Supporting information
Crystallographic Information File (CIF) https://doi.org/10.1107/S1600536807060023/cv2351sup1.cif | |
Structure factor file (CIF format) https://doi.org/10.1107/S1600536807060023/cv2351Isup2.hkl |
CCDC reference: 672764
Key indicators
- Single-crystal X-ray study
- T = 293 K
- Mean (C-C) = 0.009 Å
- R factor = 0.054
- wR factor = 0.152
- Data-to-parameter ratio = 29.2
checkCIF/PLATON results
No syntax errors found
Alert level B PLAT220_ALERT_2_B Large Non-Solvent C Ueq(max)/Ueq(min) ... 3.80 Ratio PLAT413_ALERT_2_B Short Inter XH3 .. XHn H10B .. H18E .. 2.08 Ang.
Alert level C SHFSU01_ALERT_2_C The absolute value of parameter shift to su ratio > 0.05 Absolute value of the parameter shift to su ratio given 0.078 Additional refinement cycles may be required. PLAT080_ALERT_2_C Maximum Shift/Error ............................ 0.08 PLAT094_ALERT_2_C Ratio of Maximum / Minimum Residual Density .... 2.31 PLAT220_ALERT_2_C Large Non-Solvent C Ueq(max)/Ueq(min) ... 3.19 Ratio PLAT220_ALERT_2_C Large Non-Solvent O Ueq(max)/Ueq(min) ... 2.90 Ratio PLAT222_ALERT_3_C Large Non-Solvent H Ueq(max)/Ueq(min) ... 3.70 Ratio PLAT222_ALERT_3_C Large Non-Solvent H Ueq(max)/Ueq(min) ... 3.65 Ratio PLAT342_ALERT_3_C Low Bond Precision on C-C Bonds (x 1000) Ang ... 9 PLAT601_ALERT_2_C Structure Contains Solvent Accessible VOIDS of . 31.00 A 3 PLAT720_ALERT_4_C Number of Unusual/Non-Standard Label(s) ........ 28
Alert level G REFLT03_ALERT_4_G Please check that the estimate of the number of Friedel pairs is correct. If it is not, please give the correct count in the _publ_section_exptl_refinement section of the submitted CIF. From the CIF: _diffrn_reflns_theta_max 32.50 From the CIF: _reflns_number_total 34763 Count of symmetry unique reflns 18940 Completeness (_total/calc) 183.54% TEST3: Check Friedels for noncentro structure Estimate of Friedel pairs measured 15823 Fraction of Friedel pairs measured 0.835 Are heavy atom types Z>Si present yes PLAT199_ALERT_1_G Check the Reported _cell_measurement_temperature 293 K PLAT200_ALERT_1_G Check the Reported _diffrn_ambient_temperature . 293 K
0 ALERT level A = In general: serious problem 2 ALERT level B = Potentially serious problem 10 ALERT level C = Check and explain 3 ALERT level G = General alerts; check 2 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 3 ALERT type 3 Indicator that the structure quality may be low 2 ALERT type 4 Improvement, methodology, query or suggestion 0 ALERT type 5 Informative message, check
For details of the pharmacological and biological properties of sulfonylamide derivatives, see: Kishino & Saito (1979); Xu & Angell (2000). For the structural analogues of phosphorylated sulfonylamides, see: Amirkhanov et al. (1996); Borzechowska et al. (2002); Burgi & Dunitz (1994); Malandrino et al. (1998); Pietraszkiewicz et al. (2002); Skopenko et al. (2004); Trush et al. (2001). For calculation of polyhedra of lanthanide anions, see: Porai-Koshits & Aslanov (1972). For the synthesis of the ligand, see: Kirsanov (1952); Kirsanov & Shevchenko (1954).
The synthesis of HL was carried out according to the method by Kirsanov (Kirsanov, 1952; Kirsanov & Shevchenko, 1954).
Nd(NO3)35H2O (0,42 g, 1 mmol) was dissolved in acetone (10 ml) and added to 10 ml of an acetone solution of NaL (1,48 g, 4 mmol). After 20 min the precipitate of NaNO3 was filtered off and i-PrOH (10 ml) was added to filtrate. The resulting clear solution was left at ambient temperature for crystallization in air. The crystals were separated by filtration after 48 h, washed with cool i–PrOH (10 ml) and finally dried in air. Yield: 85–90%. Analysis found: C 31.3, H 3.8, N 4.6, S 10.2%; C32H44N4NaNdO20P4S4 requires: C 31.4, H 3.6, N 4.6, S 10.5%; IR (KBr pellet, cm-1): 1240, 1060 (s, SO2) and 1170 (s, PO).
All H atoms were placed at calculated positions and treated as riding on their parent atoms [C—H = 0.93 and 0.96 Å, and Uiso(H) = 1.2 and 1.5Ueq(C)].
Data collection: CrysAlis CCD (Oxford Diffraction, 2006); cell refinement: CrysAlis RED (Oxford Diffraction, 2006); data reduction: CrysAlis RED (Oxford Diffraction, 2006); program(s) used to solve structure: SHELXS97 (Sheldrick, 1997); program(s) used to refine structure: SHELXL97 (Sheldrick, 1997); molecular graphics: ORTEP-3 (Farrugia, 1997); software used to prepare material for publication: WinGX (Farrugia, 1999).
[NaNd(C8H11NO5PS)4] | F(000) = 4952 |
Mr = 1224.10 | Dx = 1.659 Mg m−3 |
Orthorhombic, P212121 | Mo Kα radiation, λ = 0.71073 Å |
Hall symbol: P 2ac 2ab | Cell parameters from 18882 reflections |
a = 20.276 (2) Å | θ = 2.8–35.7° |
b = 21.9129 (9) Å | µ = 1.45 mm−1 |
c = 22.058 (2) Å | T = 293 K |
V = 9800.5 (14) Å3 | Prism, violet |
Z = 8 | 0.5 × 0.2 × 0.1 mm |
Oxford Diffraction Xcalibur-3 diffractometer | 34763 independent reflections |
Radiation source: Enhance (Mo) X-ray Source | 20694 reflections with I > 2σ(I) |
Graphite monochromator | Rint = 0.047 |
Detector resolution: 16.1827 pixels mm-1 | θmax = 32.5°, θmin = 2.6° |
ω–scans | h = −30→30 |
Absorption correction: multi-scan (Blessing, 1995) | k = −32→33 |
Tmin = 0.705, Tmax = 0.855 | l = −32→33 |
104650 measured reflections |
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)] = 0.054 | H-atom parameters constrained |
wR(F2) = 0.152 | w = 1/[σ2(Fo2) + (0.0935P)2] where P = (Fo2 + 2Fc2)/3 |
S = 0.90 | (Δ/σ)max = 0.078 |
34763 reflections | Δρmax = 4.50 e Å−3 |
1189 parameters | Δρmin = −1.95 e Å−3 |
0 restraints | Absolute structure: Flack (1983), 15958 Friedel pairs |
Primary atom site location: structure-invariant direct methods | Absolute structure parameter: −0.063 (8) |
[NaNd(C8H11NO5PS)4] | V = 9800.5 (14) Å3 |
Mr = 1224.10 | Z = 8 |
Orthorhombic, P212121 | Mo Kα radiation |
a = 20.276 (2) Å | µ = 1.45 mm−1 |
b = 21.9129 (9) Å | T = 293 K |
c = 22.058 (2) Å | 0.5 × 0.2 × 0.1 mm |
Oxford Diffraction Xcalibur-3 diffractometer | 34763 independent reflections |
Absorption correction: multi-scan (Blessing, 1995) | 20694 reflections with I > 2σ(I) |
Tmin = 0.705, Tmax = 0.855 | Rint = 0.047 |
104650 measured reflections |
R[F2 > 2σ(F2)] = 0.054 | H-atom parameters constrained |
wR(F2) = 0.152 | Δρmax = 4.50 e Å−3 |
S = 0.90 | Δρmin = −1.95 e Å−3 |
34763 reflections | Absolute structure: Flack (1983), 15958 Friedel pairs |
1189 parameters | Absolute structure parameter: −0.063 (8) |
0 restraints |
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 | ||
Na1A | 0.31989 (10) | −0.00395 (10) | 0.00630 (8) | 0.0228 (4) | |
Na1B | −0.25624 (12) | 0.05492 (10) | 0.24305 (9) | 0.0308 (5) | |
Nd1A | 0.248935 (14) | 0.043855 (11) | 0.255686 (10) | 0.01692 (5) | |
Nd1B | −0.242758 (13) | −0.001980 (12) | 0.493901 (11) | 0.01890 (6) | |
