The crystal structure of the title compound, {[Gd2(C8H4O4)3(C5H11NO)2]·H2O}n, consists of chains of Gd atoms interconnected by a benzene-1,4-dicarboxylate (BDC) linker. The chains are also intraconnected by carboxylate groups from the BDC linker, thus generating a three-dimensional framework with large cavities. The coordination of the eight carboxylate O atoms around the GdIII ion is distorted dodecahedral, due to the steric constraints of the carboxylate groups. The large anisotropic displacement parameters of the atoms of the coordinated diethylformamide (DEF) and the disorder in their positions indicate loose bonding to the framework, and hence solvent exchange may be possible. Additionally, one water molecule is located in the cavity.
Supporting information
CCDC reference: 277710
Key indicators
- Single-crystal X-ray study
- T = 100 K
- Mean (C-C) = 0.002 Å
- H-atom completeness 95%
- Disorder in main residue
- R factor = 0.022
- wR factor = 0.054
- Data-to-parameter ratio = 41.0
checkCIF/PLATON results
No syntax errors found
Alert level A
PLAT220_ALERT_2_A Large Non-Solvent C Ueq(max)/Ueq(min) ... 10.00 Ratio
| Author Response: The DEF molecule is only loosely attached to the framework and
is placed in channels, which makes it prone to significant thermal motion.
|
PLAT222_ALERT_3_A Large Non-Solvent H Ueq(max)/Ueq(min) ... 9.29 Ratio
| Author Response: The DEF molecule is only loosely attached to the framework and
is placed in channels, which makes it prone to significant thermal motion.
|
Alert level C
CHEMW01_ALERT_1_C The difference between the given and expected weight for
compound is greater 1 mass unit. Check that all hydrogen
atoms have been taken into account.
PLAT041_ALERT_1_C Calc. and Rep. SumFormula Strings Differ .... ?
PLAT042_ALERT_1_C Calc. and Rep. MoietyFormula Strings Differ .... ?
PLAT045_ALERT_1_C Calculated and Reported Z Differ by ............ 0.50 Ratio
PLAT094_ALERT_2_C Ratio of Maximum / Minimum Residual Density .... 2.69
PLAT213_ALERT_2_C Atom C20 has ADP max/min Ratio ............. 3.90 prolat
PLAT220_ALERT_2_C Large Non-Solvent O Ueq(max)/Ueq(min) ... 2.74 Ratio
| Author Response: The DEF molecule is only loosely attached to the framework and
is placed in channels, which makes it prone to significant thermal motion.
|
PLAT241_ALERT_2_C Check High Ueq as Compared to Neighbors for C15
PLAT301_ALERT_3_C Main Residue Disorder ......................... 13.00 Perc.
PLAT302_ALERT_4_C Anion/Solvent Disorder ......................... 50.00 Perc.
PLAT764_ALERT_4_C Overcomplete CIF Bond List Detected (Rep/Expd) . 1.38 Ratio
Alert level G
FORMU01_ALERT_2_G 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:C34 H36 Gd2 N2 O15
Atom count from the _atom_site data: C34 H34 Gd2 N2 O15
CELLZ01_ALERT_1_G Difference between formula and atom_site contents detected.
CELLZ01_ALERT_1_G WARNING: H atoms missing from atom site list. Is this intentional?
From the CIF: _cell_formula_units_Z 4
From the CIF: _chemical_formula_sum C34 H36 Gd2 N2 O15
TEST: Compare cell contents of formula and atom_site data
atom Z*formula cif sites diff
C 136.00 136.00 0.00
H 144.00 136.00 8.00
Gd 8.00 8.00 0.00
N 8.00 8.00 0.00
O 60.00 60.00 0.00
REFLT03_ALERT_1_G ALERT: Expected hkl max differ from CIF values
From the CIF: _diffrn_reflns_theta_max 43.01
From the CIF: _reflns_number_total 11366
From the CIF: _diffrn_reflns_limit_ max hkl 29. 20. 32.
From the CIF: _diffrn_reflns_limit_ min hkl -33. -20. -33.
