6)	C9—C12	1.467 (3)
Dy1—O4ⁱ	2.361 (2)	C10—C11	1.376 (4)
Dy1—O9	2.3961 (19)	N3—C13	1.3900
Dy1—O2W	2.782 (4)	N3—C17	1.3900
O1—N2	1.236 (4)	C13—C14	1.3900
O2—N2	1.205 (4)	C14—C15	1.3900
O3—C12	1.263 (3)	C15—C16	1.3900
O4—C12	1.251 (4)	C15—C18	1.524 (6)
O4—Dy1ⁱⁱ	2.361 (2)	C16—C17	1.3900
O5—N4	1.233 (8)	N3A—C13A	1.3900
O5A—N4A	1.302 (15)	N3A—C17A	1.3900
O6—N4	1.142 (9)	C13A—C14A	1.3900
O6A—N4A	1.217 (18)	C14A—C15A	1.3900
O7—C24	1.236 (4)	C15A—C16A	1.3900
O8—C24	1.275 (4)	C15A—C18	1.616 (9)
O8—Dy1ⁱⁱ	2.320 (3)	C16A—C17A	1.3900
O9—C36	1.225 (4)	C18—C19	1.356 (8)
O10—C36	1.253 (4)	C18—C23	1.396 (7)
O10—Dy1ⁱⁱ	2.2587 (19)	C19—C20	1.350 (7)
O11—N6	1.197 (6)	C20—C21	1.386 (5)
O12—N6	1.193 (5)	C21—C22	1.359 (5)
N1—C1	1.314 (7)	C21—C24	1.508 (5)
N1—C5	1.392 (6)	C22—C23	1.398 (6)
N2—C7	1.423 (5)	C25—C26	1.362 (7)
N4—C19	1.648 (8)	C26—C27	1.288 (7)
N4A—C19	1.421 (11)	C27—C28	1.301 (9)
N5—C29	1.264 (8)	C27—C30	1.519 (5)
N5—C25	1.280 (9)	C28—C29	1.502 (9)
N6—C35	1.479 (5)	C30—C35	1.374 (7)
C1—C2	1.372 (5)	C30—C31	1.393 (6)
C2—C3	1.388 (5)	C31—C32	1.374 (5)
C3—C4	1.396 (6)	C32—C33	1.412 (5)
C3—C6	1.480 (4)	C33—C34	1.351 (5)
C4—C5	1.379 (5)	C33—C36	1.559 (4)
C6—C11	1.370 (6)	C34—C35	1.410 (5)

O10ⁱ—Dy1—O7	92.12 (8)	C9—C10—C11	122.0 (3)
O10ⁱ—Dy1—O3	164.81 (8)	C6—C11—C10	122.5 (3)
O7—Dy1—O3	81.17 (8)	O4—C12—O3	124.8 (2)
O10ⁱ—Dy1—O8ⁱ	78.36 (9)	O4—C12—C9	116.4 (2)
O7—Dy1—O8ⁱ	73.05 (8)	O3—C12—C9	118.7 (3)
O3—Dy1—O8ⁱ	86.64 (8)	C13—N3—C17	120.0
O10ⁱ—Dy1—O1W	89.79 (14)	C14—C13—N3	120.0
O7—Dy1—O1W	145.12 (13)	C13—C14—C15	120.0
O3—Dy1—O1W	103.52 (14)	C16—C15—C14	120.0
O8ⁱ—Dy1—O1W	141.04 (13)	C16—C15—C18	121.0 (3)
O10ⁱ—Dy1—O4ⁱ	101.35 (7)	C14—C15—C18	117.0 (3)
O7—Dy1—O4ⁱ	143.07 (8)	C15—C16—C17	120.0
O3—Dy1—O4ⁱ	77.00 (8)	C16—C17—N3	120.0
O8ⁱ—Dy1—O4ⁱ	76.25 (9)	C13A—N3A—C17A	120.0
O1W—Dy1—O4ⁱ	69.88 (14)	C14A—C13A—N3A	120.0
O10ⁱ—Dy1—O9	84.79 (8)	C13A—C14A—C15A	120.0
O7—Dy1—O9	73.42 (8)	C16A—C15A—C14A	120.0
O3—Dy1—O9	106.05 (7)	C16A—C15A—C18	107.4 (5)
O8ⁱ—Dy1—O9	141.63 (9)	C14A—C15A—C18	132.2 (5)
O1W—Dy1—O9	72.08 (13)	C17A—C16A—C15A	120.0
O4ⁱ—Dy1—O9	141.39 (9)	C16A—C17A—N3A	120.0
O10ⁱ—Dy1—O2W	140.26 (9)	C19—C18—C23	116.2 (4)
O7—Dy1—O2W	109.47 (11)	C19—C18—C15	115.3 (5)
O3—Dy1—O2W	54.82 (8)	C23—C18—C15	127.8 (5)
O8ⁱ—Dy1—O2W	139.02 (8)	C19—C18—C15A	142.4 (6)
O1W—Dy1—O2W	53.46 (14)	C23—C18—C15A	99.3 (5)
O4ⁱ—Dy1—O2W	81.35 (11)	C15—C18—C15A	35.2 (4)
O9—Dy1—O2W	70.87 (10)	C20—C19—C18	125.4 (5)
C12—O3—Dy1	136.9 (2)	C20—C19—N4A	123.5 (6)
C12—O4—Dy1ⁱⁱ	131.01 (16)	C18—C19—N4A	107.2 (6)
C24—O7—Dy1	155.9 (2)	C20—C19—N4	109.8 (4)
C24—O8—Dy1ⁱⁱ	140.7 (2)	C18—C19—N4	124.0 (4)
C36—O9—Dy1	124.63 (18)	N4A—C19—N4	33.7 (4)
C36—O10—Dy1ⁱⁱ	141.6 (2)	C19—C20—C21	117.5 (4)
C1—N1—C5	116.6 (3)	C22—C21—C20	120.7 (4)
O2—N2—O1	121.6 (3)	C22—C21—C24	122.0 (3)
O2—N2—C7	120.4 (3)	C20—C21—C24	117.4 (3)
O1—N2—C7	117.9 (3)	C21—C22—C23	119.7 (4)
O6—N4—O5	130.1 (7)	C18—C23—C22	120.5 (4)
O6—N4—C19	120.4 (6)	O7—C24—O8	126.2 (3)
O5—N4—C19	109.1 (5)	O7—C24—C21	118.0 (3)
O6A—N4A—O5A	125.3 (12)	O8—C24—C21	115.8 (3)
O6A—N4A—C19	106.0 (11)	N5—C25—C26	122.2 (5)
O5A—N4A—C19	127.2 (9)	C27—C26—C25	124.8 (6)
C29—N5—C25	118.5 (5)	C26—C27—C28	114.6 (5)
O12—N6—O11	121.6 (4)	C26—C27—C30	124.1 (5)
O12—N6—C35	116.9 (5)	C28—C27—C30	121.0 (4)
O11—N6—C35	121.4 (3)	C27—C28—C29	120.8 (6)
N1—C1—C2	124.8 (4)	N5—C29—C28	118.8 (7)
C1—C2—C3	119.5 (4)	C35—C30—C31	117.8 (3)
C2—C3—C4	117.4 (3)	C35—C30—C27	124.5 (4)
C2—C3—C6	121.0 (4)	C31—C30—C27	117.6 (4)
C4—C3—C6	121.0 (3)	C32—C31—C30	121.9 (4)
C5—C4—C3	119.9 (4)	C31—C32—C33	119.2 (3)
C4—C5—N1	121.7 (5)	C34—C33—C32	119.8 (3)
C11—C6—C7	116.3 (3)	C34—C33—C36	120.5 (3)
C11—C6—C3	117.7 (3)	C32—C33—C36	119.7 (3)
C7—C6—C3	125.9 (3)	C33—C34—C35	120.1 (4)
C8—C7—C6	121.6 (3)	C30—C35—C34	121.1 (4)
C8—C7—N2	117.5 (3)	C30—C35—N6	123.6 (3)
C6—C7—N2	120.7 (3)	C34—C35—N6	115.3 (4)
C7—C8—C9	121.0 (3)	O9—C36—O10	127.7 (3)
C10—C9—C8	116.6 (2)	O9—C36—C33	116.5 (3)
C10—C9—C12	122.1 (3)	O10—C36—C33	115.8 (3)
C8—C9—C12	121.3 (2)