S1A | 0.30001 (6) | 0.12309 (6) | 0.11316 (6) | 0.0190 (2) | |
P1A | 0.38553 (7) | 0.14088 (6) | 0.21158 (6) | 0.0215 (3) | |
S4A | 0.32373 (7) | −0.05224 (6) | 0.13521 (6) | 0.0214 (3) | |
S2A | 0.19740 (6) | 0.12772 (6) | 0.39493 (6) | 0.0201 (2) | |
S3A | 0.17303 (6) | −0.04805 (6) | 0.37917 (5) | 0.0179 (2) | |
P3A | 0.30991 (6) | −0.04396 (7) | 0.38386 (6) | 0.0180 (2) | |
S3B | −0.15431 (7) | −0.01199 (7) | 0.34484 (6) | 0.0264 (3) | |
S1B | −0.33835 (7) | −0.07169 (6) | 0.62316 (6) | 0.0240 (3) | |
S4B | −0.14056 (7) | 0.00743 (8) | 0.63551 (7) | 0.0302 (3) | |
P2B | −0.37113 (7) | −0.04943 (7) | 0.38790 (6) | 0.0213 (3) | |
S2B | −0.33767 (7) | 0.07335 (6) | 0.36820 (6) | 0.0230 (3) | |
P2A | 0.11519 (7) | 0.14624 (7) | 0.29394 (6) | 0.0234 (3) | |
P4A | 0.18659 (7) | −0.04864 (7) | 0.13143 (6) | 0.0227 (3) | |
P1B | −0.36680 (7) | 0.05289 (7) | 0.60228 (6) | 0.0218 (3) | |
P3B | −0.12031 (7) | 0.09140 (7) | 0.41599 (7) | 0.0267 (3) | |
P4B | −0.10897 (8) | −0.09204 (8) | 0.55909 (7) | 0.0309 (3) | |
O14A | 0.17013 (17) | −0.01282 (17) | 0.32340 (16) | 0.0199 (7) | |
O19A | 0.32611 (19) | −0.01557 (18) | 0.19049 (17) | 0.0232 (8) | |
O1A | 0.25385 (18) | 0.09189 (15) | 0.15375 (13) | 0.0192 (6) | |
O4A | 0.33863 (18) | 0.11358 (17) | 0.25542 (17) | 0.0216 (8) | |
O9A | 0.24397 (19) | 0.09624 (14) | 0.35513 (14) | 0.0200 (6) | |
O13A | 0.35939 (18) | −0.01317 (19) | 0.42924 (17) | 0.0256 (8) | |
O11B | −0.15789 (19) | 0.06905 (18) | 0.46978 (18) | 0.0267 (8) | |
O16A | 0.18266 (18) | −0.02189 (19) | 0.19306 (16) | 0.0231 (8) | |
O6A | 0.16206 (18) | 0.11558 (18) | 0.25205 (18) | 0.0243 (8) | |
O20A | 0.3783 (2) | −0.04113 (19) | 0.09404 (18) | 0.0292 (9) | |
O1B | −0.32340 (17) | 0.05402 (17) | 0.54805 (16) | 0.0211 (7) | |
O11A | 0.31541 (18) | −0.01940 (17) | 0.32081 (16) | 0.0200 (8) | |
O4B | −0.29617 (19) | −0.07223 (17) | 0.56942 (17) | 0.0236 (8) | |
O17A | 0.1611 (2) | −0.11590 (19) | 0.1343 (2) | 0.0368 (11) | |
O5A | 0.30675 (19) | 0.09454 (17) | 0.05458 (16) | 0.0247 (8) | |
O2A | 0.45775 (18) | 0.11663 (19) | 0.22033 (18) | 0.0272 (8) | |
O15A | 0.11878 (18) | −0.03708 (18) | 0.42070 (16) | 0.0238 (8) | |
O19B | −0.18847 (19) | 0.02765 (19) | 0.59044 (17) | 0.0280 (9) | |
O18A | 0.1364 (2) | −0.01928 (19) | 0.08576 (19) | 0.0310 (9) | |
O6B | −0.32740 (18) | −0.05602 (17) | 0.44166 (16) | 0.0228 (8) | |
O9B | −0.29341 (18) | 0.07156 (17) | 0.42016 (17) | 0.0238 (8) | |
O10A | 0.1876 (2) | 0.09848 (18) | 0.45320 (17) | 0.0278 (8) | |
O10B | −0.3112 (2) | 0.10557 (19) | 0.31667 (18) | 0.0298 (9) | |
O8A | 0.04239 (19) | 0.12444 (19) | 0.28378 (18) | 0.0287 (9) | |
O3B | −0.4405 (2) | 0.0679 (2) | 0.5854 (2) | 0.0354 (10) | |
O2B | −0.3559 (2) | 0.10833 (18) | 0.64584 (18) | 0.0279 (9) | |
O14B | −0.19272 (17) | −0.03540 (17) | 0.39616 (16) | 0.0235 (8) | |
O16B | −0.16265 (19) | −0.07776 (19) | 0.51560 (17) | 0.0273 (8) | |
O8B | −0.3681 (2) | −0.10607 (18) | 0.34444 (18) | 0.0282 (9) | |
O3A | 0.3933 (2) | 0.21049 (19) | 0.2281 (2) | 0.0315 (9) | |
O12A | 0.3344 (2) | −0.11157 (17) | 0.38361 (17) | 0.0249 (8) | |
O7A | 0.1108 (2) | 0.2149 (2) | 0.2746 (2) | 0.0401 (11) | |
O15B | −0.1914 (2) | −0.0096 (2) | 0.28950 (18) | 0.0378 (10) | |
O5B | −0.3090 (2) | −0.1023 (2) | 0.67577 (18) | 0.0330 (10) | |
N3A | 0.2390 (2) | −0.03994 (18) | 0.41528 (16) | 0.0191 (8) | |
O20B | −0.1689 (2) | −0.0003 (2) | 0.6944 (2) | 0.0469 (13) | |
O7B | −0.44491 (19) | −0.0548 (2) | 0.41161 (19) | 0.0374 (10) | |
O13B | −0.0474 (2) | 0.1064 (2) | 0.4320 (2) | 0.0428 (12) | |
N2A | 0.1294 (2) | 0.1408 (2) | 0.3644 (2) | 0.0273 (10) | |
N1B | −0.3645 (2) | −0.0068 (2) | 0.6408 (2) | 0.0274 (10) | |
N1A | 0.3690 (2) | 0.1333 (2) | 0.1413 (2) | 0.0235 (9) | |
O12B | −0.1481 (3) | 0.1555 (2) | 0.3984 (2) | 0.0409 (11) | |
N4A | 0.2575 (2) | −0.04653 (19) | 0.09954 (17) | 0.0237 (8) | |
N3B | −0.1200 (2) | 0.0490 (2) | 0.3569 (2) | 0.0319 (11) | |
O18B | −0.1122 (3) | −0.1594 (2) | 0.5830 (2) | 0.0531 (14) | |
C27A | 0.3299 (3) | −0.1283 (2) | 0.1613 (2) | 0.0217 (10) | |
O17B | −0.0437 (2) | −0.0923 (3) | 0.5218 (3) | 0.0613 (16) | |
C3A | 0.2634 (3) | 0.1951 (2) | 0.1001 (2) | 0.0217 (10) | |
N2B | −0.3626 (2) | 0.0090 (2) | 0.3458 (2) | 0.0288 (11) | |
C11A | 0.2363 (3) | 0.1988 (2) | 0.4112 (2) | 0.0217 (10) | |
C1A | 0.4692 (3) | 0.0509 (3) | 0.2174 (3) | 0.0333 (13) | |
H1AA | 0.5153 | 0.0427 | 0.2231 | 0.050* | |
H1AB | 0.4557 | 0.0358 | 0.1784 | 0.050* | |
H1AC | 0.4442 | 0.0309 | 0.2485 | 0.050* | |
C5A | 0.2618 (4) | 0.2887 (3) | 0.0448 (3) | 0.0364 (15) | |
H5AA | 0.2803 | 0.3147 | 0.0162 | 0.044* | |
C19A | 0.1694 (2) | −0.1250 (2) | 0.3557 (2) | 0.0216 (10) | |
C11B | −0.4077 (3) | 0.1155 (3) | 0.3909 (3) | 0.0253 (11) | |
C10A | 0.0301 (3) | 0.0590 (3) | 0.2793 (3) | 0.0359 (14) | |
H10A | −0.0162 | 0.0520 | 0.2735 | 0.054* | |
H10B | 0.0443 | 0.0394 | 0.3160 | 0.054* | |
H10C | 0.0542 | 0.0426 | 0.2456 | 0.054* | |
C28A | 0.3402 (3) | −0.1406 (2) | 0.2219 (3) | 0.0288 (12) | |
H28A | 0.3433 | −0.1086 | 0.2493 | 0.035* | |
C16B | −0.4551 (3) | 0.1321 (3) | 0.3486 (3) | 0.0287 (12) | |
H16A | −0.4507 | 0.1205 | 0.3082 | 0.034* | |
C4B | −0.4504 (3) | −0.1362 (3) | 0.6504 (3) | 0.0290 (12) | |
H4BA | −0.4425 | −0.1257 | 0.6906 | 0.035* | |
C19B | −0.0907 (3) | −0.0650 (3) | 0.3314 (3) | 0.0290 (12) | |
C18A | 0.3639 (3) | 0.0523 (3) | 0.4349 (3) | 0.0374 (15) | |
H18A | 0.3966 | 0.0624 | 0.4646 | 0.056* | |
H18B | 0.3219 | 0.0683 | 0.4472 | 0.056* | |
H18C | 0.3760 | 0.0696 | 0.3965 | 0.056* | |
C8A | 0.2089 (3) | 0.2137 (3) | 0.1332 (3) | 0.0272 (11) | |
H8AA | 0.1921 | 0.1891 | 0.1639 | 0.033* | |
C10B | −0.3090 (3) | −0.1170 (3) | 0.3087 (3) | 0.0313 (13) | |
H10D | −0.3149 | −0.1530 | 0.2846 | 0.047* | |
H10E | −0.2720 | −0.1224 | 0.3353 | 0.047* | |
H10F | −0.3011 | −0.0826 | 0.2827 | 0.047* | |
C12A | 0.2913 (3) | 0.2162 (3) | 0.3778 (3) | 0.0271 (12) | |
H12A | 0.3067 | 0.1921 | 0.3461 | 0.033* | |
C15A | 0.2433 (3) | 0.2885 (2) | 0.4717 (3) | 0.0349 (13) | |
H15A | 0.2278 | 0.3129 | 0.5031 | 0.042* | |
C6A | 0.2065 (4) | 0.3067 (3) | 0.0757 (3) | 0.0412 (16) | |
H6AA | 0.1868 | 0.3440 | 0.0670 | 0.049* | |
C22A | 0.1722 (3) | −0.2462 (3) | 0.3219 (3) | 0.0363 (14) | |
H22A | 0.1734 | −0.2871 | 0.3106 | 0.044* | |
N4B | −0.1010 (3) | −0.0482 (3) | 0.6160 (3) | 0.0413 (14) | |
C14B | −0.5162 (3) | 0.1834 (3) | 0.4265 (3) | 0.0334 (13) | |
H14A | −0.5531 | 0.2058 | 0.4382 | 0.040* | |
C4A | 0.2902 (3) | 0.2331 (3) | 0.0553 (3) | 0.0329 (13) | |
H4AA | 0.3268 | 0.2207 | 0.0331 | 0.040* | |
C12B | −0.4146 (3) | 0.1326 (3) | 0.4511 (3) | 0.0325 (14) | |
H12B | −0.3832 | 0.1209 | 0.4796 | 0.039* | |
C5B | −0.5047 (3) | −0.1709 (3) | 0.6350 (3) | 0.0383 (15) | |
