Supporting information
Crystallographic Information File (CIF) https://doi.org/10.1107/S1600536807053354/lh2527sup1.cif | |
Structure factor file (CIF format) https://doi.org/10.1107/S1600536807053354/lh2527Isup2.hkl |
CCDC reference: 672573
Key indicators
- Single-crystal X-ray study
- T = 293 K
- Mean (C-C) = 0.006 Å
- Disorder in solvent or counterion
- R factor = 0.033
- wR factor = 0.089
- Data-to-parameter ratio = 15.8
checkCIF/PLATON results
No syntax errors found
Alert level A PLAT250_ALERT_2_A Large U3/U1 Ratio for Average U(i,j) Tensor .... 10.37
Author Response: This is due to the disorder of one solvent molecule |
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 0.069 Additional refinement cycles may be required. PLAT041_ALERT_1_C Calc. and Rep. SumFormula Strings Differ .... ? PLAT042_ALERT_1_C Calc. and Rep. MoietyFormula Strings Differ .... ? PLAT045_ALERT_1_C Calculated and Reported Z Differ by ............ 0.25 Ratio PLAT062_ALERT_4_C Rescale T(min) & T(max) by ..................... 0.98 PLAT080_ALERT_2_C Maximum Shift/Error ............................ 0.07 PLAT152_ALERT_1_C Supplied and Calc Volume s.u. Inconsistent ..... ? PLAT154_ALERT_1_C The su's on the Cell Angles are Equal (x 10000) 100 Deg. PLAT155_ALERT_4_C The Triclinic Unitcell is NOT Reduced .......... ? PLAT156_ALERT_4_C Axial System Input Cell not Standard ........... ? PLAT180_ALERT_3_C Check Cell Rounding: # of Values Ending with 0 = 4 PLAT220_ALERT_2_C Large Non-Solvent C Ueq(max)/Ueq(min) ... 3.05 Ratio PLAT220_ALERT_2_C Large Non-Solvent C Ueq(max)/Ueq(min) ... 2.98 Ratio PLAT241_ALERT_2_C Check High Ueq as Compared to Neighbors for C53 PLAT241_ALERT_2_C Check High Ueq as Compared to Neighbors for C107 PLAT242_ALERT_2_C Check Low Ueq as Compared to Neighbors for C31 PLAT242_ALERT_2_C Check Low Ueq as Compared to Neighbors for C38 PLAT242_ALERT_2_C Check Low Ueq as Compared to Neighbors for C42 PLAT242_ALERT_2_C Check Low Ueq as Compared to Neighbors for C45 PLAT242_ALERT_2_C Check Low Ueq as Compared to Neighbors for C81 PLAT242_ALERT_2_C Check Low Ueq as Compared to Neighbors for C88 PLAT242_ALERT_2_C Check Low Ueq as Compared to Neighbors for C99 PLAT242_ALERT_2_C Check Low Ueq as Compared to Neighbors for C102 PLAT243_ALERT_4_C High 'Solvent' Ueq as Compared to Neighbors for C118 PLAT243_ALERT_4_C High 'Solvent' Ueq as Compared to Neighbors for C120 PLAT243_ALERT_4_C High 'Solvent' Ueq as Compared to Neighbors for C125 PLAT244_ALERT_4_C Low 'Solvent' Ueq as Compared to Neighbors for C116 PLAT244_ALERT_4_C Low 'Solvent' Ueq as Compared to Neighbors for C117 PLAT244_ALERT_4_C Low 'Solvent' Ueq as Compared to Neighbors for C119 PLAT244_ALERT_4_C Low 'Solvent' Ueq as Compared to Neighbors for C121 PLAT244_ALERT_4_C Low 'Solvent' Ueq as Compared to Neighbors for C124 PLAT244_ALERT_4_C Low 'Solvent' Ueq as Compared to Neighbors for C128 PLAT244_ALERT_4_C Low 'Solvent' Ueq as Compared to Neighbors for C130 PLAT302_ALERT_4_C Anion/Solvent Disorder ......................... 13.00 Perc. PLAT332_ALERT_2_C Large Phenyl C-C Range C123 -C128 0.20 Ang. PLAT369_ALERT_2_C Long C(sp2)-C(sp2) Bond C72 - C92 ... 1.53 Ang. PLAT380_ALERT_4_C Check Incorrectly? Oriented X(sp2)-Methyl Moiety C115 PLAT380_ALERT_4_C Check Incorrectly? Oriented X(sp2)-Methyl Moiety C122 PLAT380_ALERT_4_C Check Incorrectly? Oriented X(sp2)-Methyl Moiety C129 PLAT413_ALERT_2_C Short Inter XH3 .. XHn H13C .. H54 .. 2.13 Ang. PLAT720_ALERT_4_C Number of Unusual/Non-Standard Label(s) ........ 1
Alert level G PLAT199_ALERT_1_G Check the Reported _cell_measurement_temperature 293 K PLAT200_ALERT_1_G Check the Reported _diffrn_ambient_temperature . 293 K PLAT860_ALERT_3_G Note: Number of Least-Squares Restraints ....... 154
1 ALERT level A = In general: serious problem 0 ALERT level B = Potentially serious problem 41 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 18 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 18 ALERT type 4 Improvement, methodology, query or suggestion 0 ALERT type 5 Informative message, check
n-BuLi (3.0 ml, 1.6 mol/l in hexane, 4.8 mmol) was added slowly over a period of 30 min to a solution of (Me3Si)2NH (0.78 g, 4.8 mmol) in THF (15 ml) cooled in an ice bath. The reaction mixture was stirred, warmed up slowly to room temperature and stirred for another 12 h until a clear pale yellow solution was obtained. Then the resultant solution was transferred slowly to a suspension of SmCl3 (0.41 g, 1.6 mmol) in THF (10 ml). The reaction mixture was stirred for 24 h at room temperature until all of the SmCl3 was consumed. The resulting solution was centrifuged and filtered. The filtrate was transferred to a solution of 5,10,15,20-tetrakis(4-methyl phenyl)porphyrin (0.20 g, 0.32 mmol) in bis(2-methoxyethyl)ether (8 ml) under a nitrogen atmosphere. The resulting solution was refluxed 24 h and the progress of the reaction was monitored by UV-Vis absorption spectroscopy. After the reaction, the mixture was cooled to room temperature, potassium hydridotris(pyrazole-1-yl)borate (0.1 g, 0.40 mmol) was added and the resulting solution was magnetically stirred at room temperature for 12 h. Then all solvent was removed under vacuum and chloroform (5 ml) was added. After filtration, methanol was diffused into the filtrate and a purple solid crystallized. Yield: 89%. The single-crystal suitable for data analysis were obtained from slow evaporation of toluene solution of sample at room temperature for two weeks.
All hydrogen atoms were geometrically constrained and refined in riding mode as follows: methyl d(C—H) = 0.96 Å, Uiso(H) = 1.5Ueq(C); aromatic d(C—H) = 0.93 Å, Uiso(H) = 1.2Ueq(C).
Data collection: SMART (Bruker, 1998); cell refinement: SAINT-Plus (Bruker, 1998); data reduction: SAINT-Plus (Bruker, 1998); program(s) used to solve structure: SHELXS97 (Sheldrick, 1997); program(s) used to refine structure: SHELXL97 (Sheldrick, 1997); molecular graphics: ORTEP-3 for Windows (Farrugia, 1997); software used to prepare material for publication: WinGX (Farrugia, 1999).
[Sm(C9H10BN6)(C48H36N4)]·1.75C7H8 | Z = 4 |
Mr = 1193.43 | F(000) = 2450 |
Triclinic, P1 | Dx = 1.322 Mg m−3 |
Hall symbol: -P 1 | Mo Kα radiation, λ = 0.71073 Å |
a = 16.6210 (2) Å | Cell parameters from 42602 reflections |
b = 16.5696 (2) Å | θ = 1.5–28.6° |
c = 25.4414 (3) Å | µ = 1.03 mm−1 |
α = 79.318 (1)° | T = 293 K |
β = 79.064 (1)° | Block, purple |
γ = 61.248 (1)° | 0.30 × 0.30 × 0.30 mm |
V = 5995.10 (12) Å3 |
Bruker SMART 1K CCD diffractometer | 21056 independent reflections |
Radiation source: fine-focus sealed tube | 17078 reflections with I > 2σ(I) |
Graphite monochromator | Rint = 0.030 |
ϕ and ω scans | θmax = 25.0°, θmin = 1.5° |
Absorption correction: multi-scan (SADABS; Sheldrick, 2002) | h = −19→19 |
Tmin = 0.748, Tmax = 0.748 | k = −19→19 |
73453 measured reflections | l = −30→30 |
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: inferred from neighbouring sites |
wR(F2) = 0.089 | H-atom parameters constrained |
S = 1.02 | w = 1/[σ2(Fo2) + (0.0403P)2 + 6.7364P] where P = (Fo2 + 2Fc2)/3 |
21056 reflections | (Δ/σ)max = 0.069 |
1335 parameters | Δρmax = 0.88 e Å−3 |
154 restraints | Δρmin = −0.47 e Å−3 |
[Sm(C9H10BN6)(C48H36N4)]·1.75C7H8 | γ = 61.248 (1)° |
Mr = 1193.43 | V = 5995.10 (12) Å3 |
Triclinic, P1 | Z = 4 |
a = 16.6210 (2) Å | Mo Kα radiation |
b = 16.5696 (2) Å | µ = 1.03 mm−1 |
c = 25.4414 (3) Å | T = 293 K |
α = 79.318 (1)° | 0.30 × 0.30 × 0.30 mm |
β = 79.064 (1)° |
Bruker SMART 1K CCD diffractometer | 21056 independent reflections |
Absorption correction: multi-scan (SADABS; Sheldrick, 2002) | 17078 reflections with I > 2σ(I) |
Tmin = 0.748, Tmax = 0.748 | Rint = 0.030 |
73453 measured reflections |
R[F2 > 2σ(F2)] = 0.033 | 154 restraints |
wR(F2) = 0.089 | H-atom parameters constrained |
