Supporting information
Crystallographic Information File (CIF) https://doi.org/10.1107/S160053680500615X/bt6611sup1.cif | |
Structure factor file (CIF format) https://doi.org/10.1107/S160053680500615X/bt6611Isup2.hkl |
CCDC reference: 270232
Key indicators
- Single-crystal X-ray study
- T = 293 K
- Mean (N-C) = 0.004 Å
- H-atom completeness 97%
- Disorder in main residue
- R factor = 0.025
- wR factor = 0.069
- Data-to-parameter ratio = 20.3
checkCIF/PLATON results
No syntax errors found
Alert level B PLAT411_ALERT_2_B Short Inter H...H Contact H22A .. H22A .. 2.08 Ang.
Alert level C PLAT041_ALERT_1_C Calc. and Rep. SumFormula Strings Differ .... ? PLAT042_ALERT_1_C Calc. and Rep. MoietyFormula Strings Differ .... ? PLAT068_ALERT_1_C Reported F000 Differs from Calcd (or Missing)... ? PLAT125_ALERT_4_C No _symmetry_space_group_name_Hall Given ....... ? PLAT199_ALERT_1_C Check the Reported cell_measurement_temperature 293 PLAT200_ALERT_1_C Check the Reported cell_ambient_temperature .... 293 PLAT242_ALERT_2_C Check Low Ueq as Compared to Neighbors for Nd1 PLAT301_ALERT_3_C Main Residue Disorder ......................... 5.00 Perc. PLAT311_ALERT_2_C Isolated Disordered Oxygen Atom (No H's ?) ..... >O4' PLAT311_ALERT_2_C Isolated Disordered Oxygen Atom (No H's ?) ..... <O3' PLAT355_ALERT_3_C Long O-H Bond (0.82A) O4 - H4B ... 1.04 Ang. PLAT411_ALERT_2_C Short Inter H...H Contact H24A .. H24A .. 2.12 Ang. PLAT431_ALERT_2_C Short Inter HL..A Contact Cl3 .. O4' .. 3.17 Ang. PLAT431_ALERT_2_C Short Inter HL..A Contact Cl4 .. O3' .. 3.23 Ang.
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:C12 H50 Cl3 N8 Nd1 O13 Atom count from the _atom_site data: C12 H48 Cl3 N8 Nd1 O13 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 2 From the CIF: _chemical_formula_sum C12 H50 Cl3 N8 Nd O13 TEST: Compare cell contents of formula and atom_site data atom Z*formula cif sites diff C 24.00 24.00 0.00 H 100.00 96.00 4.00 Cl 6.00 6.00 0.00 N 16.00 16.00 0.00 Nd 2.00 2.00 0.00 O 26.00 26.00 0.00
0 ALERT level A = In general: serious problem 1 ALERT level B = Potentially serious problem 14 ALERT level C = Check and explain 3 ALERT level G = General alerts; check 7 ALERT type 1 CIF construction/syntax error, inconsistent or missing data 8 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 1 ALERT type 4 Improvement, methodology, query or suggestion
Data collection: KM-4 Software (Kuma, 1993); cell refinement: KM-4 Software; data reduction: DATAPROC (Gałdecki et al., 1998); program(s) used to solve structure: SHELXS97 (Sheldrick, 1990a); program(s) used to refine structure: SHELXL97 (Sheldrick, 1997); molecular graphics: XP in SHELXTL/PC (Sheldrick, 1990b) ORTEP-3 (Farrugia, 1997); software used to prepare material for publication: SHELXL97.
