2,2′,2′′-Nitrilo­tris­(ethyl­ammonium) tris­(pyridine-2,6-di­carboxyl­ato-κ³O,N,O′)­terbate(III) hexahydrate

The asymmetric unit of the title compound, (C₆H₂₁N₄)[Tb(C₇H₃NO₄)₃]·6H₂O, consists of a (C₆H₂₁N₄)³⁺ cation, and a [(C₇H₃NO₄)₃Tb]³⁻ anion, and six molecules of water. In the anion, three pyridine-2,6-di­carboxyl­ate ligands are coordinated to the Tb^III atom via the N atom of the pyridine ring and two O atoms of different carboxyl­ate groups. The coordination polyhedron around Tb may be described as a pseudo-tricapped trigonal prism. The crystal packing is stabilized by electrostatic interactions and intermolecular hydrogen bonds involving the cation, anion and water mol­ecules.

Key indicators

• Single-crystal X-ray study
• T = 296 K
• Mean [sigma](C-C) = 0.007 Å
• H-atom completeness 79%
• R factor = 0.033
• wR factor = 0.089
• Data-to-parameter ratio = 12.2

checkCIF results

No syntax errors found

ADDSYM reports no extra symmetry

General Notes



FORMU_01  There is a discrepancy between the atom counts in the
          _chemical_formula_sum and the formula from the _atom_site* data.
          Atom count from _chemical_formula_sum:C27 H42 N7 O18 Tb1
          Atom count from the _atom_site data:  C27 H33 N7 O18 Tb1

ABSTM_02  When printed, the submitted absorption T values will be replaced
          by the scaled T values. Since the ratio of scaled T's is
          identical to the ratio of reported T values, the scaling does
          not imply a change to the absorption corrections used in the
          study.
          Ratio of Tmax expected/reported      0.375
          Tmax scaled      0.357 Tmin scaled      0.298

CELLZ_01
         From the CIF: _cell_formula_units_Z    2
         From the CIF: _chemical_formula_sum  C27 H42 N7 O18 Tb
         TEST: Compare cell contents of formula and atom_site data

         atom    Z*formula  cif sites diff
         C         54.00     54.00    0.00
         H         84.00     66.00   18.00
         N         14.00     14.00    0.00
         O         36.00     36.00    0.00
         Tb         2.00      2.00    0.00
          Difference between formula and atom_site contents detected.
          WARNING: H atoms missing from atom site list. Is this intentional?

CHEMW_03
         From the CIF: _cell_formula_units_Z                    2
         From the CIF: _chemical_formula_weight           911.60
         TEST: Calculate formula weight from _atom_site_*
         atom     mass    num     sum
         C        12.01   27.00  324.30
         H         1.01   33.00   33.26
         N        14.01    7.00   98.05
         O        16.00   18.00  287.98
         Tb      158.93    1.00  158.93
         Calculated formula weight              902.52
          The ratio of given/expected molecular weight as calculated
          from the _atom_site* data lies outside
          the range 0.99 <> 1.01

---

Computing details

Data collection: XSCANS (Siemens, 1991); cell refinement: XSCANS; data reduction: SHELXTL (Sheldrick, 1997a); program(s) used to solve structure: SHELXS97 (Sheldrick, 1990); program(s) used to refine structure: SHELXL97 (Sheldrick, 1997b); molecular graphics: ORTEP-3 for Windows (Farrugia, 1997); software used to prepare material for publication: SHELXTL.

2,2',2''-Nitrilotris(ethylammonium) tris(pyridine-2,6-dicarboxylato-κ³O,N,O')terbate(III) hexahydrate

Crystal data

[Tb(C7H3NO4)3](C6H21N4)·6H2O	Z = 2
Mr = 911.60	F(000) = 924
Triclinic, P1	Dx = 1.761 Mg m^−3
Hall symbol: -P 1	Mo Kα radiation, λ = 0.71073 Å
a = 10.538 (2) Å	Cell parameters from 38 reflections
b = 12.068 (3) Å	θ = 4.1–15.5°
c = 15.747 (3) Å	µ = 2.15 mm^−1
α = 87.31 (1)°	T = 296 K
β = 71.24 (2)°	Triclinic, colorless
γ = 65.66 (2)°	0.58 × 0.58 × 0.48 mm
V = 1719.1 (6) Å^3

Data collection

Siemens P4 diffractometer	5440 reflections with I > 2σ(I)
Radiation source: normal-focus sealed tube	Rint = 0.070
Graphite monochromator	θmax = 25.0°, θmin = 1.9°
ω scans	h = 0→12
Absorption correction: empirical (using intensity measurements) (SADABS; Sheldrick, 1996)	k = −13→14
Tmin = 0.795, Tmax = 0.951	l = −17→18
6350 measured reflections	3 standard reflections every 97 reflections
6011 independent reflections	intensity decay: 6.6%

Refinement

Refinement on F^2	Primary atom site location: structure-invariant direct methods
Least-squares matrix: full	Secondary atom site location: difference Fourier map
R[F^2 > 2σ(F^2)] = 0.033	Hydrogen site location: inferred from neighbouring sites
wR(F^2) = 0.089	H atoms treated by a mixture of independent and constrained refinement
S = 1.03	w = 1/[σ^2(Fo^2) + (0.0686P)^2] where P = (Fo^2 + 2Fc^2)/3
6011 reflections	(Δ/σ)max = 0.001
493 parameters	Δρmax = 2.42 e Å^−3
5 restraints	Δρmin = −1.24 e Å^−3

Special details

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

Refinement. Refinement of F² against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F², conventional R-factors R are based on F, with F set to zero for negative F². The threshold expression of F² > σ(F²) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F² are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger.

Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Ų)

	x	y	z	Uiso*/Ueq
Tb	0.23697 (2)	0.252096 (16)	0.241070 (12)	0.02105 (9)
O1	0.3033 (3)	0.0406 (3)	0.19483 (19)	0.0286 (6)
O2	0.4715 (3)	−0.1427 (3)	0.1246 (2)	0.0345 (7)
O3	0.3671 (3)	0.3749 (3)	0.1762 (2)	0.0342 (7)
O4	0.5567 (4)	0.4034 (3)	0.0790 (2)	0.0427 (8)
O5	0.4179 (3)	0.1516 (3)	0.3176 (2)	0.0324 (7)
O6	0.4977 (4)	0.1474 (4)	0.4339 (3)	0.0535 (10)
O7	0.0456 (3)	0.4555 (3)	0.2733 (2)	0.0377 (7)
O8	−0.0395 (5)	0.6494 (3)	0.3233 (3)	0.0667 (12)
O9	0.1790 (3)	0.2959 (3)	0.10251 (19)	0.0303 (6)
O10	0.0312 (4)	0.3252 (4)	0.0213 (2)	0.0452 (9)
O11	0.1075 (3)	0.1846 (3)	0.37600 (18)	0.0296 (6)
O12	−0.0787 (4)	0.1421 (3)	0.4581 (2)	0.0445 (8)
N1	0.4800 (4)	0.1448 (3)	0.1205 (2)	0.0231 (7)
N2	0.2207 (4)	0.3801 (3)	0.3685 (2)	0.0259 (7)
N3	0.0038 (4)	0.2437 (3)	0.2414 (2)	0.0261 (7)
C1	0.4284 (5)	−0.0310 (4)	0.1419 (3)	0.0248 (8)
C2	0.5331 (4)	0.0260 (3)	0.0957 (2)	0.0231 (8)
C3	0.6712 (5)	−0.0378 (4)	0.0342 (3)	0.0326 (10)
H3	0.7040	−0.1203	0.0171	0.039*
C4	0.7611 (5)	0.0218 (5)	−0.0019 (3)	0.0363 (10)
H4	0.8561	−0.0206	−0.0420	0.044*
C5	0.7072 (5)	0.1451 (4)	0.0226 (3)	0.0330 (10)
H5	0.7649	0.1875	−0.0011	0.040*
C6	0.5652 (5)	0.2047 (4)	0.0833 (3)	0.0256 (8)
C7	0.4909 (5)	0.3392 (4)	0.1148 (3)	0.0280 (9)
C8	0.4182 (5)	0.1999 (4)	0.3888 (3)	0.0323 (10)
C9	0.3121 (5)	0.3328 (4)	0.4155 (3)	0.0290 (9)
C10	0.3088 (6)	0.4044 (5)	0.4833 (3)	0.0440 (12)
H10	0.3721	0.3709	0.5166	0.053*
C11	0.2116 (7)	0.5246 (5)	0.5006 (4)	0.0512 (14)
H11	0.2080	0.5730	0.5463	0.061*
C12	0.1190 (6)	0.5747 (4)	0.4511 (3)	0.0413 (12)
H12	0.0539	0.6569	0.4614	0.050*
C13	0.1260 (5)	0.4985 (4)	0.3853 (3)	0.0291 (9)
C14	0.0354 (5)	0.5392 (4)	0.3236 (3)	0.0344 (10)
C15	0.0629 (5)	0.3022 (4)	0.0912 (3)	0.0283 (9)
C16	−0.0431 (5)	0.2742 (4)	0.1709 (3)	0.0275 (9)
C17	−0.1751 (5)	0.2778 (4)	0.1699 (3)	0.0359 (10)
H17	−0.2051	0.2994	0.1198	0.043*
C18	−0.2617 (5)	0.2483 (4)	0.2461 (3)	0.0422 (12)
H18	−0.3524	0.2514	0.2483	0.051*
C19	−0.2125 (5)	0.2142 (5)	0.3184 (3)	0.0399 (11)
H19	−0.2686	0.1924	0.3693	0.048*
C20	−0.0796 (4)	0.2126 (4)	0.3149 (3)	0.0262 (9)
C21	−0.0133 (5)	0.1762 (4)	0.3895 (3)	0.0291 (9)
N4	0.4953 (4)	0.3149 (3)	−0.2934 (2)	0.0329 (8)
N5	0.6247 (5)	0.3344 (4)	−0.1493 (3)	0.0484 (11)
H5A	0.5491	0.3981	−0.1133	0.058*
H5B	0.7021	0.3124	−0.1304	0.058*
H5C	0.5996	0.2723	−0.1480	0.058*
N6	0.7286 (5)	0.0306 (4)	−0.4569 (3)	0.0438 (10)
H6A	0.6827	0.0289	−0.4951	0.053*
H6B	0.7729	−0.0447	−0.4428	0.053*
H6C	0.7957	0.0595	−0.4827	0.053*
N7	0.2528 (4)	0.2817 (3)	−0.1512 (2)	0.0352 (8)
H7A	0.2448	0.2268	−0.1825	0.042*
H7B	0.1841	0.3008	−0.0968	0.042*
H7C	0.3419	0.2505	−0.1454	0.042*
C22	0.5344 (6)	0.4124 (4)	−0.2754 (3)	0.0401 (11)
H22A	0.4497	0.4740	−0.2309	0.048*
H22B	0.5573	0.4508	−0.3304	0.048*
C23	0.6634 (6)	0.3683 (5)	−0.2420 (4)	0.0431 (12)
H23A	0.7436	0.2980	−0.2814	0.052*
H23B	0.6974	0.4322	−0.2440	0.052*
C24	0.6036 (6)	0.2387 (4)	−0.3780 (3)	0.0395 (11)
H24A	0.6986	0.2401	−0.3876	0.047*
H24B	0.5713	0.2725	−0.4284	0.047*
C25	0.6198 (6)	0.1104 (5)	−0.3745 (3)	0.0481 (13)
H25A	0.6500	0.0777	−0.3232	0.058*
H25B	0.5247	0.1096	−0.3654	0.058*
C26	0.3433 (5)	0.3634 (5)	−0.2933 (3)	0.0398 (11)
H26A	0.3322	0.3038	−0.3261	0.048*
H26B	0.3229	0.4368	−0.3245	0.048*
C27	0.2322 (5)	0.3933 (4)	−0.1992 (3)	0.0374 (10)
H27A	0.2434	0.4523	−0.1659	0.045*
H27B	0.1331	0.4298	−0.2025	0.045*
O13	0.6959 (4)	−0.0604 (4)	0.2573 (3)	0.0533 (9)
O14	0.1129 (5)	−0.0760 (4)	0.2469 (4)	0.0668 (12)
O15	0.1312 (5)	0.1096 (4)	0.6273 (3)	0.0652 (11)
O16	0.3028 (8)	0.4321 (6)	−0.0215 (4)	0.098 (2)
O17	0.1104 (6)	0.6665 (6)	0.1194 (4)	0.100 (2)
O18	−0.0377 (6)	−0.0752 (6)	0.1299 (4)	0.108 (2)
H13A	0.631 (6)	0.009 (3)	0.274 (5)	0.10 (3)*
H14A	0.064 (5)	−0.055 (3)	0.213 (3)	0.032 (15)*
H16A	0.265 (8)	0.393 (6)	0.014 (4)	0.11 (3)*