H5BA | −0.5330 | −0.1844 | 0.6653 | 0.046* | |
C8B | −0.4208 (3) | −0.1306 (3) | 0.5448 (3) | 0.0296 (12) | |
H8BA | −0.3933 | −0.1158 | 0.5144 | 0.036* | |
C16A | 0.2110 (3) | 0.2350 (3) | 0.4578 (3) | 0.0313 (13) | |
H16B | 0.1733 | 0.2233 | 0.4788 | 0.038* | |
C13B | −0.4696 (3) | 0.1681 (3) | 0.4689 (3) | 0.0377 (15) | |
H13A | −0.4741 | 0.1809 | 0.5089 | 0.045* | |
C26A | 0.1342 (3) | 0.0468 (3) | 0.0749 (3) | 0.0320 (13) | |
H26A | 0.1004 | 0.0558 | 0.0457 | 0.048* | |
H26B | 0.1761 | 0.0603 | 0.0597 | 0.048* | |
H26C | 0.1245 | 0.0675 | 0.1122 | 0.048* | |
C23A | 0.1806 (3) | −0.2011 (3) | 0.2791 (3) | 0.0362 (15) | |
H23A | 0.1877 | −0.2119 | 0.2388 | 0.043* | |
C14A | 0.2988 (3) | 0.3065 (3) | 0.4392 (3) | 0.0357 (14) | |
H14B | 0.3198 | 0.3430 | 0.4486 | 0.043* | |
C3B | −0.4077 (3) | −0.1171 (2) | 0.6048 (3) | 0.0260 (11) | |
C15B | −0.5092 (3) | 0.1662 (3) | 0.3672 (3) | 0.0361 (14) | |
H15B | −0.5410 | 0.1775 | 0.3390 | 0.043* | |
C20A | 0.1611 (3) | −0.1704 (3) | 0.3991 (3) | 0.0350 (14) | |
H20A | 0.1550 | −0.1601 | 0.4396 | 0.042* | |
C29B | −0.0171 (3) | 0.1440 (3) | 0.5958 (3) | 0.0423 (16) | |
H29A | −0.0028 | 0.1646 | 0.5613 | 0.051* | |
C24A | 0.1787 (3) | −0.1395 (3) | 0.2952 (3) | 0.0293 (12) | |
H24A | 0.1836 | −0.1091 | 0.2661 | 0.035* | |
C28B | −0.0614 (3) | 0.0964 (3) | 0.5904 (3) | 0.0345 (14) | |
H28B | −0.0765 | 0.0841 | 0.5525 | 0.041* | |
C24B | −0.0672 (3) | −0.0996 (3) | 0.3792 (3) | 0.0359 (14) | |
H24B | −0.0847 | −0.0948 | 0.4179 | 0.043* | |
C20B | −0.0647 (3) | −0.0707 (3) | 0.2736 (3) | 0.0397 (16) | |
H20B | −0.0807 | −0.0470 | 0.2418 | 0.048* | |
C31A | 0.3280 (4) | −0.2347 (3) | 0.1408 (4) | 0.049 (2) | |
H31A | 0.3238 | −0.2665 | 0.1132 | 0.059* | |
C13A | 0.3227 (3) | 0.2704 (3) | 0.3930 (3) | 0.0364 (15) | |
H13B | 0.3602 | 0.2824 | 0.3719 | 0.044* | |
C27B | −0.0828 (3) | 0.0675 (3) | 0.6423 (3) | 0.0288 (12) | |
C7B | −0.4749 (3) | −0.1661 (3) | 0.5300 (3) | 0.0377 (15) | |
H7BA | −0.4827 | −0.1767 | 0.4898 | 0.045* | |
C29A | 0.3460 (4) | −0.1999 (3) | 0.2423 (3) | 0.0385 (15) | |
H29B | 0.3547 | −0.2079 | 0.2829 | 0.046* | |
C31B | −0.0147 (4) | 0.1321 (3) | 0.7028 (4) | 0.0465 (19) | |
H31B | 0.0012 | 0.1442 | 0.7405 | 0.056* | |
C23B | −0.0174 (3) | −0.1412 (3) | 0.3685 (4) | 0.0488 (19) | |
H23B | −0.0013 | −0.1651 | 0.4001 | 0.059* | |
C6B | −0.5177 (3) | −0.1861 (3) | 0.5756 (3) | 0.0410 (16) | |
H6BA | −0.5546 | −0.2094 | 0.5659 | 0.049* | |
C21B | −0.0157 (4) | −0.1112 (4) | 0.2642 (4) | 0.054 (2) | |
H21A | 0.0022 | −0.1150 | 0.2255 | 0.064* | |
C1B | −0.2946 (4) | 0.1154 (3) | 0.6781 (3) | 0.0393 (16) | |
H1BA | −0.2964 | 0.1516 | 0.7025 | 0.059* | |
H1BB | −0.2590 | 0.1188 | 0.6496 | 0.059* | |
H1BC | −0.2875 | 0.0806 | 0.7036 | 0.059* | |
C17A | 0.3338 (4) | −0.1480 (3) | 0.4382 (3) | 0.0423 (16) | |
H17A | 0.3505 | −0.1880 | 0.4295 | 0.063* | |
H17B | 0.2894 | −0.1511 | 0.4531 | 0.063* | |
H17C | 0.3610 | −0.1289 | 0.4684 | 0.063* | |
C21A | 0.1621 (4) | −0.2304 (3) | 0.3814 (3) | 0.0409 (16) | |
H21B | 0.1557 | −0.2609 | 0.4102 | 0.049* | |
C30B | 0.0062 (4) | 0.1613 (3) | 0.6519 (4) | 0.0467 (18) | |
H30A | 0.0364 | 0.1931 | 0.6549 | 0.056* | |
C32B | −0.0603 (3) | 0.0837 (3) | 0.6986 (3) | 0.0359 (14) | |
H32A | −0.0747 | 0.0633 | 0.7331 | 0.043* | |
C30A | 0.3386 (3) | −0.2479 (3) | 0.2009 (3) | 0.0406 (16) | |
H30B | 0.3408 | −0.2882 | 0.2139 | 0.049* | |
C32A | 0.3235 (4) | −0.1758 (3) | 0.1210 (3) | 0.0436 (18) | |
H32B | 0.3162 | −0.1677 | 0.0802 | 0.052* | |
C7A | 0.1799 (3) | 0.2690 (3) | 0.1201 (3) | 0.0377 (15) | |
H7AA | 0.1423 | 0.2812 | 0.1411 | 0.045* | |
C18B | 0.0010 (4) | 0.0596 (4) | 0.4399 (4) | 0.057 (2) | |
H18D | 0.0426 | 0.0778 | 0.4501 | 0.085* | |
H18E | 0.0053 | 0.0368 | 0.4030 | 0.085* | |
H18F | −0.0125 | 0.0328 | 0.4720 | 0.085* | |
C2A | 0.4342 (4) | 0.2487 (4) | 0.1891 (4) | 0.056 (2) | |
H2AA | 0.4348 | 0.2896 | 0.2047 | 0.084* | |
H2AB | 0.4164 | 0.2488 | 0.1488 | 0.084* | |
H2AC | 0.4783 | 0.2328 | 0.1883 | 0.084* | |
C25A | 0.1546 (4) | −0.1524 (3) | 0.0805 (4) | 0.054 (2) | |
H25A | 0.1384 | −0.1921 | 0.0911 | 0.081* | |
H25B | 0.1969 | −0.1563 | 0.0612 | 0.081* | |
H25C | 0.1243 | −0.1332 | 0.0531 | 0.081* | |
C22B | 0.0087 (4) | −0.1475 (4) | 0.3104 (4) | 0.059 (3) | |
H22B | 0.0421 | −0.1755 | 0.3028 | 0.070* | |
C25B | 0.0208 (4) | −0.0957 (5) | 0.5471 (4) | 0.074 (3) | |
H25D | 0.0529 | −0.0950 | 0.5151 | 0.112* | |
H25E | 0.0252 | −0.1329 | 0.5697 | 0.112* | |
H25F | 0.0277 | −0.0615 | 0.5735 | 0.112* | |
C17B | −0.1336 (6) | 0.1828 (4) | 0.3428 (4) | 0.077 (3) | |
H17D | −0.1551 | 0.2218 | 0.3405 | 0.116* | |
H17E | −0.1489 | 0.1572 | 0.3105 | 0.116* | |
H17F | −0.0867 | 0.1883 | 0.3393 | 0.116* | |
C2B | −0.4780 (4) | 0.0260 (4) | 0.5525 (4) | 0.056 (2) | |
H2BA | −0.5215 | 0.0420 | 0.5463 | 0.084* | |
H2BB | −0.4808 | −0.0117 | 0.5746 | 0.084* | |
H2BC | −0.4574 | 0.0187 | 0.5140 | 0.084* | |
C9B | −0.4991 (3) | −0.0479 (4) | 0.3695 (3) | 0.059 (2) | |
H9BA | −0.5401 | −0.0526 | 0.3907 | 0.088* | |
H9BB | −0.4958 | −0.0785 | 0.3385 | 0.088* | |
H9BC | −0.4972 | −0.0082 | 0.3513 | 0.088* | |
C9A | 0.0787 (6) | 0.2570 (4) | 0.3137 (5) | 0.081 (3) | |
H9AA | 0.0798 | 0.2970 | 0.2959 | 0.122* | |
H9AB | 0.1009 | 0.2578 | 0.3522 | 0.122* | |
H9AC | 0.0337 | 0.2447 | 0.3195 | 0.122* | |
C26B | −0.1582 (6) | −0.1736 (4) | 0.6266 (5) | 0.082 (3) | |
H26D | −0.1546 | −0.2160 | 0.6370 | 0.124* | |
H26E | −0.2017 | −0.1655 | 0.6111 | 0.124* | |
H26F | −0.1506 | −0.1491 | 0.6620 | 0.124* |
U11 | U22 | U33 | U12 | U13 | U23 | |
Na1A | 0.0243 (9) | 0.0283 (12) | 0.0158 (9) | −0.0001 (9) | −0.0007 (7) | −0.0010 (8) |
Na1B | 0.0395 (14) | 0.0298 (11) | 0.0232 (10) | 0.0019 (11) | 0.0037 (11) | 0.0036 (8) |
Nd1A | 0.01981 (12) | 0.01566 (10) | 0.01529 (10) | 0.00057 (13) | −0.00040 (10) | 0.00040 (8) |
Nd1B | 0.01793 (11) | 0.02086 (12) | 0.01791 (11) | 0.00030 (13) | −0.00023 (9) | 0.00121 (8) |
S1A | 0.0194 (6) | 0.0183 (6) | 0.0194 (6) | −0.0004 (4) | 0.0011 (4) | 0.0012 (4) |
P1A | 0.0164 (6) | 0.0216 (7) | 0.0266 (7) | −0.0012 (5) | −0.0009 (5) | −0.0012 (5) |
S4A | 0.0295 (7) | 0.0220 (7) | 0.0127 (6) | 0.0062 (5) | −0.0012 (5) | −0.0016 (5) |
S2A | 0.0222 (6) | 0.0169 (6) | 0.0212 (6) | −0.0008 (5) | 0.0022 (5) | −0.0009 (4) |
S3A | 0.0184 (5) | 0.0189 (6) | 0.0162 (6) | −0.0003 (5) | 0.0009 (4) | 0.0017 (4) |
P3A | 0.0190 (6) | 0.0192 (7) | 0.0158 (6) | −0.0003 (5) | −0.0039 (4) | 0.0019 (5) |
S3B | 0.0278 (7) | 0.0296 (8) | 0.0217 (6) | 0.0046 (6) | 0.0070 (5) | 0.0010 (5) |
S1B | 0.0250 (7) | 0.0231 (7) | 0.0240 (6) | −0.0016 (5) | 0.0005 (5) | 0.0030 (5) |
S4B | 0.0313 (7) | 0.0356 (9) | 0.0237 (7) | −0.0061 (6) | −0.0101 (5) | 0.0024 (6) |