[Nd(H2O)9]Cl3·2C6H12N4·4H2O | Z = 2 |
Mr = 765.19 | F(000) = 786 |
Triclinic, P1 | Dx = 1.638 Mg m−3 |
a = 9.8155 (6) Å | Mo Kα radiation, λ = 0.71073 Å |
b = 11.7230 (9) Å | Cell parameters from 99 reflections |
c = 14.0699 (12) Å | θ = 2–25° |
α = 85.964 (6)° | µ = 2.00 mm−1 |
β = 76.178 (6)° | T = 293 K |
γ = 80.879 (6)° | Prism, pale violet |
V = 1551.3 (2) Å3 | 0.56 × 0.28 × 0.24 mm |
Kuma KM-4 diffractometer | 6791 reflections with I > 2σ(I) |
Radiation source: fine-focus sealed tube | Rint = 0.021 |
Graphite monochromator | θmax = 27.6°, θmin = 1.8° |
ω–2θ scans | h = −12→0 |
Absorption correction: numerical (X-RED; Stoe & Cie (1999) | k = −15→15 |
Tmin = 0.381, Tmax = 0.683 | l = −18→17 |
7597 measured reflections | 3 standard reflections every 100 reflections |
7179 independent reflections | intensity decay: 43.7% |
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)] = 0.025 | Hydrogen site location: difference Fourier map |
wR(F2) = 0.069 | H-atom parameters constrained |
S = 1.09 | w = 1/[σ2(Fo2) + (0.0398P)2 + 1.1931P] where P = (Fo2 + 2Fc2)/3 |
7179 reflections | (Δ/σ)max = 0.002 |
354 parameters | Δρmax = 1.77 e Å−3 |
0 restraints | Δρmin = −0.96 e Å−3 |
Experimental. The crystal was measured in glass capillary |
Geometry. All e.s.d.'s (except the e.s.d. in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell e.s.d.'s are taken into account individually in the estimation of e.s.d.'s in distances, angles and torsion angles; correlations between e.s.d.'s in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell e.s.d.'s is used for estimating e.s.d.'s involving l.s. planes. |
Refinement. Refinement of F2 against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F2, conventional R-factors R are based on F, with F set to zero for negative F2. The threshold expression of F2 > σ(F2) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F2 are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. |
x | y | z | Uiso*/Ueq | Occ. (<1) | |
Nd1 | 0.790374 (11) | 0.298886 (10) | 0.260505 (8) | 0.02151 (5) | |
O1 | 0.8445 (2) | 0.07789 (15) | 0.25525 (15) | 0.0368 (4) | |
H1A | 0.8722 | 0.0575 | 0.1961 | 0.055* | |
H1B | 0.8388 | 0.0230 | 0.3000 | 0.055* | |
O2 | 0.6298 (2) | 0.41799 (18) | 0.39545 (14) | 0.0377 (4) | |
H2A | 0.5772 | 0.4705 | 0.3706 | 0.057* | |
H2B | 0.6391 | 0.4171 | 0.4542 | 0.057* | |
O3 | 0.7794 (2) | 0.22498 (17) | 0.10137 (13) | 0.0340 (4) | |
H3A | 0.6929 | 0.2268 | 0.1002 | 0.051* | |
H3B | 0.8455 | 0.2033 | 0.0546 | 0.051* | |