Atomic displacement parameters (Ų)

	U^11	U^22	U^33	U^12	U^13	U^23
Tb	0.02433 (12)	0.01976 (12)	0.02033 (12)	−0.01165 (8)	−0.00532 (8)	−0.00153 (7)
O1	0.0302 (16)	0.0241 (15)	0.0302 (15)	−0.0147 (13)	−0.0031 (13)	−0.0040 (12)
O2	0.0402 (17)	0.0236 (16)	0.0420 (18)	−0.0158 (14)	−0.0130 (15)	0.0007 (13)
O3	0.0395 (18)	0.0250 (16)	0.0370 (17)	−0.0207 (14)	−0.0010 (14)	−0.0034 (13)
O4	0.0461 (19)	0.0365 (19)	0.050 (2)	−0.0290 (16)	−0.0062 (16)	0.0050 (15)
O5	0.0351 (17)	0.0264 (16)	0.0342 (16)	−0.0104 (13)	−0.0121 (14)	−0.0042 (13)
O6	0.060 (2)	0.055 (2)	0.048 (2)	−0.0146 (19)	−0.034 (2)	0.0075 (18)
O7	0.0365 (17)	0.0220 (16)	0.053 (2)	−0.0045 (13)	−0.0222 (16)	−0.0076 (14)
O8	0.072 (3)	0.027 (2)	0.108 (4)	−0.0108 (19)	−0.051 (3)	−0.004 (2)
O9	0.0274 (15)	0.0355 (17)	0.0282 (15)	−0.0160 (13)	−0.0057 (13)	0.0016 (12)
O10	0.0391 (19)	0.072 (3)	0.0265 (17)	−0.0233 (18)	−0.0141 (15)	0.0130 (16)
O11	0.0326 (16)	0.0359 (17)	0.0237 (14)	−0.0204 (14)	−0.0058 (13)	0.0028 (12)
O12	0.049 (2)	0.061 (2)	0.0311 (17)	−0.0361 (19)	−0.0067 (15)	0.0108 (16)
N1	0.0293 (18)	0.0242 (18)	0.0210 (16)	−0.0153 (15)	−0.0097 (14)	0.0025 (13)
N2	0.0320 (18)	0.0233 (18)	0.0247 (17)	−0.0158 (15)	−0.0063 (15)	−0.0004 (14)
N3	0.0236 (17)	0.0300 (19)	0.0210 (16)	−0.0114 (15)	−0.0018 (14)	−0.0036 (14)
C1	0.032 (2)	0.026 (2)	0.0226 (19)	−0.0161 (18)	−0.0127 (18)	0.0053 (16)
C2	0.031 (2)	0.021 (2)	0.0213 (19)	−0.0134 (17)	−0.0099 (17)	0.0022 (15)
C3	0.037 (2)	0.027 (2)	0.028 (2)	−0.0108 (19)	−0.0080 (19)	−0.0007 (17)
C4	0.032 (2)	0.041 (3)	0.029 (2)	−0.012 (2)	−0.0039 (19)	−0.0010 (19)
C5	0.033 (2)	0.042 (3)	0.029 (2)	−0.022 (2)	−0.0076 (19)	0.0039 (19)
C6	0.031 (2)	0.031 (2)	0.0213 (19)	−0.0183 (18)	−0.0094 (17)	0.0055 (16)
C7	0.035 (2)	0.030 (2)	0.029 (2)	−0.0219 (19)	−0.0111 (19)	0.0057 (17)
C8	0.033 (2)	0.038 (3)	0.032 (2)	−0.020 (2)	−0.012 (2)	0.0060 (19)
C9	0.037 (2)	0.036 (2)	0.0211 (19)	−0.023 (2)	−0.0084 (18)	0.0012 (17)