S = 1.02 | Δρmax = 0.88 e Å−3 |
21056 reflections | Δρmin = −0.47 e Å−3 |
1335 parameters |
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) | |
Sm1 | 0.482762 (11) | 0.261500 (10) | 0.657833 (6) | 0.03049 (5) | |
Sm2 | 0.836393 (12) | 0.385772 (11) | 0.877913 (7) | 0.03729 (6) | |
N1 | 0.57515 (18) | 0.33192 (16) | 0.60674 (10) | 0.0332 (6) | |
N2 | 0.61809 (18) | 0.13848 (16) | 0.61386 (11) | 0.0343 (6) | |
N3 | 0.42424 (18) | 0.19426 (16) | 0.60740 (11) | 0.0340 (6) | |
N4 | 0.37984 (18) | 0.38779 (16) | 0.60053 (11) | 0.0340 (6) | |
N5 | 0.5620 (2) | 0.2652 (2) | 0.73429 (12) | 0.0493 (7) | |
N6 | 0.5280 (2) | 0.2599 (2) | 0.78690 (11) | 0.0465 (7) | |
N7 | 0.4574 (2) | 0.1496 (2) | 0.73743 (12) | 0.0525 (8) | |
N8 | 0.4453 (2) | 0.1652 (2) | 0.78978 (12) | 0.0504 (8) | |
N9 | 0.3531 (2) | 0.3617 (2) | 0.72682 (12) | 0.0495 (7) | |
N10 | 0.3560 (2) | 0.3373 (2) | 0.78131 (12) | 0.0475 (7) | |
N11 | 0.72354 (19) | 0.3572 (2) | 0.94114 (12) | 0.0436 (7) | |
N12 | 0.7011 (2) | 0.53405 (19) | 0.88392 (12) | 0.0437 (7) | |
N13 | 0.88912 (19) | 0.48524 (19) | 0.90085 (11) | 0.0409 (6) | |
N14 | 0.91109 (19) | 0.30930 (19) | 0.95994 (11) | 0.0411 (7) | |
N15 | 0.8714 (3) | 0.2294 (2) | 0.84721 (13) | 0.0581 (9) | |
N16 | 0.9031 (3) | 0.2101 (2) | 0.79554 (13) | 0.0592 (9) | |
N17 | 0.7806 (2) | 0.4239 (2) | 0.78406 (13) | 0.0578 (8) | |
N18 | 0.8272 (3) | 0.3681 (2) | 0.74437 (13) | 0.0600 (9) | |
N19 | 0.9848 (2) | 0.3372 (2) | 0.80925 (12) | 0.0515 (8) | |
N20 | 0.9935 (2) | 0.2984 (2) | 0.76415 (12) | 0.0544 (8) | |
B1 | 0.4381 (3) | 0.2529 (3) | 0.80599 (17) | 0.0478 (10) | |
H1 | 0.4263 | 0.2510 | 0.8453 | 0.057* | |
B2 | 0.9177 (4) | 0.2795 (4) | 0.75097 (19) | 0.0613 (13) | |
H2B1 | 0.9391 | 0.2516 | 0.7170 | 0.074* | |
C1 | 0.5421 (2) | 0.4265 (2) | 0.59702 (12) | 0.0338 (7) | |
C2 | 0.6185 (2) | 0.4470 (2) | 0.58272 (14) | 0.0424 (8) | |
H2 | 0.6148 | 0.5057 | 0.5756 | 0.051* | |
C3 | 0.6963 (3) | 0.3663 (2) | 0.58138 (15) | 0.0433 (8) | |
H3 | 0.7562 | 0.3588 | 0.5723 | 0.052* | |
C4 | 0.6697 (2) | 0.2937 (2) | 0.59658 (13) | 0.0352 (7) | |
C5 | 0.7315 (2) | 0.1991 (2) | 0.59826 (13) | 0.0366 (7) | |
C6 | 0.7067 (2) | 0.1276 (2) | 0.60636 (13) | 0.0361 (7) | |
C7 | 0.7713 (2) | 0.0313 (2) | 0.60227 (16) | 0.0473 (9) | |
H7 | 0.8354 | 0.0051 | 0.5986 | 0.057* | |
C8 | 0.7214 (2) | −0.0131 (2) | 0.60476 (16) | 0.0474 (9) | |
H8 | 0.7448 | −0.0761 | 0.6029 | 0.057* | |
C9 | 0.6254 (2) | 0.0533 (2) | 0.61076 (13) | 0.0369 (7) | |
C10 | 0.5523 (2) | 0.0355 (2) | 0.60797 (13) | 0.0354 (7) | |
C11 | 0.4588 (2) | 0.1013 (2) | 0.60601 (13) | 0.0359 (7) | |
C12 | 0.3857 (2) | 0.0817 (2) | 0.60086 (14) | 0.0432 (8) | |
H12D | 0.3911 | 0.0235 | 0.5999 | 0.052* | |
C13 | 0.3081 (2) | 0.1622 (2) | 0.59768 (15) | 0.0444 (8) | |
H13 | 0.2498 | 0.1702 | 0.5946 | 0.053* | |
C14 | 0.3321 (2) | 0.2337 (2) | 0.59998 (13) | 0.0359 (7) | |
C15 | 0.2721 (2) | 0.3287 (2) | 0.59151 (13) | 0.0358 (7) | |
C16 | 0.2965 (2) | 0.3996 (2) | 0.58994 (13) | 0.0355 (7) | |
C17 | 0.2375 (2) | 0.4961 (2) | 0.57527 (15) | 0.0452 (8) | |
H17 | 0.1776 | 0.5221 | 0.5664 | 0.054* | |
C18 | 0.2857 (2) | 0.5415 (2) | 0.57690 (15) | 0.0454 (9) | |
H18 | 0.2648 | 0.6050 | 0.5697 | 0.054* | |
C19 | 0.3758 (2) | 0.4737 (2) | 0.59192 (13) | 0.0358 (7) | |
C20 | 0.4494 (2) | 0.4923 (2) | 0.59349 (13) | 0.0349 (7) | |
C21 | 0.83363 (11) | 0.17318 (17) | 0.58430 (9) | 0.0386 (7) | |
C22 | 0.88201 (15) | 0.18067 (18) | 0.62054 (8) | 0.0565 (10) | |
H22 | 0.8525 | 0.2000 | 0.6541 | 0.068* | |
C23 | 0.97456 (15) | 0.1592 (2) | 0.60660 (10) | 0.0654 (12) | |
H23 | 1.0069 | 0.1642 | 0.6308 | 0.079* | |
C24 | 1.01873 (12) | 0.13027 (19) | 0.55641 (11) | 0.0554 (10) | |
C25 | 0.97036 (16) | 0.1228 (2) | 0.52016 (8) | 0.0642 (11) | |
H25 | 0.9999 | 0.1034 | 0.4866 | 0.077* | |
C26 | 0.87781 (15) | 0.14423 (19) | 0.53411 (8) | 0.0578 (10) | |
H26 | 0.8454 | 0.1392 | 0.5099 | 0.069* | |
C27 | 1.1214 (3) | 0.1058 (4) | 0.5413 (2) | 0.0821 (15) | |
H27A | 1.1548 | 0.0701 | 0.5714 | 0.123* | |
H27B | 1.1273 | 0.1617 | 0.5320 | 0.123* | |
H27C | 1.1460 | 0.0703 | 0.5111 | 0.123* | |
C28 | 0.57628 (17) | −0.06230 (11) | 0.60141 (9) | 0.0380 (7) | |
C29 | 0.58805 (19) | −0.08589 (13) | 0.54983 (7) | 0.0554 (10) | |
H29 | 0.5829 | −0.0421 | 0.5202 | 0.067* | |
C30 | 0.60747 (19) | −0.17488 (15) | 0.54261 (8) | 0.0590 (11) | |
H30 | 0.6153 | −0.1907 | 0.5081 | 0.071* | |
C31 | 0.61512 (18) | −0.24027 (11) | 0.58696 (10) | 0.0485 (9) | |
C32 | 0.60335 (19) | −0.21668 (13) | 0.63854 (8) | 0.0606 (11) | |
H32 | 0.6085 | −0.2604 | 0.6682 | 0.073* | |
C33 | 0.58393 (19) | −0.12769 (14) | 0.64576 (7) | 0.0548 (10) | |
H33 | 0.5761 | −0.1119 | 0.6803 | 0.066* | |
C34 | 0.6364 (3) | −0.3371 (2) | 0.5793 (2) | 0.0718 (13) | |
H34A | 0.5914 | −0.3529 | 0.6015 | 0.108* | |
H34B | 0.6968 | −0.3801 | 0.5892 | 0.108* | |
H34C | 0.6347 | −0.3399 | 0.5422 | 0.108* | |
C35 | 0.17531 (12) | 0.35731 (16) | 0.57932 (9) | 0.0371 (7) | |
C36 | 0.16265 (14) | 0.33895 (18) | 0.53122 (9) | 0.0587 (10) | |
H36 | 0.2132 | 0.3113 | 0.5059 | 0.070* | |
C37 | 0.07448 (17) | 0.3619 (2) | 0.52100 (9) | 0.0657 (12) | |
H37 | 0.0660 | 0.3496 | 0.4888 | 0.079* | |
C38 | −0.00104 (13) | 0.40317 (19) | 0.55889 (11) | 0.0574 (10) | |
C39 | 0.01161 (13) | 0.42154 (19) | 0.60699 (10) | 0.0670 (12) | |
H39 | −0.0389 | 0.4492 | 0.6323 | 0.080* | |
C40 | 0.09979 (15) | 0.39861 (18) | 0.61721 (8) | 0.0552 (10) | |
H40 | 0.1083 | 0.4109 | 0.6494 | 0.066* | |
C41 | −0.0978 (3) | 0.4262 (4) | 0.5474 (2) | 0.0895 (17) | |
H41A | −0.1412 | 0.4469 | 0.5788 | 0.134* | |
H41B | −0.0965 | 0.3719 | 0.5382 | 0.134* | |
H41C | −0.1162 | 0.4743 | 0.5179 | 0.134* | |
C42 | 0.42917 (18) | 0.59212 (11) | 0.58439 (8) | 0.0366 (7) | |
C43 | 0.4098 (2) | 0.64024 (15) | 0.62826 (7) | 0.0590 (11) | |
H43 | 0.4113 | 0.6101 | 0.6630 | 0.071* | |
C44 | 0.3883 (2) | 0.73339 (15) | 0.62018 (9) | 0.0721 (13) | |
H44 | 0.3754 | 0.7656 | 0.6495 | 0.086* | |
C45 | 0.3861 (2) | 0.77844 (11) | 0.56822 (11) | 0.0551 (10) | |
C46 | 0.4055 (2) | 0.73032 (15) | 0.52435 (8) | 0.0660 (12) | |
H46 | 0.4040 | 0.7605 | 0.4896 | 0.079* | |
C47 | 0.4270 (2) | 0.63716 (14) | 0.53243 (7) | 0.0634 (12) | |
H47 | 0.4400 | 0.6050 | 0.5031 | 0.076* | |
C48 | 0.3611 (4) | 0.8805 (3) | 0.5584 (3) | 0.0918 (18) | |
H48A | 0.3245 | 0.9092 | 0.5290 | 0.138* | |
H48B | 0.4165 | 0.8872 | 0.5499 | 0.138* | |
H48C | 0.3264 | 0.9097 | 0.5903 | 0.138* | |
C49 | 0.6371 (3) | 0.2746 (3) | 0.73369 (17) | 0.0662 (12) | |
H49 | 0.6745 | 0.2804 | 0.7026 | 0.079* | |
C50 | 0.6529 (3) | 0.2747 (4) | 0.78521 (19) | 0.0753 (14) | |
H50 | 0.7010 | 0.2799 | 0.7953 | 0.090* | |
C51 | 0.5826 (3) | 0.2656 (3) | 0.81738 (17) | 0.0625 (11) | |
H51 | 0.5733 | 0.2635 | 0.8547 | 0.075* | |
C52 | 0.4525 (4) | 0.0720 (3) | 0.73958 (18) | 0.0801 (15) | |
H52 | 0.4579 | 0.0446 | 0.7095 | 0.096* | |
C53 | 0.4384 (5) | 0.0365 (4) | 0.7919 (2) | 0.104 (2) | |
H53 | 0.4331 | −0.0175 | 0.8037 | 0.124* | |
C54 | 0.4340 (4) | 0.0974 (3) | 0.82229 (18) | 0.0786 (15) | |
H54 | 0.4246 | 0.0929 | 0.8597 | 0.094* | |
C55 | 0.2720 (3) | 0.4349 (3) | 0.72112 (17) | 0.0562 (10) | |
H55 | 0.2515 | 0.4662 | 0.6882 | 0.067* | |
C56 | 0.2217 (3) | 0.4589 (3) | 0.77061 (18) | 0.0631 (11) | |
H56 | 0.1629 | 0.5075 | 0.7774 | 0.076* | |
C57 | 0.2776 (3) | 0.3952 (3) | 0.80749 (17) | 0.0580 (10) | |
H57 | 0.2630 | 0.3928 | 0.8447 | 0.070* | |
C58 | 0.7418 (2) | 0.2770 (2) | 0.97547 (14) | 0.0447 (8) | |
C59 | 0.6632 (3) | 0.2596 (3) | 0.98277 (17) | 0.0558 (10) | |
H59 | 0.6582 | 0.2095 | 1.0037 | 0.067* | |
C60 | 0.5982 (3) | 0.3290 (3) | 0.95392 (17) | 0.0573 (10) | |
H60 | 0.5408 | 0.3348 | 0.9506 | 0.069* | |
C61 | 0.6343 (2) | 0.3919 (3) | 0.92943 (15) | 0.0457 (8) | |
C62 | 0.5815 (2) | 0.4807 (3) | 0.90399 (15) | 0.0461 (8) | |