TEST1: Expected hkl limits for theta max
Calculated maximum hkl 34. 21. 35.
Calculated minimum hkl -34. -21. -35.
2 ALERT level A = In general: serious problem
0 ALERT level B = Potentially serious problem
11 ALERT level C = Check and explain
4 ALERT level G = General alerts; check
7 ALERT type 1 CIF construction/syntax error, inconsistent or missing data
6 ALERT type 2 Indicator that the structure model may be wrong or deficient
2 ALERT type 3 Indicator that the structure quality may be low
2 ALERT type 4 Improvement, methodology, query or suggestion
Data collection: Please provide missing details; cell refinement: SAINT-Plus; data reduction: SAINT-Plus (Bruker, 2004); program(s) used to solve structure: SHELXS97 (Sheldrick, 1997); program(s) used to refine structure: SHELXL97 (Sheldrick, 1997); molecular graphics: SHELXTL (Bruker, 2004); software used to prepare material for publication: enCIFer (version 1.1; Allen et al., 2004).
poly[[tris(µ
4-benzene-1,4-dicarboxylato)bis(µ
2–
N,
N-diethylformamide)digadolinium(III)] monohydrate]
top
Crystal data top
[Gd2(C8H4O4)3(C5H11NO)2]·H2O | F(000) = 2000 |
Mr = 1025.13 | Dx = 1.864 Mg m−3 |
Monoclinic, C2/c | Mo Kα radiation, λ = 0.71073 Å |
Hall symbol: -C 2yc | Cell parameters from 7811 reflections |
a = 18.0582 (5) Å | θ = 2.8–42.4° |
b = 11.4381 (3) Å | µ = 3.67 mm−1 |
c = 18.6791 (4) Å | T = 100 K |
β = 108.796 (1)° | Block, white |
V = 3652.44 (16) Å3 | 0.20 × 0.05 × 0.05 mm |
Z = 4 | |
Data collection top
Bruker SMART APEXII CCD-based diffractometer | 11366 independent reflections |
Radiation source: fine-focus sealed tube, Siemens K FFMO 2K 90 | 9378 reflections with I > 2σ(I) |
Graphite monochromator | Rint = 0.039 |
Detector resolution: 83.33 pixels mm-1 | θmax = 43.0°, θmin = 2.1° |
φ and ω scans | h = −33→29 |
Absorption correction: multi-scan (Blessing, 1995) | k = −20→20 |
Tmin = 0.741, Tmax = 0.830 | l = −33→32 |
61459 measured reflections | |
Refinement top
Refinement on F2 | Primary atom site location: structure-invariant direct methods |
Least-squares matrix: full | Secondary atom site location: difference Fourier map |
R[F2 > 2σ(F2)] = 0.022 | Hydrogen site location: inferred from neighbouring sites |
wR(F2) = 0.054 | H-atom parameters constrained |
S = 0.95 | w = 1/[σ2(Fo2) + (0.0284P)2] where P = (Fo2 + 2Fc2)/3 |