C10	0.056 (3)	0.052 (3)	0.031 (2)	−0.024 (3)	−0.020 (2)	−0.002 (2)
C11	0.073 (4)	0.048 (3)	0.040 (3)	−0.031 (3)	−0.020 (3)	−0.011 (2)
C12	0.051 (3)	0.033 (3)	0.037 (3)	−0.021 (2)	−0.005 (2)	−0.010 (2)
C13	0.031 (2)	0.026 (2)	0.028 (2)	−0.0164 (19)	−0.0009 (18)	−0.0029 (17)
C14	0.028 (2)	0.024 (2)	0.046 (3)	−0.0099 (19)	−0.005 (2)	−0.0025 (19)
C15	0.029 (2)	0.026 (2)	0.028 (2)	−0.0103 (18)	−0.0072 (18)	0.0005 (17)
C16	0.029 (2)	0.025 (2)	0.025 (2)	−0.0107 (18)	−0.0042 (17)	−0.0037 (16)
C17	0.033 (2)	0.046 (3)	0.035 (2)	−0.020 (2)	−0.015 (2)	0.002 (2)
C18	0.032 (3)	0.056 (3)	0.049 (3)	−0.027 (2)	−0.016 (2)	0.007 (3)
C19	0.036 (3)	0.050 (3)	0.039 (3)	−0.026 (2)	−0.007 (2)	0.005 (2)
C20	0.029 (2)	0.022 (2)	0.024 (2)	−0.0129 (17)	0.0001 (17)	−0.0021 (16)
C21	0.031 (2)	0.029 (2)	0.024 (2)	−0.0142 (19)	−0.0015 (18)	−0.0019 (17)
N4	0.039 (2)	0.031 (2)	0.0270 (18)	−0.0159 (17)	−0.0053 (16)	−0.0021 (15)
N5	0.053 (3)	0.042 (3)	0.065 (3)	−0.030 (2)	−0.027 (2)	0.008 (2)
N6	0.058 (3)	0.038 (2)	0.035 (2)	−0.027 (2)	−0.0043 (19)	−0.0044 (17)
N7	0.036 (2)	0.040 (2)	0.0313 (19)	−0.0182 (18)	−0.0100 (17)	0.0020 (16)
C22	0.052 (3)	0.025 (2)	0.039 (3)	−0.019 (2)	−0.006 (2)	0.0005 (19)
C23	0.048 (3)	0.031 (3)	0.055 (3)	−0.026 (2)	−0.010 (2)	0.003 (2)
C24	0.050 (3)	0.036 (3)	0.026 (2)	−0.021 (2)	−0.001 (2)	−0.0004 (19)
C25	0.060 (3)	0.036 (3)	0.036 (3)	−0.022 (3)	0.002 (2)	0.001 (2)
C26	0.049 (3)	0.045 (3)	0.029 (2)	−0.021 (2)	−0.017 (2)	0.008 (2)
C27	0.035 (2)	0.039 (3)	0.035 (2)	−0.011 (2)	−0.013 (2)	0.003 (2)
O13	0.050 (2)	0.048 (2)	0.055 (2)	−0.015 (2)	−0.0135 (19)	−0.0100 (19)
O14	0.054 (3)	0.051 (3)	0.097 (4)	−0.030 (2)	−0.016 (3)	0.014 (2)
O15	0.077 (3)	0.051 (2)	0.058 (2)	−0.024 (2)	−0.011 (2)	−0.0125 (19)
O16	0.176 (6)	0.129 (5)	0.079 (3)	−0.129 (5)	−0.078 (4)	0.060 (3)
O17	0.078 (4)	0.144 (6)	0.104 (4)	−0.064 (4)	−0.045 (3)	0.039 (4)
O18	0.077 (4)	0.172 (6)	0.089 (4)	−0.070 (4)	−0.021 (3)	0.018 (4)