O4 | 1.04509 (19) | 0.23052 (16) | 0.22012 (14) | 0.0353 (4) | |
H4A | 1.0780 | 0.1571 | 0.2280 | 0.053* | |
H4B | 1.1298 | 0.2632 | 0.1736 | 0.053* | |
O5 | 0.59680 (19) | 0.43631 (16) | 0.20223 (14) | 0.0348 (4) | |
H5A | 0.5045 | 0.4440 | 0.2284 | 0.052* | |
H5B | 0.5906 | 0.4989 | 0.1642 | 0.052* | |
O6 | 0.9177 (2) | 0.44862 (18) | 0.31345 (16) | 0.0411 (5) | |
H6A | 1.0129 | 0.4544 | 0.2973 | 0.062* | |
H6B | 0.8949 | 0.5202 | 0.3309 | 0.062* | |
O7 | 0.8991 (2) | 0.42546 (18) | 0.11860 (15) | 0.0398 (4) | |
H7A | 0.9490 | 0.4815 | 0.1167 | 0.060* | |
H7B | 0.9053 | 0.4155 | 0.0547 | 0.060* | |
O8 | 0.8352 (2) | 0.21832 (18) | 0.41702 (13) | 0.0362 (4) | |
H8A | 0.9185 | 0.2254 | 0.4327 | 0.054* | |
H8B | 0.7951 | 0.1797 | 0.4725 | 0.054* | |
O9 | 0.5737 (2) | 0.20749 (17) | 0.30905 (15) | 0.0383 (4) | |
H9A | 0.5249 | 0.2325 | 0.3639 | 0.057* | |
H9B | 0.5741 | 0.1369 | 0.2867 | 0.057* | |
C10 | 0.0834 (3) | 0.1184 (2) | 0.5537 (2) | 0.0371 (6) | |
H10A | −0.0057 | 0.1204 | 0.6007 | 0.056* | |
H10B | 0.0993 | 0.0489 | 0.5179 | 0.056* | |
N10 | 0.1975 (3) | 0.1163 (2) | 0.60564 (17) | 0.0355 (5) | |
C11 | 0.1725 (3) | 0.2244 (3) | 0.6586 (2) | 0.0416 (6) | |
H11A | 0.0844 | 0.2279 | 0.7069 | 0.062* | |
H11B | 0.2468 | 0.2243 | 0.6923 | 0.062* | |
N11 | 0.1674 (3) | 0.3275 (2) | 0.59270 (18) | 0.0362 (5) | |
C12 | 0.3028 (3) | 0.3192 (3) | 0.5190 (2) | 0.0397 (6) | |
H12A | 0.3010 | 0.3855 | 0.4749 | 0.059* | |
H12B | 0.3785 | 0.3199 | 0.5511 | 0.059* | |
N12 | 0.3305 (2) | 0.2136 (2) | 0.46262 (17) | 0.0348 (5) | |
C13 | 0.2136 (3) | 0.2136 (3) | 0.41398 (19) | 0.0354 (5) | |
H13A | 0.2300 | 0.1446 | 0.3774 | 0.053* | |
H13B | 0.2109 | 0.2787 | 0.3688 | 0.053* | |
N13 | 0.0760 (2) | 0.2192 (2) | 0.48541 (16) | 0.0325 (4) | |
C14 | 0.0531 (3) | 0.3246 (3) | 0.5410 (2) | 0.0403 (6) | |
H14A | −0.0362 | 0.3290 | 0.5879 | 0.060* | |
H14B | 0.0488 | 0.3909 | 0.4970 | 0.060* | |
C15 | 0.3326 (3) | 0.1138 (2) | 0.5317 (2) | 0.0385 (6) | |
H15A | 0.4083 | 0.1134 | 0.5642 | 0.058* | |
H15B | 0.3508 | 0.0439 | 0.4962 | 0.058* | |
C20 | 0.2881 (3) | 0.1661 (3) | 1.0044 (2) | 0.0382 (6) | |
H20A | 0.2069 | 0.1767 | 0.9761 | 0.057* | |
H20B | 0.2882 | 0.0947 | 1.0423 | 0.057* | |
N20 | 0.2770 (2) | 0.26219 (18) | 1.06917 (16) | 0.0312 (4) | |
C21 | 0.4028 (3) | 0.2441 (2) | 1.11123 (19) | 0.0325 (5) | |
H21A | 0.4047 | 0.1728 | 1.1492 | 0.049* | |
H21B | 0.3970 | 0.3057 | 1.1543 | 0.049* | |
N21 | 0.5347 (2) | 0.24053 (18) | 1.03395 (17) | 0.0309 (4) | |