O10ⁱ—Dy1—O3—C12	41.0 (5)	C16A—C15A—C18—C23	145.1 (3)
O7—Dy1—O3—C12	−23.6 (3)	C14A—C15A—C18—C23	−42.8 (7)
O8ⁱ—Dy1—O3—C12	49.7 (3)	C16A—C15A—C18—C15	−2.5 (6)
O1W—Dy1—O3—C12	−168.3 (3)	C14A—C15A—C18—C15	169.6 (11)
O4ⁱ—Dy1—O3—C12	126.4 (3)	C23—C18—C19—C20	−2.5 (6)
O9—Dy1—O3—C12	−93.4 (3)	C15—C18—C19—C20	168.7 (4)
O2W—Dy1—O3—C12	−145.1 (3)	C15A—C18—C19—C20	−161.3 (7)
O10ⁱ—Dy1—O7—C24	137.6 (4)	C23—C18—C19—N4A	155.8 (4)
O3—Dy1—O7—C24	−56.1 (4)	C15—C18—C19—N4A	−33.1 (5)
O8ⁱ—Dy1—O7—C24	−145.3 (4)	C15A—C18—C19—N4A	−3.0 (8)
O1W—Dy1—O7—C24	44.9 (5)	C23—C18—C19—N4	−171.5 (4)
O4ⁱ—Dy1—O7—C24	−110.3 (4)	C15—C18—C19—N4	−0.4 (6)
O9—Dy1—O7—C24	53.6 (4)	C15A—C18—C19—N4	29.6 (9)
O2W—Dy1—O7—C24	−8.5 (4)	O6A—N4A—C19—C20	−43.6 (9)
O10ⁱ—Dy1—O9—C36	−166.2 (3)	O5A—N4A—C19—C20	122.9 (9)
O7—Dy1—O9—C36	−72.4 (3)	O6A—N4A—C19—C18	157.7 (8)
O3—Dy1—O9—C36	3.0 (3)	O5A—N4A—C19—C18	−35.9 (10)
O8ⁱ—Dy1—O9—C36	−102.4 (3)	O6A—N4A—C19—N4	31.3 (7)
O1W—Dy1—O9—C36	102.4 (3)	O5A—N4A—C19—N4	−162.2 (14)
O4ⁱ—Dy1—O9—C36	92.2 (3)	O6—N4—C19—C20	−38.7 (6)
O2W—Dy1—O9—C36	45.8 (3)	O5—N4—C19—C20	134.8 (4)
C5—N1—C1—C2	−3.8 (8)	O6—N4—C19—C18	131.8 (6)
N1—C1—C2—C3	3.1 (8)	O5—N4—C19—C18	−54.6 (6)
C1—C2—C3—C4	−1.1 (7)	O6—N4—C19—N4A	−159.9 (10)
C1—C2—C3—C6	170.5 (4)	O5—N4—C19—N4A	13.6 (7)
C2—C3—C4—C5	0.0 (7)	C18—C19—C20—C21	3.0 (6)
C6—C3—C4—C5	−171.6 (5)	N4A—C19—C20—C21	−151.9 (5)
C3—C4—C5—N1	−0.7 (9)	N4—C19—C20—C21	173.4 (3)
C1—N1—C5—C4	2.5 (8)	C19—C20—C21—C22	−0.7 (4)
C2—C3—C6—C11	−55.0 (6)	C19—C20—C21—C24	−179.9 (3)
C4—C3—C6—C11	116.3 (5)	C20—C21—C22—C23	−1.9 (4)
C2—C3—C6—C7	128.4 (5)	C24—C21—C22—C23	177.3 (3)
C4—C3—C6—C7	−60.4 (6)	C19—C18—C23—C22	−0.3 (5)
C11—C6—C7—C8	−0.2 (6)	C15—C18—C23—C22	−170.2 (4)
C3—C6—C7—C8	176.5 (4)	C15A—C18—C23—C22	166.8 (4)
C11—C6—C7—N2	174.6 (4)	C21—C22—C23—C18	2.4 (5)
C3—C6—C7—N2	−8.7 (6)	Dy1—O7—C24—O8	4.6 (6)
O2—N2—C7—C8	152.9 (4)	Dy1—O7—C24—C21	−176.8 (3)
O1—N2—C7—C8	−22.8 (6)	Dy1ⁱⁱ—O8—C24—O7	25.4 (4)
O2—N2—C7—C6	−22.2 (6)	Dy1ⁱⁱ—O8—C24—C21	−153.2 (2)
O1—N2—C7—C6	162.1 (4)	C22—C21—C24—O7	169.8 (2)
C6—C7—C8—C9	0.1 (6)	C20—C21—C24—O7	−11.0 (4)
N2—C7—C8—C9	−175.0 (4)	C22—C21—C24—O8	−11.5 (4)
C7—C8—C9—C10	0.8 (6)	C20—C21—C24—O8	167.8 (2)
C7—C8—C9—C12	−179.2 (3)	C29—N5—C25—C26	0.3 (10)
C8—C9—C10—C11	−1.5 (6)	N5—C25—C26—C27	−2.8 (10)
C12—C9—C10—C11	178.5 (4)	C25—C26—C27—C28	−0.2 (9)
C7—C6—C11—C10	−0.5 (6)	C25—C26—C27—C30	173.5 (6)
C3—C6—C11—C10	−177.5 (4)	C26—C27—C28—C29	4.9 (9)
C9—C10—C11—C6	1.4 (7)	C30—C27—C28—C29	−169.1 (6)
Dy1ⁱⁱ—O4—C12—O3	8.2 (5)	C25—N5—C29—C28	4.3 (10)
Dy1ⁱⁱ—O4—C12—C9	−167.3 (2)	C27—C28—C29—N5	−7.3 (11)
Dy1—O3—C12—O4	82.8 (4)	C26—C27—C30—C35	83.5 (7)
Dy1—O3—C12—C9	−101.7 (3)	C28—C27—C30—C35	−103.1 (7)
C10—C9—C12—O4	1.5 (6)	C26—C27—C30—C31	−93.0 (6)
C8—C9—C12—O4	−178.5 (3)	C28—C27—C30—C31	80.3 (7)
C10—C9—C12—O3	−174.3 (4)	C35—C30—C31—C32	−2.8 (7)
C8—C9—C12—O3	5.7 (5)	C27—C30—C31—C32	174.0 (4)
C17—N3—C13—C14	0.0	C30—C31—C32—C33	0.3 (7)
N3—C13—C14—C15	0.0	C31—C32—C33—C34	2.2 (6)
C13—C14—C15—C16	0.0	C31—C32—C33—C36	−177.1 (4)
C13—C14—C15—C18	164.0 (4)	C32—C33—C34—C35	−2.0 (6)
C14—C15—C16—C17	0.0	C36—C33—C34—C35	177.3 (3)
C18—C15—C16—C17	−163.3 (4)	C31—C30—C35—C34	3.0 (7)
C15—C16—C17—N3	0.0	C27—C30—C35—C34	−173.6 (4)
C13—N3—C17—C16	0.0	C31—C30—C35—N6	−178.2 (4)
C17A—N3A—C13A—C14A	0.0	C27—C30—C35—N6	5.2 (7)
N3A—C13A—C14A—C15A	0.0	C33—C34—C35—C30	−0.6 (6)
C13A—C14A—C15A—C16A	0.0	C33—C34—C35—N6	−179.5 (4)
C13A—C14A—C15A—C18	−171.3 (8)	O12—N6—C35—C30	2.8 (7)
C14A—C15A—C16A—C17A	0.0	O11—N6—C35—C30	−179.4 (5)
C18—C15A—C16A—C17A	173.2 (6)	O12—N6—C35—C34	−178.3 (5)
C15A—C16A—C17A—N3A	0.0	O11—N6—C35—C34	−0.6 (7)
C13A—N3A—C17A—C16A	0.0	Dy1—O9—C36—O10	−7.9 (6)
C16—C15—C18—C19	−56.7 (5)	Dy1—O9—C36—C33	175.8 (2)
C14—C15—C18—C19	139.5 (4)	Dy1ⁱⁱ—O10—C36—O9	98.3 (5)
C16—C15—C18—C23	113.3 (5)	Dy1ⁱⁱ—O10—C36—C33	−85.3 (4)
C14—C15—C18—C23	−50.5 (5)	C34—C33—C36—O9	−13.8 (5)
C16—C15—C18—C15A	155.3 (8)	C32—C33—C36—O9	165.4 (4)
C14—C15—C18—C15A	−8.5 (7)	C34—C33—C36—O10	169.4 (3)
C16A—C15A—C18—C19	−54.1 (8)	C32—C33—C36—O10	−11.4 (5)
C14A—C15A—C18—C19	118.0 (8)

Symmetry codes: (i) x−y, x, z+1/6; (ii) y, −x+y, z−1/6.

Poly[diaquatris[µ₂-3-nitro-4-(pyridin-4-yl)benzoato-κ²O:O']terbium(III)] (1502117) top

Crystal data top

[Tb(C₁₂H₇N₂O₄)₃(H₂O)₂]	D_x = 1.705 Mg m⁻³
M_r = 924.54	Mo Kα radiation, λ = 0.71073 Å
Hexagonal, P6₅	Cell parameters from 6881 reflections
Hall symbol: P 65	θ = 2.7–26.9°
a = 14.9349 (17) Å	µ = 2.04 mm⁻¹
c = 27.969 (3) Å	T = 296 K
V = 5402.7 (11) Å³	Rodlike, colorless
Z = 6	0.16 × 0.13 × 0.12 mm
F(000) = 2760

Data collection top

Bruker APEXII CCD diffractometer	6785 independent reflections
Radiation source: fine-focus sealed tube	5885 reflections with I > 2σ(I)
Graphite monochromator	R_int = 0.075
ω scans	θ_max = 26.0°, θ_min = 1.6°
Absorption correction: multi-scan (SADABS; Sheldrick, 2003)	h = −18→18
T_min = 0.734, T_max = 0.782	k = −17→16
39771 measured reflections	l = −34→32

Refinement top

Refinement on F²	Secondary atom site location: difference Fourier map
Least-squares matrix: full	Hydrogen site location: inferred from neighbouring sites
R[F² > 2σ(F²)] = 0.049	H atoms treated by a mixture of independent and constrained refinement
wR(F²) = 0.129	w = 1/[σ²(F_o²) + (0.0773P)² + 3.460P] where P = (F_o² + 2F_c²)/3
S = 1.06	(Δ/σ)_max = 0.007
6785 reflections	Δρ_max = 1.79 e Å⁻³
579 parameters	Δρ_min = −1.29 e Å⁻³
205 restraints	Absolute structure: Flack (1983), 3176 Friedel pairs
Primary atom site location: structure-invariant direct methods	Absolute structure parameter: 0.02 (2)