11366 reflections | (Δ/σ)max = 0.001 |
277 parameters | Δρmax = 2.59 e Å−3 |
0 restraints | Δρmin = −0.96 e Å−3 |
Special details top
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 (Å2) top | x | y | z | Uiso*/Ueq | Occ. (<1) |
Gd1 | 0.001829 (3) | 0.559920 (4) | 0.102180 (3) | 0.00726 (2) | |
O1 | 0.08900 (6) | 0.56023 (9) | 0.22407 (6) | 0.01713 (18) | |
O31 | −0.07784 (6) | 0.43229 (9) | 0.00789 (7) | 0.01854 (19) | |
C1 | 0.11733 (7) | 0.56150 (10) | 0.29411 (7) | 0.01022 (17) | |
O11 | −0.08653 (5) | 0.51300 (8) | 0.16110 (5) | 0.01153 (14) | |
O14 | 0.10513 (6) | 0.68267 (9) | 0.09204 (6) | 0.01663 (17) | |
O21 | −0.02661 (7) | 0.74494 (9) | 0.15146 (6) | 0.01815 (18) | |
O41 | −0.07090 (6) | 0.67660 (9) | 0.00048 (5) | 0.01924 (19) | |
C11 | 0.18656 (7) | 0.69969 (11) | 0.01577 (7) | 0.0142 (2) | |
C2 | 0.19404 (7) | 0.62278 (11) | 0.32888 (7) | 0.01196 (18) | |
C3 | 0.22907 (8) | 0.68160 (13) | 0.28281 (7) | 0.0176 (2) | |
H3 | 0.2064 | 0.6782 | 0.2294 | 0.021* | |
C12 | 0.19865 (8) | 0.67711 (12) | −0.05289 (8) | 0.0165 (2) | |
H12 | 0.1636 | 0.6276 | −0.0891 | 0.020* | |
C7 | 0.22854 (8) | 0.62536 (12) | 0.40715 (7) | 0.0144 (2) | |
H7 | 0.2053 | 0.5841 | 0.4386 | 0.017* | |
C10 | 0.11899 (7) | 0.64679 (11) | 0.03387 (7) | 0.0142 (2) | |
O13 | 0.07687 (8) | 0.39149 (12) | 0.11365 (6) | 0.0318 (3) | |
C6 | 0.29705 (8) | 0.68840 (12) | 0.43921 (7) | 0.0169 (2) | |
H6 | 0.3209 | 0.6894 | 0.4926 | 0.020* | |
C13 | 0.23812 (8) | 0.77300 (13) | 0.06843 (8) | 0.0182 (2) | |
H13 | 0.2299 | 0.7889 | 0.1152 | 0.022* | |
C5 | 0.33072 (9) | 0.75001 (13) | 0.39337 (7) | 0.0188 (2) | |
C41 | −0.09999 (9) | 0.67298 (13) | −0.07060 (8) | 0.0216 (3) | |
C4 | 0.29713 (9) | 0.74512 (14) | 0.31507 (8) | 0.0223 (3) | |
H4 | 0.3209 | 0.7854 | 0.2837 | 0.027* | |
N16 | −0.05939 (13) | 0.93673 (12) | 0.13197 (13) | 0.0370 (4) | |
C15 | −0.02170 (15) | 0.84050 (15) | 0.12457 (15) | 0.0436 (6) | |
H15 | 0.0126 | 0.8466 | 0.0954 | 0.052* | |
C19 | −0.1864 (2) | 0.9755 (4) | 0.1531 (3) | 0.0573 (14) | 0.622 (6) |
H19A | −0.2109 | 0.9768 | 0.1929 | 0.086* | 0.622 (6) |
H19B | −0.2134 | 0.9186 | 0.1143 | 0.086* | 0.622 (6) |
H19C | −0.1901 | 1.0533 | 0.1303 | 0.086* | 0.622 (6) |
C20 | −0.0182 (3) | 1.1406 (4) | 0.1242 (5) | 0.105 (3) | 0.622 (6) |