C22 | 0.5288 (3) | 0.3494 (2) | 0.9754 (2) | 0.0354 (6) | |
H22A | 0.5245 | 0.4125 | 1.0166 | 0.053* | |
H22B | 0.6141 | 0.3475 | 0.9246 | 0.053* | |
N22 | 0.4061 (3) | 0.3695 (2) | 0.93100 (17) | 0.0351 (5) | |
C23 | 0.4147 (4) | 0.2702 (3) | 0.8692 (2) | 0.0455 (7) | |
H23A | 0.3342 | 0.2812 | 0.8402 | 0.068* | |
H23B | 0.4985 | 0.2676 | 0.8171 | 0.068* | |
N23 | 0.4185 (3) | 0.1594 (2) | 0.92546 (18) | 0.0386 (5) | |
C24 | 0.5417 (3) | 0.1457 (2) | 0.9701 (2) | 0.0374 (6) | |
H24A | 0.5457 | 0.0740 | 1.0074 | 0.056* | |
H24B | 0.6269 | 0.1425 | 0.9192 | 0.056* | |
C25 | 0.2769 (3) | 0.3708 (2) | 1.0106 (2) | 0.0367 (6) | |
H25A | 0.2702 | 0.4338 | 1.0523 | 0.055* | |
H25B | 0.1951 | 0.3835 | 0.9828 | 0.055* | |
Cl1 | 0.66506 (9) | 0.14196 (7) | 0.62208 (6) | 0.04897 (18) | |
Cl2 | 0.75514 (9) | 0.50367 (8) | 0.73817 (7) | 0.0574 (2) | |
O91 | 0.1863 (3) | 1.0053 (2) | 0.2211 (2) | 0.0630 (7) | |
H91A | 0.2236 | 0.9623 | 0.2600 | 0.094* | |
H91B | 0.1235 | 0.9749 | 0.1940 | 0.094* | |
O92 | 0.6069 (3) | 0.40931 (19) | 0.59876 (17) | 0.0496 (5) | |
H92A | 0.6484 | 0.4241 | 0.6313 | 0.074* | |
H92B | 0.6231 | 0.3511 | 0.6068 | 0.074* | |
O93 | 0.5541 (3) | −0.0017 (2) | 0.23620 (18) | 0.0577 (6) | |
H93A | 0.5043 | −0.0410 | 0.2738 | 0.087* | |
H93B | 0.5788 | −0.0376 | 0.1823 | 0.087* | |
Cl3 | −0.0204 (2) | 0.1166 (2) | 0.90897 (15) | 0.0525 (6) | 0.532 (6) |
O4' | −0.0573 (6) | 0.3904 (7) | 0.8993 (4) | 0.0470 (12) | 0.532 (6) |
Cl4 | 0.0294 (3) | 0.6623 (3) | 0.08671 (15) | 0.0458 (7) | 0.468 (6) |
O3' | 0.0072 (12) | 0.9386 (12) | 0.0993 (6) | 0.091 (3) | 0.468 (6) |
U11 | U22 | U33 | U12 | U13 | U23 | |
Nd1 | 0.02086 (7) | 0.02285 (7) | 0.01997 (7) | −0.00352 (4) | −0.00322 (4) | 0.00064 (4) |
O1 | 0.0466 (11) | 0.0229 (8) | 0.0365 (10) | −0.0040 (8) | −0.0025 (8) | 0.0021 (7) |
O2 | 0.0366 (10) | 0.0441 (11) | 0.0291 (9) | 0.0084 (8) | −0.0083 (8) | −0.0094 (8) |
O3 | 0.0307 (9) | 0.0431 (10) | 0.0284 (9) | −0.0016 (8) | −0.0077 (7) | −0.0075 (8) |
O4 | 0.0238 (8) | 0.0300 (9) | 0.0448 (11) | −0.0002 (7) | 0.0017 (7) | 0.0053 (8) |
O5 | 0.0290 (9) | 0.0352 (9) | 0.0349 (9) | 0.0018 (7) | −0.0043 (7) | 0.0089 (8) |
O6 | 0.0355 (10) | 0.0362 (10) | 0.0520 (12) | −0.0133 (8) | −0.0015 (9) | −0.0170 (9) |
O7 | 0.0476 (11) | 0.0390 (10) | 0.0344 (10) | −0.0186 (9) | −0.0084 (8) | 0.0119 (8) |
O8 | 0.0322 (9) | 0.0511 (11) | 0.0267 (9) | −0.0094 (8) | −0.0103 (7) | 0.0085 (8) |
O9 | 0.0331 (9) | 0.0362 (10) | 0.0419 (10) | −0.0142 (8) | 0.0073 (8) | −0.0120 (8) |