Special details top

Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å²) top

	x	y	z	U_iso*/U_eq	Occ. (<1)
Tb1	0.039099 (9)	−0.028764 (9)	0.182093 (12)	0.02911 (3)
O1W	0.1712 (3)	−0.0640 (3)	0.19989 (16)	0.1734 (17)
H1WA	0.2336 (4)	−0.0170 (7)	0.2048 (4)	0.208*
H1WB	0.1547 (5)	−0.1149 (3)	0.2181 (2)	0.208*
O1	0.1948 (3)	0.3566 (3)	0.27166 (14)	0.1031 (14)
O2W	0.2190 (3)	0.0354 (2)	0.14020 (14)	0.1734 (17)
H2WA	0.2199 (6)	0.0795 (4)	0.11766 (18)	0.208*
H2WB	0.2082 (4)	−0.0189 (3)	0.1227 (3)	0.208*
O2	0.1223 (3)	0.4453 (2)	0.27615 (13)	0.0915 (12)
O3	0.11667 (15)	0.12215 (14)	0.13793 (8)	0.0347 (7)
O4	0.06402 (17)	0.15764 (17)	0.07018 (9)	0.0448 (7)
O5	−0.5106 (4)	−0.1837 (5)	0.2019 (2)	0.101 (2)	0.650 (4)
O5A	−0.5471 (6)	−0.2678 (7)	0.1771 (4)	0.087 (3)	0.350 (4)
O6	−0.3713 (5)	−0.0387 (6)	0.2120 (3)	0.127 (3)	0.650 (4)
O6A	−0.4277 (9)	−0.1308 (9)	0.2090 (5)	0.100 (3)	0.350 (4)
O7	−0.09368 (16)	−0.06146 (19)	0.13130 (10)	0.0455 (8)
O8	−0.09453 (18)	−0.0556 (2)	0.05183 (11)	0.0557 (10)
O9	0.01950 (18)	−0.16554 (15)	0.13000 (8)	0.0430 (7)
O10	0.09266 (16)	−0.06670 (14)	0.06557 (9)	0.0379 (7)
O11	−0.1709 (3)	−0.5395 (3)	0.11016 (16)	0.1041 (17)
O12	−0.1538 (4)	−0.6104 (4)	0.0500 (2)	0.1424 (15)
N1	0.1435 (3)	0.7401 (3)	0.2123 (2)	0.105 (2)
N2	0.1509 (2)	0.3976 (2)	0.25242 (12)	0.0491 (10)
N4	−0.4266 (3)	−0.1118 (4)	0.1902 (3)	0.0703 (19)	0.650 (4)
N4A	−0.4618 (6)	−0.1868 (7)	0.1733 (3)	0.050 (2)	0.350 (4)
N5	−0.0134 (3)	−0.6643 (3)	−0.07719 (19)	0.0895 (16)
N6	−0.1342 (3)	−0.5340 (2)	0.07283 (19)	0.0830 (16)
C1	0.2246 (4)	0.7194 (4)	0.2201 (3)	0.099 (2)
H1A	0.2855	0.7704	0.2340	0.119*
C2	0.2169 (3)	0.6280 (3)	0.2081 (2)	0.0809 (19)
H2A	0.2745	0.6196	0.2096	0.097*
C3	0.1203 (3)	0.5458 (2)	0.19330 (18)	0.0534 (13)
C4	0.0417 (3)	0.5679 (3)	0.1878 (2)	0.0669 (15)
H4A	−0.0234	0.5153	0.1786	0.080*
C5	0.0559 (3)	0.6611 (3)	0.1952 (3)	0.099 (2)
H5A	0.0018	0.6728	0.1880	0.119*
C6	0.1117 (2)	0.4496 (2)	0.17493 (14)	0.0408 (10)
C7	0.1304 (2)	0.3803 (2)	0.20184 (13)	0.0370 (10)
C8	0.1251 (2)	0.2936 (2)	0.18286 (15)	0.0385 (9)
H8A	0.1391	0.2510	0.2019	0.046*
C9	0.0983 (2)	0.2686 (2)	0.13448 (12)	0.0366 (10)
C10	0.0772 (3)	0.3341 (2)	0.10858 (14)	0.0492 (12)
H10A	0.0566	0.3177	0.0769	0.059*
C11	0.0853 (3)	0.4222 (3)	0.12749 (16)	0.0576 (13)
H11A	0.0727	0.4651	0.1079	0.069*
C12	0.0916 (2)	0.1765 (2)	0.11367 (12)	0.0359 (10)
N3	−0.7389 (2)	−0.1566 (3)	0.0978 (2)	0.163 (4)	0.584 (4)
C13	−0.7362 (3)	−0.2414 (4)	0.0790 (3)	0.123 (4)	0.584 (4)
H13A	−0.7940	−0.2935	0.0636	0.147*	0.584 (4)
C14	−0.6471 (4)	−0.2483 (5)	0.0833 (3)	0.109 (4)	0.584 (4)
H14A	−0.6453	−0.3050	0.0707	0.130*	0.584 (4)
C15	−0.5607 (3)	−0.1704 (5)	0.1063 (3)	0.073 (2)	0.584 (4)
C16	−0.5634 (3)	−0.0856 (5)	0.1251 (3)	0.083 (3)	0.584 (4)
H16A	−0.5056	−0.0334	0.1405	0.099*	0.584 (4)
C17	−0.6525 (3)	−0.0787 (4)	0.1208 (3)	0.189 (6)	0.584 (4)
H17A	−0.6543	−0.0220	0.1334	0.226*	0.584 (4)
N3A	−0.7914 (4)	−0.3191 (5)	0.0716 (2)	0.103 (4)	0.416 (4)
C13A	−0.7385 (5)	−0.3572 (6)	0.0455 (3)	0.129 (5)	0.416 (4)
H13B	−0.7745	−0.4133	0.0251	0.155*	0.416 (4)
C14A	−0.6318 (5)	−0.3114 (7)	0.0498 (3)	0.091 (4)	0.416 (4)
H14B	−0.5963	−0.3369	0.0323	0.110*	0.416 (4)
C15A	−0.5780 (4)	−0.2275 (7)	0.0802 (4)	0.057 (3)	0.416 (4)
C16A	−0.6309 (5)	−0.1894 (6)	0.1063 (4)	0.102 (5)	0.416 (4)
H16B	−0.5950	−0.1332	0.1266	0.122*	0.416 (4)
C17A	−0.7376 (5)	−0.2352 (6)	0.1020 (3)	0.099 (3)	0.416 (4)
H17B	−0.7731	−0.2097	0.1194	0.118*	0.416 (4)
C18	−0.4570 (3)	−0.1610 (4)	0.0959 (2)	0.0907 (17)
C19	−0.3938 (3)	−0.1314 (4)	0.1364 (2)	0.0997 (18)
C20	−0.2948 (3)	−0.1040 (3)	0.13494 (16)	0.0571 (12)
H20A	−0.2563	−0.0851	0.1630	0.069*
C21	−0.2490 (2)	−0.1032 (2)	0.09313 (15)	0.0381 (10)
C22	−0.3061 (2)	−0.1315 (3)	0.05134 (16)	0.0513 (13)
H22A	−0.2762	−0.1314	0.0222	0.062*
C23	−0.4106 (3)	−0.1602 (4)	0.0545 (2)	0.0720 (17)
H23A	−0.4499	−0.1798	0.0267	0.086*
C24	−0.1375 (2)	−0.0724 (2)	0.09224 (13)	0.0380 (10)
C25	0.0374 (5)	−0.6341 (4)	−0.0379 (3)	0.109 (2)
H25A	0.0746	−0.6646	−0.0268	0.131*
C26	0.0359 (4)	−0.5567 (4)	−0.0126 (3)	0.0983 (18)
H26A	0.0826	−0.5291	0.0126	0.118*
C27	−0.0213 (4)	−0.5183 (4)	−0.0194 (2)	0.0836 (19)
C28	−0.0766 (5)	−0.5489 (5)	−0.0596 (3)	0.140 (3)
H28A	−0.1185	−0.5220	−0.0683	0.168*
C29	−0.0703 (6)	−0.6273 (5)	−0.0903 (3)	0.137 (3)
H29A	−0.1074	−0.6490	−0.1187	0.165*
C30	−0.0118 (3)	−0.4248 (3)	0.00573 (19)	0.0706 (16)
C31	0.0509 (3)	−0.3255 (3)	−0.01200 (19)	0.0676 (16)
H31A	0.0823	−0.3175	−0.0416	0.081*
C32	0.0680 (3)	−0.2394 (3)	0.01254 (18)	0.0582 (12)
H32A	0.1101	−0.1741	−0.0004	0.070*
C33	0.0215 (2)	−0.2499 (2)	0.05754 (12)	0.0340 (9)
C34	−0.0440 (3)	−0.3459 (2)	0.07560 (16)	0.0492 (12)
H34A	−0.0767	−0.3534	0.1048	0.059*
C35	−0.0607 (3)	−0.4308 (3)	0.0500 (2)	0.0632 (16)
C36	0.0446 (2)	−0.1547 (2)	0.08730 (14)	0.0377 (10)

Atomic displacement parameters (Å²) top

	U¹¹	U²²	U³³	U¹²	U¹³	U²³
Tb1	0.04141 (5)	0.02562 (4)	0.02127 (6)	0.01749 (4)	−0.00137 (7)	−0.00110 (6)
O1W	0.168 (2)	0.156 (2)	0.221 (3)	0.0996 (14)	0.000 (2)	−0.029 (2)
O1	0.138 (2)	0.1160 (18)	0.076 (2)	0.0798 (14)	−0.0185 (19)	−0.0172 (18)
O2W	0.168 (2)	0.156 (2)	0.221 (3)	0.0996 (14)	0.000 (2)	−0.029 (2)
O2	0.1289 (18)	0.1200 (16)	0.060 (2)	0.0878 (12)	−0.0062 (17)	−0.0316 (15)
O3	0.0442 (9)	0.0253 (8)	0.0317 (13)	0.0153 (6)	−0.0033 (9)	0.0006 (8)
O4	0.0511 (10)	0.0585 (11)	0.0327 (13)	0.0333 (8)	−0.0105 (10)	−0.0124 (10)
O5	0.082 (2)	0.121 (3)	0.098 (3)	0.0486 (19)	0.041 (2)	0.028 (3)
O5A	0.083 (4)	0.111 (4)	0.073 (5)	0.054 (3)	0.000 (4)	0.036 (4)
O6	0.107 (3)	0.155 (4)	0.105 (5)	0.054 (3)	0.023 (3)	−0.030 (4)
O6A	0.104 (4)	0.098 (4)	0.092 (5)	0.046 (3)	−0.003 (4)	0.000 (4)
O7	0.0351 (9)	0.0714 (13)	0.0296 (14)	0.0263 (8)	−0.0129 (9)	−0.0082 (11)
O8	0.0324 (10)	0.0857 (17)	0.0361 (15)	0.0199 (10)	0.0008 (10)	−0.0115 (13)
O9	0.0902 (12)	0.0326 (8)	0.0149 (11)	0.0372 (7)	0.0015 (10)	−0.0060 (8)
O10	0.0469 (10)	0.0244 (8)	0.0430 (14)	0.0184 (7)	−0.0075 (10)	−0.0033 (9)
O11	0.127 (3)	0.0671 (19)	0.090 (3)	0.0278 (18)	0.017 (2)	0.013 (2)
O12	0.145 (2)	0.1291 (19)	0.143 (2)	0.0610 (13)	0.0264 (18)	−0.0120 (18)
N1	0.102 (2)	0.0722 (18)	0.159 (5)	0.0576 (14)	0.001 (3)	−0.023 (2)
N2	0.0680 (14)	0.0506 (12)	0.0395 (18)	0.0377 (10)	−0.0079 (14)	−0.0096 (12)
N4	0.0496 (19)	0.091 (3)	0.082 (4)	0.0440 (16)	0.023 (2)	0.023 (3)
N4A	0.042 (3)	0.062 (3)	0.042 (4)	0.025 (2)	0.006 (3)	0.007 (3)
N5	0.089 (2)	0.0715 (19)	0.102 (3)	0.0355 (15)	0.015 (2)	−0.017 (2)
N6	0.0641 (18)	0.0293 (13)	0.144 (4)	0.0147 (12)	0.015 (2)	−0.0239 (19)
C1	0.074 (2)	0.075 (2)	0.147 (5)	0.0356 (19)	−0.009 (3)	−0.029 (3)
C2	0.0652 (18)	0.0506 (15)	0.142 (5)	0.0405 (12)	−0.018 (2)	−0.036 (2)
C3	0.0480 (14)	0.0323 (12)	0.085 (3)	0.0241 (10)	−0.0115 (18)	−0.0108 (16)
C4	0.0692 (18)	0.0453 (14)	0.094 (4)	0.0346 (12)	−0.015 (2)	−0.017 (2)
C5	0.0702 (17)	0.0748 (18)	0.179 (7)	0.0557 (12)	−0.021 (3)	−0.034 (3)
C6	0.0527 (14)	0.0269 (11)	0.041 (2)	0.0187 (10)	−0.0033 (15)	−0.0039 (13)
C7	0.0392 (13)	0.0343 (13)	0.0361 (18)	0.0173 (10)	−0.0007 (13)	0.0040 (13)
C8	0.0354 (12)	0.0407 (13)	0.0330 (17)	0.0143 (10)	0.0021 (16)	0.0033 (16)
C9	0.0404 (14)	0.0381 (14)	0.0220 (16)	0.0126 (11)	−0.0038 (13)	0.0038 (13)
C10	0.0761 (17)	0.0488 (14)	0.032 (2)	0.0385 (12)	−0.0070 (16)	0.0028 (14)
C11	0.0820 (18)	0.0473 (15)	0.052 (2)	0.0385 (12)	−0.0189 (18)	0.0066 (15)
C12	0.0338 (13)	0.0396 (14)	0.0281 (17)	0.0137 (10)	−0.0010 (12)	0.0031 (13)
N3	0.136 (5)	0.183 (6)	0.210 (8)	0.109 (3)	0.010 (6)	0.021 (6)
C13	0.071 (4)	0.140 (7)	0.131 (7)	0.033 (4)	−0.045 (5)	−0.010 (6)
C14	0.060 (4)	0.117 (6)	0.133 (7)	0.033 (4)	−0.009 (5)	−0.002 (6)
C15	0.0414 (19)	0.104 (3)	0.105 (6)	0.0589 (17)	0.013 (3)	0.020 (3)
C16	0.069 (3)	0.101 (4)	0.085 (5)	0.048 (3)	0.031 (4)	0.039 (4)
C17	0.210 (8)	0.191 (8)	0.158 (9)	0.095 (5)	−0.033 (7)	0.026 (7)
N3A	0.096 (6)	0.108 (6)	0.095 (7)	0.044 (4)	0.002 (5)	0.027 (5)
C13A	0.115 (7)	0.132 (7)	0.154 (9)	0.072 (5)	−0.005 (6)	0.030 (7)
C14A	0.075 (5)	0.090 (6)	0.097 (7)	0.033 (4)	0.000 (5)	0.026 (6)
C15A	0.053 (3)	0.058 (3)	0.053 (4)	0.023 (2)	0.008 (3)	0.011 (3)
C16A	0.087 (5)	0.138 (7)	0.101 (8)	0.072 (4)	0.005 (6)	−0.008 (6)
C17A	0.091 (4)	0.106 (4)	0.092 (5)	0.044 (3)	0.005 (4)	0.008 (4)
C18	0.0483 (15)	0.124 (3)	0.107 (3)	0.0486 (15)	0.018 (2)	0.058 (2)
C19	0.0922 (18)	0.156 (3)	0.097 (4)	0.0964 (15)	0.045 (2)	0.049 (3)
C20	0.0662 (16)	0.0853 (19)	0.039 (2)	0.0519 (12)	0.0162 (16)	0.0231 (16)
C21	0.0301 (11)	0.0372 (13)	0.049 (2)	0.0185 (9)	0.0034 (14)	0.0065 (14)
C22	0.0189 (13)	0.062 (2)	0.054 (2)	0.0054 (13)	−0.0068 (15)	−0.0039 (19)
C23	0.0317 (16)	0.082 (2)	0.089 (3)	0.0192 (16)	−0.012 (2)	0.018 (2)
C24	0.0309 (12)	0.0480 (15)	0.0283 (18)	0.0146 (11)	0.0032 (13)	−0.0036 (14)
C25	0.152 (4)	0.054 (2)	0.118 (4)	0.049 (2)	0.025 (4)	−0.014 (3)
C26	0.132 (3)	0.073 (2)	0.102 (3)	0.0599 (16)	0.031 (3)	−0.005 (2)
C27	0.074 (3)	0.064 (2)	0.091 (3)	0.0186 (19)	−0.002 (3)	−0.046 (2)
C28	0.140 (4)	0.154 (4)	0.150 (6)	0.091 (3)	−0.023 (4)	−0.069 (4)
C29	0.126 (4)	0.128 (4)	0.154 (6)	0.060 (3)	−0.039 (4)	−0.068 (4)
C30	0.072 (2)	0.0521 (17)	0.085 (3)	0.0287 (14)	0.016 (2)	−0.0239 (19)
C31	0.071 (2)	0.0451 (17)	0.070 (3)	0.0170 (16)	0.017 (2)	−0.0200 (19)
C32	0.0764 (17)	0.0482 (14)	0.060 (3)	0.0386 (11)	0.016 (2)	−0.0004 (18)
C33	0.0432 (13)	0.0308 (11)	0.0306 (17)	0.0205 (9)	0.0052 (13)	−0.0095 (12)
C34	0.0627 (17)	0.0328 (13)	0.054 (2)	0.0254 (11)	0.0001 (17)	−0.0074 (15)
C35	0.0505 (18)	0.0383 (17)	0.092 (3)	0.0156 (14)	0.002 (2)	−0.013 (2)
C36	0.0382 (13)	0.0298 (12)	0.046 (2)	0.0178 (9)	−0.0070 (14)	−0.0138 (13)