H20A | −0.0230 | 1.2082 | 0.0907 | 0.158* | 0.622 (6) |
H20B | 0.0368 | 1.1165 | 0.1439 | 0.158* | 0.622 (6) |
H20C | −0.0366 | 1.1620 | 0.1664 | 0.158* | 0.622 (6) |
C19A | −0.1394 (7) | 0.9902 (10) | 0.2082 (7) | 0.089 (4) | 0.378 (6) |
H19D | −0.1923 | 0.9792 | 0.2108 | 0.134* | 0.378 (6) |
H19E | −0.1298 | 1.0737 | 0.2034 | 0.134* | 0.378 (6) |
H19F | −0.1011 | 0.9596 | 0.2544 | 0.134* | 0.378 (6) |
C20A | −0.0652 (5) | 1.0785 (6) | 0.0379 (5) | 0.056 (2) | 0.378 (6) |
H20D | −0.0436 | 1.1513 | 0.0253 | 0.085* | 0.378 (6) |
H20E | −0.1208 | 1.0894 | 0.0313 | 0.085* | 0.378 (6) |
H20F | −0.0592 | 1.0158 | 0.0044 | 0.085* | 0.378 (6) |
C17 | −0.0658 (3) | 1.0433 (3) | 0.0815 (3) | 0.0497 (13) | 0.626 (7) |
H17A | −0.0478 | 1.0226 | 0.0384 | 0.060* | 0.626 (7) |
H17B | −0.1212 | 1.0680 | 0.0610 | 0.060* | 0.626 (7) |
C18 | −0.1019 (2) | 0.9415 (2) | 0.1867 (2) | 0.0290 (7) | 0.626 (7) |
H18A | −0.0756 | 0.9984 | 0.2268 | 0.035* | 0.626 (7) |
H18B | −0.0989 | 0.8639 | 0.2109 | 0.035* | 0.626 (7) |
C17A | −0.0219 (4) | 1.0459 (4) | 0.1193 (4) | 0.0326 (14) | 0.374 (7) |
H17C | 0.0344 | 1.0332 | 0.1271 | 0.039* | 0.374 (7) |
H17D | −0.0273 | 1.1080 | 0.1542 | 0.039* | 0.374 (7) |
C18A | −0.1320 (5) | 0.9287 (5) | 0.1438 (5) | 0.0387 (18) | 0.374 (7) |
H18C | −0.1433 | 0.8450 | 0.1491 | 0.046* | 0.374 (7) |
H18D | −0.1726 | 0.9584 | 0.0981 | 0.046* | 0.374 (7) |
O99 | −0.0274 (3) | 1.2785 (5) | 0.2561 (4) | 0.106 (2)* | 0.50 |
Atomic displacement parameters (Å2) top | U11 | U22 | U33 | U12 | U13 | U23 |
Gd1 | 0.00684 (2) | 0.00960 (2) | 0.00528 (3) | −0.00035 (2) | 0.00190 (2) | 0.00008 (2) |
O1 | 0.0128 (4) | 0.0305 (5) | 0.0068 (4) | −0.0046 (3) | 0.0012 (3) | 0.0011 (3) |
O31 | 0.0150 (4) | 0.0224 (5) | 0.0208 (5) | −0.0110 (3) | 0.0094 (4) | −0.0105 (4) |
C1 | 0.0095 (4) | 0.0136 (4) | 0.0073 (4) | 0.0013 (3) | 0.0025 (3) | 0.0000 (3) |
O11 | 0.0112 (3) | 0.0154 (4) | 0.0095 (4) | −0.0018 (3) | 0.0053 (3) | −0.0020 (3) |
O14 | 0.0173 (4) | 0.0220 (4) | 0.0138 (4) | −0.0087 (4) | 0.0094 (3) | −0.0059 (4) |
O21 | 0.0257 (5) | 0.0151 (4) | 0.0142 (4) | 0.0010 (4) | 0.0071 (4) | −0.0028 (3) |
O41 | 0.0256 (5) | 0.0213 (4) | 0.0083 (4) | 0.0115 (4) | 0.0019 (3) | 0.0022 (3) |
C11 | 0.0137 (5) | 0.0174 (5) | 0.0140 (5) | −0.0072 (4) | 0.0080 (4) | −0.0055 (4) |