P2B | 0.0193 (6) | 0.0244 (7) | 0.0201 (6) | 0.0005 (5) | −0.0003 (5) | −0.0015 (5) |
S2B | 0.0232 (6) | 0.0246 (7) | 0.0211 (6) | 0.0044 (5) | 0.0011 (5) | 0.0032 (5) |
P2A | 0.0208 (7) | 0.0223 (7) | 0.0271 (7) | 0.0023 (5) | 0.0009 (5) | 0.0013 (5) |
P4A | 0.0296 (7) | 0.0180 (7) | 0.0204 (7) | −0.0020 (6) | −0.0095 (5) | −0.0009 (5) |
P1B | 0.0231 (6) | 0.0227 (7) | 0.0197 (6) | −0.0007 (5) | 0.0014 (5) | −0.0008 (5) |
P3B | 0.0265 (7) | 0.0220 (7) | 0.0317 (8) | −0.0015 (6) | 0.0071 (6) | 0.0012 (6) |
P4B | 0.0303 (8) | 0.0278 (8) | 0.0345 (8) | 0.0043 (6) | −0.0126 (6) | 0.0018 (6) |
O14A | 0.0217 (17) | 0.0210 (19) | 0.0170 (17) | −0.0005 (14) | −0.0011 (13) | 0.0002 (13) |
O19A | 0.032 (2) | 0.020 (2) | 0.0180 (18) | 0.0054 (15) | −0.0031 (15) | −0.0028 (14) |
O1A | 0.0192 (16) | 0.0197 (15) | 0.0186 (14) | −0.0012 (15) | 0.0003 (14) | 0.0026 (11) |
O4A | 0.0204 (18) | 0.024 (2) | 0.0200 (19) | −0.0017 (15) | 0.0007 (14) | −0.0025 (15) |
O9A | 0.0246 (18) | 0.0167 (15) | 0.0188 (15) | 0.0005 (15) | 0.0009 (15) | −0.0023 (11) |
O13A | 0.0244 (19) | 0.031 (2) | 0.0210 (18) | −0.0012 (16) | −0.0009 (14) | 0.0009 (15) |
O11B | 0.0185 (18) | 0.028 (2) | 0.033 (2) | −0.0061 (15) | 0.0044 (16) | −0.0012 (16) |
O16A | 0.0248 (19) | 0.029 (2) | 0.0149 (18) | −0.0106 (15) | −0.0038 (14) | 0.0026 (14) |
O6A | 0.0214 (19) | 0.029 (2) | 0.022 (2) | 0.0060 (16) | 0.0022 (15) | −0.0015 (16) |
O20A | 0.035 (2) | 0.029 (2) | 0.023 (2) | 0.0047 (18) | −0.0038 (16) | −0.0033 (17) |
O1B | 0.0202 (18) | 0.022 (2) | 0.0208 (17) | 0.0022 (14) | 0.0038 (13) | 0.0037 (14) |
O11A | 0.0247 (19) | 0.0212 (19) | 0.0140 (17) | 0.0044 (14) | −0.0011 (13) | −0.0022 (13) |
O4B | 0.0250 (19) | 0.019 (2) | 0.0265 (19) | −0.0013 (15) | 0.0000 (15) | 0.0005 (14) |
O17A | 0.047 (3) | 0.025 (2) | 0.039 (2) | −0.0103 (19) | −0.024 (2) | 0.0026 (18) |
O5A | 0.035 (2) | 0.0194 (19) | 0.0201 (18) | 0.0003 (16) | 0.0030 (15) | 0.0005 (14) |
O2A | 0.0197 (19) | 0.033 (2) | 0.028 (2) | 0.0021 (16) | −0.0037 (15) | −0.0018 (16) |
O15A | 0.0197 (18) | 0.032 (2) | 0.0196 (18) | −0.0009 (16) | −0.0003 (14) | 0.0020 (15) |
O19B | 0.027 (2) | 0.033 (2) | 0.024 (2) | −0.0045 (16) | −0.0024 (15) | −0.0064 (16) |
O18A | 0.031 (2) | 0.030 (2) | 0.032 (2) | −0.0028 (17) | −0.0101 (17) | −0.0022 (17) |
O6B | 0.0240 (19) | 0.024 (2) | 0.0203 (18) | −0.0038 (15) | −0.0058 (14) | 0.0044 (14) |
O9B | 0.0230 (19) | 0.027 (2) | 0.0218 (18) | 0.0053 (15) | −0.0007 (14) | 0.0051 (14) |
O10A | 0.036 (2) | 0.023 (2) | 0.025 (2) | −0.0008 (16) | 0.0050 (16) | 0.0020 (15) |
O10B | 0.033 (2) | 0.031 (2) | 0.026 (2) | 0.0048 (17) | 0.0066 (17) | 0.0028 (16) |
O8A | 0.023 (2) | 0.030 (2) | 0.033 (2) | 0.0032 (16) | −0.0007 (16) | −0.0072 (17) |
O3B | 0.021 (2) | 0.051 (3) | 0.034 (2) | 0.0014 (19) | −0.0024 (17) | 0.001 (2) |
O2B | 0.035 (2) | 0.021 (2) | 0.028 (2) | 0.0017 (16) | −0.0006 (17) | −0.0056 (15) |
O14B | 0.0210 (18) | 0.027 (2) | 0.0228 (18) | −0.0009 (15) | 0.0044 (14) | 0.0024 (14) |
O16B | 0.0220 (19) | 0.036 (2) | 0.0239 (19) | 0.0060 (16) | −0.0058 (15) | −0.0004 (16) |
O8B | 0.029 (2) | 0.030 (2) | 0.026 (2) | −0.0052 (17) | 0.0045 (16) | −0.0059 (16) |
O3A | 0.031 (2) | 0.024 (2) | 0.040 (2) | −0.0060 (17) | 0.0005 (18) | −0.0051 (17) |
O12A | 0.030 (2) | 0.019 (2) | 0.026 (2) | 0.0063 (15) | −0.0027 (16) | 0.0041 (14) |
O7A | 0.049 (3) | 0.025 (2) | 0.045 (3) | 0.014 (2) | 0.001 (2) | 0.0001 (19) |
O15B | 0.040 (2) | 0.047 (3) | 0.026 (2) | 0.014 (2) | −0.0010 (17) | 0.0037 (19) |
O5B | 0.041 (3) | 0.033 (2) | 0.024 (2) | −0.0029 (19) | −0.0086 (18) | 0.0045 (16) |
N3A | 0.023 (2) | 0.022 (2) | 0.0128 (16) | −0.0041 (17) | −0.0023 (14) | 0.0004 (13) |
O20B | 0.049 (3) | 0.060 (3) | 0.032 (2) | −0.023 (3) | −0.007 (2) | 0.005 (2) |
O7B | 0.0184 (19) | 0.065 (3) | 0.028 (2) | 0.001 (2) | 0.0006 (16) | 0.001 (2) |
O13B | 0.031 (2) | 0.053 (3) | 0.044 (3) | −0.009 (2) | 0.003 (2) | 0.003 (2) |
N2A | 0.017 (2) | 0.029 (3) | 0.036 (3) | 0.0019 (18) | 0.0028 (18) | −0.007 (2) |
N1B | 0.036 (3) | 0.027 (3) | 0.019 (2) | 0.001 (2) | 0.0051 (18) | −0.0023 (18) |
N1A | 0.022 (2) | 0.023 (2) | 0.026 (2) | 0.0012 (17) | 0.0002 (17) | 0.0048 (17) |
O12B | 0.060 (3) | 0.032 (3) | 0.031 (2) | 0.006 (2) | −0.001 (2) | 0.0081 (18) |
N4A | 0.030 (2) | 0.025 (2) | 0.0164 (17) | 0.005 (2) | −0.0042 (17) | −0.0014 (14) |
N3B | 0.031 (3) | 0.027 (3) | 0.038 (3) | −0.001 (2) | 0.019 (2) | 0.004 (2) |
O18B | 0.092 (4) | 0.035 (3) | 0.032 (3) | 0.014 (3) | −0.015 (3) | 0.001 (2) |
C27A | 0.023 (3) | 0.018 (3) | 0.025 (3) | 0.0087 (19) | −0.0057 (19) | −0.0061 (19) |
O17B | 0.030 (3) | 0.098 (5) | 0.055 (3) | 0.010 (3) | −0.010 (2) | 0.007 (3) |
C3A | 0.026 (3) | 0.013 (2) | 0.027 (2) | 0.0000 (18) | −0.005 (2) | −0.0001 (16) |
N2B | 0.040 (3) | 0.030 (3) | 0.016 (2) | 0.001 (2) | −0.0113 (18) | 0.0001 (18) |
C11A | 0.024 (3) | 0.016 (2) | 0.025 (2) | 0.0031 (19) | −0.0043 (19) | 0.0003 (17) |
C1A | 0.026 (3) | 0.037 (4) | 0.037 (3) | 0.010 (2) | −0.010 (2) | 0.003 (3) |
C5A | 0.061 (4) | 0.019 (3) | 0.030 (3) | 0.002 (3) | 0.005 (3) | 0.010 (2) |
C19A | 0.017 (2) | 0.019 (3) | 0.028 (3) | −0.0076 (19) | −0.0051 (19) | 0.0024 (19) |
C11B | 0.021 (3) | 0.026 (3) | 0.030 (3) | 0.005 (2) | 0.001 (2) | 0.001 (2) |
C10A | 0.032 (3) | 0.031 (3) | 0.045 (4) | −0.005 (3) | 0.001 (3) | 0.001 (3) |
C28A | 0.042 (3) | 0.017 (3) | 0.027 (3) | 0.005 (2) | 0.014 (2) | 0.001 (2) |
C16B | 0.034 (3) | 0.023 (3) | 0.029 (3) | 0.003 (2) | −0.006 (2) | 0.003 (2) |
C4B | 0.028 (3) | 0.029 (3) | 0.030 (3) | 0.002 (2) | 0.003 (2) | −0.001 (2) |
C19B | 0.015 (2) | 0.032 (3) | 0.040 (3) | 0.000 (2) | −0.003 (2) | −0.009 (2) |
C18A | 0.040 (4) | 0.035 (4) | 0.038 (3) | −0.006 (3) | −0.013 (3) | 0.001 (3) |
C8A | 0.025 (3) | 0.025 (3) | 0.032 (3) | 0.003 (2) | 0.002 (2) | 0.005 (2) |
C10B | 0.029 (3) | 0.041 (4) | 0.024 (3) | 0.005 (3) | 0.009 (2) | −0.004 (2) |
C12A | 0.026 (3) | 0.022 (3) | 0.033 (3) | 0.005 (2) | −0.002 (2) | −0.005 (2) |
C15A | 0.046 (4) | 0.022 (3) | 0.036 (3) | 0.003 (3) | 0.001 (3) | −0.011 (2) |
C6A | 0.058 (5) | 0.022 (3) | 0.043 (4) | 0.005 (3) | −0.014 (3) | 0.001 (3) |
C22A | 0.045 (4) | 0.013 (3) | 0.051 (4) | 0.000 (2) | 0.002 (3) | −0.005 (2) |
N4B | 0.042 (3) | 0.028 (3) | 0.054 (4) | 0.003 (2) | −0.025 (3) | 0.000 (2) |
C14B | 0.026 (3) | 0.035 (4) | 0.038 (3) | 0.007 (2) | 0.003 (2) | 0.003 (3) |
C4A | 0.046 (4) | 0.028 (3) | 0.024 (3) | −0.006 (3) | 0.007 (3) | 0.004 (2) |
C12B | 0.034 (3) | 0.037 (4) | 0.026 (3) | 0.016 (3) | −0.004 (2) | 0.004 (2) |
C5B | 0.035 (3) | 0.037 (4) | 0.043 (4) | −0.005 (3) | 0.011 (3) | 0.007 (3) |
C8B | 0.030 (3) | 0.029 (3) | 0.030 (3) | −0.010 (2) | −0.003 (2) | 0.008 (2) |