C63 | 0.6114 (2) | 0.5482 (2) | 0.88756 (15) | 0.0471 (9) | |
C64 | 0.5520 (3) | 0.6445 (3) | 0.87306 (18) | 0.0595 (11) | |
H64 | 0.4884 | 0.6720 | 0.8725 | 0.071* | |
C65 | 0.6050 (3) | 0.6872 (3) | 0.86049 (18) | 0.0614 (11) | |
H65 | 0.5847 | 0.7500 | 0.8494 | 0.074* | |
C66 | 0.6991 (3) | 0.6189 (2) | 0.86710 (15) | 0.0477 (9) | |
C67 | 0.7752 (3) | 0.6366 (2) | 0.85929 (15) | 0.0490 (9) | |
C68 | 0.8648 (3) | 0.5729 (2) | 0.87425 (14) | 0.0447 (8) | |
C69 | 0.9417 (3) | 0.5923 (3) | 0.86766 (16) | 0.0535 (10) | |
H69 | 0.9437 | 0.6460 | 0.8501 | 0.064* | |
C70 | 1.0104 (3) | 0.5186 (3) | 0.89149 (16) | 0.0522 (9) | |
H70 | 1.0688 | 0.5117 | 0.8932 | 0.063* | |
C71 | 0.9772 (2) | 0.4528 (2) | 0.91367 (14) | 0.0435 (8) | |
C72 | 1.0247 (2) | 0.3694 (2) | 0.94671 (14) | 0.0417 (8) | |
C73 | 0.9894 (2) | 0.3082 (2) | 0.97117 (14) | 0.0425 (8) | |
C74 | 1.0267 (3) | 0.2377 (3) | 1.01523 (15) | 0.0532 (10) | |
H74 | 1.0798 | 0.2224 | 1.0302 | 0.064* | |
C75 | 0.9705 (3) | 0.1984 (3) | 1.03051 (15) | 0.0523 (9) | |
H75 | 0.9776 | 0.1510 | 1.0582 | 0.063* | |
C76 | 0.8975 (2) | 0.2427 (2) | 0.99650 (14) | 0.0429 (8) | |
C77 | 0.8220 (2) | 0.2243 (2) | 1.00157 (14) | 0.0450 (8) | |
C78 | 0.48192 (12) | 0.50799 (18) | 0.89787 (10) | 0.0480 (9) | |
C79 | 0.45767 (15) | 0.51111 (19) | 0.84789 (8) | 0.0578 (10) | |
H79 | 0.5028 | 0.4939 | 0.8184 | 0.069* | |
C80 | 0.36602 (17) | 0.5400 (2) | 0.84192 (9) | 0.0640 (11) | |
H80 | 0.3498 | 0.5421 | 0.8085 | 0.077* | |
C81 | 0.29863 (12) | 0.56571 (19) | 0.88593 (11) | 0.0570 (10) | |
C82 | 0.32287 (14) | 0.5626 (2) | 0.93591 (9) | 0.0677 (12) | |
H82 | 0.2778 | 0.5798 | 0.9654 | 0.081* | |
C83 | 0.41452 (16) | 0.5337 (2) | 0.94188 (8) | 0.0673 (12) | |
H83 | 0.4307 | 0.5316 | 0.9753 | 0.081* | |
C84 | 0.1964 (3) | 0.6028 (4) | 0.8796 (2) | 0.0860 (16) | |
H84A | 0.1663 | 0.5832 | 0.9116 | 0.129* | |
H84B | 0.1916 | 0.5792 | 0.8493 | 0.129* | |
H84C | 0.1673 | 0.6692 | 0.8740 | 0.129* | |
C85 | 0.7594 (2) | 0.73294 (14) | 0.83665 (11) | 0.0548 (10) | |
C86 | 0.7408 (3) | 0.76536 (19) | 0.78365 (11) | 0.0844 (15) | |
H86 | 0.7391 | 0.7271 | 0.7618 | 0.101* | |
C87 | 0.7246 (3) | 0.8550 (2) | 0.76327 (11) | 0.0950 (18) | |
H87 | 0.7122 | 0.8767 | 0.7278 | 0.114* | |
C88 | 0.7271 (2) | 0.91228 (15) | 0.79588 (15) | 0.0833 (15) | |
C89 | 0.7457 (3) | 0.87986 (18) | 0.84888 (14) | 0.0903 (17) | |
H89 | 0.7474 | 0.9182 | 0.8707 | 0.108* | |
C90 | 0.7618 (2) | 0.7902 (2) | 0.86926 (10) | 0.0760 (13) | |
H90 | 0.7743 | 0.7685 | 0.9047 | 0.091* | |
C91 | 0.7080 (5) | 1.0114 (3) | 0.7720 (3) | 0.125 (3) | |
H91A | 0.6778 | 1.0280 | 0.7402 | 0.187* | |
H91B | 0.7653 | 1.0144 | 0.7629 | 0.187* | |
H91C | 0.6690 | 1.0537 | 0.7980 | 0.187* | |
C92 | 1.12048 (12) | 0.34652 (17) | 0.95883 (10) | 0.0458 (8) | |
C93 | 1.13340 (14) | 0.40831 (14) | 0.98216 (11) | 0.0550 (10) | |
H93 | 1.0832 | 0.4639 | 0.9913 | 0.066* | |
C94 | 1.22140 (17) | 0.38707 (18) | 0.99181 (11) | 0.0609 (11) | |
H94 | 1.2300 | 0.4284 | 1.0074 | 0.073* | |
C95 | 1.29646 (12) | 0.3040 (2) | 0.97812 (12) | 0.0636 (11) | |
C96 | 1.28354 (13) | 0.24225 (16) | 0.95479 (12) | 0.0655 (11) | |
H96 | 1.3338 | 0.1867 | 0.9456 | 0.079* | |
C97 | 1.19555 (16) | 0.26349 (15) | 0.94514 (11) | 0.0569 (10) | |
H97 | 1.1869 | 0.2221 | 0.9295 | 0.068* | |
C98 | 1.3932 (3) | 0.2829 (5) | 0.9880 (3) | 0.105 (2) | |
H98A | 1.3945 | 0.2812 | 1.0258 | 0.158* | |
H98B | 1.4081 | 0.3303 | 0.9683 | 0.158* | |
H98C | 1.4377 | 0.2240 | 0.9761 | 0.158* | |
C99 | 0.82433 (19) | 0.14297 (14) | 1.04081 (9) | 0.0479 (9) | |
C100 | 0.8828 (2) | 0.05375 (17) | 1.02709 (10) | 0.0803 (15) | |
H100 | 0.9194 | 0.0448 | 0.9940 | 0.096* | |
C101 | 0.8864 (2) | −0.02211 (13) | 1.06279 (12) | 0.0907 (17) | |
H101 | 0.9255 | −0.0818 | 1.0536 | 0.109* | |
C102 | 0.8317 (2) | −0.00875 (16) | 1.11219 (11) | 0.0704 (12) | |
C103 | 0.7733 (2) | 0.08048 (19) | 1.12591 (9) | 0.0846 (16) | |
H103 | 0.7367 | 0.0894 | 1.1590 | 0.101* | |
C104 | 0.7696 (2) | 0.15634 (14) | 1.09022 (10) | 0.0752 (14) | |
H104 | 0.7305 | 0.2160 | 1.0994 | 0.090* | |
C105 | 0.8367 (5) | −0.0927 (4) | 1.1519 (2) | 0.107 (2) | |
H10A | 0.7771 | −0.0777 | 1.1718 | 0.160* | |
H10B | 0.8809 | −0.1084 | 1.1763 | 0.160* | |
H10C | 0.8554 | −0.1443 | 1.1323 | 0.160* | |
C106 | 0.8696 (4) | 0.1533 (3) | 0.8743 (2) | 0.0813 (15) | |
H106 | 0.8511 | 0.1467 | 0.9110 | 0.098* | |
C107 | 0.8985 (5) | 0.0862 (4) | 0.8408 (2) | 0.0979 (19) | |
H107 | 0.9030 | 0.0273 | 0.8499 | 0.118* | |
C108 | 0.9192 (4) | 0.1245 (3) | 0.7915 (2) | 0.0807 (15) | |
H108 | 0.9410 | 0.0956 | 0.7601 | 0.097* | |
C109 | 0.7038 (3) | 0.4920 (3) | 0.76419 (17) | 0.0660 (12) | |
H109 | 0.6592 | 0.5409 | 0.7829 | 0.079* | |
C110 | 0.6990 (4) | 0.4808 (4) | 0.7129 (2) | 0.0838 (15) | |
H110 | 0.6525 | 0.5182 | 0.6911 | 0.101* | |
C111 | 0.7784 (4) | 0.4021 (4) | 0.70145 (17) | 0.0775 (14) | |
H111 | 0.7962 | 0.3760 | 0.6692 | 0.093* | |
C112 | 1.0653 (3) | 0.3376 (3) | 0.80769 (16) | 0.0552 (10) | |
H112 | 1.0793 | 0.3604 | 0.8336 | 0.066* | |
C113 | 1.1254 (3) | 0.3001 (3) | 0.76312 (17) | 0.0617 (11) | |
H113 | 1.1852 | 0.2927 | 0.7532 | 0.074* | |
C114 | 1.0772 (3) | 0.2766 (3) | 0.73732 (17) | 0.0630 (11) | |
H114 | 1.0991 | 0.2492 | 0.7054 | 0.076* | |
C115 | 0.9965 (8) | 0.7857 (9) | 0.7792 (3) | 0.305 (8) | |
H11A | 1.0375 | 0.7236 | 0.7926 | 0.458* | |
H11B | 0.9378 | 0.7896 | 0.7764 | 0.458* | |
H11C | 0.9880 | 0.8278 | 0.8034 | 0.458* | |
C116 | 1.0362 (5) | 0.8099 (5) | 0.7259 (2) | 0.164 (3) | |
C117 | 1.1209 (4) | 0.7460 (3) | 0.7028 (3) | 0.152 (3) | |
H117 | 1.1525 | 0.6877 | 0.7212 | 0.183* | |
C118 | 1.1584 (4) | 0.7693 (5) | 0.6523 (3) | 0.197 (5) | |
H18A | 1.2151 | 0.7265 | 0.6369 | 0.237* | |
C119 | 1.1112 (6) | 0.8565 (6) | 0.6249 (2) | 0.169 (4) | |
H119 | 1.1363 | 0.8720 | 0.5911 | 0.203* | |
C120 | 1.0265 (5) | 0.9204 (4) | 0.6480 (3) | 0.183 (4) | |
H120 | 0.9949 | 0.9787 | 0.6297 | 0.220* | |
C121 | 0.9890 (4) | 0.8971 (4) | 0.6985 (3) | 0.154 (3) | |
H121 | 0.9323 | 0.9399 | 0.7140 | 0.184* | |
C122 | 1.0363 (5) | 0.2584 (4) | 0.4021 (2) | 0.141 (3) | |
H12A | 0.9780 | 0.2634 | 0.3976 | 0.211* | |
H12B | 1.0330 | 0.2744 | 0.4372 | 0.211* | |
H12C | 1.0838 | 0.1960 | 0.3987 | 0.211* | |
C123 | 1.0580 (5) | 0.3216 (3) | 0.3608 (2) | 0.1055 (19) | |
C124 | 1.1425 (4) | 0.3241 (4) | 0.3612 (3) | 0.0979 (18) | |
H12F | 1.1819 | 0.2863 | 0.3869 | 0.117* | |
C125 | 1.1641 (5) | 0.3806 (5) | 0.3246 (3) | 0.125 (2) | |
H125 | 1.2191 | 0.3823 | 0.3250 | 0.151* | |
C126 | 1.1028 (6) | 0.4416 (4) | 0.2828 (3) | 0.120 (2) | |
H126 | 1.1179 | 0.4815 | 0.2570 | 0.144* | |
C127 | 1.0276 (6) | 0.4361 (5) | 0.2842 (3) | 0.119 (2) | |
H127 | 0.9881 | 0.4728 | 0.2583 | 0.143* | |
C128 | 1.0022 (4) | 0.3769 (3) | 0.3231 (2) | 0.0951 (17) | |
H128 | 0.9467 | 0.3762 | 0.3227 | 0.114* | |
C129 | 0.1921 (5) | 1.0193 (4) | 0.6989 (2) | 0.150 (3) | |
H12H | 0.1336 | 1.0202 | 0.7003 | 0.225* | |
H12I | 0.2151 | 1.0298 | 0.6621 | 0.225* | |
H12J | 0.1846 | 1.0672 | 0.7185 | 0.225* | |
C130 | 0.2587 (3) | 0.9280 (2) | 0.72326 (13) | 0.0985 (18) | |
C131 | 0.2295 (3) | 0.8614 (3) | 0.74347 (17) | 0.111 (2) | |
H131 | 0.1690 | 0.8743 | 0.7416 | 0.133* | |
C132 | 0.2907 (4) | 0.7753 (3) | 0.76648 (17) | 0.123 (2) | |
H132 | 0.2711 | 0.7306 | 0.7800 | 0.148* | |
C133 | 0.3810 (4) | 0.7559 (3) | 0.76928 (16) | 0.124 (2) | |
H133 | 0.4220 | 0.6983 | 0.7847 | 0.149* | |
C134 | 0.4103 (2) | 0.8225 (4) | 0.74906 (18) | 0.122 (2) | |
H124 | 0.4707 | 0.8096 | 0.7509 | 0.147* | |
C135 | 0.3491 (3) | 0.9086 (3) | 0.72606 (15) | 0.0981 (17) | |
H135 | 0.3687 | 0.9533 | 0.7125 | 0.118* | |
C136 | 0.430 (2) | −0.0286 (14) | 0.9639 (11) | 0.370 (17) | 0.50 |
H13A | 0.3782 | −0.0247 | 0.9899 | 0.555* | 0.50 |
H13B | 0.4664 | −0.0911 | 0.9552 | 0.555* | 0.50 |
H13C | 0.4074 | 0.0117 | 0.9319 | 0.555* | 0.50 |