Geometric parameters (Å, º) top

Tb1—O10ⁱ	2.277 (3)	C6—C7	1.417 (5)
Tb1—O7	2.285 (2)	C7—C8	1.364 (5)
Tb1—O3	2.310 (2)	C8—C9	1.408 (5)
Tb1—O1W	2.335 (5)	C9—C10	1.374 (6)
Tb1—O8ⁱ	2.343 (2)	C9—C12	1.449 (5)
Tb1—O4ⁱ	2.363 (3)	C10—C11	1.367 (6)
Tb1—O9	2.405 (2)	N3—C13	1.3900
Tb1—O2W	2.633 (4)	N3—C17	1.3900
O1—N2	1.224 (6)	C13—C14	1.3900
O2—N2	1.198 (5)	C14—C15	1.3900
O3—C12	1.251 (5)	C15—C16	1.3900
O4—C12	1.270 (4)	C15—C18	1.512 (6)
O4—Tb1ⁱⁱ	2.363 (3)	C16—C17	1.3900
O5—N4	1.219 (7)	N3A—C13A	1.3900
O5A—N4A	1.248 (10)	N3A—C17A	1.3900
O6—N4	1.160 (9)	C13A—C14A	1.3900
O6A—N4A	1.237 (15)	C14A—C15A	1.3900
O7—C24	1.241 (4)	C15A—C16A	1.3900
O8—C24	1.261 (5)	C15A—C18	1.628 (7)
O8—Tb1ⁱⁱ	2.343 (2)	C16A—C17A	1.3900
O9—C36	1.238 (4)	C18—C23	1.346 (8)
O10—C36	1.292 (4)	C18—C19	1.398 (8)
O10—Tb1ⁱⁱ	2.277 (3)	C19—C20	1.322 (6)
O11—N6	1.163 (7)	C20—C21	1.351 (6)
O12—N6	1.210 (7)	C21—C22	1.383 (6)
N1—C5	1.337 (6)	C21—C24	1.491 (5)
N1—C1	1.408 (8)	C22—C23	1.399 (6)
N2—C7	1.443 (5)	C25—C26	1.366 (9)
N4—C19	1.654 (10)	C26—C27	1.259 (10)
N4A—C19	1.393 (10)	C27—C28	1.332 (10)
N5—C29	1.276 (11)	C27—C30	1.507 (7)
N5—C25	1.283 (9)	C28—C29	1.492 (12)
N6—C35	1.516 (5)	C30—C31	1.391 (6)
C1—C2	1.354 (8)	C30—C35	1.417 (7)
C2—C3	1.411 (5)	C31—C32	1.364 (6)
C3—C4	1.379 (6)	C32—C33	1.408 (6)
C3—C6	1.469 (5)	C33—C34	1.366 (4)
C4—C5	1.315 (6)	C33—C36	1.530 (5)
C6—C11	1.386 (6)	C34—C35	1.366 (6)

O10ⁱ—Tb1—O7	92.49 (8)	C11—C10—C9	122.7 (4)
O10ⁱ—Tb1—O3	163.67 (8)	C10—C11—C6	122.0 (4)
O7—Tb1—O3	80.46 (8)	O3—C12—O4	123.0 (3)
O10ⁱ—Tb1—O1W	88.76 (10)	O3—C12—C9	119.8 (3)
O7—Tb1—O1W	145.59 (13)	O4—C12—C9	117.2 (3)
O3—Tb1—O1W	105.40 (10)	C13—N3—C17	120.0
O10ⁱ—Tb1—O8ⁱ	77.98 (10)	N3—C13—C14	120.0
O7—Tb1—O8ⁱ	73.48 (10)	C15—C14—C13	120.0
O3—Tb1—O8ⁱ	85.87 (11)	C14—C15—C16	120.0
O1W—Tb1—O8ⁱ	139.89 (13)	C14—C15—C18	117.9 (4)
O10ⁱ—Tb1—O4ⁱ	101.18 (9)	C16—C15—C18	118.9 (4)
O7—Tb1—O4ⁱ	143.39 (9)	C17—C16—C15	120.0
O3—Tb1—O4ⁱ	77.03 (8)	C16—C17—N3	120.0
O1W—Tb1—O4ⁱ	69.23 (11)	C13A—N3A—C17A	120.0
O8ⁱ—Tb1—O4ⁱ	76.42 (9)	C14A—C13A—N3A	120.0
O10ⁱ—Tb1—O9	84.72 (8)	C15A—C14A—C13A	120.0
O7—Tb1—O9	73.60 (10)	C14A—C15A—C16A	120.0
O3—Tb1—O9	107.06 (8)	C14A—C15A—C18	132.9 (6)
O1W—Tb1—O9	72.28 (12)	C16A—C15A—C18	107.1 (6)
O8ⁱ—Tb1—O9	141.85 (10)	C17A—C16A—C15A	120.0
O4ⁱ—Tb1—O9	140.85 (8)	C16A—C17A—N3A	120.0
O10ⁱ—Tb1—O2W	136.92 (10)	C23—C18—C19	115.5 (4)
O7—Tb1—O2W	114.81 (11)	C23—C18—C15	131.7 (6)
O3—Tb1—O2W	58.97 (11)	C19—C18—C15	111.8 (6)
O1W—Tb1—O2W	49.74 (13)	C23—C18—C15A	100.5 (5)
O8ⁱ—Tb1—O2W	139.70 (12)	C19—C18—C15A	141.3 (6)
O4ⁱ—Tb1—O2W	76.91 (9)	C15—C18—C15A	39.0 (5)
O9—Tb1—O2W	73.03 (9)	C20—C19—N4A	125.3 (7)
C12—O3—Tb1	139.16 (18)	C20—C19—C18	123.1 (6)
C12—O4—Tb1ⁱⁱ	131.4 (3)	N4A—C19—C18	103.6 (5)
C24—O7—Tb1	156.8 (2)	C20—C19—N4	111.0 (5)
C24—O8—Tb1ⁱⁱ	141.2 (2)	N4A—C19—N4	40.4 (5)
C36—O9—Tb1	124.98 (19)	C18—C19—N4	125.5 (5)
C36—O10—Tb1ⁱⁱ	142.7 (2)	C19—C20—C21	120.8 (4)
C5—N1—C1	115.5 (4)	C20—C21—C22	119.8 (3)
O2—N2—O1	119.6 (4)	C20—C21—C24	120.0 (3)
O2—N2—C7	122.9 (4)	C22—C21—C24	120.2 (3)
O1—N2—C7	117.4 (4)	C21—C22—C23	117.6 (4)
O6—N4—O5	128.6 (8)	C18—C23—C22	123.2 (5)
O6—N4—C19	120.7 (5)	O7—C24—O8	125.5 (3)
O5—N4—C19	110.7 (5)	O7—C24—C21	117.4 (3)
O6A—N4A—O5A	117.5 (10)	O8—C24—C21	117.1 (3)
O6A—N4A—C19	105.3 (7)	N5—C25—C26	119.0 (7)
O5A—N4A—C19	136.7 (9)	C27—C26—C25	127.5 (7)
C29—N5—C25	119.9 (6)	C26—C27—C28	114.7 (7)
O11—N6—O12	121.7 (4)	C26—C27—C30	125.5 (5)
O11—N6—C35	121.8 (4)	C28—C27—C30	117.8 (6)
O12—N6—C35	116.5 (5)	C27—C28—C29	118.8 (8)
C2—C1—N1	122.3 (5)	N5—C29—C28	119.4 (7)
C1—C2—C3	119.0 (5)	C31—C30—C35	115.5 (4)
C4—C3—C2	116.5 (4)	C31—C30—C27	121.5 (4)
C4—C3—C6	121.8 (3)	C35—C30—C27	122.9 (4)
C2—C3—C6	120.4 (4)	C32—C31—C30	122.3 (5)
C5—C4—C3	122.0 (4)	C31—C32—C33	119.7 (3)
C4—C5—N1	124.0 (5)	C34—C33—C32	120.1 (3)
C11—C6—C7	115.1 (3)	C34—C33—C36	119.0 (3)
C11—C6—C3	119.7 (4)	C32—C33—C36	120.9 (3)
C7—C6—C3	125.2 (4)	C35—C34—C33	118.9 (4)
C8—C7—C6	123.2 (3)	C34—C35—C30	123.4 (4)
C8—C7—N2	117.3 (3)	C34—C35—N6	115.2 (4)
C6—C7—N2	119.4 (3)	C30—C35—N6	121.4 (4)
C7—C8—C9	120.0 (4)	O9—C36—O10	124.4 (3)
C10—C9—C8	117.0 (3)	O9—C36—C33	119.4 (3)
C10—C9—C12	122.1 (3)	O10—C36—C33	116.2 (3)
C8—C9—C12	120.9 (3)