C16A | 0.041 (3) | 0.025 (3) | 0.027 (3) | −0.006 (2) | 0.008 (2) | 0.000 (2) |
C13B | 0.035 (3) | 0.044 (4) | 0.034 (3) | 0.015 (3) | 0.002 (3) | 0.000 (3) |
C26A | 0.026 (3) | 0.033 (3) | 0.037 (3) | 0.004 (2) | −0.006 (2) | 0.003 (3) |
C23A | 0.047 (4) | 0.022 (3) | 0.039 (4) | −0.002 (3) | 0.011 (3) | −0.009 (2) |
C14A | 0.044 (4) | 0.023 (3) | 0.040 (4) | −0.014 (3) | −0.002 (3) | −0.004 (2) |
C3B | 0.028 (3) | 0.016 (3) | 0.033 (3) | −0.001 (2) | 0.000 (2) | 0.002 (2) |
C15B | 0.030 (3) | 0.036 (4) | 0.042 (4) | 0.008 (3) | −0.009 (3) | 0.001 (3) |
C20A | 0.053 (4) | 0.024 (3) | 0.028 (3) | −0.006 (3) | −0.005 (3) | 0.001 (2) |
C29B | 0.030 (3) | 0.041 (4) | 0.056 (4) | −0.004 (3) | −0.009 (3) | 0.006 (3) |
C24A | 0.041 (3) | 0.024 (3) | 0.023 (3) | −0.009 (2) | 0.010 (2) | −0.001 (2) |
C28B | 0.024 (3) | 0.045 (4) | 0.035 (3) | 0.001 (3) | −0.011 (2) | 0.008 (3) |
C24B | 0.019 (3) | 0.033 (4) | 0.056 (4) | −0.002 (2) | 0.006 (3) | 0.004 (3) |
C20B | 0.038 (4) | 0.047 (4) | 0.035 (3) | −0.005 (3) | 0.005 (3) | −0.023 (3) |
C31A | 0.053 (4) | 0.017 (3) | 0.077 (6) | 0.006 (3) | −0.023 (4) | −0.014 (3) |
C13A | 0.026 (3) | 0.027 (3) | 0.057 (4) | −0.008 (2) | 0.009 (3) | −0.010 (3) |
C27B | 0.022 (3) | 0.029 (3) | 0.035 (3) | 0.004 (2) | −0.003 (2) | −0.008 (2) |
C7B | 0.031 (3) | 0.050 (4) | 0.032 (3) | −0.009 (3) | 0.001 (3) | 0.003 (3) |
C29A | 0.052 (4) | 0.030 (3) | 0.034 (3) | 0.007 (3) | 0.007 (3) | 0.012 (2) |
C31B | 0.044 (4) | 0.042 (4) | 0.053 (5) | 0.006 (3) | −0.011 (3) | −0.023 (3) |
C23B | 0.027 (3) | 0.035 (4) | 0.084 (6) | −0.004 (3) | −0.015 (4) | 0.008 (4) |
C6B | 0.029 (3) | 0.040 (4) | 0.053 (4) | −0.011 (3) | −0.002 (3) | 0.001 (3) |
C21B | 0.032 (4) | 0.066 (6) | 0.063 (5) | −0.003 (3) | 0.005 (3) | −0.034 (4) |
C1B | 0.057 (4) | 0.022 (3) | 0.039 (4) | −0.005 (3) | −0.009 (3) | −0.001 (2) |
C17A | 0.054 (4) | 0.034 (4) | 0.038 (4) | 0.009 (3) | 0.001 (3) | 0.010 (3) |
C21A | 0.053 (4) | 0.018 (3) | 0.052 (4) | −0.007 (3) | −0.005 (3) | 0.011 (3) |
C30B | 0.035 (4) | 0.040 (4) | 0.066 (5) | −0.003 (3) | −0.010 (3) | −0.005 (3) |
C32B | 0.026 (3) | 0.043 (4) | 0.038 (3) | 0.006 (3) | −0.004 (2) | −0.021 (3) |
C30A | 0.040 (4) | 0.018 (3) | 0.064 (5) | −0.002 (3) | 0.004 (3) | 0.002 (3) |
C32A | 0.062 (5) | 0.028 (3) | 0.041 (4) | 0.013 (3) | −0.019 (3) | −0.018 (3) |
C7A | 0.033 (3) | 0.030 (4) | 0.050 (4) | 0.011 (3) | 0.007 (3) | 0.004 (3) |
C18B | 0.040 (4) | 0.079 (6) | 0.051 (5) | 0.012 (4) | 0.004 (3) | 0.022 (4) |
C2A | 0.073 (6) | 0.037 (4) | 0.057 (5) | −0.021 (4) | 0.007 (4) | 0.000 (3) |
C25A | 0.076 (6) | 0.033 (4) | 0.053 (5) | −0.004 (4) | −0.027 (4) | −0.002 (3) |
C22B | 0.028 (4) | 0.048 (5) | 0.100 (7) | 0.006 (3) | −0.004 (4) | −0.040 (5) |
C25B | 0.039 (5) | 0.131 (10) | 0.053 (5) | −0.008 (5) | −0.015 (4) | 0.008 (6) |
C17B | 0.147 (10) | 0.043 (5) | 0.040 (5) | 0.019 (6) | 0.002 (5) | 0.011 (4) |
C2B | 0.031 (4) | 0.050 (5) | 0.087 (6) | −0.004 (3) | −0.007 (4) | 0.003 (4) |
C9B | 0.024 (3) | 0.103 (7) | 0.049 (5) | 0.005 (4) | −0.004 (3) | −0.009 (5) |
C9A | 0.120 (10) | 0.028 (5) | 0.096 (8) | 0.010 (5) | −0.012 (7) | −0.006 (4) |
C26B | 0.119 (9) | 0.044 (6) | 0.084 (8) | −0.013 (6) | 0.017 (7) | 0.006 (5) |
Na1A—O10Ai | 2.385 (4) | C19A—C24A | 1.385 (8) |
Na1A—O20A | 2.411 (4) | C19A—C20A | 1.390 (8) |
Na1A—O5A | 2.421 (4) | C11B—C12B | 1.388 (8) |
Na1A—O15Ai | 2.433 (4) | C11B—C16B | 1.388 (7) |
Na1A—N3Ai | 2.526 (4) | C10A—H10A | 0.9600 |
Na1A—N4A | 2.589 (5) | C10A—H10B | 0.9600 |
Na1B—O15B | 2.186 (5) | C10A—H10C | 0.9600 |
Na1B—O20Bii | 2.211 (5) | C28A—C29A | 1.379 (8) |
Na1B—O5Bii | 2.242 (5) | C28A—H28A | 0.9300 |
Na1B—O10B | 2.261 (4) | C16B—C15B | 1.389 (8) |
Nd1A—O6A | 2.362 (4) | C16B—H16A | 0.9300 |
Nd1A—O4A | 2.375 (4) | C4B—C5B | 1.381 (9) |
Nd1A—O16A | 2.406 (4) | C4B—C3B | 1.391 (8) |
Nd1A—O11A | 2.409 (4) | C4B—H4BA | 0.9300 |
Nd1A—O9A | 2.478 (3) | C19B—C24B | 1.383 (9) |
Nd1A—O1A | 2.485 (3) | C19B—C20B | 1.386 (8) |
Nd1A—O19A | 2.492 (4) | C18A—H18A | 0.9600 |
Nd1A—O14A | 2.515 (4) | C18A—H18B | 0.9600 |
Nd1B—O1B | 2.368 (4) | C18A—H18C | 0.9600 |
Nd1B—O16B | 2.372 (4) | C8A—C7A | 1.379 (8) |
Nd1B—O11B | 2.380 (4) | C8A—H8AA | 0.9300 |
Nd1B—O6B | 2.382 (4) | C10B—H10D | 0.9600 |
Nd1B—O19B | 2.484 (4) | C10B—H10E | 0.9600 |
Nd1B—O14B | 2.493 (4) | C10B—H10F | 0.9600 |
Nd1B—O4B | 2.513 (4) | C12A—C13A | 1.388 (8) |
Nd1B—O9B | 2.509 (4) | C12A—H12A | 0.9300 |
S1A—O5A | 1.442 (4) | C15A—C16A | 1.378 (8) |
S1A—O1A | 1.465 (3) | C15A—C14A | 1.391 (9) |
S1A—N1A | 1.547 (5) | C15A—H15A | 0.9300 |
S1A—C3A | 1.767 (5) | C6A—C7A | 1.391 (9) |
P1A—O4A | 1.482 (4) | C6A—H6AA | 0.9300 |
P1A—O2A | 1.570 (4) | C22A—C21A | 1.372 (10) |
P1A—O3A | 1.576 (4) | C22A—C23A | 1.378 (9) |
P1A—N1A | 1.595 (5) | C22A—H22A | 0.9300 |
S4A—O20A | 1.452 (4) | C14B—C15B | 1.369 (9) |
S4A—O19A | 1.461 (4) | C14B—C13B | 1.372 (9) |
S4A—N4A | 1.561 (4) | C14B—H14A | 0.9300 |
S4A—C27A | 1.769 (5) | C4A—H4AA | 0.9300 |
S2A—O10A | 1.450 (4) | C12B—C13B | 1.416 (8) |
S2A—O9A | 1.462 (4) | C12B—H12B | 0.9300 |
S2A—N2A | 1.561 (5) | C5B—C6B | 1.376 (10) |
S2A—C11A | 1.783 (5) | C5B—H5BA | 0.9300 |
S3A—O15A | 1.452 (4) | C8B—C3B | 1.382 (8) |
S3A—O14A | 1.453 (4) | C8B—C7B | 1.384 (8) |
S3A—N3A | 1.566 (4) | C8B—H8BA | 0.9300 |
S3A—C19A | 1.766 (5) | C16A—H16B | 0.9300 |
S3A—Na1Aiii | 3.030 (2) | C13B—H13A | 0.9300 |
P3A—O11A | 1.495 (4) | C26A—H26A | 0.9600 |
P3A—O12A | 1.563 (4) | C26A—H26B | 0.9600 |
P3A—O13A | 1.570 (4) | C26A—H26C | 0.9600 |
P3A—N3A | 1.599 (4) | C23A—C24A | 1.397 (8) |
S3B—O15B | 1.435 (4) | C23A—H23A | 0.9300 |
S3B—O14B | 1.467 (4) | C14A—C13A | 1.378 (9) |
S3B—N3B | 1.530 (5) | C14A—H14B | 0.9300 |
S3B—C19B | 1.761 (6) | C15B—H15B | 0.9300 |
S1B—O4B | 1.462 (4) | C20A—C21A | 1.373 (8) |
S1B—O5B | 1.467 (4) | C20A—H20A | 0.9300 |
S1B—N1B | 1.567 (5) | C29B—C30B | 1.376 (10) |
S1B—C3B | 1.770 (6) | C29B—C28B | 1.383 (9) |
S1B—Na1Biv | 3.287 (2) | C29B—H29A | 0.9300 |
S4B—O20B | 1.431 (5) | C24A—H24A | 0.9300 |
S4B—O19B | 1.459 (4) | C28B—C27B | 1.379 (9) |
S4B—N4B | 1.521 (6) | C28B—H28B | 0.9300 |
S4B—C27B | 1.769 (6) | C24B—C23B | 1.382 (9) |
P2B—O6B | 1.488 (4) | C24B—H24B | 0.9300 |
P2B—O8B | 1.570 (4) | C20B—C21B | 1.348 (10) |
P2B—O7B | 1.589 (4) | C20B—H20B | 0.9300 |
P2B—N2B | 1.591 (5) | C31A—C32A | 1.367 (9) |
S2B—O10B | 1.442 (4) | C31A—C30A | 1.372 (11) |
S2B—O9B | 1.456 (4) | C31A—H31A | 0.9300 |
S2B—N2B | 1.578 (5) | C13A—H13B | 0.9300 |
S2B—C11B | 1.767 (5) | C27B—C32B | 1.369 (8) |
P2A—O6A | 1.486 (4) | C7B—C6B | 1.399 (9) |
P2A—O7A | 1.565 (5) | C7B—H7BA | 0.9300 |
P2A—O8A | 1.567 (4) | C29A—C30A | 1.400 (9) |
P2A—N2A | 1.584 (5) | C29A—H29B | 0.9300 |
P4A—O16A | 1.483 (4) | C31B—C30B | 1.361 (11) |