Geometric parameters (Å, º)

Tb—O7	2.393 (3)	C13—C14	1.504 (7)
Tb—O3	2.398 (3)	C15—C16	1.519 (6)
Tb—O9	2.428 (3)	C16—C17	1.379 (6)
Tb—O1	2.431 (3)	C17—C18	1.387 (6)
Tb—O11	2.435 (3)	C17—H17	0.93
Tb—O5	2.448 (3)	C18—C19	1.377 (7)
Tb—N1	2.492 (3)	C18—H18	0.93
Tb—N3	2.499 (3)	C19—C20	1.376 (6)
Tb—N2	2.508 (3)	C19—H19	0.93
O1—C1	1.265 (5)	C20—C21	1.513 (6)
O2—C1	1.243 (5)	N4—C26	1.461 (6)
O3—C7	1.260 (5)	N4—C22	1.463 (6)
O4—C7	1.244 (5)	N4—C24	1.481 (6)
O5—C8	1.290 (5)	N5—C23	1.472 (6)
O6—C8	1.229 (6)	N5—H5A	0.89
O7—C14	1.261 (5)	N5—H5B	0.89
O8—C14	1.236 (6)	N5—H5C	0.89
O9—C15	1.264 (5)	N6—C25	1.476 (6)
O10—C15	1.239 (5)	N6—H6A	0.89
O11—C21	1.268 (5)	N6—H6B	0.89
O12—C21	1.235 (5)	N6—H6C	0.89
N1—C2	1.330 (5)	N7—C27	1.484 (6)
N1—C6	1.353 (5)	N7—H7A	0.89
N2—C9	1.330 (6)	N7—H7B	0.89
N2—C13	1.341 (6)	N7—H7C	0.89
N3—C16	1.333 (6)	C22—C23	1.498 (7)
N3—C20	1.351 (5)	C22—H22A	0.97
C1—C2	1.511 (5)	C22—H22B	0.97
C2—C3	1.374 (6)	C23—H23A	0.97
C3—C4	1.383 (6)	C23—H23B	0.97
C3—H3	0.93	C24—C25	1.487 (7)
C4—C5	1.379 (7)	C24—H24A	0.97
C4—H4	0.93	C24—H24B	0.97
C5—C6	1.388 (6)	C25—H25A	0.97
C5—H5	0.93	C25—H25B	0.97
C6—C7	1.507 (6)	C26—C27	1.511 (6)
C8—C9	1.511 (7)	C26—H26A	0.97
C9—C10	1.388 (6)	C26—H26B	0.97
C10—C11	1.364 (8)	C27—H27A	0.97
C10—H10	0.93	C27—H27B	0.97
C11—C12	1.373 (8)	O13—H13A	0.82 (4)
C11—H11	0.93	O14—H14A	0.82 (5)
C12—C13	1.381 (6)	O16—H16A	0.83 (7)
C12—H12	0.93
O7—Tb—O3	76.76 (11)	C13—C12—H12	121.2
O7—Tb—O9	75.65 (11)	N2—C13—C12	122.0 (4)
O3—Tb—O9	78.48 (10)	N2—C13—C14	113.5 (4)
O7—Tb—O1	145.15 (10)	C12—C13—C14	124.4 (4)
O3—Tb—O1	127.82 (10)	O8—C14—O7	124.6 (5)
O9—Tb—O1	85.11 (10)	O8—C14—C13	119.5 (4)
O7—Tb—O11	92.44 (11)	O7—C14—C13	115.9 (4)
O3—Tb—O11	148.33 (10)	O10—C15—O9	126.1 (4)
O9—Tb—O11	128.12 (10)	O10—C15—C16	118.2 (4)
O1—Tb—O11	76.83 (10)	O9—C15—C16	115.7 (4)
O7—Tb—O5	128.33 (10)	N3—C16—C17	122.9 (4)
O3—Tb—O5	88.92 (11)	N3—C16—C15	114.1 (4)
O9—Tb—O5	149.74 (10)	C17—C16—C15	123.0 (4)
O1—Tb—O5	81.12 (10)	C16—C17—C18	117.8 (4)
O11—Tb—O5	74.46 (10)	C16—C17—H17	121.1
O7—Tb—N1	135.31 (11)	C18—C17—H17	121.1
O3—Tb—N1	64.06 (10)	C19—C18—C17	119.6 (4)
O9—Tb—N1	76.23 (10)	C19—C18—H18	120.2
O1—Tb—N1	63.99 (10)	C17—C18—H18	120.2
O11—Tb—N1	132.23 (10)	C20—C19—C18	119.5 (4)
O5—Tb—N1	73.52 (10)	C20—C19—H19	120.3
O7—Tb—N3	71.48 (11)	C18—C19—H19	120.3
O3—Tb—N3	135.41 (11)	N3—C20—C19	121.1 (4)
O9—Tb—N3	64.02 (10)	N3—C20—C21	114.4 (4)