O10ⁱ—Tb1—O3—C12	−40.0 (5)	C14A—C15A—C18—C19	−122.3 (10)
O7—Tb1—O3—C12	25.3 (3)	C16A—C15A—C18—C19	54.0 (10)
O1W—Tb1—O3—C12	170.6 (3)	C14A—C15A—C18—C15	−175.7 (12)
O8ⁱ—Tb1—O3—C12	−48.6 (3)	C16A—C15A—C18—C15	0.6 (6)
O4ⁱ—Tb1—O3—C12	−125.6 (3)	O6A—N4A—C19—C20	63.2 (13)
O9—Tb1—O3—C12	94.8 (3)	O5A—N4A—C19—C20	−125.3 (14)
O2W—Tb1—O3—C12	152.0 (4)	O6A—N4A—C19—C18	−147.5 (10)
O10ⁱ—Tb1—O7—C24	−138.6 (6)	O5A—N4A—C19—C18	24.0 (17)
O3—Tb1—O7—C24	56.3 (6)	O6A—N4A—C19—N4	−18.0 (9)
O1W—Tb1—O7—C24	−47.1 (7)	O5A—N4A—C19—N4	154 (2)
O8ⁱ—Tb1—O7—C24	144.8 (7)	C23—C18—C19—C20	0.2 (8)
O4ⁱ—Tb1—O7—C24	108.9 (6)	C15—C18—C19—C20	−170.2 (5)
O9—Tb1—O7—C24	−54.8 (6)	C15A—C18—C19—C20	156.9 (8)
O2W—Tb1—O7—C24	7.1 (7)	C23—C18—C19—N4A	−150.0 (7)
O10ⁱ—Tb1—O9—C36	166.6 (3)	C15—C18—C19—N4A	39.7 (8)
O7—Tb1—O9—C36	72.5 (3)	C15A—C18—C19—N4A	6.7 (12)
O3—Tb1—O9—C36	−1.8 (3)	C23—C18—C19—N4	172.2 (5)
O1W—Tb1—O9—C36	−103.0 (3)	C15—C18—C19—N4	1.8 (8)
O8ⁱ—Tb1—O9—C36	103.8 (3)	C15A—C18—C19—N4	−31.1 (12)
O4ⁱ—Tb1—O9—C36	−92.1 (3)	O6—N4—C19—C20	39.7 (10)
O2W—Tb1—O9—C36	−50.7 (3)	O5—N4—C19—C20	−138.4 (6)
C5—N1—C1—C2	4.3 (10)	O6—N4—C19—N4A	159.9 (12)
N1—C1—C2—C3	−8.7 (10)	O5—N4—C19—N4A	−18.1 (8)
C1—C2—C3—C4	5.9 (8)	O6—N4—C19—C18	−133.1 (8)
C1—C2—C3—C6	173.1 (5)	O5—N4—C19—C18	48.8 (9)
C2—C3—C4—C5	1.1 (9)	N4A—C19—C20—C21	143.8 (7)
C6—C3—C4—C5	−165.9 (6)	C18—C19—C20—C21	0.1 (8)
C3—C4—C5—N1	−5.8 (11)	N4—C19—C20—C21	−172.9 (4)
C1—N1—C5—C4	3.1 (11)	C19—C20—C21—C22	−0.2 (7)
C4—C3—C6—C11	52.6 (6)	C19—C20—C21—C24	−179.8 (4)
C2—C3—C6—C11	−113.9 (5)	C20—C21—C22—C23	0.0 (6)
C4—C3—C6—C7	−128.7 (5)	C24—C21—C22—C23	179.6 (4)
C2—C3—C6—C7	64.8 (6)	C19—C18—C23—C22	−0.4 (8)
C11—C6—C7—C8	1.1 (5)	C15—C18—C23—C22	167.6 (6)
C3—C6—C7—C8	−177.6 (3)	C15A—C18—C23—C22	−165.8 (6)
C11—C6—C7—N2	−175.4 (3)	C21—C22—C23—C18	0.3 (7)
C3—C6—C7—N2	5.9 (5)	Tb1—O7—C24—O8	−5.3 (9)
O2—N2—C7—C8	−152.5 (3)	Tb1—O7—C24—C21	177.8 (4)
O1—N2—C7—C8	23.6 (4)	Tb1ⁱⁱ—O8—C24—O7	−23.6 (7)
O2—N2—C7—C6	24.2 (4)	Tb1ⁱⁱ—O8—C24—C21	153.3 (3)
O1—N2—C7—C6	−159.6 (3)	C20—C21—C24—O7	9.2 (5)
C6—C7—C8—C9	−1.0 (5)	C22—C21—C24—O7	−170.4 (4)
N2—C7—C8—C9	175.6 (3)	C20—C21—C24—O8	−168.0 (4)
C7—C8—C9—C10	−0.8 (4)	C22—C21—C24—O8	12.4 (5)
C7—C8—C9—C12	−179.6 (3)	C29—N5—C25—C26	−5.1 (8)
C8—C9—C10—C11	2.6 (5)	N5—C25—C26—C27	10.5 (9)
C12—C9—C10—C11	−178.6 (3)	C25—C26—C27—C28	−9.0 (9)
C9—C10—C11—C6	−2.5 (6)	C25—C26—C27—C30	−172.5 (5)
C7—C6—C11—C10	0.6 (5)	C26—C27—C28—C29	3.1 (8)
C3—C6—C11—C10	179.4 (3)	C30—C27—C28—C29	168.0 (5)
Tb1—O3—C12—O4	−83.2 (4)	C25—N5—C29—C28	0.2 (9)
Tb1—O3—C12—C9	99.9 (3)	C27—C28—C29—N5	1.0 (10)
Tb1ⁱⁱ—O4—C12—O3	−9.0 (4)	C26—C27—C30—C31	88.9 (8)
Tb1ⁱⁱ—O4—C12—C9	167.92 (19)	C28—C27—C30—C31	−74.1 (7)
C10—C9—C12—O3	176.3 (3)	C26—C27—C30—C35	−87.3 (7)
C8—C9—C12—O3	−5.0 (4)	C28—C27—C30—C35	109.6 (6)
C10—C9—C12—O4	−0.8 (4)	C35—C30—C31—C32	2.8 (8)
C8—C9—C12—O4	178.0 (3)	C27—C30—C31—C32	−173.7 (5)
C17—N3—C13—C14	0.0	C30—C31—C32—C33	0.3 (8)
N3—C13—C14—C15	0.0	C31—C32—C33—C34	−2.9 (6)
C13—C14—C15—C16	0.0	C31—C32—C33—C36	176.1 (4)
C13—C14—C15—C18	−159.5 (5)	C32—C33—C34—C35	2.1 (6)
C14—C15—C16—C17	0.0	C36—C33—C34—C35	−177.0 (4)
C18—C15—C16—C17	159.3 (5)	C33—C34—C35—C30	1.3 (7)
C15—C16—C17—N3	0.0	C33—C34—C35—N6	179.8 (4)
C13—N3—C17—C16	0.0	C31—C30—C35—C34	−3.6 (8)
C17A—N3A—C13A—C14A	0.0	C27—C30—C35—C34	172.8 (5)
N3A—C13A—C14A—C15A	0.0	C31—C30—C35—N6	177.9 (5)
C13A—C14A—C15A—C16A	0.0	C27—C30—C35—N6	−5.7 (8)
C13A—C14A—C15A—C18	175.9 (8)	O11—N6—C35—C34	−2.1 (7)
C14A—C15A—C16A—C17A	0.0	O12—N6—C35—C34	176.9 (5)
C18—C15A—C16A—C17A	−176.9 (6)	O11—N6—C35—C30	176.5 (5)
C15A—C16A—C17A—N3A	0.0	O12—N6—C35—C30	−4.5 (8)
C13A—N3A—C17A—C16A	0.0	Tb1—O9—C36—O10	5.9 (5)
C14—C15—C18—C23	47.7 (8)	Tb1—O9—C36—C33	−176.2 (2)
C16—C15—C18—C23	−112.0 (7)	Tb1ⁱⁱ—O10—C36—O9	−100.6 (4)
C14—C15—C18—C19	−144.0 (4)	Tb1ⁱⁱ—O10—C36—C33	81.5 (5)
C16—C15—C18—C19	56.3 (6)	C34—C33—C36—O9	13.1 (5)
C14—C15—C18—C15A	3.2 (7)	C32—C33—C36—O9	−166.0 (4)
C16—C15—C18—C15A	−156.5 (9)	C34—C33—C36—O10	−168.9 (4)
C14A—C15A—C18—C23	36.4 (9)	C32—C33—C36—O10	12.1 (5)
C16A—C15A—C18—C23	−147.3 (4)

Symmetry codes: (i) y, −x+y, z+1/6; (ii) x−y, x, z−1/6.

Poly[diaquatris[µ₂-3-nitro-4-(pyridin-4-yl)benzoato-κ²O:O']terbium(III)] (1502118) top

Crystal data top

[Tb(C₁₂H₇N₂O₄)₃(H₂O)₂]	D_x = 1.699 Mg m⁻³
M_r = 924.54	Mo Kα radiation, λ = 0.71073 Å
Hexagonal, P6₁	Cell parameters from 8187 reflections
Hall symbol: P 61	θ = 2.7–27.0°
a = 14.962 (2) Å	µ = 2.04 mm⁻¹
c = 27.974 (5) Å	T = 296 K
V = 5423.2 (15) Å³	Rodlike, colorless
Z = 6	0.16 × 0.12 × 0.12 mm
F(000) = 2760

Data collection top

Bruker APEXII CCD diffractometer	6932 independent reflections
Radiation source: fine-focus sealed tube	6262 reflections with I > 2σ(I)
Graphite monochromator	R_int = 0.066
ω scans	θ_max = 26.0°, θ_min = 1.6°
Absorption correction: multi-scan (SADABS; Sheldrick, 2003)	h = −18→18
T_min = 0.746, T_max = 0.783	k = −17→18
40050 measured reflections	l = −34→34

Refinement top

Refinement on F²	Secondary atom site location: difference Fourier map
Least-squares matrix: full	Hydrogen site location: inferred from neighbouring sites
R[F² > 2σ(F²)] = 0.048	H atoms treated by a mixture of independent and constrained refinement
wR(F²) = 0.115	w = 1/[σ²(F_o²) + (0.0525P)² + 15.9885P] where P = (F_o² + 2F_c²)/3
S = 1.05	(Δ/σ)_max = 0.010
6932 reflections	Δρ_max = 1.55 e Å⁻³
573 parameters	Δρ_min = −1.06 e Å⁻³
222 restraints	Absolute structure: Flack (1983), 3298 Friedel pairs
Primary atom site location: structure-invariant direct methods	Absolute structure parameter: 0.025 (19)