C2 | 0.0137 (5) | 0.0140 (4) | 0.0080 (4) | −0.0027 (4) | 0.0032 (4) | −0.0006 (4) |
C3 | 0.0208 (5) | 0.0241 (6) | 0.0072 (5) | −0.0099 (5) | 0.0034 (4) | −0.0007 (4) |
C12 | 0.0165 (5) | 0.0216 (5) | 0.0139 (5) | −0.0096 (4) | 0.0085 (4) | −0.0069 (4) |
C7 | 0.0162 (5) | 0.0183 (5) | 0.0080 (5) | −0.0054 (4) | 0.0030 (4) | −0.0002 (4) |
C10 | 0.0135 (5) | 0.0174 (5) | 0.0138 (5) | −0.0062 (4) | 0.0074 (4) | −0.0035 (4) |
O13 | 0.0444 (7) | 0.0370 (6) | 0.0103 (4) | 0.0311 (6) | 0.0038 (4) | 0.0006 (4) |
C6 | 0.0211 (5) | 0.0197 (5) | 0.0078 (5) | −0.0082 (5) | 0.0018 (4) | −0.0006 (4) |
C13 | 0.0186 (5) | 0.0253 (6) | 0.0142 (5) | −0.0124 (5) | 0.0101 (4) | −0.0086 (5) |
C5 | 0.0236 (6) | 0.0216 (6) | 0.0091 (5) | −0.0128 (5) | 0.0025 (4) | −0.0012 (4) |
C41 | 0.0292 (7) | 0.0234 (6) | 0.0100 (5) | 0.0163 (5) | 0.0032 (5) | 0.0028 (5) |
C4 | 0.0283 (7) | 0.0281 (7) | 0.0085 (5) | −0.0173 (6) | 0.0033 (5) | −0.0003 (5) |
N16 | 0.0540 (11) | 0.0133 (5) | 0.0559 (12) | −0.0004 (6) | 0.0345 (10) | 0.0001 (6) |
C15 | 0.0628 (14) | 0.0153 (6) | 0.0760 (16) | −0.0070 (7) | 0.0546 (14) | −0.0074 (8) |
C19 | 0.0315 (18) | 0.050 (2) | 0.087 (4) | 0.0063 (17) | 0.014 (2) | −0.009 (2) |
C20 | 0.048 (2) | 0.037 (2) | 0.187 (7) | −0.0153 (19) | −0.024 (3) | 0.056 (3) |
C19A | 0.092 (8) | 0.099 (8) | 0.106 (9) | −0.034 (6) | 0.074 (7) | −0.067 (7) |
C20A | 0.049 (4) | 0.045 (3) | 0.070 (5) | 0.012 (3) | 0.013 (4) | 0.037 (3) |
C17 | 0.058 (3) | 0.0241 (14) | 0.070 (3) | 0.0105 (16) | 0.025 (3) | 0.0231 (17) |
C18 | 0.0346 (16) | 0.0220 (11) | 0.0317 (18) | 0.0042 (10) | 0.0127 (14) | −0.0075 (11) |
C17A | 0.036 (3) | 0.0129 (16) | 0.051 (4) | −0.0009 (16) | 0.016 (3) | 0.0037 (18) |
C18A | 0.046 (4) | 0.025 (2) | 0.058 (5) | 0.000 (2) | 0.034 (4) | −0.003 (2) |
Geometric parameters (Å, º) top
Gd1—O11 | 2.2754 (9) | C5—C41iv | 1.5007 (19) |
Gd1—O1 | 2.3135 (10) | C41—O13i | 1.2574 (17) |
Gd1—O13 | 2.3253 (11) | C41—C5v | 1.5007 (19) |
Gd1—O41 | 2.3468 (10) | C4—H4 | 0.9500 |
Gd1—O31 | 2.3811 (10) | N16—C15 | 1.325 (2) |
Gd1—O14 | 2.3905 (9) | N16—C18A | 1.401 (6) |
Gd1—O21 | 2.4278 (10) | N16—C18 | 1.464 (4) |
Gd1—O31i | 2.8175 (11) | N16—C17A | 1.475 (5) |
Gd1—Gd1i | 4.0364 (1) | N16—C17 | 1.522 (4) |
O1—C1 | 1.2418 (15) | C15—H15 | 0.9500 |
O31—C10i | 1.2670 (15) | C19—C18 | 1.503 (6) |
O31—Gd1i | 2.8175 (11) | C19—H19A | 0.9800 |