O1—Tb—N3	74.02 (11)	C19—C20—C21	124.5 (4)
O11—Tb—N3	64.31 (10)	O12—C21—O11	124.8 (4)
O5—Tb—N3	135.46 (11)	O12—C21—C20	119.3 (4)
N1—Tb—N3	123.68 (10)	O11—C21—C20	115.9 (4)
O7—Tb—N2	63.94 (11)	C26—N4—C22	111.6 (4)
O3—Tb—N2	72.80 (10)	C26—N4—C24	112.7 (4)
O9—Tb—N2	134.45 (11)	C22—N4—C24	110.3 (4)
O1—Tb—N2	140.41 (11)	C23—N5—H5A	109.5
O11—Tb—N2	75.70 (10)	C23—N5—H5B	109.5
O5—Tb—N2	64.39 (10)	H5A—N5—H5B	109.5
N1—Tb—N2	118.99 (11)	C23—N5—H5C	109.5
N3—Tb—N2	117.31 (11)	H5A—N5—H5C	109.5
C1—O1—Tb	124.2 (2)	H5B—N5—H5C	109.5
C7—O3—Tb	126.3 (3)	C25—N6—H6A	109.5
C8—O5—Tb	124.0 (3)	C25—N6—H6B	109.5
C14—O7—Tb	125.1 (3)	H6A—N6—H6B	109.5
C15—O9—Tb	125.2 (3)	C25—N6—H6C	109.5
C21—O11—Tb	125.1 (3)	H6A—N6—H6C	109.5
C2—N1—C6	118.5 (3)	H6B—N6—H6C	109.5
C2—N1—Tb	121.0 (2)	C27—N7—H7A	109.5
C6—N1—Tb	120.3 (3)	C27—N7—H7B	109.5
C9—N2—C13	120.0 (4)	H7A—N7—H7B	109.5
C9—N2—Tb	120.2 (3)	C27—N7—H7C	109.5
C13—N2—Tb	119.8 (3)	H7A—N7—H7C	109.5
C16—N3—C20	119.0 (4)	H7B—N7—H7C	109.5
C16—N3—Tb	120.7 (3)	N4—C22—C23	113.3 (4)
C20—N3—Tb	120.2 (3)	N4—C22—H22A	108.9
O2—C1—O1	125.9 (4)	C23—C22—H22A	108.9
O2—C1—C2	117.9 (4)	N4—C22—H22B	108.9
O1—C1—C2	116.3 (3)	C23—C22—H22B	108.9
N1—C2—C3	122.5 (4)	H22A—C22—H22B	107.7
N1—C2—C1	113.8 (3)	N5—C23—C22	111.7 (4)
C3—C2—C1	123.8 (4)	N5—C23—H23A	109.3
C2—C3—C4	119.4 (4)	C22—C23—H23A	109.3
C2—C3—H3	120.3	N5—C23—H23B	109.3
C4—C3—H3	120.3	C22—C23—H23B	109.3
C5—C4—C3	118.8 (4)	H23A—C23—H23B	107.9
C5—C4—H4	120.6	N4—C24—C25	111.1 (4)
C3—C4—H4	120.6	N4—C24—H24A	109.4
C4—C5—C6	118.8 (4)	C25—C24—H24A	109.4
C4—C5—H5	120.6	N4—C24—H24B	109.4
C6—C5—H5	120.6	C25—C24—H24B	109.4
N1—C6—C5	121.9 (4)	H24A—C24—H24B	108.0
N1—C6—C7	113.4 (3)	N6—C25—C24	113.0 (4)
C5—C6—C7	124.7 (4)	N6—C25—H25A	109.0
O4—C7—O3	126.5 (4)	C24—C25—H25A	109.0
O4—C7—C6	117.9 (4)	N6—C25—H25B	109.0
O3—C7—C6	115.6 (3)	C24—C25—H25B	109.0
O6—C8—O5	125.5 (5)	H25A—C25—H25B	107.8
O6—C8—C9	119.3 (4)	N4—C26—C27	112.5 (4)
O5—C8—C9	115.2 (4)	N4—C26—H26A	109.1
N2—C9—C10	120.6 (4)	C27—C26—H26A	109.1
N2—C9—C8	115.7 (4)	N4—C26—H26B	109.1
C10—C9—C8	123.6 (4)	C27—C26—H26B	109.1
C11—C10—C9	119.2 (5)	H26A—C26—H26B	107.8
C11—C10—H10	120.4	N7—C27—C26	110.9 (4)
C9—C10—H10	120.4	N7—C27—H27A	109.5
C10—C11—C12	120.6 (4)	C26—C27—H27A	109.5
C10—C11—H11	119.7	N7—C27—H27B	109.5
C12—C11—H11	119.7	C26—C27—H27B	109.5
C11—C12—C13	117.6 (5)	H27A—C27—H27B	108.0
C11—C12—H12	121.2
O7—Tb—O1—C1	141.1 (3)	O11—Tb—N3—C20	2.9 (3)