P4A—O17A | 1.564 (4) | C31B—C32B | 1.411 (10) |
P4A—O18A | 1.569 (4) | C31B—H31B | 0.9300 |
P4A—N4A | 1.601 (5) | C23B—C22B | 1.394 (12) |
P1B—O1B | 1.485 (4) | C23B—H23B | 0.9300 |
P1B—N1B | 1.560 (5) | C6B—H6BA | 0.9300 |
P1B—O2B | 1.565 (4) | C21B—C22B | 1.384 (12) |
P1B—O3B | 1.574 (4) | C21B—H21A | 0.9300 |
P3B—O11B | 1.493 (4) | C1B—H1BA | 0.9600 |
P3B—O13B | 1.555 (5) | C1B—H1BB | 0.9600 |
P3B—O12B | 1.562 (5) | C1B—H1BC | 0.9600 |
P3B—N3B | 1.600 (5) | C17A—H17A | 0.9600 |
P4B—O16B | 1.484 (4) | C17A—H17B | 0.9600 |
P4B—O17B | 1.559 (6) | C17A—H17C | 0.9600 |
P4B—O18B | 1.570 (5) | C21A—H21B | 0.9300 |
P4B—N4B | 1.589 (6) | C30B—H30A | 0.9300 |
O13A—C18A | 1.442 (8) | C32B—H32A | 0.9300 |
O17A—C25A | 1.438 (8) | C30A—H30B | 0.9300 |
O2A—C1A | 1.461 (7) | C32A—H32B | 0.9300 |
O15A—Na1Aiii | 2.433 (4) | C7A—H7AA | 0.9300 |
O18A—C26A | 1.469 (7) | C18B—H18D | 0.9600 |
O10A—Na1Aiii | 2.385 (4) | C18B—H18E | 0.9600 |
O8A—C10A | 1.458 (7) | C18B—H18F | 0.9600 |
O3B—C2B | 1.396 (8) | C2A—H2AA | 0.9600 |
O2B—C1B | 1.440 (8) | C2A—H2AB | 0.9600 |
O8B—C10B | 1.454 (6) | C2A—H2AC | 0.9600 |
O3A—C2A | 1.457 (8) | C25A—H25A | 0.9600 |
O12A—C17A | 1.445 (7) | C25A—H25B | 0.9600 |
O7A—C9A | 1.422 (10) | C25A—H25C | 0.9600 |
O5B—Na1Biv | 2.242 (5) | C22B—H22B | 0.9300 |
N3A—Na1Aiii | 2.526 (4) | C25B—H25D | 0.9600 |
O20B—Na1Biv | 2.211 (5) | C25B—H25E | 0.9600 |
O7B—C9B | 1.446 (8) | C25B—H25F | 0.9600 |
O13B—C18B | 1.429 (9) | C17B—H17D | 0.9600 |
O12B—C17B | 1.396 (9) | C17B—H17E | 0.9600 |
O18B—C26B | 1.375 (11) | C17B—H17F | 0.9600 |
C27A—C32A | 1.373 (7) | C2B—H2BA | 0.9600 |
C27A—C28A | 1.379 (8) | C2B—H2BB | 0.9600 |
O17B—C25B | 1.422 (9) | C2B—H2BC | 0.9600 |
C3A—C8A | 1.385 (7) | C9B—H9BA | 0.9600 |
C3A—C4A | 1.403 (7) | C9B—H9BB | 0.9600 |
C11A—C12A | 1.390 (8) | C9B—H9BC | 0.9600 |
C11A—C16A | 1.395 (7) | C9A—H9AA | 0.9600 |
C1A—H1AA | 0.9600 | C9A—H9AB | 0.9600 |
C1A—H1AB | 0.9600 | C9A—H9AC | 0.9600 |
C1A—H1AC | 0.9600 | C26B—H26D | 0.9600 |
C5A—C4A | 1.367 (8) | C26B—H26E | 0.9600 |
C5A—C6A | 1.369 (10) | C26B—H26F | 0.9600 |
C5A—H5AA | 0.9300 | ||
O10Ai—Na1A—O20A | 97.60 (16) | C28A—C27A—S4A | 120.7 (4) |
O10Ai—Na1A—O5A | 169.50 (17) | C25B—O17B—P4B | 125.0 (5) |
O20A—Na1A—O5A | 90.13 (15) | C8A—C3A—C4A | 120.4 (5) |
O10Ai—Na1A—O15Ai | 88.43 (15) | C8A—C3A—S1A | 120.8 (4) |
O20A—Na1A—O15Ai | 119.79 (16) | C4A—C3A—S1A | 118.8 (4) |
O5A—Na1A—O15Ai | 93.91 (15) | S2B—N2B—P2B | 124.9 (3) |
O10Ai—Na1A—N3Ai | 84.84 (14) | C12A—C11A—C16A | 122.0 (5) |
O20A—Na1A—N3Ai | 177.28 (17) | C12A—C11A—S2A | 119.2 (4) |
O5A—Na1A—N3Ai | 87.60 (14) | C16A—C11A—S2A | 118.8 (4) |
O15Ai—Na1A—N3Ai | 58.92 (13) | O2A—C1A—H1AA | 109.5 |
O10Ai—Na1A—N4A | 92.63 (15) | O2A—C1A—H1AB | 109.5 |
O20A—Na1A—N4A | 58.69 (15) | H1AA—C1A—H1AB | 109.5 |
O5A—Na1A—N4A | 85.30 (14) | O2A—C1A—H1AC | 109.5 |
O15Ai—Na1A—N4A | 178.26 (16) | H1AA—C1A—H1AC | 109.5 |
N3Ai—Na1A—N4A | 122.54 (16) | H1AB—C1A—H1AC | 109.5 |
O15B—Na1B—O20Bii | 106.9 (2) | C4A—C5A—C6A | 121.2 (6) |
O15B—Na1B—O5Bii | 104.8 (2) | C4A—C5A—H5AA | 119.4 |
O20Bii—Na1B—O5Bii | 109.55 (17) | C6A—C5A—H5AA | 119.4 |
O15B—Na1B—O10B | 106.11 (17) | C24A—C19A—C20A | 121.1 (5) |
O20Bii—Na1B—O10B | 105.98 (19) | C24A—C19A—S3A | 119.8 (4) |
O5Bii—Na1B—O10B | 122.60 (19) | C20A—C19A—S3A | 119.1 (4) |
O6A—Nd1A—O4A | 98.22 (12) | C12B—C11B—C16B | 120.3 (5) |
O6A—Nd1A—O16A | 87.85 (14) | C12B—C11B—S2B | 119.5 (4) |
O4A—Nd1A—O16A | 144.23 (13) | C16B—C11B—S2B | 120.2 (4) |
O6A—Nd1A—O11A | 145.13 (13) | O8A—C10A—H10A | 109.5 |
O4A—Nd1A—O11A | 86.74 (13) | O8A—C10A—H10B | 109.5 |
O16A—Nd1A—O11A | 108.08 (14) | H10A—C10A—H10B | 109.5 |
O6A—Nd1A—O9A | 72.03 (13) | O8A—C10A—H10C | 109.5 |
O4A—Nd1A—O9A | 74.65 (12) | H10A—C10A—H10C | 109.5 |
O16A—Nd1A—O9A | 139.73 (12) | H10B—C10A—H10C | 109.5 |
O11A—Nd1A—O9A | 76.19 (11) | C27A—C28A—C29A | 120.9 (6) |
O6A—Nd1A—O1A | 73.58 (13) | C27A—C28A—H28A | 119.6 |
O4A—Nd1A—O1A | 72.22 (12) | C29A—C28A—H28A | 119.6 |
O16A—Nd1A—O1A | 75.91 (12) | C11B—C16B—C15B | 119.2 (6) |
O11A—Nd1A—O1A | 139.56 (12) | C11B—C16B—H16A | 120.4 |
O9A—Nd1A—O1A | 127.34 (11) | C15B—C16B—H16A | 120.4 |
O6A—Nd1A—O19A | 142.77 (13) | C5B—C4B—C3B | 118.9 (6) |
O4A—Nd1A—O19A | 81.60 (13) | C5B—C4B—H4BA | 120.6 |
O16A—Nd1A—O19A | 72.94 (12) | C3B—C4B—H4BA | 120.6 |
O11A—Nd1A—O19A | 72.07 (12) | C24B—C19B—C20B | 121.4 (6) |
O9A—Nd1A—O19A | 141.11 (12) | C24B—C19B—S3B | 119.0 (5) |
O1A—Nd1A—O19A | 70.97 (12) | C20B—C19B—S3B | 119.6 (5) |
O6A—Nd1A—O14A | 82.82 (13) | O13A—C18A—H18A | 109.5 |
O4A—Nd1A—O14A | 143.65 (12) | O13A—C18A—H18B | 109.5 |
O16A—Nd1A—O14A | 71.97 (12) | H18A—C18A—H18B | 109.5 |
O11A—Nd1A—O14A | 73.57 (11) | O13A—C18A—H18C | 109.5 |
O9A—Nd1A—O14A | 71.17 (11) | H18A—C18A—H18C | 109.5 |
O1A—Nd1A—O14A | 140.54 (12) | H18B—C18A—H18C | 109.5 |
O19A—Nd1A—O14A | 118.92 (13) | C7A—C8A—C3A | 119.2 (6) |
O1B—Nd1B—O16B | 137.22 (12) | C7A—C8A—H8AA | 120.4 |
O1B—Nd1B—O11B | 105.85 (13) | C3A—C8A—H8AA | 120.4 |
O16B—Nd1B—O11B | 90.45 (15) | O8B—C10B—H10D | 109.5 |
O1B—Nd1B—O6B | 90.24 (14) | O8B—C10B—H10E | 109.5 |
O16B—Nd1B—O6B | 104.06 (13) | H10D—C10B—H10E | 109.5 |
O11B—Nd1B—O6B | 137.53 (13) | O8B—C10B—H10F | 109.5 |
O1B—Nd1B—O19B | 74.81 (13) | H10D—C10B—H10F | 109.5 |
O16B—Nd1B—O19B | 72.93 (13) | H10E—C10B—H10F | 109.5 |
O11B—Nd1B—O19B | 72.56 (13) | C13A—C12A—C11A | 118.3 (5) |
O6B—Nd1B—O19B | 149.77 (13) | C13A—C12A—H12A | 120.9 |
O1B—Nd1B—O14B | 150.42 (12) | C11A—C12A—H12A | 120.9 |
O16B—Nd1B—O14B | 71.95 (13) | C16A—C15A—C14A | 120.7 (5) |
O11B—Nd1B—O14B | 72.82 (13) | C16A—C15A—H15A | 119.6 |
O6B—Nd1B—O14B | 74.26 (13) | C14A—C15A—H15A | 119.6 |
O19B—Nd1B—O14B | 129.64 (13) | C5A—C6A—C7A | 119.8 (6) |
O1B—Nd1B—O4B | 71.67 (12) | C5A—C6A—H6AA | 120.1 |
O16B—Nd1B—O4B | 74.48 (13) | C7A—C6A—H6AA | 120.1 |
O11B—Nd1B—O4B | 149.32 (13) | C21A—C22A—C23A | 119.6 (6) |
O6B—Nd1B—O4B | 72.89 (12) | C21A—C22A—H22A | 120.2 |
O19B—Nd1B—O4B | 77.46 (13) | C23A—C22A—H22A | 120.2 |
O14B—Nd1B—O4B | 124.66 (12) | S4B—N4B—P4B | 130.8 (3) |
O1B—Nd1B—O9B | 73.23 (12) | C15B—C14B—C13B | 120.8 (6) |
O16B—Nd1B—O9B | 149.40 (13) | C15B—C14B—H14A | 119.6 |
O11B—Nd1B—O9B | 74.40 (13) | C13B—C14B—H14A | 119.6 |
O6B—Nd1B—O9B | 73.19 (13) | C5A—C4A—C3A | 119.0 (6) |
O19B—Nd1B—O9B | 124.70 (13) | C5A—C4A—H4AA | 120.5 |
O14B—Nd1B—O9B | 78.15 (12) | C3A—C4A—H4AA | 120.5 |
O4B—Nd1B—O9B | 130.28 (13) | C11B—C12B—C13B | 119.5 (5) |
O5A—S1A—O1A | 113.9 (2) | C11B—C12B—H12B | 120.3 |
O5A—S1A—N1A | 109.6 (2) | C13B—C12B—H12B | 120.3 |
O1A—S1A—N1A | 113.6 (2) | C6B—C5B—C4B | 121.3 (6) |
O5A—S1A—C3A | 106.3 (2) | C6B—C5B—H5BA | 119.3 |
O1A—S1A—C3A | 104.3 (2) | C4B—C5B—H5BA | 119.3 |
N1A—S1A—C3A | 108.5 (2) | C3B—C8B—C7B | 119.9 (6) |
O4A—P1A—O2A | 112.4 (2) | C3B—C8B—H8BA | 120.1 |