C1—O11ii | 1.2715 (15) | C19—H19B | 0.9800 |
C1—C2 | 1.5007 (17) | C19—H19C | 0.9800 |
O11—C1ii | 1.2715 (15) | C20—C17 | 1.474 (8) |
O14—C10 | 1.2598 (15) | C20—H20A | 0.9800 |
O21—C15 | 1.218 (2) | C20—H20B | 0.9800 |
O41—C41 | 1.2613 (17) | C20—H20C | 0.9800 |
C11—C12 | 1.3926 (17) | C19A—C18A | 1.436 (10) |
C11—C13 | 1.3955 (18) | C19A—H19D | 0.9800 |
C11—C10 | 1.4952 (16) | C19A—H19E | 0.9800 |
C2—C7 | 1.3927 (17) | C19A—H19F | 0.9800 |
C2—C3 | 1.3944 (17) | C20A—C17A | 1.516 (11) |
C3—C4 | 1.3872 (19) | C20A—H20D | 0.9800 |
C3—H3 | 0.9500 | C20A—H20E | 0.9800 |
C12—C13iii | 1.3883 (17) | C20A—H20F | 0.9800 |
C12—H12 | 0.9500 | C17—H17A | 0.9900 |
C7—C6 | 1.3898 (18) | C17—H17B | 0.9900 |
C7—H7 | 0.9500 | C18—H18A | 0.9900 |
C10—O31i | 1.2670 (15) | C18—H18B | 0.9900 |
O13—C41i | 1.2574 (17) | C17A—H17C | 0.9900 |
C6—C5 | 1.3911 (19) | C17A—H17D | 0.9900 |
C6—H6 | 0.9500 | C18A—H18C | 0.9900 |
C13—C12iii | 1.3883 (17) | C18A—H18D | 0.9900 |
C13—H13 | 0.9500 | O99—O99ii | 1.086 (11) |
C5—C4 | 1.3923 (19) | | |
| | | |
O11—Gd1—O1 | 83.40 (3) | C6—C5—C41iv | 119.21 (12) |
O11—Gd1—O13 | 103.81 (5) | C4—C5—C41iv | 120.84 (12) |
O1—Gd1—O13 | 73.68 (4) | O13i—C41—O41 | 125.52 (13) |
O11—Gd1—O41 | 103.23 (4) | O13i—C41—C5v | 117.27 (12) |
O1—Gd1—O41 | 145.25 (4) | O41—C41—C5v | 117.20 (12) |
O13—Gd1—O41 | 134.69 (4) | C3—C4—C5 | 120.16 (12) |
O11—Gd1—O31 | 82.09 (3) | C3—C4—H4 | 119.9 |
O1—Gd1—O31 | 141.83 (4) | C5—C4—H4 | 119.9 |
O13—Gd1—O31 | 75.85 (4) | C15—N16—C18A | 120.0 (3) |
O41—Gd1—O31 | 72.71 (4) | C15—N16—C18 | 120.43 (19) |
O11—Gd1—O14 | 149.72 (3) | C15—N16—C17A | 114.1 (3) |
O1—Gd1—O14 | 77.07 (3) | C18A—N16—C17A | 125.6 (3) |
O13—Gd1—O14 | 92.72 (5) | C18—N16—C17A | 116.8 (3) |
O41—Gd1—O14 | 81.33 (4) | C15—N16—C17 | 122.7 (2) |
O31—Gd1—O14 | 127.05 (3) | C18A—N16—C17 | 105.2 (4) |
O11—Gd1—O21 | 75.83 (3) | C18—N16—C17 | 116.8 (2) |
O1—Gd1—O21 | 77.61 (4) | O21—C15—N16 | 126.48 (18) |
O13—Gd1—O21 | 151.10 (4) | O21—C15—H15 | 116.8 |
O41—Gd1—O21 | 71.31 (4) | N16—C15—H15 | 116.8 |
O31—Gd1—O21 | 131.58 (4) | C18—C19—H19A | 109.5 |
O14—Gd1—O21 | 77.52 (4) | C18—C19—H19B | 109.5 |
O11—Gd1—O31i | 160.55 (3) | H19A—C19—H19B | 109.5 |
O1—Gd1—O31i | 112.41 (4) | C18—C19—H19C | 109.5 |
O13—Gd1—O31i | 71.76 (4) | H19A—C19—H19C | 109.5 |