C137 | 0.4882 (19) | 0.0007 (9) | 0.9872 (9) | 0.370 (17) | 0.50 |
C138 | 0.457 (2) | 0.0311 (12) | 1.0381 (9) | 0.370 (17) | 0.50 |
H138 | 0.4023 | 0.0330 | 1.0565 | 0.444* | 0.50 |
C139 | 0.508 (3) | 0.0587 (11) | 1.0614 (8) | 0.370 (17) | 0.50 |
H139 | 0.4868 | 0.0791 | 1.0954 | 0.444* | 0.50 |
C140 | 0.590 (2) | 0.0559 (10) | 1.0339 (10) | 0.370 (17) | 0.50 |
H140 | 0.6234 | 0.0744 | 1.0496 | 0.444* | 0.50 |
C141 | 0.621 (2) | 0.0255 (11) | 0.9831 (10) | 0.370 (17) | 0.50 |
H141 | 0.6755 | 0.0236 | 0.9647 | 0.444* | 0.50 |
C142 | 0.570 (2) | −0.0022 (9) | 0.9598 (7) | 0.370 (17) | 0.50 |
H142 | 0.5909 | −0.0225 | 0.9257 | 0.444* | 0.50 |
U11 | U22 | U33 | U12 | U13 | U23 | |
Sm1 | 0.03464 (9) | 0.02702 (8) | 0.03449 (9) | −0.01687 (7) | −0.00639 (7) | −0.00408 (6) |
Sm2 | 0.04230 (11) | 0.04041 (10) | 0.03538 (10) | −0.02316 (8) | −0.00873 (8) | −0.00238 (7) |
N1 | 0.0364 (15) | 0.0282 (13) | 0.0394 (15) | −0.0167 (11) | −0.0076 (12) | −0.0052 (11) |
N2 | 0.0375 (15) | 0.0273 (13) | 0.0421 (15) | −0.0172 (12) | −0.0073 (12) | −0.0039 (11) |
N3 | 0.0361 (15) | 0.0257 (12) | 0.0440 (15) | −0.0154 (11) | −0.0082 (12) | −0.0056 (11) |
N4 | 0.0376 (15) | 0.0280 (13) | 0.0425 (15) | −0.0183 (12) | −0.0070 (12) | −0.0066 (11) |
N5 | 0.0531 (19) | 0.066 (2) | 0.0404 (17) | −0.0346 (16) | −0.0094 (14) | −0.0081 (14) |
N6 | 0.0550 (19) | 0.0529 (17) | 0.0384 (17) | −0.0274 (15) | −0.0106 (14) | −0.0081 (13) |
N7 | 0.078 (2) | 0.0490 (18) | 0.0410 (17) | −0.0397 (17) | −0.0012 (16) | −0.0051 (13) |
N8 | 0.067 (2) | 0.0486 (17) | 0.0398 (17) | −0.0318 (16) | −0.0041 (15) | −0.0002 (13) |
N9 | 0.0477 (18) | 0.0492 (17) | 0.0443 (18) | −0.0145 (15) | −0.0048 (14) | −0.0120 (14) |
N10 | 0.0522 (19) | 0.0498 (17) | 0.0417 (17) | −0.0243 (15) | 0.0000 (14) | −0.0116 (13) |
N11 | 0.0398 (16) | 0.0472 (16) | 0.0473 (17) | −0.0231 (14) | −0.0102 (13) | 0.0008 (13) |
N12 | 0.0464 (17) | 0.0446 (16) | 0.0476 (17) | −0.0259 (14) | −0.0132 (14) | −0.0002 (13) |
N13 | 0.0406 (16) | 0.0445 (16) | 0.0415 (16) | −0.0213 (13) | −0.0103 (13) | −0.0030 (12) |
N14 | 0.0401 (16) | 0.0460 (16) | 0.0392 (16) | −0.0213 (13) | −0.0071 (13) | −0.0023 (12) |
N15 | 0.083 (2) | 0.0540 (19) | 0.0503 (19) | −0.0418 (18) | −0.0057 (17) | −0.0091 (15) |
N16 | 0.079 (2) | 0.061 (2) | 0.054 (2) | −0.0434 (19) | −0.0017 (17) | −0.0176 (16) |
N17 | 0.068 (2) | 0.070 (2) | 0.0427 (18) | −0.0360 (19) | −0.0159 (16) | −0.0021 (16) |
N18 | 0.080 (2) | 0.075 (2) | 0.0427 (19) | −0.049 (2) | −0.0120 (17) | −0.0047 (16) |
N19 | 0.058 (2) | 0.0579 (19) | 0.0475 (18) | −0.0334 (16) | −0.0004 (15) | −0.0134 (15) |
N20 | 0.070 (2) | 0.0601 (19) | 0.0417 (17) | −0.0373 (18) | 0.0041 (16) | −0.0147 (15) |
B1 | 0.060 (3) | 0.054 (2) | 0.032 (2) | −0.029 (2) | −0.0063 (19) | −0.0050 (18) |
B2 | 0.091 (4) | 0.070 (3) | 0.042 (2) | −0.050 (3) | −0.002 (2) | −0.018 (2) |
C1 | 0.0435 (19) | 0.0308 (16) | 0.0360 (17) | −0.0233 (15) | −0.0050 (14) | −0.0058 (13) |
C2 | 0.050 (2) | 0.0330 (17) | 0.056 (2) | −0.0273 (16) | −0.0086 (17) | −0.0049 (15) |
C3 | 0.046 (2) | 0.0426 (19) | 0.055 (2) | −0.0307 (17) | −0.0066 (17) | −0.0076 (16) |
C4 | 0.0391 (18) | 0.0349 (16) | 0.0388 (18) | −0.0207 (15) | −0.0074 (14) | −0.0073 (13) |
C5 | 0.0372 (18) | 0.0351 (17) | 0.0416 (18) | −0.0181 (14) | −0.0070 (14) | −0.0073 (14) |
C6 | 0.0373 (18) | 0.0327 (16) | 0.0415 (18) | −0.0176 (14) | −0.0062 (14) | −0.0053 (13) |
C7 | 0.0352 (19) | 0.0334 (17) | 0.070 (3) | −0.0130 (15) | −0.0048 (17) | −0.0084 (16) |
C8 | 0.042 (2) | 0.0278 (16) | 0.071 (3) | −0.0148 (15) | −0.0045 (18) | −0.0095 (16) |
C9 | 0.0402 (18) | 0.0286 (15) | 0.0439 (19) | −0.0176 (14) | −0.0034 (15) | −0.0049 (13) |
C10 | 0.0438 (19) | 0.0255 (15) | 0.0402 (18) | −0.0185 (14) | −0.0037 (15) | −0.0052 (13) |
C11 | 0.0448 (19) | 0.0308 (16) | 0.0396 (18) | −0.0220 (15) | −0.0063 (15) | −0.0062 (13) |
C12 | 0.052 (2) | 0.0346 (17) | 0.057 (2) | −0.0292 (17) | −0.0089 (17) | −0.0092 (15) |
C13 | 0.043 (2) | 0.0385 (18) | 0.064 (2) | −0.0248 (16) | −0.0142 (17) | −0.0069 (16) |
C14 | 0.0376 (18) | 0.0371 (17) | 0.0408 (18) | −0.0217 (15) | −0.0065 (14) | −0.0071 (14) |
C15 | 0.0368 (18) | 0.0366 (17) | 0.0395 (18) | −0.0191 (14) | −0.0093 (14) | −0.0053 (14) |
C16 | 0.0389 (18) | 0.0328 (16) | 0.0389 (18) | −0.0169 (14) | −0.0123 (14) | −0.0046 (13) |
C17 | 0.043 (2) | 0.0358 (17) | 0.058 (2) | −0.0148 (16) | −0.0223 (17) | −0.0006 (15) |
C18 | 0.050 (2) | 0.0264 (16) | 0.061 (2) | −0.0154 (15) | −0.0209 (18) | 0.0001 (15) |
C19 | 0.0423 (18) | 0.0266 (15) | 0.0420 (18) | −0.0168 (14) | −0.0099 (15) | −0.0042 (13) |
C20 | 0.0454 (19) | 0.0272 (15) | 0.0371 (17) | −0.0195 (14) | −0.0063 (14) | −0.0053 (13) |
C21 | 0.0353 (18) | 0.0339 (16) | 0.050 (2) | −0.0176 (14) | −0.0054 (15) | −0.0062 (14) |
C22 | 0.042 (2) | 0.069 (3) | 0.062 (3) | −0.0202 (19) | −0.0074 (18) | −0.027 (2) |
C23 | 0.042 (2) | 0.080 (3) | 0.079 (3) | −0.022 (2) | −0.016 (2) | −0.028 (2) |
C24 | 0.039 (2) | 0.048 (2) | 0.078 (3) | −0.0196 (17) | −0.008 (2) | −0.0050 (19) |
C25 | 0.053 (2) | 0.088 (3) | 0.059 (3) | −0.039 (2) | 0.008 (2) | −0.020 (2) |
C26 | 0.052 (2) | 0.081 (3) | 0.054 (2) | −0.039 (2) | −0.0016 (19) | −0.018 (2) |
C27 | 0.042 (2) | 0.093 (4) | 0.107 (4) | −0.029 (2) | −0.003 (2) | −0.012 (3) |
C28 | 0.0402 (18) | 0.0260 (15) | 0.051 (2) | −0.0171 (14) | −0.0043 (15) | −0.0075 (14) |
C29 | 0.081 (3) | 0.0353 (18) | 0.052 (2) | −0.0303 (19) | −0.001 (2) | −0.0077 (16) |
C30 | 0.077 (3) | 0.041 (2) | 0.063 (3) | −0.028 (2) | 0.000 (2) | −0.0207 (18) |
C31 | 0.040 (2) | 0.0282 (17) | 0.080 (3) | −0.0174 (15) | −0.0029 (18) | −0.0130 (17) |
C32 | 0.077 (3) | 0.0316 (18) | 0.069 (3) | −0.0249 (19) | −0.008 (2) | 0.0037 (17) |
C33 | 0.076 (3) | 0.0367 (19) | 0.052 (2) | −0.0246 (19) | −0.011 (2) | −0.0046 (16) |
C34 | 0.065 (3) | 0.033 (2) | 0.121 (4) | −0.0239 (19) | −0.002 (3) | −0.022 (2) |
C35 | 0.0380 (18) | 0.0340 (16) | 0.0452 (19) | −0.0204 (14) | −0.0125 (15) | 0.0007 (14) |
C36 | 0.047 (2) | 0.077 (3) | 0.061 (3) | −0.029 (2) | −0.0092 (19) | −0.023 (2) |
C37 | 0.061 (3) | 0.086 (3) | 0.068 (3) | −0.042 (2) | −0.022 (2) | −0.013 (2) |
C38 | 0.045 (2) | 0.055 (2) | 0.078 (3) | −0.0279 (19) | −0.024 (2) | 0.011 (2) |
C39 | 0.041 (2) | 0.086 (3) | 0.068 (3) | −0.024 (2) | −0.004 (2) | −0.010 (2) |
C40 | 0.046 (2) | 0.069 (3) | 0.050 (2) | −0.022 (2) | −0.0098 (18) | −0.0119 (19) |
C41 | 0.054 (3) | 0.102 (4) | 0.122 (5) | −0.042 (3) | −0.034 (3) | 0.010 (3) |
C42 | 0.0402 (18) | 0.0269 (15) | 0.048 (2) | −0.0173 (14) | −0.0090 (15) | −0.0065 (14) |
C43 | 0.087 (3) | 0.044 (2) | 0.050 (2) | −0.035 (2) | 0.004 (2) | −0.0128 (17) |
C44 | 0.100 (4) | 0.045 (2) | 0.075 (3) | −0.037 (2) | 0.012 (3) | −0.028 (2) |
C45 | 0.049 (2) | 0.0269 (17) | 0.092 (3) | −0.0182 (16) | −0.008 (2) | −0.0085 (19) |
C46 | 0.102 (4) | 0.043 (2) | 0.062 (3) | −0.039 (2) | −0.032 (2) | 0.0134 (19) |
C47 | 0.114 (4) | 0.040 (2) | 0.049 (2) | −0.041 (2) | −0.023 (2) | −0.0004 (17) |
C48 | 0.084 (4) | 0.030 (2) | 0.160 (5) | −0.025 (2) | −0.014 (3) | −0.013 (3) |
C49 | 0.064 (3) | 0.103 (3) | 0.054 (3) | −0.055 (3) | −0.007 (2) | −0.014 (2) |
C50 | 0.072 (3) | 0.118 (4) | 0.065 (3) | −0.059 (3) | −0.019 (2) | −0.018 (3) |
C51 | 0.074 (3) | 0.077 (3) | 0.049 (2) | −0.038 (2) | −0.022 (2) | −0.011 (2) |
C52 | 0.143 (5) | 0.070 (3) | 0.056 (3) | −0.077 (3) | 0.007 (3) | −0.009 (2) |
C53 | 0.196 (7) | 0.085 (4) | 0.063 (3) | −0.103 (4) | 0.012 (4) | −0.004 (3) |
C54 | 0.128 (4) | 0.072 (3) | 0.049 (3) | −0.065 (3) | 0.001 (3) | 0.005 (2) |
C55 | 0.048 (2) | 0.055 (2) | 0.056 (2) | −0.0122 (19) | −0.0090 (19) | −0.0158 (19) |
C56 | 0.049 (2) | 0.061 (3) | 0.068 (3) | −0.013 (2) | 0.000 (2) | −0.025 (2) |
C57 | 0.056 (2) | 0.068 (3) | 0.051 (2) | −0.030 (2) | 0.009 (2) | −0.024 (2) |