O4A—P1A—O3A | 107.7 (2) | C7B—C8B—H8BA | 120.1 |
O2A—P1A—O3A | 101.9 (2) | C15A—C16A—C11A | 118.2 (5) |
O4A—P1A—N1A | 117.2 (2) | C15A—C16A—H16B | 120.9 |
O2A—P1A—N1A | 106.2 (2) | C11A—C16A—H16B | 120.9 |
O3A—P1A—N1A | 110.3 (2) | C14B—C13B—C12B | 119.2 (6) |
O20A—S4A—O19A | 113.9 (2) | C14B—C13B—H13A | 120.4 |
O20A—S4A—N4A | 109.1 (2) | C12B—C13B—H13A | 120.4 |
O19A—S4A—N4A | 113.9 (2) | O18A—C26A—H26A | 109.5 |
O20A—S4A—C27A | 107.9 (3) | O18A—C26A—H26B | 109.5 |
O19A—S4A—C27A | 104.2 (2) | H26A—C26A—H26B | 109.5 |
N4A—S4A—C27A | 107.5 (2) | O18A—C26A—H26C | 109.5 |
O20A—S4A—Na1A | 51.33 (16) | H26A—C26A—H26C | 109.5 |
O19A—S4A—Na1A | 126.23 (17) | H26B—C26A—H26C | 109.5 |
N4A—S4A—Na1A | 58.53 (16) | C22A—C23A—C24A | 121.0 (6) |
C27A—S4A—Na1A | 129.45 (18) | C22A—C23A—H23A | 119.5 |
O10A—S2A—O9A | 114.3 (2) | C24A—C23A—H23A | 119.5 |
O10A—S2A—N2A | 110.1 (3) | C13A—C14A—C15A | 120.2 (5) |
O9A—S2A—N2A | 113.4 (2) | C13A—C14A—H14B | 119.9 |
O10A—S2A—C11A | 105.5 (2) | C15A—C14A—H14B | 119.9 |
O9A—S2A—C11A | 104.3 (2) | C8B—C3B—C4B | 120.6 (5) |
N2A—S2A—C11A | 108.5 (2) | C8B—C3B—S1B | 119.4 (4) |
O15A—S3A—O14A | 114.6 (2) | C4B—C3B—S1B | 119.9 (5) |
O15A—S3A—N3A | 107.9 (2) | C14B—C15B—C16B | 120.9 (6) |
O14A—S3A—N3A | 113.9 (2) | C14B—C15B—H15B | 119.6 |
O15A—S3A—C19A | 108.2 (2) | C16B—C15B—H15B | 119.6 |
O14A—S3A—C19A | 104.9 (2) | C21A—C20A—C19A | 119.2 (6) |
N3A—S3A—C19A | 107.0 (2) | C21A—C20A—H20A | 120.4 |
O15A—S3A—Na1Aiii | 52.38 (15) | C19A—C20A—H20A | 120.4 |
O14A—S3A—Na1Aiii | 125.82 (16) | C30B—C29B—C28B | 120.6 (7) |
N3A—S3A—Na1Aiii | 56.38 (15) | C30B—C29B—H29A | 119.7 |
C19A—S3A—Na1Aiii | 129.24 (19) | C28B—C29B—H29A | 119.7 |
O11A—P3A—O12A | 108.3 (2) | C19A—C24A—C23A | 118.1 (5) |
O11A—P3A—O13A | 113.0 (2) | C19A—C24A—H24A | 120.9 |
O12A—P3A—O13A | 101.9 (2) | C23A—C24A—H24A | 120.9 |
O11A—P3A—N3A | 116.8 (2) | C27B—C28B—C29B | 118.6 (6) |
O12A—P3A—N3A | 109.9 (2) | C27B—C28B—H28B | 120.7 |
O13A—P3A—N3A | 106.0 (2) | C29B—C28B—H28B | 120.7 |
O15B—S3B—O14B | 113.0 (3) | C23B—C24B—C19B | 118.9 (7) |
O15B—S3B—N3B | 110.8 (3) | C23B—C24B—H24B | 120.6 |
O14B—S3B—N3B | 114.4 (2) | C19B—C24B—H24B | 120.6 |
O15B—S3B—C19B | 105.3 (3) | C21B—C20B—C19B | 118.8 (8) |
O14B—S3B—C19B | 106.8 (3) | C21B—C20B—H20B | 120.6 |
N3B—S3B—C19B | 105.8 (3) | C19B—C20B—H20B | 120.6 |
O14B—S3B—Na1B | 109.83 (16) | C32A—C31A—C30A | 121.2 (6) |
N3B—S3B—Na1B | 90.8 (2) | C32A—C31A—H31A | 119.4 |
C19B—S3B—Na1B | 128.4 (2) | C30A—C31A—H31A | 119.4 |
O4B—S1B—O5B | 113.6 (3) | C14A—C13A—C12A | 120.6 (6) |
O4B—S1B—N1B | 114.0 (2) | C14A—C13A—H13B | 119.7 |
O5B—S1B—N1B | 110.9 (3) | C12A—C13A—H13B | 119.7 |
O4B—S1B—C3B | 106.0 (3) | C32B—C27B—C28B | 122.0 (6) |
O5B—S1B—C3B | 104.3 (3) | C32B—C27B—S4B | 119.4 (5) |
N1B—S1B—C3B | 107.3 (3) | C28B—C27B—S4B | 118.6 (5) |
O4B—S1B—Na1Biv | 108.17 (17) | C8B—C7B—C6B | 119.9 (6) |
N1B—S1B—Na1Biv | 84.05 (19) | C8B—C7B—H7BA | 120.1 |
C3B—S1B—Na1Biv | 135.3 (2) | C6B—C7B—H7BA | 120.1 |
O20B—S4B—O19B | 112.8 (3) | C28A—C29A—C30A | 119.0 (6) |
O20B—S4B—N4B | 111.9 (3) | C28A—C29A—H29B | 120.5 |
O19B—S4B—N4B | 113.7 (3) | C30A—C29A—H29B | 120.5 |
O20B—S4B—C27B | 106.1 (3) | C30B—C31B—C32B | 120.2 (7) |
O19B—S4B—C27B | 105.8 (3) | C30B—C31B—H31B | 119.9 |
N4B—S4B—C27B | 105.8 (3) | C32B—C31B—H31B | 119.9 |
O6B—P2B—O8B | 112.8 (2) | C24B—C23B—C22B | 120.0 (7) |
O6B—P2B—O7B | 107.0 (2) | C24B—C23B—H23B | 120.0 |
O8B—P2B—O7B | 100.3 (2) | C22B—C23B—H23B | 120.0 |
O6B—P2B—N2B | 118.6 (2) | C5B—C6B—C7B | 119.3 (6) |
O8B—P2B—N2B | 106.0 (2) | C5B—C6B—H6BA | 120.3 |
O7B—P2B—N2B | 110.8 (3) | C7B—C6B—H6BA | 120.3 |
O10B—S2B—O9B | 113.9 (2) | C20B—C21B—C22B | 121.9 (8) |
O10B—S2B—N2B | 108.1 (3) | C20B—C21B—H21A | 119.1 |
O9B—S2B—N2B | 114.8 (2) | C22B—C21B—H21A | 119.1 |
O10B—S2B—C11B | 105.5 (3) | O2B—C1B—H1BA | 109.5 |
O9B—S2B—C11B | 106.7 (2) | O2B—C1B—H1BB | 109.5 |
N2B—S2B—C11B | 107.4 (3) | H1BA—C1B—H1BB | 109.5 |
O9B—S2B—Na1B | 110.68 (17) | O2B—C1B—H1BC | 109.5 |
N2B—S2B—Na1B | 77.58 (19) | H1BA—C1B—H1BC | 109.5 |
C11B—S2B—Na1B | 135.7 (2) | H1BB—C1B—H1BC | 109.5 |
O6A—P2A—O7A | 107.5 (2) | O12A—C17A—H17A | 109.5 |
O6A—P2A—O8A | 112.1 (2) | O12A—C17A—H17B | 109.5 |
O7A—P2A—O8A | 101.5 (3) | H17A—C17A—H17B | 109.5 |
O6A—P2A—N2A | 117.4 (2) | O12A—C17A—H17C | 109.5 |
O7A—P2A—N2A | 110.5 (3) | H17A—C17A—H17C | 109.5 |
O8A—P2A—N2A | 106.8 (2) | H17B—C17A—H17C | 109.5 |
O16A—P4A—O17A | 108.5 (2) | C20A—C21A—C22A | 121.0 (6) |
O16A—P4A—O18A | 113.1 (2) | C20A—C21A—H21B | 119.5 |
O17A—P4A—O18A | 101.4 (2) | C22A—C21A—H21B | 119.5 |
O16A—P4A—N4A | 116.1 (2) | C31B—C30B—C29B | 120.4 (7) |
O17A—P4A—N4A | 110.0 (3) | C31B—C30B—H30A | 119.8 |
O18A—P4A—N4A | 106.8 (2) | C29B—C30B—H30A | 119.8 |
O1B—P1B—N1B | 115.8 (2) | C27B—C32B—C31B | 118.2 (7) |
O1B—P1B—O2B | 113.4 (2) | C27B—C32B—H32A | 120.9 |
N1B—P1B—O2B | 108.2 (2) | C31B—C32B—H32A | 120.9 |
O1B—P1B—O3B | 111.6 (2) | C31A—C30A—C29A | 119.2 (6) |
N1B—P1B—O3B | 109.4 (3) | C31A—C30A—H30B | 120.4 |
O2B—P1B—O3B | 96.7 (2) | C29A—C30A—H30B | 120.4 |
O11B—P3B—O13B | 112.0 (3) | C31A—C32A—C27A | 120.1 (7) |
O11B—P3B—O12B | 108.0 (3) | C31A—C32A—H32B | 120.0 |
O13B—P3B—O12B | 102.1 (3) | C27A—C32A—H32B | 120.0 |
O11B—P3B—N3B | 117.3 (2) | C8A—C7A—C6A | 120.3 (6) |
O13B—P3B—N3B | 107.7 (3) | C8A—C7A—H7AA | 119.8 |
O12B—P3B—N3B | 108.7 (3) | C6A—C7A—H7AA | 119.8 |
O16B—P4B—O17B | 106.4 (3) | O13B—C18B—H18D | 109.5 |
O16B—P4B—O18B | 112.6 (3) | O13B—C18B—H18E | 109.5 |
O17B—P4B—O18B | 102.1 (3) | H18D—C18B—H18E | 109.5 |
O16B—P4B—N4B | 117.3 (3) | O13B—C18B—H18F | 109.5 |
O17B—P4B—N4B | 109.5 (3) | H18D—C18B—H18F | 109.5 |
O18B—P4B—N4B | 107.9 (3) | H18E—C18B—H18F | 109.5 |
S3A—O14A—Nd1A | 137.7 (2) | O3A—C2A—H2AA | 109.5 |
S4A—O19A—Nd1A | 138.4 (2) | O3A—C2A—H2AB | 109.5 |
S1A—O1A—Nd1A | 140.9 (2) | H2AA—C2A—H2AB | 109.5 |
P1A—O4A—Nd1A | 138.8 (2) | O3A—C2A—H2AC | 109.5 |
S2A—O9A—Nd1A | 140.9 (2) | H2AA—C2A—H2AC | 109.5 |
C18A—O13A—P3A | 121.5 (4) | H2AB—C2A—H2AC | 109.5 |
P3B—O11B—Nd1B | 139.6 (2) | O17A—C25A—H25A | 109.5 |
P4A—O16A—Nd1A | 137.1 (2) | O17A—C25A—H25B | 109.5 |
P2A—O6A—Nd1A | 139.2 (2) | H25A—C25A—H25B | 109.5 |
S4A—O20A—Na1A | 100.6 (2) | O17A—C25A—H25C | 109.5 |
P1B—O1B—Nd1B | 143.8 (2) | H25A—C25A—H25C | 109.5 |
P3A—O11A—Nd1A | 136.1 (2) | H25B—C25A—H25C | 109.5 |
S1B—O4B—Nd1B | 141.7 (2) | C21B—C22B—C23B | 119.0 (7) |
C25A—O17A—P4A | 121.4 (5) | C21B—C22B—H22B | 120.5 |
S1A—O5A—Na1A | 142.3 (2) | C23B—C22B—H22B | 120.5 |
C1A—O2A—P1A | 118.5 (3) | O17B—C25B—H25D | 109.5 |
S3A—O15A—Na1Aiii | 99.42 (19) | O17B—C25B—H25E | 109.5 |
S4B—O19B—Nd1B | 143.1 (2) | H25D—C25B—H25E | 109.5 |
C26A—O18A—P4A | 121.9 (4) | O17B—C25B—H25F | 109.5 |
P2B—O6B—Nd1B | 140.1 (2) | H25D—C25B—H25F | 109.5 |
