Supporting information
Crystallographic Information File (CIF) https://doi.org/10.1107/S1600536806023683/ng2034sup1.cif | |
Structure factor file (CIF format) https://doi.org/10.1107/S1600536806023683/ng2034Isup2.hkl |
CCDC reference: 618290
Key indicators
- Single-crystal X-ray study
- T = 298 K
- Mean (C-C) = 0.007 Å
- H-atom completeness 66%
- Disorder in solvent or counterion
- R factor = 0.033
- wR factor = 0.074
- Data-to-parameter ratio = 12.2
checkCIF/PLATON results
No syntax errors found
Alert level A PLAT306_ALERT_2_A Isolated Oxygen Atom (H-atoms Missing ?) ....... O2W
Author Response: H-atoms were not located |
PROBLEM: Isolated Oxygen Atom (H-atoms Missing ?) ....... O3W RESPONSE: H-atoms were not located H-atoms were not located PLAT306_ALERT_2_A Isolated Oxygen Atom (H-atoms Missing ?) ....... O3W
Author Response: H-atoms were not located |
PROBLEM: Isolated Oxygen Atom (H-atoms Missing ?) ....... O3W RESPONSE: H-atoms were not located H-atoms were not located PLAT430_ALERT_2_A Short Inter D...A Contact O4W' .. O3W .. 2.48 Ang.
Author Response: Disordered crystallization water molecules |
PROBLEM: Short Inter D...A Contact O4W .. O5W .. 2.19 Ang. RESPONSE: Disordered crystallization water molecules Disordered crystallization water molecules PLAT430_ALERT_2_A Short Inter D...A Contact O4W .. O5W .. 2.19 Ang.
Author Response: Disordered crystallization water molecules |
PROBLEM: Short Inter D...A Contact O4W .. O5W .. 2.19 Ang. RESPONSE: Disordered crystallization water molecules Disordered crystallization water molecules
Alert level B PLAT430_ALERT_2_B Short Inter D...A Contact O4W' .. O5W .. 2.77 Ang.
Author Response: Disordered crystallization water molecules |
PROBLEM: Short Inter D...A Contact O4W .. O5W .. 2.19 Ang. RESPONSE: Disordered crystallization water molecules Disordered crystallization water molecules PLAT430_ALERT_2_B Short Inter D...A Contact O2W .. O3 .. 2.70 Ang.
Author Response: Disordered crystallization water molecules |
PROBLEM: Short Inter D...A Contact O4W .. O5W .. 2.19 Ang. RESPONSE: Disordered crystallization water molecules Disordered crystallization water molecules PLAT430_ALERT_2_B Short Inter D...A Contact O2W .. O7 .. 2.81 Ang.
Author Response: Disordered crystallization water molecules |
PROBLEM: Short Inter D...A Contact O4W .. O5W .. 2.19 Ang. RESPONSE: Disordered crystallization water molecules Disordered crystallization water molecules PLAT430_ALERT_2_B Short Inter D...A Contact O5W .. O8 .. 2.81 Ang.
Author Response: Disordered crystallization water molecules |
PROBLEM: Short Inter D...A Contact O4W .. O5W .. 2.19 Ang. RESPONSE: Disordered crystallization water molecules Disordered crystallization water molecules
Alert level C CHEMW03_ALERT_2_C The ratio of given/expected molecular weight as calculated from the _atom_site* data lies outside the range 0.99 <> 1.01 From the CIF: _cell_formula_units_Z 1 From the CIF: _chemical_formula_weight 1037.02 TEST: Calculate formula weight from _atom_site_* atom mass num sum C 12.01 16.00 192.18 H 1.01 26.00 26.21 N 14.01 6.00 84.04 O 16.00 27.00 431.97 Nd 144.24 2.00 288.48 Calculated formula weight 1022.88 PLAT041_ALERT_1_C Calc. and Rep. SumFormula Strings Differ .... ? PLAT042_ALERT_1_C Calc. and Rep. MoietyFormula Strings Differ .... ? PLAT043_ALERT_1_C Check Reported Molecular Weight ................ 1037.02 PLAT044_ALERT_1_C Calculated and Reported Dx Differ .............. ? PLAT062_ALERT_4_C Rescale T(min) & T(max) by ..................... 1.02 PLAT068_ALERT_1_C Reported F000 Differs from Calcd (or Missing)... ? PLAT302_ALERT_4_C Anion/Solvent Disorder ......................... 17.00 Perc. PLAT369_ALERT_2_C Long C(sp2)-C(sp2) Bond C7 - C7_a ... 1.54 Ang. PLAT430_ALERT_2_C Short Inter D...A Contact O2W .. O3W .. 2.85 Ang.