C58 | 0.046 (2) | 0.047 (2) | 0.043 (2) | −0.0255 (17) | −0.0033 (16) | 0.0001 (15) |
C59 | 0.055 (2) | 0.058 (2) | 0.062 (3) | −0.037 (2) | −0.008 (2) | 0.0064 (19) |
C60 | 0.046 (2) | 0.067 (3) | 0.070 (3) | −0.036 (2) | −0.012 (2) | 0.001 (2) |
C61 | 0.040 (2) | 0.054 (2) | 0.048 (2) | −0.0254 (17) | −0.0079 (16) | −0.0036 (16) |
C62 | 0.040 (2) | 0.056 (2) | 0.047 (2) | −0.0241 (17) | −0.0104 (16) | −0.0045 (17) |
C63 | 0.044 (2) | 0.050 (2) | 0.051 (2) | −0.0209 (17) | −0.0161 (17) | −0.0037 (16) |
C64 | 0.044 (2) | 0.052 (2) | 0.081 (3) | −0.0163 (19) | −0.023 (2) | −0.003 (2) |
C65 | 0.055 (2) | 0.042 (2) | 0.086 (3) | −0.0179 (19) | −0.025 (2) | 0.001 (2) |
C66 | 0.052 (2) | 0.0418 (19) | 0.054 (2) | −0.0222 (17) | −0.0183 (18) | −0.0007 (16) |
C67 | 0.057 (2) | 0.044 (2) | 0.051 (2) | −0.0254 (18) | −0.0134 (18) | −0.0024 (16) |
C68 | 0.052 (2) | 0.0458 (19) | 0.043 (2) | −0.0274 (17) | −0.0081 (17) | −0.0044 (15) |
C69 | 0.059 (2) | 0.053 (2) | 0.061 (2) | −0.037 (2) | −0.006 (2) | −0.0025 (18) |
C70 | 0.050 (2) | 0.062 (2) | 0.059 (2) | −0.036 (2) | −0.0069 (19) | −0.0093 (19) |
C71 | 0.043 (2) | 0.052 (2) | 0.043 (2) | −0.0253 (17) | −0.0030 (16) | −0.0144 (16) |
C72 | 0.0377 (19) | 0.051 (2) | 0.0407 (19) | −0.0211 (16) | −0.0061 (15) | −0.0104 (16) |
C73 | 0.0366 (19) | 0.052 (2) | 0.0389 (19) | −0.0191 (16) | −0.0049 (15) | −0.0088 (15) |
C74 | 0.044 (2) | 0.063 (2) | 0.049 (2) | −0.0209 (19) | −0.0160 (18) | 0.0016 (18) |
C75 | 0.049 (2) | 0.055 (2) | 0.047 (2) | −0.0210 (19) | −0.0134 (18) | 0.0073 (17) |
C76 | 0.042 (2) | 0.0443 (19) | 0.0372 (19) | −0.0177 (16) | −0.0041 (15) | −0.0001 (15) |
C77 | 0.046 (2) | 0.0457 (19) | 0.041 (2) | −0.0220 (17) | −0.0022 (16) | 0.0000 (15) |
C78 | 0.043 (2) | 0.050 (2) | 0.055 (2) | −0.0224 (17) | −0.0164 (18) | −0.0030 (17) |
C79 | 0.050 (2) | 0.074 (3) | 0.056 (2) | −0.032 (2) | −0.0090 (19) | −0.010 (2) |
C80 | 0.058 (3) | 0.082 (3) | 0.064 (3) | −0.037 (2) | −0.022 (2) | −0.007 (2) |
C81 | 0.043 (2) | 0.048 (2) | 0.087 (3) | −0.0203 (18) | −0.020 (2) | −0.014 (2) |
C82 | 0.046 (2) | 0.084 (3) | 0.077 (3) | −0.026 (2) | −0.006 (2) | −0.031 (2) |
C83 | 0.050 (2) | 0.096 (3) | 0.060 (3) | −0.029 (2) | −0.009 (2) | −0.026 (2) |
C84 | 0.049 (3) | 0.093 (4) | 0.122 (4) | −0.026 (3) | −0.024 (3) | −0.031 (3) |
C85 | 0.055 (2) | 0.045 (2) | 0.068 (3) | −0.0255 (18) | −0.013 (2) | −0.0022 (18) |
C86 | 0.119 (4) | 0.063 (3) | 0.080 (3) | −0.045 (3) | −0.044 (3) | 0.014 (2) |
C87 | 0.122 (5) | 0.070 (3) | 0.097 (4) | −0.049 (3) | −0.049 (4) | 0.030 (3) |
C88 | 0.071 (3) | 0.046 (2) | 0.123 (5) | −0.023 (2) | −0.015 (3) | 0.007 (3) |
C89 | 0.111 (4) | 0.060 (3) | 0.108 (4) | −0.048 (3) | 0.005 (4) | −0.022 (3) |
C90 | 0.102 (4) | 0.060 (3) | 0.074 (3) | −0.045 (3) | −0.003 (3) | −0.009 (2) |
C91 | 0.118 (5) | 0.048 (3) | 0.192 (7) | −0.034 (3) | −0.027 (5) | 0.021 (4) |
C92 | 0.041 (2) | 0.062 (2) | 0.0390 (19) | −0.0260 (18) | −0.0048 (16) | −0.0083 (16) |
C93 | 0.044 (2) | 0.069 (3) | 0.058 (2) | −0.0272 (19) | −0.0049 (18) | −0.019 (2) |
C94 | 0.054 (2) | 0.084 (3) | 0.060 (3) | −0.039 (2) | −0.008 (2) | −0.018 (2) |
C95 | 0.041 (2) | 0.097 (3) | 0.058 (3) | −0.038 (2) | −0.0065 (19) | −0.004 (2) |
C96 | 0.041 (2) | 0.076 (3) | 0.072 (3) | −0.020 (2) | −0.003 (2) | −0.013 (2) |
C97 | 0.046 (2) | 0.062 (2) | 0.064 (3) | −0.023 (2) | −0.0038 (19) | −0.017 (2) |
C98 | 0.051 (3) | 0.149 (6) | 0.128 (5) | −0.049 (3) | −0.017 (3) | −0.025 (4) |
C99 | 0.049 (2) | 0.048 (2) | 0.045 (2) | −0.0240 (18) | −0.0050 (17) | 0.0023 (16) |
C100 | 0.085 (3) | 0.053 (3) | 0.065 (3) | −0.013 (2) | 0.018 (3) | −0.002 (2) |
C101 | 0.109 (4) | 0.042 (2) | 0.083 (4) | −0.016 (3) | 0.011 (3) | 0.000 (2) |
C102 | 0.092 (3) | 0.058 (3) | 0.059 (3) | −0.037 (3) | −0.014 (2) | 0.011 (2) |
C103 | 0.129 (5) | 0.065 (3) | 0.049 (3) | −0.048 (3) | 0.016 (3) | −0.001 (2) |
C104 | 0.102 (4) | 0.056 (3) | 0.055 (3) | −0.034 (3) | 0.012 (3) | −0.006 (2) |
C105 | 0.155 (6) | 0.068 (3) | 0.089 (4) | −0.055 (4) | −0.016 (4) | 0.024 (3) |
C106 | 0.133 (5) | 0.061 (3) | 0.063 (3) | −0.059 (3) | −0.002 (3) | −0.006 (2) |
C107 | 0.161 (6) | 0.063 (3) | 0.088 (4) | −0.070 (4) | 0.001 (4) | −0.013 (3) |
C108 | 0.116 (4) | 0.067 (3) | 0.078 (3) | −0.054 (3) | −0.001 (3) | −0.029 (3) |
C109 | 0.069 (3) | 0.079 (3) | 0.051 (2) | −0.034 (2) | −0.023 (2) | 0.007 (2) |
C110 | 0.100 (4) | 0.103 (4) | 0.060 (3) | −0.052 (4) | −0.040 (3) | 0.013 (3) |
C111 | 0.115 (4) | 0.106 (4) | 0.040 (2) | −0.071 (4) | −0.027 (3) | 0.004 (2) |
C112 | 0.061 (3) | 0.058 (2) | 0.051 (2) | −0.033 (2) | −0.0010 (19) | −0.0078 (18) |
C113 | 0.061 (3) | 0.065 (3) | 0.061 (3) | −0.035 (2) | 0.012 (2) | −0.013 (2) |
C114 | 0.079 (3) | 0.063 (3) | 0.051 (2) | −0.040 (2) | 0.012 (2) | −0.015 (2) |
C115 | 0.296 (11) | 0.352 (12) | 0.286 (11) | −0.188 (9) | −0.010 (8) | 0.009 (8) |
C116 | 0.161 (7) | 0.187 (7) | 0.188 (7) | −0.118 (6) | −0.036 (6) | 0.003 (6) |
C117 | 0.140 (6) | 0.133 (5) | 0.225 (8) | −0.075 (5) | −0.063 (6) | −0.037 (5) |
C118 | 0.177 (8) | 0.219 (8) | 0.246 (9) | −0.103 (7) | −0.035 (7) | −0.096 (7) |
C119 | 0.178 (7) | 0.212 (8) | 0.177 (7) | −0.123 (6) | −0.039 (6) | −0.038 (6) |
C120 | 0.206 (8) | 0.175 (7) | 0.219 (8) | −0.115 (6) | −0.072 (7) | −0.011 (6) |
C121 | 0.154 (6) | 0.137 (6) | 0.186 (7) | −0.070 (5) | −0.060 (6) | −0.006 (5) |
C122 | 0.195 (7) | 0.117 (5) | 0.129 (5) | −0.096 (5) | 0.003 (5) | −0.008 (4) |
C123 | 0.142 (5) | 0.083 (4) | 0.095 (4) | −0.051 (4) | −0.012 (4) | −0.019 (3) |
C124 | 0.075 (3) | 0.109 (4) | 0.124 (5) | −0.044 (3) | −0.012 (3) | −0.042 (4) |
C125 | 0.117 (5) | 0.129 (5) | 0.132 (6) | −0.058 (4) | −0.001 (4) | −0.029 (4) |
C126 | 0.144 (6) | 0.108 (5) | 0.113 (5) | −0.073 (4) | 0.015 (4) | −0.013 (4) |
C127 | 0.132 (5) | 0.112 (5) | 0.118 (5) | −0.055 (4) | −0.017 (4) | −0.023 (4) |
C128 | 0.107 (4) | 0.085 (4) | 0.100 (4) | −0.044 (3) | −0.032 (3) | −0.006 (3) |
C129 | 0.170 (6) | 0.116 (5) | 0.134 (6) | −0.042 (5) | −0.028 (5) | −0.005 (4) |
C130 | 0.131 (5) | 0.096 (4) | 0.071 (3) | −0.051 (4) | −0.016 (3) | −0.017 (3) |
C131 | 0.137 (5) | 0.121 (5) | 0.110 (4) | −0.088 (4) | −0.016 (4) | −0.008 (4) |
C132 | 0.155 (6) | 0.125 (5) | 0.118 (5) | −0.082 (5) | −0.028 (4) | −0.011 (4) |
C133 | 0.156 (6) | 0.114 (5) | 0.096 (4) | −0.051 (4) | −0.035 (4) | −0.012 (4) |
C134 | 0.116 (5) | 0.152 (6) | 0.108 (5) | −0.070 (5) | −0.006 (4) | −0.021 (4) |
C135 | 0.112 (4) | 0.117 (4) | 0.087 (4) | −0.073 (4) | −0.005 (3) | −0.010 (3) |
C136 | 0.58 (4) | 0.090 (10) | 0.193 (13) | 0.028 (14) | −0.003 (16) | −0.013 (8) |
C137 | 0.58 (4) | 0.090 (10) | 0.193 (13) | 0.028 (14) | −0.003 (16) | −0.013 (8) |
C138 | 0.58 (4) | 0.090 (10) | 0.193 (13) | 0.028 (14) | −0.003 (16) | −0.013 (8) |
C139 | 0.58 (4) | 0.090 (10) | 0.193 (13) | 0.028 (14) | −0.003 (16) | −0.013 (8) |
C140 | 0.58 (4) | 0.090 (10) | 0.193 (13) | 0.028 (14) | −0.003 (16) | −0.013 (8) |
C141 | 0.58 (4) | 0.090 (10) | 0.193 (13) | 0.028 (14) | −0.003 (16) | −0.013 (8) |
C142 | 0.58 (4) | 0.090 (10) | 0.193 (13) | 0.028 (14) | −0.003 (16) | −0.013 (8) |
Sm1—N4 | 2.409 (3) | C58—C59 | 1.439 (5) |
Sm1—N1 | 2.411 (3) | C59—C60 | 1.350 (5) |
Sm1—N3 | 2.425 (2) | C59—H59 | 0.9300 |
Sm1—N2 | 2.438 (3) | C60—C61 | 1.433 (5) |
Sm1—N5 | 2.572 (3) | C60—H60 | 0.9300 |
Sm1—N9 | 2.585 (3) | C61—C62 | 1.405 (5) |
Sm1—N7 | 2.598 (3) | C62—C63 | 1.399 (5) |
Sm1—B1 | 3.690 (4) | C62—C78 | 1.523 (4) |
Sm2—N11 | 2.400 (3) | C63—C64 | 1.435 (5) |
Sm2—N13 | 2.401 (3) | C64—C65 | 1.337 (6) |
Sm2—N12 | 2.410 (3) | C64—H64 | 0.9300 |
Sm2—N14 | 2.448 (3) | C65—C66 | 1.444 (5) |
Sm2—N17 | 2.584 (3) | C65—H65 | 0.9300 |
Sm2—N19 | 2.600 (3) | C66—C67 | 1.402 (5) |
Sm2—N15 | 2.606 (3) | C67—C68 | 1.424 (5) |
Sm2—B2 | 3.677 (4) | C67—C85 | 1.503 (4) |
N1—C4 | 1.373 (4) | C68—C69 | 1.436 (5) |