O3—Tb—O1—C1	13.6 (4)	O5—Tb—N3—C20	27.0 (4)
O9—Tb—O1—C1	85.0 (3)	N1—Tb—N3—C20	128.1 (3)
O11—Tb—O1—C1	−144.0 (3)	N2—Tb—N3—C20	−53.2 (3)
O5—Tb—O1—C1	−68.0 (3)	Tb—O1—C1—O2	171.6 (3)
N1—Tb—O1—C1	7.9 (3)	Tb—O1—C1—C2	−8.8 (5)
N3—Tb—O1—C1	149.3 (3)	C6—N1—C2—C3	0.4 (6)
N2—Tb—O1—C1	−96.9 (3)	Tb—N1—C2—C3	−175.1 (3)
O7—Tb—O3—C7	−158.0 (4)	C6—N1—C2—C1	179.8 (3)
O9—Tb—O3—C7	−80.2 (4)	Tb—N1—C2—C1	4.3 (4)
O1—Tb—O3—C7	−5.8 (4)	O2—C1—C2—N1	−177.7 (3)
O11—Tb—O3—C7	129.4 (3)	O1—C1—C2—N1	2.6 (5)
O5—Tb—O3—C7	72.1 (4)	O2—C1—C2—C3	1.7 (6)
N1—Tb—O3—C7	0.0 (3)	O1—C1—C2—C3	−178.0 (4)
N3—Tb—O3—C7	−112.7 (3)	N1—C2—C3—C4	1.8 (6)
N2—Tb—O3—C7	135.6 (4)	C1—C2—C3—C4	−177.6 (4)
O7—Tb—O5—C8	5.1 (4)	C2—C3—C4—C5	−2.2 (7)
O3—Tb—O5—C8	77.3 (3)	C3—C4—C5—C6	0.6 (7)
O9—Tb—O5—C8	141.9 (3)	C2—N1—C6—C5	−2.1 (6)
O1—Tb—O5—C8	−154.2 (3)	Tb—N1—C6—C5	173.4 (3)
O11—Tb—O5—C8	−75.5 (3)	C2—N1—C6—C7	178.3 (3)
N1—Tb—O5—C8	140.5 (3)	Tb—N1—C6—C7	−6.2 (4)
N3—Tb—O5—C8	−97.9 (3)	C4—C5—C6—N1	1.6 (6)
N2—Tb—O5—C8	5.9 (3)	C4—C5—C6—C7	−178.8 (4)
O3—Tb—O7—C14	−64.5 (4)	Tb—O3—C7—O4	177.7 (3)
O9—Tb—O7—C14	−145.8 (4)	Tb—O3—C7—C6	−3.0 (5)
O1—Tb—O7—C14	155.7 (3)	N1—C6—C7—O4	−174.7 (4)
O11—Tb—O7—C14	85.4 (4)	C5—C6—C7—O4	5.7 (6)
O5—Tb—O7—C14	13.4 (4)	N1—C6—C7—O3	5.9 (5)
N1—Tb—O7—C14	−93.2 (4)	C5—C6—C7—O3	−173.7 (4)
N3—Tb—O7—C14	147.3 (4)	Tb—O5—C8—O6	172.1 (4)
N2—Tb—O7—C14	12.6 (3)	Tb—O5—C8—C9	−8.9 (5)
O7—Tb—O9—C15	−72.3 (3)	C13—N2—C9—C10	1.1 (6)
O3—Tb—O9—C15	−151.4 (3)	Tb—N2—C9—C10	176.9 (3)
O1—Tb—O9—C15	78.4 (3)	C13—N2—C9—C8	−177.7 (4)
O11—Tb—O9—C15	9.3 (4)	Tb—N2—C9—C8	−2.0 (5)
O5—Tb—O9—C15	141.4 (3)	O6—C8—C9—N2	−174.2 (4)
N1—Tb—O9—C15	142.7 (3)	O5—C8—C9—N2	6.8 (5)
N3—Tb—O9—C15	3.8 (3)	O6—C8—C9—C10	7.0 (7)
N2—Tb—O9—C15	−99.9 (3)	O5—C8—C9—C10	−172.0 (4)
O7—Tb—O11—C21	67.0 (3)	N2—C9—C10—C11	−0.7 (7)
O3—Tb—O11—C21	135.4 (3)	C8—C9—C10—C11	178.1 (5)
O9—Tb—O11—C21	−6.7 (4)	C9—C10—C11—C12	−0.7 (8)
O1—Tb—O11—C21	−79.5 (3)	C10—C11—C12—C13	1.5 (8)
O5—Tb—O11—C21	−163.8 (3)	C9—N2—C13—C12	−0.3 (6)
N1—Tb—O11—C21	−114.4 (3)	Tb—N2—C13—C12	−176.0 (3)
N3—Tb—O11—C21	−1.1 (3)	C9—N2—C13—C14	177.3 (4)
N2—Tb—O11—C21	129.3 (3)	Tb—N2—C13—C14	1.5 (5)
O7—Tb—N1—C2	−149.6 (3)	C11—C12—C13—N2	−1.0 (7)
O3—Tb—N1—C2	179.0 (3)	C11—C12—C13—C14	−178.3 (4)
O9—Tb—N1—C2	−97.3 (3)	Tb—O7—C14—O8	161.5 (4)
O1—Tb—N1—C2	−6.0 (3)	Tb—O7—C14—C13	−16.6 (6)
O11—Tb—N1—C2	32.2 (3)	N2—C13—C14—O8	−169.3 (4)
O5—Tb—N1—C2	82.0 (3)	C12—C13—C14—O8	8.3 (7)