Author Response: Disordered crystallization water molecules |
PROBLEM: Short Inter D...A Contact O4W .. O5W .. 2.19 Ang. RESPONSE: Disordered crystallization water molecules Disordered crystallization water molecules PLAT720_ALERT_4_C Number of Unusual/Non-Standard Label(s) ........ 1 PLAT731_ALERT_1_C Bond Calc 0.85(4), Rep 0.841(19) ...... 2.11 su-Rat O1W -H1A 1.555 1.555 PLAT735_ALERT_1_C D-H Calc 0.85(4), Rep 0.841(19) ...... 2.11 su-Rat O1W -H1A 1.555 1.555 PLAT764_ALERT_4_C Overcomplete CIF Bond List Detected (Rep/Expd) . 1.28 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:C16 H40 N6 Nd2 O27 Atom count from the _atom_site data: C16 H26 N6 Nd2 O27 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 1 From the CIF: _chemical_formula_sum C16 H40 N6 Nd2 O27 TEST: Compare cell contents of formula and atom_site data atom Z*formula cif sites diff C 16.00 16.00 0.00 H 40.00 26.00 14.00 N 6.00 6.00 0.00 Nd 2.00 2.00 0.00 O 27.00 27.00 0.00
4 ALERT level A = In general: serious problem 4 ALERT level B = Potentially serious problem 14 ALERT level C = Check and explain 3 ALERT level G = General alerts; check 9 ALERT type 1 CIF construction/syntax error, inconsistent or missing data 12 ALERT type 2 Indicator that the structure model may be wrong or deficient 0 ALERT type 3 Indicator that the structure quality may be low 4 ALERT type 4 Improvement, methodology, query or suggestion
Data collection: COLLECT (Nonius, 1998); cell refinement: HKL (Otwinowski & Minor, 1997); data reduction: HKL; program(s) used to solve structure: SHELXS97 (Sheldrick, 1997a); program(s) used to refine structure: SHELXL97 (Sheldrick, 1997a); molecular graphics: SHELXTL (Sheldrick, 1997b); software used to prepare material for publication: SHELXTL.