N1—C1 | 1.379 (4) | C69—C70 | 1.345 (5) |
N2—C6 | 1.373 (4) | C69—H69 | 0.9300 |
N2—C9 | 1.374 (4) | C70—C71 | 1.430 (5) |
N3—C11 | 1.366 (4) | C70—H70 | 0.9300 |
N3—C14 | 1.381 (4) | C71—C72 | 1.418 (5) |
N4—C19 | 1.370 (4) | C72—C73 | 1.400 (5) |
N4—C16 | 1.374 (4) | C72—C92 | 1.528 (4) |
N5—C49 | 1.328 (5) | C73—C74 | 1.444 (5) |
N5—N6 | 1.355 (4) | C74—C75 | 1.341 (5) |
N6—C51 | 1.345 (5) | C74—H74 | 0.9300 |
N6—B1 | 1.535 (5) | C75—C76 | 1.438 (5) |
N7—C52 | 1.318 (5) | C75—H75 | 0.9300 |
N7—N8 | 1.363 (4) | C76—C77 | 1.406 (5) |
N8—C54 | 1.335 (5) | C77—C99 | 1.509 (4) |
N8—B1 | 1.526 (5) | C78—C79 | 1.3900 |
N9—C55 | 1.322 (5) | C78—C83 | 1.3900 |
N9—N10 | 1.373 (4) | C79—C80 | 1.3900 |
N10—C57 | 1.329 (5) | C79—H79 | 0.9300 |
N10—B1 | 1.541 (5) | C80—C81 | 1.3900 |
N11—C58 | 1.380 (4) | C80—H80 | 0.9300 |
N11—C61 | 1.380 (4) | C81—C82 | 1.3900 |
N12—C66 | 1.377 (4) | C81—C84 | 1.534 (4) |
N12—C63 | 1.381 (4) | C82—C83 | 1.3900 |
N13—C71 | 1.377 (4) | C82—H82 | 0.9300 |
N13—C68 | 1.381 (4) | C83—H83 | 0.9300 |
N14—C73 | 1.376 (4) | C84—H84A | 0.9600 |
N14—C76 | 1.384 (4) | C84—H84B | 0.9600 |
N15—C106 | 1.331 (5) | C84—H84C | 0.9600 |
N15—N16 | 1.356 (4) | C85—C86 | 1.3900 |
N16—C108 | 1.331 (5) | C85—C90 | 1.3900 |
N16—B2 | 1.533 (6) | C86—C87 | 1.3900 |
N17—C109 | 1.343 (5) | C86—H86 | 0.9300 |
N17—N18 | 1.355 (5) | C87—C88 | 1.3900 |
N18—C111 | 1.355 (5) | C87—H87 | 0.9300 |
N18—B2 | 1.524 (6) | C88—C89 | 1.3900 |
N19—C112 | 1.335 (5) | C88—C91 | 1.539 (5) |
N19—N20 | 1.369 (4) | C89—C90 | 1.3900 |
N20—C114 | 1.334 (5) | C89—H89 | 0.9300 |
N20—B2 | 1.542 (6) | C90—H90 | 0.9300 |
B1—H1 | 0.9800 | C91—H91A | 0.9600 |
B2—H2B1 | 0.9800 | C91—H91B | 0.9600 |
C1—C20 | 1.404 (4) | C91—H91C | 0.9600 |
C1—C2 | 1.432 (5) | C92—C93 | 1.3900 |
C2—C3 | 1.340 (5) | C92—C97 | 1.3900 |
C2—H2 | 0.9300 | C93—C94 | 1.3900 |
C3—C4 | 1.438 (4) | C93—H93 | 0.9300 |
C3—H3 | 0.9300 | C94—C95 | 1.3900 |
C4—C5 | 1.398 (4) | C94—H94 | 0.9300 |
C5—C6 | 1.402 (4) | C95—C96 | 1.3900 |
C5—C21 | 1.523 (4) | C95—C98 | 1.533 (5) |
C6—C7 | 1.442 (4) | C96—C97 | 1.3900 |
C7—C8 | 1.334 (5) | C96—H96 | 0.9300 |
C7—H7 | 0.9300 | C97—H97 | 0.9300 |
C8—C9 | 1.435 (5) | C98—H98A | 0.9600 |
C8—H8 | 0.9300 | C98—H98B | 0.9600 |
C9—C10 | 1.398 (5) | C98—H98C | 0.9600 |
C10—C11 | 1.409 (4) | C99—C100 | 1.3900 |
C10—C28 | 1.505 (3) | C99—C104 | 1.3900 |
C11—C12 | 1.433 (4) | C100—C101 | 1.3900 |
C12—C13 | 1.339 (5) | C100—H100 | 0.9300 |
C12—H12D | 0.9300 | C101—C102 | 1.3900 |
C13—C14 | 1.433 (4) | C101—H101 | 0.9300 |
C13—H13 | 0.9300 | C102—C103 | 1.3900 |
C14—C15 | 1.402 (4) | C102—C105 | 1.536 (5) |
C15—C16 | 1.408 (4) | C103—C104 | 1.3900 |
C15—C35 | 1.520 (3) | C103—H103 | 0.9300 |
C16—C17 | 1.437 (4) | C104—H104 | 0.9300 |
C17—C18 | 1.346 (5) | C105—H10A | 0.9600 |
C17—H17 | 0.9300 | C105—H10B | 0.9600 |
C18—C19 | 1.445 (5) | C105—H10C | 0.9600 |
C18—H18 | 0.9300 | C106—C107 | 1.369 (7) |
C19—C20 | 1.407 (4) | C106—H106 | 0.9300 |
C20—C42 | 1.501 (3) | C107—C108 | 1.359 (7) |
C21—C22 | 1.3900 | C107—H107 | 0.9300 |
C21—C26 | 1.3900 | C108—H108 | 0.9300 |
C22—C23 | 1.3900 | C109—C110 | 1.372 (6) |
C22—H22 | 0.9300 | C109—H109 | 0.9300 |
C23—C24 | 1.3900 | C110—C111 | 1.366 (7) |
C23—H23 | 0.9300 | C110—H110 | 0.9300 |
C24—C25 | 1.3900 | C111—H111 | 0.9300 |
C24—C27 | 1.538 (4) | C112—C113 | 1.380 (5) |
C25—C26 | 1.3900 | C112—H112 | 0.9300 |
C25—H25 | 0.9300 | C113—C114 | 1.349 (6) |
C26—H26 | 0.9300 | C113—H113 | 0.9300 |
C27—H27A | 0.9600 | C114—H114 | 0.9300 |
C27—H27B | 0.9600 | C115—C116 | 1.465 (6) |
C27—H27C | 0.9600 | C115—H11A | 0.9600 |
C28—C29 | 1.3900 | C115—H11B | 0.9600 |
C28—C33 | 1.3900 | C115—H11C | 0.9600 |
C29—C30 | 1.3900 | C116—C117 | 1.3900 |
C29—H29 | 0.9300 | C116—C121 | 1.3900 |
C30—C31 | 1.3900 | C117—C118 | 1.3900 |
C30—H30 | 0.9300 | C117—H117 | 0.9300 |
C31—C32 | 1.3900 | C118—C119 | 1.3900 |
C31—C34 | 1.511 (4) | C118—H18A | 0.9300 |
C32—C33 | 1.3900 | C119—C120 | 1.3900 |
C32—H32 | 0.9300 | C119—H119 | 0.9300 |
C33—H33 | 0.9300 | C120—C121 | 1.3900 |
C34—H34A | 0.9600 | C120—H120 | 0.9300 |
C34—H34B | 0.9600 | C121—H121 | 0.9300 |
C34—H34C | 0.9600 | C122—C123 | 1.464 (6) |
C35—C36 | 1.3900 | C122—H12A | 0.9600 |
C35—C40 | 1.3900 | C122—H12B | 0.9600 |
C36—C37 | 1.3900 | C122—H12C | 0.9600 |
C36—H36 | 0.9300 | C123—C128 | 1.347 (8) |
C37—C38 | 1.3900 | C123—C124 | 1.426 (8) |
C37—H37 | 0.9300 | C124—C125 | 1.322 (9) |
C38—C39 | 1.3900 | C124—H12F | 0.9300 |
C38—C41 | 1.538 (4) | C125—C126 | 1.488 (10) |
C39—C40 | 1.3900 | C125—H125 | 0.9300 |
C39—H39 | 0.9300 | C126—C127 | 1.290 (9) |
C40—H40 | 0.9300 | C126—H126 | 0.9300 |
C41—H41A | 0.9600 | C127—C128 | 1.414 (9) |
C41—H41B | 0.9600 | C127—H127 | 0.9300 |
C41—H41C | 0.9600 | C128—H128 | 0.9300 |
C42—C43 | 1.3900 | C129—C130 | 1.483 (5) |
C42—C47 | 1.3900 | C129—H12H | 0.9600 |
C43—C44 | 1.3900 | C129—H12I | 0.9600 |
C43—H43 | 0.9300 | C129—H12J | 0.9600 |
C44—C45 | 1.3900 | C130—C131 | 1.3900 |
C44—H44 | 0.9300 | C130—C135 | 1.3900 |
C45—C46 | 1.3900 | C131—C132 | 1.3900 |
C45—C48 | 1.516 (4) | C131—H131 | 0.9300 |
C46—C47 | 1.3900 | C132—C133 | 1.3900 |
C46—H46 | 0.9300 | C132—H132 | 0.9300 |
C47—H47 | 0.9300 | C133—C134 | 1.3900 |
C48—H48A | 0.9600 | C133—H133 | 0.9300 |
C48—H48B | 0.9600 | C134—C135 | 1.3900 |
C48—H48C | 0.9600 | C134—H124 | 0.9300 |
C49—C50 | 1.385 (6) | C135—H135 | 0.9300 |
C49—H49 | 0.9300 | C136—C137 | 1.521 (10) |
C50—C51 | 1.349 (6) | C136—H13A | 0.9600 |
C50—H50 | 0.9300 | C136—H13B | 0.9600 |
C51—H51 | 0.9300 | C136—H13C | 0.9600 |
C52—C53 | 1.378 (6) | C137—C138 | 1.3900 |
C52—H52 | 0.9300 | C137—C142 | 1.3900 |
C53—C54 | 1.347 (7) | C138—C139 | 1.3900 |
C53—H53 | 0.9300 | C138—H138 | 0.9300 |
C54—H54 | 0.9300 | C139—C140 | 1.3900 |
C55—C56 | 1.381 (6) | C139—H139 | 0.9300 |
C55—H55 | 0.9300 | C140—C141 | 1.3900 |
C56—C57 | 1.370 (6) | C140—H140 | 0.9300 |
C56—H56 | 0.9300 | C141—C142 | 1.3900 |
C57—H57 | 0.9300 | C141—H141 | 0.9300 |
C58—C77 | 1.407 (5) | C142—H142 | 0.9300 |
N4—Sm1—N1 | 75.30 (9) | N6—C51—H51 | 125.4 |
N4—Sm1—N3 | 73.80 (8) | C50—C51—H51 | 125.4 |
N1—Sm1—N3 | 116.82 (9) | N7—C52—C53 | 111.7 (4) |
N4—Sm1—N2 | 117.18 (9) | N7—C52—H52 | 124.2 |
N1—Sm1—N2 | 73.65 (8) | C53—C52—H52 | 124.2 |
N3—Sm1—N2 | 73.88 (8) | C54—C53—C52 | 104.7 (4) |
N4—Sm1—N5 | 129.53 (9) | C54—C53—H53 | 127.6 |
N1—Sm1—N5 | 80.75 (9) | C52—C53—H53 | 127.6 |
N3—Sm1—N5 | 155.49 (9) | N8—C54—C53 | 108.7 (4) |
N2—Sm1—N5 | 96.97 (9) | N8—C54—H54 | 125.6 |
N4—Sm1—N9 | 77.72 (9) | C53—C54—H54 | 125.6 |
N1—Sm1—N9 | 114.80 (9) | N9—C55—C56 | 111.0 (4) |
N3—Sm1—N9 | 110.39 (9) | N9—C55—H55 | 124.5 |
N2—Sm1—N9 | 164.91 (9) | C56—C55—H55 | 124.5 |
N5—Sm1—N9 | 73.15 (10) | C57—C56—C55 | 104.8 (4) |
N4—Sm1—N7 | 132.95 (10) | C57—C56—H56 | 127.6 |
N1—Sm1—N7 | 150.81 (10) | C55—C56—H56 | 127.6 |
N3—Sm1—N7 | 83.44 (9) | N10—C57—C56 | 108.8 (4) |
N2—Sm1—N7 | 94.11 (9) | N10—C57—H57 | 125.6 |
N5—Sm1—N7 | 74.45 (10) | C56—C57—H57 | 125.6 |
N9—Sm1—N7 | 72.48 (10) | N11—C58—C77 | 125.2 (3) |
N4—Sm1—B1 | 121.69 (9) | N11—C58—C59 | 108.9 (3) |
N1—Sm1—B1 | 121.12 (9) | C77—C58—C59 | 125.8 (3) |
N3—Sm1—B1 | 122.05 (9) | C60—C59—C58 | 107.9 (3) |
N2—Sm1—B1 | 121.12 (9) | C60—C59—H59 | 126.1 |
N5—Sm1—B1 | 43.45 (10) | C58—C59—H59 | 126.1 |
N9—Sm1—B1 | 44.03 (9) | C59—C60—C61 | 107.0 (3) |
N7—Sm1—B1 | 43.39 (9) | C59—C60—H60 | 126.5 |
N11—Sm2—N13 | 117.64 (10) | C61—C60—H60 | 126.5 |
N11—Sm2—N12 | 74.22 (10) | N11—C61—C62 | 125.6 (3) |
N13—Sm2—N12 | 74.87 (9) | N11—C61—C60 | 109.7 (3) |
N11—Sm2—N14 | 74.56 (9) | C62—C61—C60 | 124.2 (3) |
N13—Sm2—N14 | 73.67 (9) | C63—C62—C61 | 124.8 (3) |
N12—Sm2—N14 | 117.10 (9) | C63—C62—C78 | 117.5 (3) |
N11—Sm2—N17 | 106.81 (10) | C61—C62—C78 | 117.5 (3) |
N13—Sm2—N17 | 116.77 (10) | N12—C63—C62 | 126.0 (3) |
N12—Sm2—N17 | 76.86 (10) | N12—C63—C64 | 109.3 (3) |