N3—Tb—N1—C2	−52.1 (3)	N2—C13—C14—O7	8.9 (6)
N2—Tb—N1—C2	129.2 (3)	C12—C13—C14—O7	−173.6 (4)
O7—Tb—N1—C6	35.0 (3)	Tb—O9—C15—O10	179.5 (4)
O3—Tb—N1—C6	3.6 (3)	Tb—O9—C15—C16	−2.7 (5)
O9—Tb—N1—C6	87.3 (3)	C20—N3—C16—C17	1.3 (6)
O1—Tb—N1—C6	178.6 (3)	Tb—N3—C16—C17	−176.1 (3)
O11—Tb—N1—C6	−143.2 (3)	C20—N3—C16—C15	−177.6 (3)
O5—Tb—N1—C6	−93.4 (3)	Tb—N3—C16—C15	4.9 (5)
N3—Tb—N1—C6	132.5 (3)	O10—C15—C16—N3	176.4 (4)
N2—Tb—N1—C6	−46.2 (3)	O9—C15—C16—N3	−1.6 (5)
O7—Tb—N2—C9	177.9 (3)	O10—C15—C16—C17	−2.5 (6)
O3—Tb—N2—C9	−98.8 (3)	O9—C15—C16—C17	179.5 (4)
O9—Tb—N2—C9	−152.1 (3)	N3—C16—C17—C18	0.0 (7)
O1—Tb—N2—C9	30.5 (4)	C15—C16—C17—C18	178.8 (4)
O11—Tb—N2—C9	77.9 (3)	C16—C17—C18—C19	−1.4 (7)
O5—Tb—N2—C9	−1.5 (3)	C17—C18—C19—C20	1.4 (7)
N1—Tb—N2—C9	−52.8 (3)	C16—N3—C20—C19	−1.3 (6)
N3—Tb—N2—C9	128.5 (3)	Tb—N3—C20—C19	176.2 (3)
O7—Tb—N2—C13	−6.4 (3)	C16—N3—C20—C21	178.3 (4)
O3—Tb—N2—C13	77.0 (3)	Tb—N3—C20—C21	−4.3 (4)
O9—Tb—N2—C13	23.6 (4)	C18—C19—C20—N3	−0.1 (7)
O1—Tb—N2—C13	−153.7 (3)	C18—C19—C20—C21	−179.6 (4)
O11—Tb—N2—C13	−106.4 (3)	Tb—O11—C21—O12	−179.8 (3)
O5—Tb—N2—C13	174.3 (3)	Tb—O11—C21—C20	−0.6 (5)
N1—Tb—N2—C13	123.0 (3)	N3—C20—C21—O12	−177.5 (4)
N3—Tb—N2—C13	−55.8 (3)	C19—C20—C21—O12	2.0 (7)
O7—Tb—N3—C16	78.2 (3)	N3—C20—C21—O11	3.2 (5)
O3—Tb—N3—C16	31.4 (4)	C19—C20—C21—O11	−177.4 (4)
O9—Tb—N3—C16	−4.5 (3)	C26—N4—C22—C23	159.1 (4)
O1—Tb—N3—C16	−96.8 (3)	C24—N4—C22—C23	−74.8 (5)
O11—Tb—N3—C16	−179.6 (3)	N4—C22—C23—N5	−71.4 (5)
O5—Tb—N3—C16	−155.5 (3)	C26—N4—C24—C25	−85.1 (5)
N1—Tb—N3—C16	−54.5 (3)	C22—N4—C24—C25	149.4 (4)
N2—Tb—N3—C16	124.2 (3)	N4—C24—C25—N6	−179.1 (4)
O7—Tb—N3—C20	−99.3 (3)	C22—N4—C26—C27	−79.6 (5)
O3—Tb—N3—C20	−146.1 (3)	C24—N4—C26—C27	155.7 (4)
O9—Tb—N3—C20	178.1 (3)	N4—C26—C27—N7	−62.7 (5)
O1—Tb—N3—C20	85.7 (3)

Hydrogen-bond geometry (Å, º)

D—H···A	D—H	H···A	D···A	D—H···A
O13—H13A···O5	0.82 (4)	2.10 (3)	2.880 (5)	158 (8)
O14—H14A···O18	0.82 (5)	2.02 (5)	2.789 (8)	157 (3)
O16—H16A···O9	0.83 (7)	2.01 (7)	2.837 (5)	178 (8)
N7—H7B···O10	0.89	1.97	2.855 (5)	174
N5—H5A···O4^i	0.89	2.19	2.979 (6)	147
N5—H5B···O17^i	0.89	2.15	2.971 (7)	152
N5—H5C···O2^ii	0.89	1.97	2.851 (5)	171
N6—H6C···O12^iii	0.89	1.96	2.840 (5)	172
N6—H6B···O11^ii	0.89	2.12	2.960 (5)	158
N6—H6A···O15^ii	0.89	2.44	2.838 (5)	107
N7—H7C···O2^ii	0.89	1.98	2.851 (5)	165
N7—H7A···O13^ii	0.89	2.13	2.977 (6)	160

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