C10 | 0.0350 (13) | 0.0372 (14) | 0.0417 (15) | −0.0147 (11) | −0.0092 (11) | 0.0037 (11) |
N10 | 0.0402 (12) | 0.0329 (11) | 0.0351 (11) | −0.0068 (9) | −0.0130 (9) | 0.0054 (9) |
C11 | 0.0491 (16) | 0.0492 (17) | 0.0267 (13) | −0.0092 (13) | −0.0076 (11) | −0.0031 (11) |
N11 | 0.0382 (12) | 0.0320 (11) | 0.0376 (12) | −0.0041 (9) | −0.0053 (9) | −0.0104 (9) |
C12 | 0.0425 (15) | 0.0355 (14) | 0.0429 (15) | −0.0167 (12) | −0.0048 (12) | −0.0074 (11) |
N12 | 0.0284 (10) | 0.0394 (12) | 0.0348 (11) | −0.0086 (9) | 0.0004 (9) | −0.0078 (9) |
C13 | 0.0397 (14) | 0.0417 (14) | 0.0257 (12) | −0.0095 (11) | −0.0067 (10) | −0.0026 (10) |
N13 | 0.0298 (11) | 0.0370 (11) | 0.0324 (11) | −0.0039 (9) | −0.0112 (9) | −0.0012 (9) |
C14 | 0.0359 (14) | 0.0340 (13) | 0.0482 (16) | 0.0049 (11) | −0.0101 (12) | −0.0041 (12) |
C15 | 0.0328 (13) | 0.0354 (14) | 0.0486 (16) | 0.0021 (11) | −0.0146 (12) | −0.0084 (12) |
C20 | 0.0336 (13) | 0.0372 (14) | 0.0459 (15) | −0.0110 (11) | −0.0094 (11) | −0.0026 (12) |
N20 | 0.0279 (10) | 0.0283 (10) | 0.0336 (11) | −0.0012 (8) | −0.0025 (8) | 0.0021 (8) |
C21 | 0.0375 (13) | 0.0285 (12) | 0.0310 (12) | −0.0025 (10) | −0.0090 (10) | 0.0008 (9) |
N21 | 0.0298 (10) | 0.0236 (10) | 0.0399 (12) | −0.0030 (8) | −0.0103 (9) | 0.0000 (8) |
C22 | 0.0377 (14) | 0.0252 (12) | 0.0435 (15) | −0.0093 (10) | −0.0081 (11) | 0.0035 (10) |
N22 | 0.0403 (12) | 0.0302 (11) | 0.0331 (11) | −0.0056 (9) | −0.0069 (9) | 0.0074 (9) |
C23 | 0.0578 (19) | 0.0526 (18) | 0.0273 (13) | −0.0112 (14) | −0.0094 (12) | −0.0035 (12) |
N23 | 0.0439 (13) | 0.0360 (12) | 0.0361 (12) | −0.0104 (10) | −0.0036 (10) | −0.0117 (10) |
C24 | 0.0329 (13) | 0.0251 (12) | 0.0496 (16) | 0.0003 (10) | −0.0011 (11) | −0.0093 (11) |
C25 | 0.0355 (13) | 0.0296 (12) | 0.0399 (14) | 0.0043 (10) | −0.0065 (11) | 0.0052 (11) |
Cl1 | 0.0586 (5) | 0.0446 (4) | 0.0417 (4) | −0.0146 (3) | −0.0049 (3) | 0.0051 (3) |
Cl2 | 0.0465 (4) | 0.0577 (5) | 0.0658 (5) | −0.0139 (4) | 0.0013 (4) | −0.0218 (4) |
O91 | 0.0612 (16) | 0.0461 (13) | 0.0816 (19) | 0.0007 (11) | −0.0223 (14) | −0.0013 (13) |
O92 | 0.0569 (14) | 0.0369 (11) | 0.0507 (13) | 0.0086 (10) | −0.0139 (11) | −0.0034 (9) |
O93 | 0.0765 (17) | 0.0504 (13) | 0.0498 (13) | −0.0293 (12) | −0.0052 (12) | −0.0121 (11) |
Cl3 | 0.0583 (10) | 0.0511 (12) | 0.0452 (9) | −0.0010 (8) | −0.0058 (7) | −0.0201 (8) |
O4' | 0.057 (3) | 0.033 (3) | 0.052 (3) | −0.010 (2) | −0.016 (2) | 0.002 (2) |
Cl4 | 0.0539 (12) | 0.0489 (15) | 0.0356 (9) | −0.0153 (10) | −0.0067 (7) | −0.0020 (9) |