(CH6N3)2[Nd2(C6H5O7)2(C2O4)(H2O)2]·7H2O | Z = 1 |
Mr = 1037.02 | F(000) = 514 |
Triclinic, P1 | Dx = 1.980 Mg m−3 |
Hall symbol: -P 1 | Mo Kα radiation, λ = 0.71073 Å |
a = 8.2017 (4) Å | Cell parameters from 8223 reflections |
b = 10.0447 (3) Å | θ = 3.2–25.0° |
c = 11.0222 (5) Å | µ = 3.06 mm−1 |
α = 87.892 (3)° | T = 298 K |
β = 89.505 (2)° | Plate, light pink |
γ = 73.464 (3)° | 0.16 × 0.06 × 0.02 mm |
V = 869.90 (6) Å3 |
Nonius KappaCCD area-detector diffractometer | 3033 independent reflections |
Radiation source: fine-focus sealed tube | 2588 reflections with I > 2σ(I) |
Graphite monochromator | Rint = 0.055 |
φ and ω scans | θmax = 25.0°, θmin = 3.2° |
Absorption correction: multi-scan (MULABS in PLATON; Spek, 2003) | h = −9→9 |
Tmin = 0.790, Tmax = 0.922 | k = −11→11 |
8213 measured reflections | l = −12→13 |
Refinement on F2 | Primary atom site location: structure-invariant direct methods |
Least-squares matrix: full | Secondary atom site location: difference Fourier map |
R[F2 > 2σ(F2)] = 0.033 | Hydrogen site location: mixed |
wR(F2) = 0.074 | H atoms treated by a mixture of independent and constrained refinement |
S = 1.02 | w = 1/[σ2(Fo2) + (0.0305P)2] where P = (Fo2 + 2Fc2)/3 |
3033 reflections | (Δ/σ)max = 0.001 |
248 parameters | Δρmax = 1.15 e Å−3 |
34 restraints | Δρmin = −1.01 e Å−3 |
Geometry. All e.s.d.'s (except the e.s.d. in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell e.s.d.'s are taken into account individually in the estimation of e.s.d.'s in distances, angles and torsion angles; correlations between e.s.d.'s in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell e.s.d.'s is used for estimating e.s.d.'s involving l.s. planes. |
Refinement. Refinement of F2 against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F2, conventional R-factors R are based on F, with F set to zero for negative F2. The threshold expression of F2 > σ(F2) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F2 are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. |
x | y | z | Uiso*/Ueq | Occ. (<1) | |
Nd | 0.39086 (3) | 0.33312 (3) | 0.54647 (3) | 0.02134 (11) | |
O1 | 0.6334 (5) | 0.1586 (3) | 0.4271 (3) | 0.0265 (9) | |
H1 | 0.609 (6) | 0.086 (3) | 0.445 (4) | 0.018 (14)* | |