Special details top

Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å²) top

	x	y	z	U_iso*/U_eq	Occ. (<1)
Tb1	−0.067774 (9)	−0.028271 (10)	0.116213 (11)	0.03015 (3)
O1	0.1608 (3)	0.3561 (3)	0.20552 (13)	0.0990 (15)
O1W	−0.2351 (4)	−0.0667 (4)	0.13589 (18)	0.1724 (16)
H1WA	−0.2553	−0.0321	0.1523	0.207*
H1WB	−0.2822	−0.1300	0.1369	0.207*
O2	0.3241 (3)	0.4466 (3)	0.20908 (13)	0.0934 (15)
O2W	−0.1863 (3)	0.0406 (3)	0.07406 (14)	0.1724 (16)
H2WA	−0.2211 (4)	−0.0082 (4)	0.0523 (2)	0.207*
H2WB	−0.1430 (6)	0.0955 (3)	0.0557 (2)	0.207*
O3	0.00695 (15)	0.12254 (14)	0.07239 (8)	0.0352 (6)
O4	0.09439 (16)	0.15731 (18)	0.00429 (9)	0.0466 (7)
O5	0.3255 (4)	−0.1818 (4)	0.1388 (2)	0.0970 (19)	0.599 (4)
O5A	0.2812 (5)	−0.2684 (6)	0.1121 (4)	0.091 (3)	0.401 (4)
O6	0.3339 (5)	−0.0314 (5)	0.1470 (3)	0.125 (2)	0.599 (4)
O6A	0.2988 (8)	−0.1303 (9)	0.1416 (4)	0.117 (4)	0.401 (4)
O7	0.03070 (15)	−0.06303 (17)	0.06538 (9)	0.0460 (7)
O8	0.03981 (17)	−0.05483 (17)	−0.01408 (10)	0.0543 (7)
O9	−0.18477 (17)	−0.16533 (16)	0.06420 (8)	0.0433 (8)
O10	−0.15940 (15)	−0.06735 (15)	−0.00039 (8)	0.0383 (7)
O11	−0.3651 (3)	−0.5366 (3)	0.04508 (16)	0.1127 (18)
O12	−0.4570 (4)	−0.6098 (4)	−0.0141 (2)	0.1377 (14)
N1	0.5949 (3)	0.7402 (3)	0.1463 (2)	0.100 (2)
N2	0.2472 (2)	0.3977 (2)	0.18591 (11)	0.0501 (10)
N4	0.3154 (4)	−0.1055 (4)	0.1264 (3)	0.0735 (19)	0.599 (4)
N4A	0.2811 (5)	−0.1843 (6)	0.1083 (4)	0.072 (3)	0.401 (4)
N5	−0.6503 (4)	−0.6652 (3)	−0.1424 (2)	0.1003 (18)
N6	−0.3977 (3)	−0.5324 (2)	0.0069 (2)	0.0918 (17)
C1	0.6081 (3)	0.6633 (4)	0.1304 (3)	0.101 (2)
H1A	0.6745	0.6744	0.1259	0.121*
C2	0.5247 (3)	0.5685 (3)	0.1207 (2)	0.0735 (16)
H2A	0.5362	0.5167	0.1094	0.088*
C3	0.4261 (3)	0.5469 (3)	0.12686 (17)	0.0570 (13)
C4	0.4109 (3)	0.6285 (3)	0.1417 (2)	0.0747 (17)
H4A	0.3452	0.6203	0.1439	0.090*
C5	0.4967 (4)	0.7198 (4)	0.1527 (2)	0.095 (2)
H5A	0.4872	0.7718	0.1656	0.114*
C6	0.3394 (3)	0.4496 (2)	0.10893 (15)	0.0489 (12)
C7	0.2502 (2)	0.3822 (2)	0.13547 (13)	0.0397 (10)
C8	0.1706 (2)	0.2939 (2)	0.11688 (14)	0.0382 (9)
H8A	0.1158	0.2500	0.1365	0.046*
C9	0.1705 (2)	0.2684 (2)	0.06866 (12)	0.0358 (9)
C10	0.2565 (3)	0.3343 (3)	0.04243 (14)	0.0528 (13)
H10A	0.2603	0.3186	0.0106	0.063*
C11	0.3365 (3)	0.4220 (3)	0.06161 (15)	0.0581 (14)
H11A	0.3915	0.4650	0.0419	0.070*
C12	0.0839 (2)	0.1747 (2)	0.04704 (12)	0.0364 (9)
N3	0.5836 (2)	−0.1520 (3)	0.03007 (19)	0.162 (4)	0.568 (4)
C13	0.4949 (3)	−0.2362 (4)	0.0120 (3)	0.128 (2)	0.568 (4)
H13A	0.4993	−0.2879	−0.0044	0.154*	0.568 (4)
C14	0.3995 (3)	−0.2431 (4)	0.0185 (3)	0.115 (2)	0.568 (4)
H14A	0.3401	−0.2995	0.0064	0.139*	0.568 (4)
C15	0.3928 (3)	−0.1658 (5)	0.0430 (3)	0.077 (2)	0.568 (4)
C16	0.4816 (4)	−0.0816 (5)	0.0610 (3)	0.100 (2)	0.568 (4)
H16A	0.4771	−0.0298	0.0774	0.120*	0.568 (4)
C17	0.5769 (3)	−0.0746 (4)	0.0546 (3)	0.125 (3)	0.568 (4)
H17A	0.6363	−0.0183	0.0666	0.150*	0.568 (4)
N3A	0.4721 (4)	−0.3208 (4)	0.0039 (2)	0.112 (4)	0.432 (4)
C13A	0.3796 (4)	−0.3593 (5)	−0.0209 (3)	0.157 (6)	0.432 (4)
H13B	0.3576	−0.4165	−0.0407	0.189*	0.432 (4)
C14A	0.3200 (5)	−0.3124 (7)	−0.0162 (3)	0.092 (4)	0.432 (4)
H14B	0.2581	−0.3382	−0.0328	0.111*	0.432 (4)
C15A	0.3529 (6)	−0.2269 (7)	0.0134 (4)	0.062 (3)	0.432 (4)
C16A	0.4453 (7)	−0.1884 (6)	0.0383 (4)	0.115 (3)	0.432 (4)
H16B	0.4673	−0.1313	0.0580	0.138*	0.432 (4)
C17A	0.5050 (5)	−0.2353 (5)	0.0335 (3)	0.110 (4)	0.432 (4)
H17B	0.5668	−0.2096	0.0501	0.133*	0.432 (4)
C18	0.2970 (3)	−0.1589 (3)	0.0316 (2)	0.0967 (16)
C19	0.2623 (3)	−0.1278 (4)	0.0730 (2)	0.0925 (17)
C20	0.1901 (3)	−0.1034 (3)	0.07003 (15)	0.0587 (13)
H20A	0.1688	−0.0847	0.0977	0.070*
C21	0.1447 (2)	−0.1044 (2)	0.02729 (13)	0.0354 (9)
C22	0.1757 (2)	−0.1310 (2)	−0.01413 (15)	0.0521 (11)
H22A	0.1470	−0.1299	−0.0434	0.062*
C23	0.2526 (3)	−0.1601 (3)	−0.0111 (2)	0.0766 (14)
H23A	0.2728	−0.1803	−0.0386	0.092*
C24	0.0661 (2)	−0.0704 (2)	0.02600 (12)	0.0393 (9)
C25	−0.6747 (4)	−0.6325 (4)	−0.1053 (3)	0.117 (3)
H25A	−0.7430	−0.6572	−0.0964	0.141*
C26	−0.5910 (4)	−0.5559 (4)	−0.0788 (2)	0.109 (2)
H26A	−0.6091	−0.5300	−0.0526	0.131*
C27	−0.4933 (4)	−0.5168 (3)	−0.0855 (2)	0.0893 (18)
C28	−0.4723 (5)	−0.5503 (5)	−0.1244 (3)	0.129 (3)
H28A	−0.4036	−0.5240	−0.1331	0.155*
C29	−0.5562 (6)	−0.6312 (6)	−0.1562 (3)	0.148 (3)
H29A	−0.5408	−0.6549	−0.1840	0.178*
C30	−0.4119 (3)	−0.4247 (3)	−0.05899 (19)	0.0752 (16)
C31	−0.3779 (3)	−0.3265 (3)	−0.07682 (17)	0.0686 (15)
H31A	−0.4031	−0.3188	−0.1060	0.082*
C32	−0.3068 (3)	−0.2395 (3)	−0.05196 (17)	0.0600 (13)
H32A	−0.2831	−0.1743	−0.0650	0.072*
C33	−0.2710 (2)	−0.2496 (2)	−0.00767 (12)	0.0342 (9)
C34	−0.3011 (2)	−0.3458 (2)	0.01004 (14)	0.0425 (11)
H34A	−0.2755	−0.3533	0.0392	0.051*
C35	−0.3707 (3)	−0.4329 (3)	−0.01613 (18)	0.0603 (14)
C36	−0.1986 (2)	−0.1537 (2)	0.02046 (13)	0.0342 (9)