N14—Sm2—N17 | 165.25 (10) | C62—C63—C64 | 124.6 (3) |
N11—Sm2—N19 | 153.93 (10) | C65—C64—C63 | 107.4 (3) |
N13—Sm2—N19 | 82.68 (9) | C65—C64—H64 | 126.3 |
N12—Sm2—N19 | 129.73 (10) | C63—C64—H64 | 126.3 |
N14—Sm2—N19 | 97.99 (10) | C64—C65—C66 | 108.0 (3) |
N17—Sm2—N19 | 74.24 (11) | C64—C65—H65 | 126.0 |
N11—Sm2—N15 | 82.32 (10) | C66—C65—H65 | 126.0 |
N13—Sm2—N15 | 150.23 (10) | N12—C66—C67 | 125.8 (3) |
N12—Sm2—N15 | 134.27 (10) | N12—C66—C65 | 108.6 (3) |
N14—Sm2—N15 | 92.68 (10) | C67—C66—C65 | 125.5 (3) |
N17—Sm2—N15 | 73.17 (11) | C66—C67—C68 | 125.5 (3) |
N19—Sm2—N15 | 72.99 (10) | C66—C67—C85 | 117.3 (3) |
N11—Sm2—B2 | 119.12 (11) | C68—C67—C85 | 117.1 (3) |
N13—Sm2—B2 | 123.23 (10) | N13—C68—C67 | 125.2 (3) |
N12—Sm2—B2 | 120.21 (11) | N13—C68—C69 | 109.4 (3) |
N14—Sm2—B2 | 122.65 (11) | C67—C68—C69 | 125.3 (3) |
N17—Sm2—B2 | 43.44 (12) | C70—C69—C68 | 107.3 (3) |
N19—Sm2—B2 | 44.05 (11) | C70—C69—H69 | 126.3 |
N15—Sm2—B2 | 43.56 (10) | C68—C69—H69 | 126.3 |
C4—N1—C1 | 106.3 (3) | C69—C70—C71 | 107.5 (3) |
C4—N1—Sm1 | 128.4 (2) | C69—C70—H70 | 126.3 |
C1—N1—Sm1 | 122.6 (2) | C71—C70—H70 | 126.3 |
C6—N2—C9 | 106.5 (3) | N13—C71—C72 | 124.7 (3) |
C6—N2—Sm1 | 126.04 (19) | N13—C71—C70 | 109.7 (3) |
C9—N2—Sm1 | 123.7 (2) | C72—C71—C70 | 125.5 (3) |
C11—N3—C14 | 106.2 (3) | C73—C72—C71 | 125.3 (3) |
C11—N3—Sm1 | 124.1 (2) | C73—C72—C92 | 117.1 (3) |
C14—N3—Sm1 | 122.70 (19) | C71—C72—C92 | 117.5 (3) |
C19—N4—C16 | 106.7 (3) | N14—C73—C72 | 126.0 (3) |
C19—N4—Sm1 | 122.9 (2) | N14—C73—C74 | 109.2 (3) |
C16—N4—Sm1 | 125.7 (2) | C72—C73—C74 | 124.7 (3) |
C49—N5—N6 | 105.4 (3) | C75—C74—C73 | 107.3 (3) |
C49—N5—Sm1 | 131.7 (3) | C75—C74—H74 | 126.3 |
N6—N5—Sm1 | 122.9 (2) | C73—C74—H74 | 126.3 |
C51—N6—N5 | 109.6 (3) | C74—C75—C76 | 107.9 (3) |
C51—N6—B1 | 127.4 (3) | C74—C75—H75 | 126.1 |
N5—N6—B1 | 122.9 (3) | C76—C75—H75 | 126.1 |
C52—N7—N8 | 105.0 (3) | N14—C76—C77 | 125.7 (3) |
C52—N7—Sm1 | 132.8 (3) | N14—C76—C75 | 109.0 (3) |
N8—N7—Sm1 | 122.2 (2) | C77—C76—C75 | 125.2 (3) |
C54—N8—N7 | 109.8 (3) | C76—C77—C58 | 126.3 (3) |
C54—N8—B1 | 127.2 (3) | C76—C77—C99 | 117.3 (3) |
N7—N8—B1 | 122.7 (3) | C58—C77—C99 | 116.3 (3) |
C55—N9—N10 | 106.0 (3) | C79—C78—C83 | 120.0 |
C55—N9—Sm1 | 132.1 (3) | C79—C78—C62 | 120.1 (2) |
N10—N9—Sm1 | 121.6 (2) | C83—C78—C62 | 119.8 (2) |
C57—N10—N9 | 109.5 (3) | C78—C79—C80 | 120.0 |
C57—N10—B1 | 127.2 (3) | C78—C79—H79 | 120.0 |
N9—N10—B1 | 123.3 (3) | C80—C79—H79 | 120.0 |
C58—N11—C61 | 106.4 (3) | C79—C80—C81 | 120.0 |
C58—N11—Sm2 | 125.1 (2) | C79—C80—H80 | 120.0 |
C61—N11—Sm2 | 120.9 (2) | C81—C80—H80 | 120.0 |
C66—N12—C63 | 106.7 (3) | C82—C81—C80 | 120.0 |
C66—N12—Sm2 | 125.5 (2) | C82—C81—C84 | 119.0 (3) |
C63—N12—Sm2 | 124.7 (2) | C80—C81—C84 | 120.9 (3) |
C71—N13—C68 | 106.0 (3) | C81—C82—C83 | 120.0 |
C71—N13—Sm2 | 122.5 (2) | C81—C82—H82 | 120.0 |
C68—N13—Sm2 | 121.4 (2) | C83—C82—H82 | 120.0 |
C73—N14—C76 | 106.5 (3) | C82—C83—C78 | 120.0 |
C73—N14—Sm2 | 125.2 (2) | C82—C83—H83 | 120.0 |
C76—N14—Sm2 | 126.6 (2) | C78—C83—H83 | 120.0 |
C106—N15—N16 | 105.8 (3) | C81—C84—H84A | 109.5 |
C106—N15—Sm2 | 132.1 (3) | C81—C84—H84B | 109.5 |
N16—N15—Sm2 | 122.0 (2) | H84A—C84—H84B | 109.5 |
C108—N16—N15 | 109.6 (4) | C81—C84—H84C | 109.5 |
C108—N16—B2 | 127.9 (4) | H84A—C84—H84C | 109.5 |
N15—N16—B2 | 122.5 (3) | H84B—C84—H84C | 109.5 |
C109—N17—N18 | 105.6 (3) | C86—C85—C90 | 120.0 |
C109—N17—Sm2 | 132.0 (3) | C86—C85—C67 | 120.3 (2) |
N18—N17—Sm2 | 122.3 (2) | C90—C85—C67 | 119.7 (2) |
N17—N18—C111 | 109.1 (4) | C85—C86—C87 | 120.0 |
N17—N18—B2 | 122.9 (3) | C85—C86—H86 | 120.0 |
C111—N18—B2 | 128.0 (4) | C87—C86—H86 | 120.0 |
C112—N19—N20 | 104.8 (3) | C88—C87—C86 | 120.0 |
C112—N19—Sm2 | 133.7 (3) | C88—C87—H87 | 120.0 |
N20—N19—Sm2 | 121.4 (2) | C86—C87—H87 | 120.0 |
C114—N20—N19 | 109.1 (3) | C87—C88—C89 | 120.0 |
C114—N20—B2 | 128.0 (3) | C87—C88—C91 | 118.5 (4) |
N19—N20—B2 | 122.8 (3) | C89—C88—C91 | 121.5 (4) |
N8—B1—N6 | 110.8 (3) | C90—C89—C88 | 120.0 |
N8—B1—N10 | 108.6 (3) | C90—C89—H89 | 120.0 |
N6—B1—N10 | 110.6 (3) | C88—C89—H89 | 120.0 |
N8—B1—Sm1 | 71.52 (18) | C89—C90—C85 | 120.0 |
N6—B1—Sm1 | 70.72 (18) | C89—C90—H90 | 120.0 |
N10—B1—Sm1 | 71.00 (18) | C85—C90—H90 | 120.0 |
N8—B1—H1 | 108.9 | C88—C91—H91A | 109.5 |
N6—B1—H1 | 108.9 | C88—C91—H91B | 109.5 |
N10—B1—H1 | 108.9 | H91A—C91—H91B | 109.5 |
Sm1—B1—H1 | 179.5 | C88—C91—H91C | 109.5 |
N18—B2—N16 | 110.7 (4) | H91A—C91—H91C | 109.5 |
N18—B2—N20 | 112.0 (3) | H91B—C91—H91C | 109.5 |
N16—B2—N20 | 109.0 (4) | C93—C92—C97 | 120.0 |
N18—B2—Sm2 | 71.4 (2) | C93—C92—C72 | 120.88 (19) |
N16—B2—Sm2 | 71.9 (2) | C97—C92—C72 | 119.11 (19) |
N20—B2—Sm2 | 71.72 (19) | C94—C93—C92 | 120.0 |
N18—B2—H2B1 | 108.3 | C94—C93—H93 | 120.0 |
N16—B2—H2B1 | 108.3 | C92—C93—H93 | 120.0 |
N20—B2—H2B1 | 108.3 | C93—C94—C95 | 120.0 |
Sm2—B2—H2B1 | 179.7 | C93—C94—H94 | 120.0 |
N1—C1—C20 | 125.8 (3) | C95—C94—H94 | 120.0 |
N1—C1—C2 | 109.2 (3) | C96—C95—C94 | 120.0 |
C20—C1—C2 | 124.3 (3) | C96—C95—C98 | 120.8 (3) |
C3—C2—C1 | 107.8 (3) | C94—C95—C98 | 119.2 (3) |
C3—C2—H2 | 126.1 | C95—C96—C97 | 120.0 |
C1—C2—H2 | 126.1 | C95—C96—H96 | 120.0 |
C2—C3—C4 | 107.2 (3) | C97—C96—H96 | 120.0 |
C2—C3—H3 | 126.4 | C96—C97—C92 | 120.0 |
C4—C3—H3 | 126.4 | C96—C97—H97 | 120.0 |
N1—C4—C5 | 126.1 (3) | C92—C97—H97 | 120.0 |
N1—C4—C3 | 109.5 (3) | C95—C98—H98A | 109.5 |
C5—C4—C3 | 124.4 (3) | C95—C98—H98B | 109.5 |
C4—C5—C6 | 125.4 (3) | H98A—C98—H98B | 109.5 |
C4—C5—C21 | 116.7 (3) | C95—C98—H98C | 109.5 |
C6—C5—C21 | 117.7 (3) | H98A—C98—H98C | 109.5 |
N2—C6—C5 | 125.9 (3) | H98B—C98—H98C | 109.5 |
N2—C6—C7 | 109.4 (3) | C100—C99—C104 | 120.0 |
C5—C6—C7 | 124.4 (3) | C100—C99—C77 | 119.1 (2) |
C8—C7—C6 | 106.8 (3) | C104—C99—C77 | 120.9 (2) |
C8—C7—H7 | 126.6 | C101—C100—C99 | 120.0 |
C6—C7—H7 | 126.6 | C101—C100—H100 | 120.0 |
C7—C8—C9 | 108.2 (3) | C99—C100—H100 | 120.0 |
C7—C8—H8 | 125.9 | C100—C101—C102 | 120.0 |
C9—C8—H8 | 125.9 | C100—C101—H101 | 120.0 |
N2—C9—C10 | 125.7 (3) | C102—C101—H101 | 120.0 |
N2—C9—C8 | 108.9 (3) | C103—C102—C101 | 120.0 |
C10—C9—C8 | 125.0 (3) | C103—C102—C105 | 120.1 (3) |
C9—C10—C11 | 126.6 (3) | C101—C102—C105 | 119.9 (3) |
C9—C10—C28 | 117.1 (3) | C102—C103—C104 | 120.0 |
C11—C10—C28 | 116.1 (3) | C102—C103—H103 | 120.0 |
N3—C11—C10 | 125.1 (3) | C104—C103—H103 | 120.0 |
N3—C11—C12 | 109.4 (3) | C103—C104—C99 | 120.0 |
C10—C11—C12 | 125.5 (3) | C103—C104—H104 | 120.0 |
C13—C12—C11 | 107.9 (3) | C99—C104—H104 | 120.0 |
C13—C12—H12D | 126.0 | C102—C105—H10A | 109.5 |
C11—C12—H12D | 126.0 | C102—C105—H10B | 109.5 |
C12—C13—C14 | 106.9 (3) | H10A—C105—H10B | 109.5 |
C12—C13—H13 | 126.6 | C102—C105—H10C | 109.5 |
C14—C13—H13 | 126.6 | H10A—C105—H10C | 109.5 |
N3—C14—C15 | 126.1 (3) | H10B—C105—H10C | 109.5 |
N3—C14—C13 | 109.5 (3) | N15—C106—C107 | 110.9 (4) |
C15—C14—C13 | 124.2 (3) | N15—C106—H106 | 124.6 |
C14—C15—C16 | 124.9 (3) | C107—C106—H106 | 124.6 |
C14—C15—C35 | 117.6 (3) | C108—C107—C106 | 105.0 (4) |
C16—C15—C35 | 117.4 (3) | C108—C107—H107 | 127.5 |
N4—C16—C15 | 125.9 (3) | C106—C107—H107 | 127.5 |
N4—C16—C17 | 109.8 (3) | N16—C108—C107 | 108.8 (4) |
C15—C16—C17 | 124.2 (3) | N16—C108—H108 | 125.6 |
C18—C17—C16 | 106.8 (3) | C107—C108—H108 | 125.6 |
C18—C17—H17 | 126.6 | N17—C109—C110 | 112.0 (5) |
C16—C17—H17 | 126.6 | N17—C109—H109 | 124.0 |
C17—C18—C19 | 107.8 (3) | C110—C109—H109 | 124.0 |
C17—C18—H18 | 126.1 | C111—C110—C109 | 104.0 (4) |
C19—C18—H18 | 126.1 | C111—C110—H110 | 128.0 |
N4—C19—C20 | 125.6 (3) | C109—C110—H110 | 128.0 |
N4—C19—C18 | 108.9 (3) | N18—C111—C110 | 109.4 (4) |
C20—C19—C18 | 125.3 (3) | N18—C111—H111 | 125.3 |
C1—C20—C19 | 126.3 (3) | C110—C111—H111 | 125.3 |
C1—C20—C42 | 116.4 (3) | N19—C112—C113 | 111.9 (4) |
C19—C20—C42 | 116.9 (3) | N19—C112—H112 | 124.0 |
C22—C21—C26 | 120.0 | C113—C112—H112 | 124.0 |