H1A | 0.730 (5) | 0.318 (4) | 0.637 (5) | 0.022* | |
H1B | 0.721 (5) | 0.190 (2) | 0.675 (5) | 0.022* | |
O2 | 0.3158 (5) | 0.2488 (4) | 0.3549 (4) | 0.0325 (9) | |
O3 | 0.3757 (6) | 0.2243 (5) | 0.1602 (4) | 0.0589 (13) | |
O4 | 0.5334 (4) | 0.4418 (3) | 0.3896 (3) | 0.0245 (8) | |
O5 | 0.7276 (5) | 0.5007 (3) | 0.2791 (4) | 0.0350 (10) | |
O6 | 0.5883 (5) | −0.0848 (3) | 0.4046 (4) | 0.0394 (11) | |
O7 | 0.6572 (5) | −0.2009 (3) | 0.2389 (3) | 0.0306 (9) | |
O8 | 0.0905 (4) | 0.3351 (3) | 0.5691 (3) | 0.0286 (9) | |
O9 | −0.1821 (4) | 0.4568 (3) | 0.5463 (4) | 0.0316 (9) | |
O1W | 0.6641 (5) | 0.2722 (4) | 0.6632 (4) | 0.0333 (9) | |
O2W | 0.5457 (8) | 0.2426 (7) | −0.0481 (5) | 0.0881 (19) | |
O3W | 0.1243 (11) | −0.0616 (8) | 0.0915 (8) | 0.131 (3) | |
O4W | 0.127 (4) | 0.042 (4) | 0.345 (2) | 0.128 (6) | 0.50 |
O4W' | 0.152 (4) | 0.024 (4) | 0.296 (2) | 0.128 (6) | 0.50 |
O5W | −0.010 (2) | 0.0992 (17) | 0.5153 (18) | 0.149 (6) | 0.50 |
N1 | 0.0516 (7) | 0.4560 (6) | 0.1574 (5) | 0.0514 (15) | |
H1C | −0.0515 | 0.4677 | 0.1813 | 0.062* | |
H1D | 0.1189 | 0.3734 | 0.1514 | 0.062* | |
N2 | 0.2635 (7) | 0.5457 (6) | 0.0876 (5) | 0.0556 (16) | |
H2A | 0.3291 | 0.4631 | 0.0782 | 0.067* | |
H2B | 0.2995 | 0.6165 | 0.0696 | 0.067* | |
N3 | 0.0046 (8) | 0.6918 (6) | 0.1386 (6) | 0.0658 (18) | |
H3C | −0.0987 | 0.7048 | 0.1624 | 0.079* | |
H3D | 0.0419 | 0.7619 | 0.1204 | 0.079* | |
C1 | 0.6111 (7) | 0.1685 (5) | 0.2990 (5) | 0.0219 (11) | |
C2 | 0.4193 (7) | 0.2173 (5) | 0.2686 (5) | 0.0274 (12) | |
C3 | 0.6988 (7) | 0.2752 (5) | 0.2500 (5) | 0.0302 (13) | |
H3A | 0.8207 | 0.2352 | 0.2590 | 0.036* | |
H3B | 0.6748 | 0.2907 | 0.1638 | 0.036* | |
C4 | 0.6496 (7) | 0.4141 (5) | 0.3087 (5) | 0.0250 (12) | |
C5 | 0.6940 (7) | 0.0280 (5) | 0.2420 (5) | 0.0285 (13) | |
H5A | 0.6664 | 0.0365 | 0.1562 | 0.034* | |
H5B | 0.8165 | 0.0079 | 0.2492 | 0.034* | |
C6 | 0.6420 (7) | −0.0929 (5) | 0.2966 (5) | 0.0254 (12) | |
C7 | −0.0251 (7) | 0.4399 (5) | 0.5335 (5) | 0.0252 (12) | |
C8 | 0.1062 (9) | 0.5641 (8) | 0.1300 (6) | 0.0495 (17) |
U11 | U22 | U33 | U12 | U13 | U23 | |
Nd | 0.01783 (16) | 0.01596 (15) | 0.02981 (18) | −0.00419 (11) | 0.00271 (11) | −0.00103 (10) |
O1 | 0.032 (2) | 0.0182 (18) | 0.030 (2) | −0.0082 (16) | 0.0035 (17) | −0.0016 (15) |