O41—Gd1—O31i | 70.64 (4) | H19B—C19—H19C | 109.5 |
O31—Gd1—O31i | 78.46 (3) | C17—C20—H20A | 109.5 |
O14—Gd1—O31i | 49.27 (3) | C17—C20—H20B | 109.5 |
O21—Gd1—O31i | 117.48 (3) | H20A—C20—H20B | 109.5 |
C1—O1—Gd1 | 162.85 (9) | C17—C20—H20C | 109.5 |
C10i—O31—Gd1 | 171.04 (10) | H20A—C20—H20C | 109.5 |
C10i—O31—Gd1i | 84.27 (8) | H20B—C20—H20C | 109.5 |
Gd1—O31—Gd1i | 101.54 (3) | C18A—C19A—H19D | 109.5 |
O1—C1—O11ii | 124.68 (11) | C18A—C19A—H19E | 109.5 |
O1—C1—C2 | 118.10 (11) | H19D—C19A—H19E | 109.5 |
O11ii—C1—C2 | 117.22 (11) | C18A—C19A—H19F | 109.5 |
C1ii—O11—Gd1 | 137.64 (8) | H19D—C19A—H19F | 109.5 |
C10—O14—Gd1 | 104.71 (8) | H19E—C19A—H19F | 109.5 |
C15—O21—Gd1 | 125.00 (12) | C17A—C20A—H20D | 109.5 |
C41—O41—Gd1 | 140.18 (9) | C17A—C20A—H20E | 109.5 |
C12—C11—C13 | 119.59 (11) | H20D—C20A—H20E | 109.5 |
C12—C11—C10 | 120.97 (11) | C17A—C20A—H20F | 109.5 |
C13—C11—C10 | 119.44 (11) | H20D—C20A—H20F | 109.5 |
C7—C2—C3 | 119.95 (11) | H20E—C20A—H20F | 109.5 |
C7—C2—C1 | 120.17 (11) | C20—C17—N16 | 110.8 (4) |
C3—C2—C1 | 119.82 (11) | C20—C17—H17A | 109.5 |
C4—C3—C2 | 119.95 (12) | N16—C17—H17A | 109.5 |
C4—C3—H3 | 120.0 | C20—C17—H17B | 109.5 |
C2—C3—H3 | 120.0 | N16—C17—H17B | 109.5 |
C13iii—C12—C11 | 119.99 (12) | H17A—C17—H17B | 108.1 |
C13iii—C12—H12 | 120.0 | N16—C18—C19 | 114.1 (4) |
C11—C12—H12 | 120.0 | N16—C18—H18A | 108.7 |
C6—C7—C2 | 119.89 (11) | C19—C18—H18A | 108.7 |
C6—C7—H7 | 120.1 | N16—C18—H18B | 108.7 |
C2—C7—H7 | 120.1 | C19—C18—H18B | 108.7 |
O14—C10—O31i | 121.57 (11) | H18A—C18—H18B | 107.6 |
O14—C10—C11 | 117.82 (11) | N16—C17A—C20A | 104.7 (5) |
O31i—C10—C11 | 120.61 (11) | N16—C17A—H17C | 110.8 |
O14—C10—Gd1 | 51.08 (6) | C20A—C17A—H17C | 110.8 |
O31i—C10—Gd1 | 70.63 (7) | N16—C17A—H17D | 110.8 |
C11—C10—Gd1 | 168.03 (9) | C20A—C17A—H17D | 110.8 |
C41i—O13—Gd1 | 136.94 (10) | H17C—C17A—H17D | 108.9 |
C7—C6—C5 | 120.17 (12) | N16—C18A—C19A | 116.4 (7) |
C7—C6—H6 | 119.9 | N16—C18A—H18C | 108.2 |
C5—C6—H6 | 119.9 | C19A—C18A—H18C | 108.2 |
C12iii—C13—C11 | 120.43 (12) | N16—C18A—H18D | 108.2 |
C12iii—C13—H13 | 119.8 | C19A—C18A—H18D | 108.2 |
C11—C13—H13 | 119.8 | H18C—C18A—H18D | 107.3 |
C6—C5—C4 | 119.83 (12) | | |
Symmetry codes: (i) −x, −y+1, −z; (ii) −x, y, −z+1/2; (iii) −x+1/2, −y+3/2, −z; (iv) x+1/2, −y+3/2, z+1/2; (v) x−1/2, −y+3/2, z−1/2. |