S2B—O9B—Nd1B | 141.2 (2) | H25E—C25B—H25F | 109.5 |
S2A—O10A—Na1Aiii | 145.9 (2) | O12B—C17B—H17D | 109.5 |
S2B—O10B—Na1B | 120.6 (2) | O12B—C17B—H17E | 109.5 |
C10A—O8A—P2A | 118.0 (4) | H17D—C17B—H17E | 109.5 |
C2B—O3B—P1B | 120.1 (5) | O12B—C17B—H17F | 109.5 |
C1B—O2B—P1B | 120.6 (4) | H17D—C17B—H17F | 109.5 |
S3B—O14B—Nd1B | 141.3 (2) | H17E—C17B—H17F | 109.5 |
P4B—O16B—Nd1B | 141.3 (2) | O3B—C2B—H2BA | 109.5 |
C10B—O8B—P2B | 119.5 (4) | O3B—C2B—H2BB | 109.5 |
C2A—O3A—P1A | 118.5 (4) | H2BA—C2B—H2BB | 109.5 |
C17A—O12A—P3A | 121.2 (4) | O3B—C2B—H2BC | 109.5 |
C9A—O7A—P2A | 119.0 (5) | H2BA—C2B—H2BC | 109.5 |
S3B—O15B—Na1B | 137.5 (3) | H2BB—C2B—H2BC | 109.5 |
S1B—O5B—Na1Biv | 123.5 (3) | O7B—C9B—H9BA | 109.5 |
S3A—N3A—P3A | 122.8 (2) | O7B—C9B—H9BB | 109.5 |
S3A—N3A—Na1Aiii | 92.54 (19) | H9BA—C9B—H9BB | 109.5 |
P3A—N3A—Na1Aiii | 142.2 (2) | O7B—C9B—H9BC | 109.5 |
S4B—O20B—Na1Biv | 141.3 (3) | H9BA—C9B—H9BC | 109.5 |
C9B—O7B—P2B | 119.7 (4) | H9BB—C9B—H9BC | 109.5 |
C18B—O13B—P3B | 121.9 (5) | O7A—C9A—H9AA | 109.5 |
S2A—N2A—P2A | 126.7 (3) | O7A—C9A—H9AB | 109.5 |
P1B—N1B—S1B | 129.5 (3) | H9AA—C9A—H9AB | 109.5 |
S1A—N1A—P1A | 126.5 (3) | O7A—C9A—H9AC | 109.5 |
C17B—O12B—P3B | 121.9 (5) | H9AA—C9A—H9AC | 109.5 |
S4A—N4A—P4A | 123.3 (2) | H9AB—C9A—H9AC | 109.5 |
S4A—N4A—Na1A | 90.5 (2) | O18B—C26B—H26D | 109.5 |
P4A—N4A—Na1A | 143.0 (2) | O18B—C26B—H26E | 109.5 |
S3B—N3B—P3B | 130.3 (3) | H26D—C26B—H26E | 109.5 |
C26B—O18B—P4B | 118.4 (6) | O18B—C26B—H26F | 109.5 |
C32A—C27A—C28A | 119.6 (6) | H26D—C26B—H26F | 109.5 |
C32A—C27A—S4A | 119.7 (5) | H26E—C26B—H26F | 109.5 |
Symmetry codes: (i) −x+1/2, −y, z−1/2; (ii) −x−1/2, −y, z−1/2; (iii) −x+1/2, −y, z+1/2; (iv) −x−1/2, −y, z+1/2. |
Experimental details
Crystal data | |
Chemical formula | [NaNd(C8H11NO5PS)4] |
Mr | 1224.10 |
Crystal system, space group | Orthorhombic, P212121 |
Temperature (K) | 293 |
a, b, c (Å) | 20.276 (2), 21.9129 (9), 22.058 (2) |
V (Å3) | 9800.5 (14) |
Z | 8 |
Radiation type | Mo Kα |
µ (mm−1) | 1.45 |
Crystal size (mm) | 0.5 × 0.2 × 0.1 |
Data collection | |
Diffractometer | Oxford Diffraction Xcalibur-3 diffractometer |
Absorption correction | Multi-scan (Blessing, 1995) |
Tmin, Tmax | 0.705, 0.855 |
No. of measured, independent and observed [I > 2σ(I)] reflections | 104650, 34763, 20694 |
Rint | 0.047 |
(sin θ/λ)max (Å−1) | 0.756 |
Refinement | |
R[F2 > 2σ(F2)], wR(F2), S | 0.054, 0.152, 0.90 |
No. of reflections | 34763 |
No. of parameters | 1189 |
H-atom treatment | H-atom parameters constrained |
Δρmax, Δρmin (e Å−3) | 4.50, −1.95 |
Absolute structure | Flack (1983), 15958 Friedel pairs |
Absolute structure parameter | −0.063 (8) |
Computer programs: CrysAlis CCD (Oxford Diffraction, 2006), CrysAlis RED (Oxford Diffraction, 2006), SHELXS97 (Sheldrick, 1997), SHELXL97 (Sheldrick, 1997), ORTEP-3 (Farrugia, 1997), WinGX (Farrugia, 1999).
Na1A—O10Ai | 2.385 (4) | Nd1A—O11A | 2.409 (4) |
Na1A—O20A | 2.411 (4) | Nd1A—O9A | 2.478 (3) |
Na1A—O5A | 2.421 (4) | Nd1A—O1A | 2.485 (3) |
Na1A—O15Ai | 2.433 (4) | Nd1A—O19A | 2.492 (4) |
Na1A—N3Ai | 2.526 (4) | Nd1A—O14A | 2.515 (4) |
Na1A—N4A | 2.589 (5) | Nd1B—O1B | 2.368 (4) |
Na1B—O15B | 2.186 (5) | Nd1B—O16B | 2.372 (4) |
Na1B—O20Bii | 2.211 (5) | Nd1B—O11B | 2.380 (4) |
Na1B—O5Bii | 2.242 (5) | Nd1B—O6B | 2.382 (4) |
Na1B—O10B | 2.261 (4) | Nd1B—O19B | 2.484 (4) |
Nd1A—O6A | 2.362 (4) | Nd1B—O14B | 2.493 (4) |
Nd1A—O4A | 2.375 (4) | Nd1B—O4B | 2.513 (4) |
Nd1A—O16A | 2.406 (4) | Nd1B—O9B | 2.509 (4) |
Symmetry codes: (i) −x+1/2, −y, z−1/2; (ii) −x−1/2, −y, z−1/2. |
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It is known that sulfonylamide derivatives of a general view RSO2NHPO(R1)2 are widely used in medicine and toxicology as bactericidal drugs (Xu & Angell, 2000); some sulfonyl phosphoramides are important pesticides (Kishino & Saito, 1979). Earlier systematically investigated by us carbacylamidophosphates and their coordination compounds (Skopenko et al., 2004; Amirkhanov et al., 1996) may be considered as structural analogous of phosphorylated sulfonylamides. To date the coordination chemistry of these ligands have been of great interest (Pietraszkiewicz et al., 2002), however there are no reports on the crystal structure of the complexes with dimethyl(phenylsulfonyl)amidophosphate (HL). This paper is devoted to the crystal structure of tetrakis–complex of composition {Na[Nd(L)4]}n.
The title compound contains two independent one-dimensional polymeric chains, A and B, respectively, which are formed by [Nd(L4)]- anions and sodium cations as the linkers (Figs. 1 and 2). The distinctions between the chains are in the different types of coordination polyhedra for Nd3+ and Na+ ions.
In complex anions the neodymium atoms have eight-coordinated environment formed by oxygen atoms belonging to sulfonyl and phosphoryl groups of four bidentate chelate ligands. The coordinated residues of acido ligand (L) are once deprotonated by amide group. According to the geometrical standards, which are proposed by Porai-Koshits (Porai-Koshits & Aslanov, 1972) the resulting coordination polyhedra can be described as a medium conformation between bicapped trigonal prism and square antiprism for Nd1A atom and as a slightly distorted square antiprism for Nd1B atom.
The Nd—O distances (Table 1) fall in the range 2.362 (4)–2.409 (4) Å, for phosphoryl and 2.478 (3)–2.515 (4) Å for sulfonyl groups. The average Nd—O(P) bond lengths are shorter than Nd—O(S) separation that can be explained by higher affinity of phosphoryl group to lanthanide ions. The conclusion of deprotonation of amide goups can be achieved from the analysis of the O—S—N—P—O chelate fragments (Burgi & Dunitz, 1994). The bite angles around the central atom lie in the range 72.03 (13)–73.57 (11)° for Nd1A and 71.67 (12)–73.19 (13)° for Nd1B which are typical for lanthanide complexes with oxygen donor atoms chelate ligands (Malandrino et al., 1998; Trush et al., 2001; Borzechowska et al., 2002). The metallocycles are almost flat with a deviation of the Nd atoms from the mean planes defined by the other five atoms of 0.124 (1) Å for Nd1A and 0.064 (1) Å for Nd1B.
The connection of complex anions in one-dimensional polymer structure is provided by Na ions (Fig 3). The Na polyhedron in A is a distorted octahedron and in B it can be described as a tetrahedron. The distorted octahedral environment is formed by four oxygen atoms belonging to SO groups (two from one complex anion and two from the neighbor one) and two nitrogen atoms from amide groups of different tetrakis anions. The tetrahedral environment is formed by four SO O atoms from different anions only. The Na—O, Na—N bond lengths are indicated in Table 1.