O2 | 0.026 (2) | 0.038 (2) | 0.037 (2) | −0.0118 (17) | 0.0010 (19) | −0.0050 (17) |
O3 | 0.049 (3) | 0.082 (3) | 0.033 (3) | 0.003 (3) | −0.008 (2) | −0.009 (2) |
O4 | 0.024 (2) | 0.0199 (17) | 0.029 (2) | −0.0064 (15) | 0.0076 (17) | −0.0032 (15) |
O5 | 0.040 (2) | 0.0208 (19) | 0.050 (3) | −0.0169 (18) | 0.016 (2) | −0.0037 (17) |
O6 | 0.057 (3) | 0.0217 (19) | 0.041 (3) | −0.0135 (19) | 0.021 (2) | −0.0036 (16) |
O7 | 0.038 (2) | 0.0168 (18) | 0.038 (2) | −0.0089 (16) | 0.0008 (18) | −0.0060 (16) |
O8 | 0.0176 (19) | 0.0215 (18) | 0.044 (2) | −0.0017 (16) | 0.0004 (17) | 0.0065 (16) |
O9 | 0.020 (2) | 0.0267 (19) | 0.047 (3) | −0.0071 (16) | 0.0010 (18) | 0.0069 (17) |
O1W | 0.029 (2) | 0.031 (2) | 0.042 (2) | −0.0118 (17) | −0.0060 (18) | 0.0056 (18) |
O2W | 0.099 (4) | 0.128 (5) | 0.057 (3) | −0.064 (4) | −0.011 (3) | 0.004 (3) |
O3W | 0.114 (6) | 0.131 (5) | 0.144 (6) | −0.032 (5) | 0.023 (5) | 0.021 (5) |
O4W | 0.109 (8) | 0.146 (8) | 0.157 (12) | −0.080 (6) | −0.015 (9) | −0.007 (9) |
O4W' | 0.109 (8) | 0.146 (8) | 0.157 (12) | −0.080 (6) | −0.015 (9) | −0.007 (9) |
O5W | 0.145 (10) | 0.128 (9) | 0.186 (11) | −0.057 (8) | −0.022 (8) | −0.013 (8) |
N1 | 0.034 (3) | 0.063 (4) | 0.055 (4) | −0.012 (3) | 0.004 (3) | 0.006 (3) |
N2 | 0.036 (3) | 0.055 (3) | 0.074 (4) | −0.008 (3) | 0.017 (3) | −0.004 (3) |
N3 | 0.052 (4) | 0.056 (4) | 0.082 (5) | −0.002 (3) | 0.022 (4) | −0.013 (3) |
C1 | 0.027 (3) | 0.016 (2) | 0.022 (3) | −0.006 (2) | 0.005 (2) | −0.003 (2) |
C2 | 0.033 (3) | 0.023 (3) | 0.027 (3) | −0.010 (2) | −0.002 (3) | −0.001 (2) |
C3 | 0.038 (3) | 0.024 (3) | 0.033 (3) | −0.014 (2) | 0.015 (3) | −0.007 (2) |
C4 | 0.027 (3) | 0.022 (3) | 0.028 (3) | −0.009 (2) | 0.001 (2) | −0.004 (2) |
C5 | 0.035 (3) | 0.016 (2) | 0.034 (3) | −0.007 (2) | 0.011 (3) | −0.005 (2) |
C6 | 0.019 (3) | 0.025 (3) | 0.030 (3) | −0.003 (2) | 0.002 (2) | 0.000 (2) |
C7 | 0.019 (3) | 0.023 (3) | 0.034 (3) | −0.006 (2) | 0.002 (2) | −0.003 (2) |
C8 | 0.039 (4) | 0.074 (5) | 0.034 (4) | −0.012 (4) | −0.002 (3) | −0.002 (3) |
Nd—O1 | 2.626 (3) | O9—Ndiii | 2.499 (3) |
Nd—O2 | 2.451 (4) | O1W—H1A | 0.841 (19) |
Nd—O4 | 2.470 (3) | O1W—H1B | 0.832 (19) |
Nd—O8 | 2.469 (3) | O4W—O4W' | 0.59 (5) |
Nd—O6i | 2.490 (3) | N1—C8 | 1.312 (8) |