Atomic displacement parameters (Å²) top

	U¹¹	U²²	U³³	U¹²	U¹³	U²³
Tb1	0.03251 (5)	0.02761 (5)	0.02193 (5)	0.00875 (4)	0.00026 (6)	−0.00185 (5)
O1	0.0811 (19)	0.112 (2)	0.064 (2)	0.0187 (16)	0.0083 (16)	−0.0206 (17)
O1W	0.157 (2)	0.169 (2)	0.196 (3)	0.0861 (14)	−0.005 (2)	−0.031 (2)
O2	0.0816 (18)	0.119 (2)	0.063 (2)	0.0373 (16)	−0.0210 (16)	−0.0356 (18)
O2W	0.157 (2)	0.169 (2)	0.196 (3)	0.0861 (14)	−0.005 (2)	−0.031 (2)
O3	0.0449 (9)	0.0256 (8)	0.0318 (12)	0.0151 (6)	0.0001 (9)	−0.0016 (8)
O4	0.0452 (9)	0.0642 (11)	0.0328 (12)	0.0292 (8)	−0.0065 (9)	−0.0137 (10)
O5	0.096 (2)	0.130 (3)	0.089 (3)	0.0750 (18)	0.003 (2)	0.054 (2)
O5A	0.096 (3)	0.124 (3)	0.090 (5)	0.083 (2)	0.022 (4)	0.036 (4)
O6	0.151 (3)	0.148 (3)	0.128 (5)	0.114 (2)	−0.044 (3)	−0.012 (3)
O6A	0.123 (5)	0.131 (6)	0.096 (6)	0.063 (4)	−0.015 (5)	0.005 (5)
O7	0.0583 (9)	0.0657 (10)	0.0302 (13)	0.0430 (7)	0.0009 (9)	−0.0114 (9)
O8	0.0818 (9)	0.0797 (10)	0.0365 (13)	0.0666 (6)	−0.0152 (10)	−0.0120 (9)
O9	0.0476 (11)	0.0373 (10)	0.0222 (11)	0.0041 (9)	−0.0092 (9)	−0.0115 (9)
O10	0.0384 (9)	0.0296 (8)	0.0391 (13)	0.0112 (7)	0.0037 (9)	−0.0033 (9)
O11	0.149 (3)	0.0778 (19)	0.093 (3)	0.0432 (18)	−0.005 (2)	0.017 (2)
O12	0.1449 (18)	0.1237 (17)	0.144 (2)	0.0664 (12)	−0.0222 (16)	0.0075 (16)
N1	0.0506 (19)	0.071 (2)	0.152 (5)	0.0102 (17)	−0.015 (2)	−0.013 (3)
N2	0.0509 (14)	0.0451 (13)	0.0417 (17)	0.0147 (11)	−0.0123 (13)	−0.0170 (13)
N4	0.062 (2)	0.088 (2)	0.090 (4)	0.0519 (16)	−0.014 (2)	0.025 (3)
N4A	0.074 (3)	0.103 (4)	0.072 (6)	0.068 (2)	−0.002 (4)	0.012 (4)
N5	0.117 (3)	0.0614 (18)	0.116 (4)	0.0399 (17)	−0.030 (3)	−0.019 (2)
N6	0.0694 (19)	0.0264 (13)	0.169 (4)	0.0157 (12)	−0.033 (2)	−0.028 (2)
C1	0.0375 (18)	0.077 (3)	0.167 (6)	0.0129 (18)	0.011 (3)	−0.030 (3)
C2	0.0603 (19)	0.0488 (18)	0.096 (3)	0.0157 (15)	0.015 (2)	−0.009 (2)
C3	0.0382 (14)	0.0421 (15)	0.082 (3)	0.0131 (11)	−0.0004 (17)	−0.0175 (17)
C4	0.0440 (17)	0.0486 (18)	0.124 (4)	0.0172 (14)	−0.013 (2)	−0.026 (2)
C5	0.083 (2)	0.069 (2)	0.138 (4)	0.0408 (16)	−0.016 (3)	−0.040 (2)
C6	0.0539 (16)	0.0279 (12)	0.055 (2)	0.0129 (11)	0.0077 (17)	−0.0015 (14)
C7	0.0454 (13)	0.0359 (12)	0.0372 (17)	0.0200 (10)	0.0011 (13)	−0.0055 (12)
C8	0.0364 (11)	0.0384 (12)	0.0374 (16)	0.0168 (9)	0.0013 (15)	0.0027 (14)
C9	0.0463 (12)	0.0403 (12)	0.0255 (16)	0.0251 (9)	0.0017 (12)	0.0001 (11)
C10	0.0579 (18)	0.0540 (18)	0.034 (2)	0.0185 (14)	0.0068 (16)	0.0053 (16)
C11	0.0515 (18)	0.0492 (19)	0.043 (2)	0.0022 (16)	0.0237 (16)	0.0094 (17)
C12	0.0488 (13)	0.0341 (11)	0.0320 (17)	0.0250 (9)	0.0000 (12)	−0.0002 (11)
N3	0.115 (4)	0.190 (6)	0.202 (8)	0.091 (4)	0.008 (6)	0.012 (6)
C13	0.130 (3)	0.144 (3)	0.156 (4)	0.102 (2)	0.030 (3)	−0.006 (3)
C14	0.122 (2)	0.133 (3)	0.157 (4)	0.1130 (18)	0.023 (3)	0.001 (3)
C15	0.061 (2)	0.099 (3)	0.089 (4)	0.0543 (18)	−0.005 (3)	0.010 (3)
C16	0.085 (3)	0.127 (3)	0.102 (4)	0.065 (2)	0.005 (3)	0.043 (3)
C17	0.108 (4)	0.142 (4)	0.110 (4)	0.050 (3)	0.012 (3)	0.029 (4)
N3A	0.115 (5)	0.122 (5)	0.114 (7)	0.071 (4)	0.031 (5)	0.035 (5)
C13A	0.158 (8)	0.156 (8)	0.163 (9)	0.082 (5)	0.033 (7)	0.009 (7)
C14A	0.094 (4)	0.102 (4)	0.118 (8)	0.077 (3)	0.018 (5)	0.006 (5)
C15A	0.068 (3)	0.086 (4)	0.062 (5)	0.061 (2)	0.020 (3)	0.022 (4)
C16A	0.111 (4)	0.123 (4)	0.116 (4)	0.062 (3)	0.007 (4)	−0.006 (4)
C17A	0.132 (5)	0.124 (5)	0.111 (7)	0.091 (3)	−0.013 (5)	0.032 (5)
C18	0.0754 (15)	0.134 (2)	0.119 (4)	0.0810 (12)	0.033 (2)	0.066 (2)
C19	0.0670 (19)	0.127 (3)	0.085 (3)	0.0498 (16)	−0.002 (2)	0.045 (2)
C20	0.0495 (15)	0.085 (2)	0.042 (2)	0.0338 (13)	−0.0014 (15)	0.0266 (16)
C21	0.0321 (11)	0.0381 (12)	0.0386 (17)	0.0196 (8)	0.0016 (12)	0.0076 (12)
C22	0.0671 (13)	0.0629 (13)	0.053 (2)	0.0529 (9)	0.0065 (15)	0.0035 (14)
C23	0.0759 (14)	0.0821 (16)	0.106 (4)	0.0655 (11)	0.0404 (19)	0.024 (2)
C24	0.0455 (12)	0.0509 (13)	0.0312 (17)	0.0313 (9)	−0.0047 (13)	0.0004 (12)
C25	0.108 (4)	0.073 (3)	0.126 (5)	0.012 (3)	−0.033 (4)	−0.001 (3)
C26	0.086 (3)	0.074 (3)	0.104 (4)	−0.007 (2)	−0.047 (3)	−0.002 (3)
C27	0.098 (3)	0.0522 (18)	0.112 (3)	0.0339 (17)	−0.060 (2)	−0.049 (2)
C28	0.104 (3)	0.136 (3)	0.134 (4)	0.049 (3)	−0.031 (3)	−0.072 (3)
C29	0.154 (4)	0.129 (3)	0.153 (4)	0.065 (2)	0.002 (3)	−0.044 (3)
C30	0.0680 (19)	0.0514 (17)	0.099 (3)	0.0246 (14)	−0.046 (2)	−0.030 (2)
C31	0.080 (2)	0.0498 (18)	0.066 (3)	0.0251 (15)	−0.037 (2)	−0.0237 (18)
C32	0.0627 (18)	0.0463 (16)	0.053 (2)	0.0138 (14)	−0.022 (2)	−0.0131 (19)
C33	0.0331 (12)	0.0314 (12)	0.0348 (17)	0.0136 (9)	−0.0140 (12)	−0.0109 (12)
C34	0.0412 (14)	0.0300 (13)	0.048 (2)	0.0113 (11)	−0.0062 (14)	−0.0049 (13)
C35	0.0552 (17)	0.0326 (14)	0.089 (3)	0.0189 (12)	−0.0243 (19)	−0.0207 (17)
C36	0.0219 (10)	0.0294 (11)	0.0465 (18)	0.0091 (8)	−0.0088 (12)	−0.0147 (12)

Geometric parameters (Å, º) top

Tb1—O7	2.287 (3)	C6—C7	1.415 (4)
Tb1—O10ⁱ	2.287 (2)	C7—C8	1.364 (4)
Tb1—O3	2.3068 (19)	C8—C9	1.401 (5)
Tb1—O1W	2.337 (6)	C9—C10	1.378 (4)
Tb1—O8ⁱ	2.346 (3)	C9—C12	1.481 (4)
Tb1—O4ⁱ	2.363 (2)	C10—C11	1.368 (5)
Tb1—O9	2.408 (2)	N3—C13	1.3900
Tb1—O2W	2.725 (5)	N3—C17	1.3900
O1—N2	1.247 (5)	C13—C14	1.3900
O2—N2	1.199 (4)	C14—C15	1.3900
O3—C12	1.241 (3)	C15—C16	1.3900
O4—C12	1.250 (4)	C15—C18	1.521 (7)
O4—Tb1ⁱⁱ	2.363 (2)	C16—C17	1.3900
O5—N4	1.272 (9)	N3A—C13A	1.3900
O5A—N4A	1.264 (13)	N3A—C17A	1.3900
O6—N4	1.152 (10)	C13A—C14A	1.3900
O6A—N4A	1.174 (15)	C14A—C15A	1.3900
O7—C24	1.251 (4)	C15A—C16A	1.3900
O8—C24	1.248 (4)	C15A—C18	1.686 (9)
O8—Tb1ⁱⁱ	2.346 (3)	C16A—C17A	1.3900
O9—C36	1.267 (4)	C18—C23	1.363 (8)
O10—C36	1.264 (4)	C18—C19	1.439 (9)
O10—Tb1ⁱⁱ	2.287 (2)	C19—C20	1.305 (8)
O11—N6	1.190 (7)	C20—C21	1.371 (5)
O12—N6	1.202 (6)	C21—C22	1.378 (5)
N1—C1	1.336 (8)	C21—C24	1.498 (5)
N1—C5	1.356 (7)	C22—C23	1.422 (6)
N2—C7	1.434 (5)	C25—C26	1.414 (7)
N4—C19	1.647 (9)	C26—C27	1.287 (8)
N4A—C19	1.417 (12)	C27—C28	1.301 (10)
N5—C25	1.275 (9)	C27—C30	1.502 (6)
N5—C29	1.294 (10)	C28—C29	1.521 (10)
N6—C35	1.481 (6)	C30—C35	1.381 (7)
C1—C2	1.369 (5)	C30—C31	1.385 (6)
C2—C3	1.355 (6)	C31—C32	1.388 (5)
C3—C4	1.412 (7)	C32—C33	1.388 (6)
C3—C6	1.471 (4)	C33—C34	1.369 (5)
C4—C5	1.362 (5)	C33—C36	1.515 (4)
C6—C11	1.381 (6)	C34—C35	1.400 (5)

O7—Tb1—O10ⁱ	91.71 (9)	C11—C10—C9	122.3 (4)
O7—Tb1—O3	80.78 (9)	C10—C11—C6	122.9 (3)
O10ⁱ—Tb1—O3	162.94 (9)	O3—C12—O4	126.1 (2)
O7—Tb1—O1W	145.42 (13)	O3—C12—C9	117.3 (3)
O10ⁱ—Tb1—O1W	87.35 (15)	O4—C12—C9	116.5 (2)
O3—Tb1—O1W	107.53 (15)	C13—N3—C17	120.0
O7—Tb1—O8ⁱ	73.93 (8)	C14—C13—N3	120.0
O10ⁱ—Tb1—O8ⁱ	78.03 (9)	C13—C14—C15	120.0
O3—Tb1—O8ⁱ	85.16 (8)	C14—C15—C16	120.0
O1W—Tb1—O8ⁱ	138.96 (14)	C14—C15—C18	114.5 (4)
O7—Tb1—O4ⁱ	143.75 (8)	C16—C15—C18	121.3 (4)
O10ⁱ—Tb1—O4ⁱ	101.50 (8)	C17—C16—C15	120.0
O3—Tb1—O4ⁱ	76.89 (8)	C16—C17—N3	120.0
O1W—Tb1—O4ⁱ	69.60 (15)	C13A—N3A—C17A	120.0
O8ⁱ—Tb1—O4ⁱ	76.04 (9)	N3A—C13A—C14A	120.0
O7—Tb1—O9	72.98 (8)	C15A—C14A—C13A	120.0
O10ⁱ—Tb1—O9	84.46 (8)	C16A—C15A—C14A	120.0
O3—Tb1—O9	107.60 (7)	C16A—C15A—C18	106.9 (5)
O1W—Tb1—O9	72.53 (14)	C14A—C15A—C18	132.9 (5)
O8ⁱ—Tb1—O9	141.83 (9)	C15A—C16A—C17A	120.0
O4ⁱ—Tb1—O9	141.26 (10)	C16A—C17A—N3A	120.0
O7—Tb1—O2W	115.60 (11)	C23—C18—C19	117.2 (5)
O10ⁱ—Tb1—O2W	137.33 (10)	C23—C18—C15	130.7 (6)
O3—Tb1—O2W	59.26 (9)	C19—C18—C15	111.0 (5)
O1W—Tb1—O2W	51.33 (15)	C23—C18—C15A	96.5 (5)
O8ⁱ—Tb1—O2W	138.78 (8)	C19—C18—C15A	143.7 (6)
O4ⁱ—Tb1—O2W	76.10 (10)	C15—C18—C15A	41.8 (4)
O9—Tb1—O2W	74.17 (10)	C20—C19—N4A	130.6 (6)
C12—O3—Tb1	139.7 (2)	C20—C19—C18	121.5 (5)
C12—O4—Tb1ⁱⁱ	130.05 (17)	N4A—C19—C18	99.0 (6)
C24—O7—Tb1	156.5 (3)	C20—C19—N4	112.6 (5)
C24—O8—Tb1ⁱⁱ	140.8 (3)	N4A—C19—N4	43.0 (5)
C36—O9—Tb1	124.46 (17)	C18—C19—N4	125.5 (5)
C36—O10—Tb1ⁱⁱ	142.7 (2)	C19—C20—C21	121.8 (4)
C1—N1—C5	117.5 (4)	C20—C21—C22	120.0 (4)
O2—N2—O1	120.4 (4)	C20—C21—C24	119.1 (3)
O2—N2—C7	122.2 (3)	C22—C21—C24	120.8 (3)
O1—N2—C7	117.4 (3)	C21—C22—C23	118.6 (4)
O6—N4—O5	130.4 (8)	C18—C23—C22	120.8 (5)
O6—N4—C19	120.5 (7)	O8—C24—O7	126.0 (4)
O5—N4—C19	109.1 (6)	O8—C24—C21	117.4 (3)
O6A—N4A—O5A	120.5 (12)	O7—C24—C21	116.6 (3)
O6A—N4A—C19	100.8 (10)	N5—C25—C26	115.5 (6)
O5A—N4A—C19	138.7 (10)	C27—C26—C25	129.5 (7)
C25—N5—C29	123.8 (6)	C26—C27—C28	112.7 (5)
O11—N6—O12	120.8 (5)	C26—C27—C30	124.1 (6)
O11—N6—C35	122.1 (4)	C28—C27—C30	121.7 (5)
O12—N6—C35	117.1 (5)	C27—C28—C29	122.2 (6)
N1—C1—C2	120.5 (5)	N5—C29—C28	116.2 (8)
C3—C2—C1	122.8 (5)	C35—C30—C31	117.5 (4)
C2—C3—C4	117.3 (3)	C35—C30—C27	122.8 (4)
C2—C3—C6	120.6 (4)	C31—C30—C27	119.6 (5)
C4—C3—C6	120.9 (4)	C30—C31—C32	121.2 (4)
C5—C4—C3	117.1 (5)	C33—C32—C31	120.1 (4)
N1—C5—C4	124.5 (6)	C34—C33—C32	119.7 (3)
C11—C6—C7	114.4 (3)	C34—C33—C36	120.8 (3)
C11—C6—C3	120.2 (3)	C32—C33—C36	119.5 (3)
C7—C6—C3	125.2 (4)	C33—C34—C35	119.3 (4)
C8—C7—C6	123.1 (3)	C30—C35—C34	122.0 (4)
C8—C7—N2	116.7 (3)	C30—C35—N6	123.8 (3)
C6—C7—N2	119.7 (3)	C34—C35—N6	114.2 (4)
C7—C8—C9	120.8 (3)	O10—C36—O9	124.2 (3)
C10—C9—C8	116.4 (3)	O10—C36—C33	118.4 (3)
C10—C9—C12	121.4 (3)	O9—C36—C33	117.4 (3)
C8—C9—C12	122.2 (2)