O3' | 0.150 (9) | 0.071 (6) | 0.048 (4) | −0.007 (6) | −0.020 (4) | −0.014 (4) |
Nd1—O4 | 2.4425 (17) | N12—C15 | 1.468 (4) |
Nd1—O8 | 2.4442 (18) | N12—C13 | 1.471 (3) |
Nd1—O9 | 2.4624 (18) | C13—N13 | 1.473 (3) |
Nd1—O3 | 2.4887 (18) | C13—H13A | 0.9600 |
Nd1—O2 | 2.5069 (18) | C13—H13B | 0.9600 |
Nd1—O7 | 2.5285 (18) | N13—C14 | 1.468 (4) |
Nd1—O5 | 2.5428 (18) | C14—H14A | 0.9600 |
Nd1—O6 | 2.5542 (18) | C14—H14B | 0.9600 |
Nd1—O1 | 2.5635 (18) | C15—H15A | 0.9600 |
O1—H1A | 0.8500 | C15—H15B | 0.9600 |
O1—H1B | 0.8667 | C20—N20 | 1.472 (4) |
O2—H2A | 0.8501 | C20—N23 | 1.477 (4) |
O2—H2B | 0.8529 | C20—H20A | 0.9600 |
O3—H3A | 0.8501 | C20—H20B | 0.9600 |
O3—H3B | 0.8281 | N20—C25 | 1.468 (3) |
O4—H4A | 0.8789 | N20—C21 | 1.473 (3) |
O4—H4B | 1.0352 | C21—N21 | 1.475 (3) |
O5—H5A | 0.8849 | C21—H21A | 0.9600 |
O5—H5B | 0.8805 | C21—H21B | 0.9600 |
O6—H6A | 0.9190 | N21—C24 | 1.461 (3) |
O6—H6B | 0.8706 | N21—C22 | 1.470 (3) |
O7—H7A | 0.8745 | C22—N22 | 1.465 (4) |
O7—H7B | 0.9013 | C22—H22A | 0.9600 |
O8—H8A | 0.9130 | C22—H22B | 0.9600 |
O8—H8B | 0.9105 | N22—C25 | 1.477 (3) |
O9—H9A | 0.8500 | N22—C23 | 1.481 (4) |
O9—H9B | 0.9040 | C23—N23 | 1.473 (4) |
C10—N10 | 1.472 (3) | C23—H23A | 0.9600 |
C10—N13 | 1.473 (4) | C23—H23B | 0.9600 |
C10—H10A | 0.9600 | N23—C24 | 1.473 (4) |
C10—H10B | 0.9600 | C24—H24A | 0.9600 |
N10—C11 | 1.473 (4) | C24—H24B | 0.9600 |
N10—C15 | 1.474 (4) | C25—H25A | 0.9600 |
C11—N11 | 1.473 (4) | C25—H25B | 0.9600 |
C11—H11A | 0.9600 | O91—H91A | 0.8279 |
C11—H11B | 0.9600 | O91—H91B | 0.9241 |
N11—C12 | 1.472 (4) | O92—H92A | 0.7263 |
N11—C14 | 1.481 (4) | O92—H92B | 0.6832 |
C12—N12 | 1.471 (3) | O93—H93A | 0.8030 |
C12—H12A | 0.9600 | O93—H93B | 0.8583 |
C12—H12B | 0.9600 | ||
O4—Nd1—O8 | 76.98 (6) | N12—C12—N11 | 112.1 (2) |
O4—Nd1—O9 | 135.64 (7) | N12—C12—H12A | 109.2 |
O8—Nd1—O9 | 84.62 (7) | N11—C12—H12A | 109.2 |
O4—Nd1—O3 | 88.06 (7) | N12—C12—H12B | 109.2 |
O8—Nd1—O3 | 137.46 (7) | N11—C12—H12B | 109.2 |
O9—Nd1—O3 | 78.84 (6) | H12A—C12—H12B | 107.9 |
O4—Nd1—O2 | 133.31 (7) | C15—N12—C13 | 108.6 (2) |
O8—Nd1—O2 | 71.32 (7) | C15—N12—C12 | 108.0 (2) |
O9—Nd1—O2 | 74.48 (7) | C13—N12—C12 | 108.5 (2) |
O3—Nd1—O2 | 138.05 (6) | N12—C13—N13 | 111.4 (2) |
O4—Nd1—O7 | 73.24 (7) | N12—C13—H13A | 109.3 |
O8—Nd1—O7 | 139.09 (7) | N13—C13—H13A | 109.3 |
O9—Nd1—O7 | 136.20 (7) | N12—C13—H13B | 109.3 |
O3—Nd1—O7 | 68.89 (7) | N13—C13—H13B | 109.3 |
O2—Nd1—O7 | 111.25 (7) | H13A—C13—H13B | 108.0 |