Nd—O4ii | 2.630 (3) | N1—H1C | 0.8600 |
Nd—O5ii | 2.590 (4) | N1—H1D | 0.8600 |
Nd—O6i | 2.490 (3) | N2—C8 | 1.334 (8) |
Nd—O7i | 2.751 (4) | N2—H2A | 0.8600 |
Nd—O9iii | 2.499 (3) | N2—H2B | 0.8600 |
Nd—O1w | 2.503 (4) | N3—C8 | 1.322 (9) |
O1—C1 | 1.421 (6) | N3—H3C | 0.8600 |
O1—H1 | 0.82 (2) | N3—H3D | 0.8600 |
O2—C2 | 1.257 (6) | C1—C3 | 1.532 (6) |
O3—C2 | 1.244 (7) | C1—C5 | 1.536 (7) |
O4—C4 | 1.278 (6) | C1—C2 | 1.545 (8) |
O4—Ndii | 2.630 (3) | C3—C4 | 1.506 (7) |
O5—C4 | 1.251 (6) | C3—H3A | 0.9700 |
O5—Ndii | 2.590 (4) | C3—H3B | 0.9700 |
O6—C6 | 1.264 (6) | C4—Ndii | 2.986 (5) |
O6—Ndi | 2.490 (3) | C5—C6 | 1.502 (7) |
O7—C6 | 1.252 (6) | C5—H5A | 0.9700 |
O7—Ndi | 2.751 (4) | C5—H5B | 0.9700 |
O8—C7 | 1.253 (6) | C6—Ndi | 2.990 (5) |
O9—C7 | 1.257 (6) | C7—C7iii | 1.544 (9) |
O2—Nd—O8 | 74.68 (13) | C4ii—Nd—C6i | 111.20 (14) |
O2—Nd—O4 | 75.74 (12) | C1—O1—Nd | 114.2 (3) |
O8—Nd—O4 | 131.01 (12) | C1—O1—H1 | 102 (4) |
O2—Nd—O6i | 76.40 (13) | Nd—O1—H1 | 99 (4) |
O8—Nd—O6i | 77.01 (12) | C2—O2—Nd | 122.3 (3) |
O4—Nd—O6i | 131.17 (12) | C4—O4—Nd | 142.8 (3) |
O2—Nd—O9iii | 77.03 (13) | C4—O4—Ndii | 93.1 (3) |
O8—Nd—O9iii | 65.56 (10) | Nd—O4—Ndii | 115.56 (13) |
O4—Nd—O9iii | 70.31 (11) | C4—O5—Ndii | 95.7 (3) |
O6i—Nd—O9iii | 138.52 (13) | C6—O6—Ndi | 100.5 (3) |
O2—Nd—O1W | 131.35 (13) | C6—O7—Ndi | 88.4 (3) |
O8—Nd—O1W | 140.95 (12) | C7—O8—Nd | 119.7 (3) |
O4—Nd—O1W | 87.31 (12) | C7—O9—Ndiii | 120.1 (3) |
O6i—Nd—O1W | 82.04 (13) | Nd—O1W—H1A | 112 (3) |
O9iii—Nd—O1W | 138.94 (12) | Nd—O1W—H1B | 121 (3) |
O2—Nd—O5ii | 143.69 (13) | H1A—O1W—H1B | 108 (3) |
O8—Nd—O5ii | 74.54 (12) | C8—N1—H1C | 120.0 |
O4—Nd—O5ii | 111.83 (10) | C8—N1—H1D | 120.0 |
O6i—Nd—O5ii | 114.43 (12) | H1C—N1—H1D | 120.0 |
O9iii—Nd—O5ii | 73.02 (13) | C8—N2—H2A | 120.0 |
O1W—Nd—O5ii | 84.95 (13) | C8—N2—H2B | 120.0 |
O2—Nd—O1 | 62.10 (12) | H2A—N2—H2B | 120.0 |
O8—Nd—O1 | 128.18 (11) | C8—N3—H3C | 120.0 |
O4—Nd—O1 | 65.04 (10) | C8—N3—H3D | 120.0 |
O6i—Nd—O1 | 66.60 (11) | H3C—N3—H3D | 120.0 |
O9iii—Nd—O1 | 124.78 (12) | O1—C1—C3 | 107.0 (4) |
O1W—Nd—O1 | 69.36 (12) | O1—C1—C5 | 110.9 (4) |
O5ii—Nd—O1 | 154.08 (12) | C3—C1—C5 | 109.1 (4) |
O2—Nd—O4ii | 134.82 (11) | O1—C1—C2 | 109.5 (4) |