O7—Tb1—O3—C12	−22.3 (3)	C16A—C15A—C18—C19	−55.0 (8)
O10ⁱ—Tb1—O3—C12	42.5 (5)	C14A—C15A—C18—C19	118.9 (8)
O1W—Tb1—O3—C12	−167.7 (3)	C16A—C15A—C18—C15	−3.0 (5)
O8ⁱ—Tb1—O3—C12	52.2 (3)	C14A—C15A—C18—C15	170.8 (10)
O4ⁱ—Tb1—O3—C12	129.0 (3)	O6A—N4A—C19—C20	−63.7 (9)
O9—Tb1—O3—C12	−91.0 (3)	O5A—N4A—C19—C20	114.7 (12)
O2W—Tb1—O3—C12	−149.6 (3)	O6A—N4A—C19—C18	149.9 (7)
O10ⁱ—Tb1—O7—C24	145.6 (4)	O5A—N4A—C19—C18	−31.7 (11)
O3—Tb1—O7—C24	−49.8 (4)	O6A—N4A—C19—N4	16.0 (7)
O1W—Tb1—O7—C24	57.8 (5)	O5A—N4A—C19—N4	−165.6 (13)
O8ⁱ—Tb1—O7—C24	−137.4 (5)	C23—C18—C19—C20	1.1 (6)
O4ⁱ—Tb1—O7—C24	−102.2 (4)	C15—C18—C19—C20	170.6 (4)
O9—Tb1—O7—C24	61.9 (4)	C15A—C18—C19—C20	−155.3 (7)
O2W—Tb1—O7—C24	−0.5 (5)	C23—C18—C19—N4A	151.6 (4)
O7—Tb1—O9—C36	−72.6 (3)	C15—C18—C19—N4A	−39.0 (5)
O10ⁱ—Tb1—O9—C36	−166.1 (3)	C15A—C18—C19—N4A	−4.8 (8)
O3—Tb1—O9—C36	1.5 (3)	C23—C18—C19—N4	−171.2 (4)
O1W—Tb1—O9—C36	104.9 (3)	C15—C18—C19—N4	−1.8 (7)
O8ⁱ—Tb1—O9—C36	−103.5 (3)	C15A—C18—C19—N4	32.4 (9)
O4ⁱ—Tb1—O9—C36	92.4 (3)	O6—N4—C19—C20	−41.4 (7)
O2W—Tb1—O9—C36	51.2 (3)	O5—N4—C19—C20	136.2 (5)
C5—N1—C1—C2	0.6 (10)	O6—N4—C19—N4A	−167.3 (9)
N1—C1—C2—C3	−0.6 (10)	O5—N4—C19—N4A	10.2 (6)
C1—C2—C3—C4	3.1 (9)	O6—N4—C19—C18	131.6 (7)
C1—C2—C3—C6	170.3 (5)	O5—N4—C19—C18	−50.8 (6)
C2—C3—C4—C5	−5.7 (8)	N4A—C19—C20—C21	−141.2 (6)
C6—C3—C4—C5	−172.8 (5)	C18—C19—C20—C21	−1.1 (6)
C1—N1—C5—C4	−3.7 (10)	N4—C19—C20—C21	172.2 (3)
C3—C4—C5—N1	6.3 (9)	C19—C20—C21—C22	−0.5 (5)
C2—C3—C6—C11	−53.8 (7)	C19—C20—C21—C24	−177.0 (3)
C4—C3—C6—C11	112.9 (5)	C20—C21—C22—C23	2.0 (4)
C2—C3—C6—C7	131.9 (5)	C24—C21—C22—C23	178.4 (3)
C4—C3—C6—C7	−61.4 (6)	C19—C18—C23—C22	0.4 (5)
C11—C6—C7—C8	3.8 (6)	C15—C18—C23—C22	−166.6 (5)
C3—C6—C7—C8	178.4 (4)	C15A—C18—C23—C22	166.6 (4)
C11—C6—C7—N2	174.9 (4)	C21—C22—C23—C18	−1.9 (5)
C3—C6—C7—N2	−10.5 (6)	Tb1ⁱⁱ—O8—C24—O7	26.9 (4)
O2—N2—C7—C8	151.5 (4)	Tb1ⁱⁱ—O8—C24—C21	−155.2 (2)
O1—N2—C7—C8	−26.9 (6)	Tb1—O7—C24—O8	−3.7 (6)
O2—N2—C7—C6	−20.1 (6)	Tb1—O7—C24—C21	178.4 (3)
O1—N2—C7—C6	161.4 (4)	C20—C21—C24—O8	167.6 (3)
C6—C7—C8—C9	−4.1 (6)	C22—C21—C24—O8	−8.7 (4)
N2—C7—C8—C9	−175.4 (4)	C20—C21—C24—O7	−14.2 (4)
C7—C8—C9—C10	3.1 (6)	C22—C21—C24—O7	169.4 (2)
C7—C8—C9—C12	−178.2 (4)	C29—N5—C25—C26	−1.2 (11)
C8—C9—C10—C11	−2.3 (7)	N5—C25—C26—C27	−2.7 (11)
C12—C9—C10—C11	179.0 (4)	C25—C26—C27—C28	4.6 (11)
C9—C10—C11—C6	2.4 (8)	C25—C26—C27—C30	170.6 (6)
C7—C6—C11—C10	−3.0 (7)	C26—C27—C28—C29	−2.9 (10)
C3—C6—C11—C10	−177.8 (5)	C30—C27—C28—C29	−169.3 (6)
Tb1—O3—C12—O4	79.5 (5)	C25—N5—C29—C28	2.3 (12)
Tb1—O3—C12—C9	−102.6 (4)	C27—C28—C29—N5	−0.1 (12)
Tb1ⁱⁱ—O4—C12—O3	10.3 (6)	C26—C27—C30—C35	88.7 (8)
Tb1ⁱⁱ—O4—C12—C9	−167.6 (2)	C28—C27—C30—C35	−106.4 (7)
C10—C9—C12—O3	−176.2 (4)	C26—C27—C30—C31	−89.2 (7)
C8—C9—C12—O3	5.1 (5)	C28—C27—C30—C31	75.6 (8)
C10—C9—C12—O4	1.9 (6)	C35—C30—C31—C32	−1.5 (8)
C8—C9—C12—O4	−176.7 (4)	C27—C30—C31—C32	176.5 (5)
C17—N3—C13—C14	0.0	C30—C31—C32—C33	−2.1 (7)
N3—C13—C14—C15	0.0	C31—C32—C33—C34	4.0 (6)
C13—C14—C15—C16	0.0	C31—C32—C33—C36	−176.2 (4)
C13—C14—C15—C18	157.4 (4)	C32—C33—C34—C35	−2.3 (6)
C14—C15—C16—C17	0.0	C36—C33—C34—C35	177.9 (4)
C18—C15—C16—C17	−155.8 (5)	C31—C30—C35—C34	3.3 (7)
C15—C16—C17—N3	0.0	C27—C30—C35—C34	−174.7 (5)
C13—N3—C17—C16	0.0	C31—C30—C35—N6	−178.6 (5)
C17A—N3A—C13A—C14A	0.0	C27—C30—C35—N6	3.5 (8)
N3A—C13A—C14A—C15A	0.0	C33—C34—C35—C30	−1.4 (7)
C13A—C14A—C15A—C16A	0.0	C33—C34—C35—N6	−179.7 (4)
C13A—C14A—C15A—C18	−173.2 (8)	O11—N6—C35—C30	−175.8 (5)
C14A—C15A—C16A—C17A	0.0	O12—N6—C35—C30	1.9 (8)
C18—C15A—C16A—C17A	174.8 (6)	O11—N6—C35—C34	2.6 (7)
C15A—C16A—C17A—N3A	0.0	O12—N6—C35—C34	−179.8 (5)
C13A—N3A—C17A—C16A	0.0	Tb1ⁱⁱ—O10—C36—O9	101.3 (4)
C14—C15—C18—C23	−46.3 (7)	Tb1ⁱⁱ—O10—C36—C33	−81.7 (4)
C16—C15—C18—C23	110.7 (6)	Tb1—O9—C36—O10	−6.3 (5)
C14—C15—C18—C19	146.1 (4)	Tb1—O9—C36—C33	176.7 (2)
C16—C15—C18—C19	−56.8 (6)	C34—C33—C36—O10	168.3 (3)
C14—C15—C18—C15A	−4.0 (6)	C32—C33—C36—O10	−11.5 (5)
C16—C15—C18—C15A	153.1 (8)	C34—C33—C36—O9	−14.5 (5)
C16A—C15A—C18—C23	146.0 (3)	C32—C33—C36—O9	165.7 (4)
C14A—C15A—C18—C23	−40.1 (7)

Symmetry codes: (i) x−y, x, z+1/6; (ii) y, −x+y, z−1/6.

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Format		BIBTeX
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