O4—Nd1—O5 | 142.78 (6) | C14—N13—C13 | 108.6 (2) |
O8—Nd1—O5 | 137.04 (6) | C14—N13—C10 | 108.6 (2) |
O9—Nd1—O5 | 73.48 (7) | C13—N13—C10 | 108.1 (2) |
O3—Nd1—O5 | 74.30 (6) | N13—C14—N11 | 111.9 (2) |
O2—Nd1—O5 | 67.44 (6) | N13—C14—H14A | 109.2 |
O7—Nd1—O5 | 69.88 (6) | N11—C14—H14A | 109.2 |
O4—Nd1—O6 | 71.35 (7) | N13—C14—H14B | 109.2 |
O8—Nd1—O6 | 76.79 (7) | N11—C14—H14B | 109.2 |
O9—Nd1—O6 | 142.38 (6) | H14A—C14—H14B | 107.9 |
O3—Nd1—O6 | 135.52 (7) | N12—C15—N10 | 112.0 (2) |
O2—Nd1—O6 | 68.69 (7) | N12—C15—H15A | 109.2 |
O7—Nd1—O6 | 67.54 (7) | N10—C15—H15A | 109.2 |
O5—Nd1—O6 | 98.57 (7) | N12—C15—H15B | 109.2 |
O4—Nd1—O1 | 68.03 (6) | N10—C15—H15B | 109.2 |
O8—Nd1—O1 | 70.10 (7) | H15A—C15—H15B | 107.9 |
O9—Nd1—O1 | 67.80 (7) | N20—C20—N23 | 111.5 (2) |
O3—Nd1—O1 | 67.37 (6) | N20—C20—H20A | 109.3 |
O2—Nd1—O1 | 127.53 (7) | N23—C20—H20A | 109.3 |
O7—Nd1—O1 | 121.22 (7) | N20—C20—H20B | 109.3 |
O5—Nd1—O1 | 129.38 (7) | N23—C20—H20B | 109.3 |
O6—Nd1—O1 | 131.95 (7) | H20A—C20—H20B | 108.0 |
Nd1—O1—H1A | 109.8 | C25—N20—C20 | 108.8 (2) |
Nd1—O1—H1B | 133.4 | C25—N20—C21 | 108.6 (2) |
H1A—O1—H1B | 116.8 | C20—N20—C21 | 108.2 (2) |
Nd1—O2—H2A | 108.8 | N20—C21—N21 | 111.3 (2) |
Nd1—O2—H2B | 125.6 | N20—C21—H21A | 109.4 |
H2A—O2—H2B | 124.1 | N21—C21—H21A | 109.4 |
Nd1—O3—H3A | 108.7 | N20—C21—H21B | 109.4 |
Nd1—O3—H3B | 128.7 | N21—C21—H21B | 109.4 |
H3A—O3—H3B | 122.6 | H21A—C21—H21B | 108.0 |
Nd1—O4—H4A | 120.9 | C24—N21—C22 | 108.3 (2) |
Nd1—O4—H4B | 132.5 | C24—N21—C21 | 108.3 (2) |
H4A—O4—H4B | 103.5 | C22—N21—C21 | 108.7 (2) |
Nd1—O5—H5A | 126.9 | N22—C22—N21 | 112.2 (2) |
Nd1—O5—H5B | 137.5 | N22—C22—H22A | 109.2 |
H5A—O5—H5B | 94.2 | N21—C22—H22A | 109.2 |
Nd1—O6—H6A | 128.6 | N22—C22—H22B | 109.2 |
Nd1—O6—H6B | 135.6 | N21—C22—H22B | 109.2 |
H6A—O6—H6B | 92.2 | H22A—C22—H22B | 107.9 |
Nd1—O7—H7A | 130.7 | C22—N22—C25 | 108.0 (2) |
Nd1—O7—H7B | 126.2 | C22—N22—C23 | 107.9 (2) |
H7A—O7—H7B | 102.7 | C25—N22—C23 | 107.9 (2) |
Nd1—O8—H8A | 119.6 | N23—C23—N22 | 112.2 (2) |
Nd1—O8—H8B | 142.0 | N23—C23—H23A | 109.2 |
H8A—O8—H8B | 98.4 | N22—C23—H23A | 109.2 |
Nd1—O9—H9A | 109.5 | N23—C23—H23B | 109.2 |
Nd1—O9—H9B | 119.2 | N22—C23—H23B | 109.2 |
H9A—O9—H9B | 124.8 | H23A—C23—H23B | 107.9 |
N10—C10—N13 | 111.9 (2) | C24—N23—C23 | 107.9 (2) |
N10—C10—H10A | 109.2 | C24—N23—C20 | 108.6 (2) |
N13—C10—H10A | 109.2 | C23—N23—C20 | 107.8 (2) |
N10—C10—H10B | 109.2 | N21—C24—N23 | 112.0 (2) |
N13—C10—H10B | 109.2 | N21—C24—H24A | 109.2 |