C22—C21—C5 | 120.69 (18) | C114—C113—C112 | 103.8 (4) |
C26—C21—C5 | 119.29 (18) | C114—C113—H113 | 128.1 |
C23—C22—C21 | 120.0 | C112—C113—H113 | 128.1 |
C23—C22—H22 | 120.0 | N20—C114—C113 | 110.3 (4) |
C21—C22—H22 | 120.0 | N20—C114—H114 | 124.8 |
C24—C23—C22 | 120.0 | C113—C114—H114 | 124.8 |
C24—C23—H23 | 120.0 | C116—C115—H11A | 109.5 |
C22—C23—H23 | 120.0 | C116—C115—H11B | 109.5 |
C23—C24—C25 | 120.0 | H11A—C115—H11B | 109.5 |
C23—C24—C27 | 119.9 (3) | C116—C115—H11C | 109.5 |
C25—C24—C27 | 120.1 (3) | H11A—C115—H11C | 109.5 |
C24—C25—C26 | 120.0 | H11B—C115—H11C | 109.5 |
C24—C25—H25 | 120.0 | C117—C116—C121 | 120.0 |
C26—C25—H25 | 120.0 | C117—C116—C115 | 120.2 (5) |
C25—C26—C21 | 120.0 | C121—C116—C115 | 119.8 (5) |
C25—C26—H26 | 120.0 | C118—C117—C116 | 120.0 |
C21—C26—H26 | 120.0 | C118—C117—H117 | 120.0 |
C24—C27—H27A | 109.5 | C116—C117—H117 | 120.0 |
C24—C27—H27B | 109.5 | C119—C118—C117 | 120.0 |
H27A—C27—H27B | 109.5 | C119—C118—H18A | 120.0 |
C24—C27—H27C | 109.5 | C117—C118—H18A | 120.0 |
H27A—C27—H27C | 109.5 | C120—C119—C118 | 120.0 |
H27B—C27—H27C | 109.5 | C120—C119—H119 | 120.0 |
C29—C28—C33 | 120.0 | C118—C119—H119 | 120.0 |
C29—C28—C10 | 118.67 (18) | C119—C120—C121 | 120.0 |
C33—C28—C10 | 121.30 (18) | C119—C120—H120 | 120.0 |
C28—C29—C30 | 120.0 | C121—C120—H120 | 120.0 |
C28—C29—H29 | 120.0 | C120—C121—C116 | 120.0 |
C30—C29—H29 | 120.0 | C120—C121—H121 | 120.0 |
C31—C30—C29 | 120.0 | C116—C121—H121 | 120.0 |
C31—C30—H30 | 120.0 | C123—C122—H12A | 109.5 |
C29—C30—H30 | 120.0 | C123—C122—H12B | 109.5 |
C32—C31—C30 | 120.0 | H12A—C122—H12B | 109.5 |
C32—C31—C34 | 119.9 (3) | C123—C122—H12C | 109.5 |
C30—C31—C34 | 120.1 (3) | H12A—C122—H12C | 109.5 |
C31—C32—C33 | 120.0 | H12B—C122—H12C | 109.5 |
C31—C32—H32 | 120.0 | C128—C123—C124 | 119.2 (6) |
C33—C32—H32 | 120.0 | C128—C123—C122 | 123.2 (7) |
C32—C33—C28 | 120.0 | C124—C123—C122 | 117.6 (6) |
C32—C33—H33 | 120.0 | C125—C124—C123 | 119.2 (7) |
C28—C33—H33 | 120.0 | C125—C124—H12F | 120.4 |
C31—C34—H34A | 109.5 | C123—C124—H12F | 120.4 |
C31—C34—H34B | 109.5 | C124—C125—C126 | 121.8 (7) |
H34A—C34—H34B | 109.5 | C124—C125—H125 | 119.1 |
C31—C34—H34C | 109.5 | C126—C125—H125 | 119.1 |
H34A—C34—H34C | 109.5 | C127—C126—C125 | 116.3 (7) |
H34B—C34—H34C | 109.5 | C127—C126—H126 | 121.9 |
C36—C35—C40 | 120.0 | C125—C126—H126 | 121.9 |
C36—C35—C15 | 120.02 (18) | C126—C127—C128 | 123.2 (8) |
C40—C35—C15 | 119.93 (18) | C126—C127—H127 | 118.4 |
C35—C36—C37 | 120.0 | C128—C127—H127 | 118.4 |
C35—C36—H36 | 120.0 | C123—C128—C127 | 120.3 (7) |
C37—C36—H36 | 120.0 | C123—C128—H128 | 119.8 |
C36—C37—C38 | 120.0 | C127—C128—H128 | 119.8 |
C36—C37—H37 | 120.0 | C130—C129—H12H | 109.5 |
C38—C37—H37 | 120.0 | C130—C129—H12I | 109.5 |
C39—C38—C37 | 120.0 | H12H—C129—H12I | 109.5 |
C39—C38—C41 | 120.7 (3) | C130—C129—H12J | 109.5 |
C37—C38—C41 | 119.3 (3) | H12H—C129—H12J | 109.5 |
C38—C39—C40 | 120.0 | H12I—C129—H12J | 109.5 |
C38—C39—H39 | 120.0 | C131—C130—C135 | 120.0 |
C40—C39—H39 | 120.0 | C131—C130—C129 | 118.9 (4) |
C39—C40—C35 | 120.0 | C135—C130—C129 | 121.1 (4) |
C39—C40—H40 | 120.0 | C130—C131—C132 | 120.0 |
C35—C40—H40 | 120.0 | C130—C131—H131 | 120.0 |
C38—C41—H41A | 109.5 | C132—C131—H131 | 120.0 |
C38—C41—H41B | 109.5 | C133—C132—C131 | 120.0 |
H41A—C41—H41B | 109.5 | C133—C132—H132 | 120.0 |
C38—C41—H41C | 109.5 | C131—C132—H132 | 120.0 |
H41A—C41—H41C | 109.5 | C134—C133—C132 | 120.0 |
H41B—C41—H41C | 109.5 | C134—C133—H133 | 120.0 |
C43—C42—C47 | 120.0 | C132—C133—H133 | 120.0 |
C43—C42—C20 | 119.71 (18) | C133—C134—C135 | 120.0 |
C47—C42—C20 | 120.27 (18) | C133—C134—H124 | 120.0 |
C42—C43—C44 | 120.0 | C135—C134—H124 | 120.0 |
C42—C43—H43 | 120.0 | C134—C135—C130 | 120.0 |
C44—C43—H43 | 120.0 | C134—C135—H135 | 120.0 |
C45—C44—C43 | 120.0 | C130—C135—H135 | 120.0 |
C45—C44—H44 | 120.0 | C137—C136—H13A | 109.5 |
C43—C44—H44 | 120.0 | C137—C136—H13B | 109.5 |
C46—C45—C44 | 120.0 | H13A—C136—H13B | 109.5 |
C46—C45—C48 | 119.0 (3) | C137—C136—H13C | 109.5 |
C44—C45—C48 | 121.0 (3) | H13A—C136—H13C | 109.5 |
C47—C46—C45 | 120.0 | H13B—C136—H13C | 109.5 |
C47—C46—H46 | 120.0 | C138—C137—C142 | 120.0 |
C45—C46—H46 | 120.0 | C138—C137—C136 | 117.5 (10) |
C46—C47—C42 | 120.0 | C142—C137—C136 | 122.5 (10) |
C46—C47—H47 | 120.0 | C137—C138—C139 | 120.0 |
C42—C47—H47 | 120.0 | C137—C138—H138 | 120.0 |
C45—C48—H48A | 109.5 | C139—C138—H138 | 120.0 |
C45—C48—H48B | 109.5 | C140—C139—C138 | 120.0 |
H48A—C48—H48B | 109.5 | C140—C139—H139 | 120.0 |
C45—C48—H48C | 109.5 | C138—C139—H139 | 120.0 |
H48A—C48—H48C | 109.5 | C139—C140—C141 | 120.0 |
H48B—C48—H48C | 109.5 | C139—C140—H140 | 120.0 |
N5—C49—C50 | 111.5 (4) | C141—C140—H140 | 120.0 |
N5—C49—H49 | 124.2 | C142—C141—C140 | 120.0 |
C50—C49—H49 | 124.2 | C142—C141—H141 | 120.0 |
C51—C50—C49 | 104.3 (4) | C140—C141—H141 | 120.0 |
C51—C50—H50 | 127.9 | C141—C142—C137 | 120.0 |
C49—C50—H50 | 127.9 | C141—C142—H142 | 120.0 |
N6—C51—C50 | 109.2 (4) | C137—C142—H142 | 120.0 |
Experimental details
Crystal data | |
Chemical formula | [Sm(C9H10BN6)(C48H36N4)]·1.75C7H8 |
Mr | 1193.43 |
Crystal system, space group | Triclinic, P1 |
Temperature (K) | 293 |
a, b, c (Å) | 16.6210 (2), 16.5696 (2), 25.4414 (3) |
α, β, γ (°) | 79.318 (1), 79.064 (1), 61.248 (1) |
V (Å3) | 5995.10 (12) |
Z | 4 |
Radiation type | Mo Kα |
µ (mm−1) | 1.03 |
Crystal size (mm) | 0.30 × 0.30 × 0.30 |
Data collection | |
Diffractometer | Bruker SMART 1K CCD diffractometer |
Absorption correction | Multi-scan (SADABS; Sheldrick, 2002) |
Tmin, Tmax | 0.748, 0.748 |
No. of measured, independent and observed [I > 2σ(I)] reflections | 73453, 21056, 17078 |
Rint | 0.030 |
(sin θ/λ)max (Å−1) | 0.595 |
Refinement | |
R[F2 > 2σ(F2)], wR(F2), S | 0.033, 0.089, 1.02 |
No. of reflections | 21056 |
No. of parameters | 1335 |
No. of restraints | 154 |
H-atom treatment | H-atom parameters constrained |
Δρmax, Δρmin (e Å−3) | 0.88, −0.47 |
Computer programs: SMART (Bruker, 1998), SAINT-Plus (Bruker, 1998), SHELXS97 (Sheldrick, 1997), SHELXL97 (Sheldrick, 1997), ORTEP-3 for Windows (Farrugia, 1997), WinGX (Farrugia, 1999).
Several monoporphyrinate lanthanide complexes with hydridotrispyrazolylborate anions have been reported recently (He, Guo et al., 2004; He et al. 2004a,b; Foley et al. 2003). These complexes exhibit strong luminescence in the near-infrared region and have potential in fluoroimmunoassay and photonic devices (He, Guo et al. 2004). However, light rare earth complexes are uncommon. Reported herein is the single-crystal structure of a Sm(III) complex.
In the title compound, there are two independent molecules in the asymmetric unit. In each, the SmIII ion is "sandwiched" between a porphyrin ring and a tripodal ligand. The conformation of each complex molecule is different only in the relative orientaions of the phenyl groups. In each molecule, four N atoms from a 5,10,15,20-tetrakis(4-methyl)porphyrinate ligand (TTP2-) and three N atoms from hydridotris (pyrazol-1-yl)borate anion (TpH-) ligand coordinate to the central SmIII ion to form a capped trigonal prismatic geometry. The distances between atom Sm1 and the least-squared planes N1/N2/N3/N4 and N5/N7/N9 are 1.2647 (13) and 1.8713 (17) Å, respectively. The distances between atom Sm2 and the least-squared planes N11/N12/N13/N14 and N15/N17/N19 are 1.2549 (14) and 1.8778 (18) Å, respectively. The distances Sm1···B1 and Sm2···B2 are 3.690 (4) and 3.677 (4) Å, respectively. In each independent molecules the orientation of the three arms of the tripodal ligand are different with respect to the phenyl rings. For the molecule containing Sm1 the three arms are located between the phenyl groups, whereas in the molecule containing Sm2 one arm of tripodal ligand is very close to one of the phenyl groups.