O8—Nd—O4ii | 116.37 (11) | C3—C1—C2 | 110.3 (4) |
O4—Nd—O4ii | 64.44 (13) | C5—C1—C2 | 110.0 (4) |
O6i—Nd—O4ii | 147.12 (13) | O3—C2—O2 | 123.6 (5) |
O9iii—Nd—O4ii | 70.33 (11) | O3—C2—C1 | 118.3 (5) |
O1W—Nd—O4ii | 68.98 (12) | O2—C2—C1 | 118.1 (5) |
O5ii—Nd—O4ii | 49.72 (10) | C4—C3—C1 | 116.3 (4) |
O1—Nd—O4ii | 114.22 (10) | C4—C3—H3A | 108.2 |
O2—Nd—O7i | 119.07 (11) | C1—C3—H3A | 108.2 |
O8—Nd—O7i | 69.27 (11) | C4—C3—H3B | 108.2 |
O4—Nd—O7i | 159.32 (12) | C1—C3—H3B | 108.2 |
O6i—Nd—O7i | 48.99 (11) | H3A—C3—H3B | 107.4 |
O9iii—Nd—O7i | 124.91 (11) | O5—C4—O4 | 120.5 (4) |
O1W—Nd—O7i | 72.08 (12) | O5—C4—C3 | 118.8 (5) |
O5ii—Nd—O7i | 65.82 (10) | O4—C4—C3 | 120.7 (4) |
O1—Nd—O7i | 107.45 (10) | O5—C4—Ndii | 59.6 (3) |
O4ii—Nd—O7i | 105.20 (10) | O4—C4—Ndii | 61.6 (2) |
O2—Nd—C4ii | 144.15 (13) | C3—C4—Ndii | 169.4 (4) |
O8—Nd—C4ii | 94.10 (13) | C6—C5—C1 | 115.3 (4) |
O4—Nd—C4ii | 87.76 (13) | C6—C5—H5A | 108.4 |
O6i—Nd—C4ii | 135.08 (14) | C1—C5—H5A | 108.4 |
O9iii—Nd—C4ii | 67.42 (14) | C6—C5—H5B | 108.4 |
O1W—Nd—C4ii | 78.06 (14) | C1—C5—H5B | 108.4 |
O5ii—Nd—C4ii | 24.63 (12) | H5A—C5—H5B | 107.5 |
O1—Nd—C4ii | 137.71 (13) | O7—C6—O6 | 120.7 (4) |
O4ii—Nd—C4ii | 25.30 (12) | O7—C6—C5 | 121.3 (5) |
O7i—Nd—C4ii | 86.47 (12) | O6—C6—C5 | 117.9 (5) |
O2—Nd—C6i | 96.48 (13) | O7—C6—Ndi | 66.9 (3) |
O8—Nd—C6i | 68.71 (12) | O6—C6—Ndi | 55.0 (2) |
O4—Nd—C6i | 153.03 (13) | C5—C6—Ndi | 164.8 (4) |
O6i—Nd—C6i | 24.55 (13) | O8—C7—O9 | 125.6 (4) |
O9iii—Nd—C6i | 133.91 (13) | O8—C7—C7iii | 118.6 (6) |
O1W—Nd—C6i | 78.57 (13) | O9—C7—C7iii | 115.8 (5) |
O5ii—Nd—C6i | 89.88 (13) | N1—C8—N3 | 120.9 (6) |
O1—Nd—C6i | 88.38 (12) | N1—C8—N2 | 119.9 (7) |
O4ii—Nd—C6i | 128.66 (13) | N3—C8—N2 | 119.2 (7) |
O7i—Nd—C6i | 24.74 (12) |
Symmetry codes: (i) −x+1, −y, −z+1; (ii) −x+1, −y+1, −z+1; (iii) −x, −y+1, −z+1. |
D—H···A | D—H | H···A | D···A | D—H···A |
O1—H1···O6 | 0.82 (2) | 1.85 (3) | 2.596 (5) | 151 (5) |
O1W—H1A···O9iv | 0.84 (2) | 1.99 (2) | 2.796 (5) | 162 (4) |
N1—H1C···O5v | 0.86 | 2.05 | 2.893 (7) | 166 |
N1—H1D···O3 | 0.86 | 2.21 | 2.993 (7) | 151 |
N2—H2B···O2Wvi | 0.86 | 2.16 | 2.995 (8) | 164 |
N3—H3C···O7vii | 0.86 | 2.14 | 2.964 (7) | 161 |
Symmetry codes: (iv) x+1, y, z; (v) x−1, y, z; (vi) −x+1, −y+1, −z; (vii) x−1, y+1, z. |