H10A—C10—H10B | 107.9 | N23—C24—H24A | 109.2 |
C10—N10—C11 | 108.4 (2) | N21—C24—H24B | 109.2 |
C10—N10—C15 | 108.0 (2) | N23—C24—H24B | 109.2 |
C11—N10—C15 | 107.9 (2) | H24A—C24—H24B | 107.9 |
N11—C11—N10 | 112.2 (2) | N20—C25—N22 | 111.9 (2) |
N11—C11—H11A | 109.2 | N20—C25—H25A | 109.2 |
N10—C11—H11A | 109.2 | N22—C25—H25A | 109.2 |
N11—C11—H11B | 109.2 | N20—C25—H25B | 109.2 |
N10—C11—H11B | 109.2 | N22—C25—H25B | 109.2 |
H11A—C11—H11B | 107.9 | H25A—C25—H25B | 107.9 |
C12—N11—C11 | 108.0 (2) | H91A—O91—H91B | 116.3 |
C12—N11—C14 | 107.9 (2) | H92A—O92—H92B | 94.0 |
C11—N11—C14 | 108.0 (2) | H93A—O93—H93B | 105.4 |
D—H···A | D—H | H···A | D···A | D—H···A |
O1—H1A···Cl3i | 0.85 | 2.63 | 3.333 (3) | 141 |
O1—H1A···O3′ii | 0.85 | 2.09 | 2.835 (11) | 146 |
O1—H1B···N10i | 0.87 | 2.05 | 2.910 (3) | 170 |
O2—H2A···O92iii | 0.85 | 2.08 | 2.818 (3) | 144 |
O2—H2A···O5 | 0.85 | 2.39 | 2.803 (3) | 111 |
O2—H2B···O92 | 0.85 | 1.98 | 2.811 (3) | 165 |
O3—H3A···N21iv | 0.85 | 1.97 | 2.762 (3) | 154 |
O3—H3B···Cl3v | 0.83 | 2.35 | 3.155 (3) | 163 |
O3—H3B···Cl4vi | 0.83 | 2.64 | 3.192 (3) | 126 |
O4—H4A···O91ii | 0.88 | 1.92 | 2.781 (3) | 167 |
O4—H4B···N20v | 1.04 | 1.80 | 2.771 (3) | 155 |
O5—H5A···Cl2iii | 0.88 | 2.46 | 3.326 (2) | 165 |
O5—H5B···N22iii | 0.88 | 1.97 | 2.846 (3) | 174 |
O6—H6A···Cl2vii | 0.92 | 2.34 | 3.248 (2) | 172 |
O6—H6B···N11iii | 0.87 | 2.08 | 2.932 (3) | 166 |
O7—H7A···O4′iii | 0.87 | 1.94 | 2.817 (6) | 175 |
O7—H7B···O4′v | 0.90 | 2.16 | 3.060 (6) | 174 |
O7—H7A···Cl4viii | 0.87 | 2.35 | 3.198 (3) | 162 |
O7—H7B···Cl4vi | 0.90 | 2.16 | 3.019 (3) | 159 |
O8—H8A···N13viii | 0.91 | 1.86 | 2.758 (3) | 168 |
O8—H8B···Cl1 | 0.91 | 2.24 | 3.118 (2) | 162 |
O9—H9A···N12 | 0.85 | 2.11 | 2.806 (3) | 139 |
O9—H9B···O93 | 0.90 | 1.87 | 2.774 (3) | 173 |
O91—H91A···Cl1iii | 0.83 | 2.37 | 3.190 (3) | 174 |
O91—H91B···Cl3ix | 0.92 | 2.35 | 3.252 (4) | 164 |
O91—H91B···O3′ | 0.92 | 2.05 | 2.950 (10) | 163 |
O92—H92A···Cl2 | 0.73 | 2.34 | 3.061 (3) | 170 |
O92—H92B···Cl1 | 0.68 | 2.42 | 3.104 (2) | 174 |
O93—H93A···Cl1i | 0.80 | 2.35 | 3.150 (3) | 173 |
O93—H93B···N23i | 0.86 | 2.15 | 2.968 (3) | 160 |
C20—H20A···Cl3 | 0.96 | 2.82 | 3.731 (4) | 158 |
C21—H21B···Cl2x | 0.96 | 2.80 | 3.673 (3) | 151 |
Symmetry codes: (i) −x+1, −y, −z+1; (ii) x+1, y−1, z; (iii) −x+1, −y+1, −z+1; (iv) x, y, z−1; (v) x+1, y, z−1; (vi) −x+1, −y+1, −z; (vii) −x+2, −y+1, −z+1; (viii) x+1, y, z; (ix) −x, −y+1, −z+1; (x) −x+1, −y+1, −z+2. |
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