At 173 K, the structure of the acyclic `triphosphenium' salt 1,1,1,3,3,3-hexaphenyltriphosphenium tetrachloroaluminate dichloromethane hemisolvate, [(Ph3P)2P][AlCl4]·0.5CH2Cl2, contains two cations, two anions and one solvent molecule in the asymmetric unit. There are no unusually short anion-cation distances and the structures of the ions are comparable to those that have been reported previously.
Supporting information
CCDC reference: 618282
Key indicators
- Single-crystal X-ray study
- T = 173 K
- Mean (C-C) = 0.006 Å
Some non-H atoms missing
- R factor = 0.049
- wR factor = 0.131
- Data-to-parameter ratio = 20.4
checkCIF/PLATON results
No syntax errors found
Alert level A
ABSMU01_ALERT_1_A The ratio of given/expected absorption coefficient lies
outside the range 0.90 <> 1.10
Calculated value of mu = 1.147
Value of mu given = 0.573
CHEMW01_ALERT_1_A The ratio of given/expected molecular weight as calculated
from the _chemical_formula_sum lies outside
the range 0.90 <> 1.10
Calculated formula weight = 1533.6284
Formula weight given = 766.7600
Alert level C
ABSTM02_ALERT_3_C The ratio of expected to reported Tmax/Tmin(RR') is < 0.90
Tmin and Tmax reported: 0.652 0.795
Tmin(prime) and Tmax expected: 0.746 0.795
RR(prime) = 0.874
Please check that your absorption correction is appropriate.
CHEMW01_ALERT_1_C The difference between the given and expected weight for
compound is greater 1 mass unit. Check that all hydrogen
atoms have been taken into account.
DIFMX01_ALERT_2_C The maximum difference density is > 0.1*ZMAX*0.75
_refine_diff_density_max given = 1.563
Test value = 1.275
DIFMX02_ALERT_1_C The maximum difference density is > 0.1*ZMAX*0.75
The relevant atom site should be identified.
PLAT042_ALERT_1_C Calc. and Rep. MoietyFormula Strings Differ .... ?
PLAT045_ALERT_1_C Calculated and Reported Z Differ by ............ 0.50 Ratio
PLAT061_ALERT_3_C Tmax/Tmin Range Test RR' too Large ............. 0.87
PLAT094_ALERT_2_C Ratio of Maximum / Minimum Residual Density .... 2.54
PLAT097_ALERT_2_C Maximum (Positive) Residual Density ............ 1.56 e/A
PLAT220_ALERT_2_C Large Non-Solvent C Ueq(max)/Ueq(min) ... 3.42 Ratio
PLAT220_ALERT_2_C Large Non-Solvent C Ueq(max)/Ueq(min) ... 2.85 Ratio
PLAT241_ALERT_2_C Check High Ueq as Compared to Neighbors for C13
PLAT242_ALERT_2_C Check Low Ueq as Compared to Neighbors for C11
PLAT244_ALERT_4_C Low 'Solvent' Ueq as Compared to Neighbors for Al1
PLAT244_ALERT_4_C Low 'Solvent' Ueq as Compared to Neighbors for Al2
PLAT244_ALERT_4_C Low 'Solvent' Ueq as Compared to Neighbors for C1
PLAT340_ALERT_3_C Low Bond Precision on C-C bonds (x 1000) Ang ... 6
Alert level G
FORMU01_ALERT_1_G There is a discrepancy between the atom counts in the
_chemical_formula_sum and _chemical_formula_moiety. This is
usually due to the moiety formula being in the wrong format.
Atom count from _chemical_formula_sum: C73 H62 Al2 Cl10 P6
Atom count from _chemical_formula_moiety:C36.5 H31 Al1 Cl5 P3
FORMU01_ALERT_2_G There is a discrepancy between the atom counts in the
_chemical_formula_sum and the formula from the _atom_site* data.
Atom count from _chemical_formula_sum:C73 H62 Al2 Cl10 P6
Atom count from the _atom_site data: C36.5 H31 Al1 Cl5 P3
CELLZ01_ALERT_1_G Difference between formula and atom_site contents detected.
CELLZ01_ALERT_1_G ALERT: Large difference may be due to a
symmetry error - see SYMMG tests
From the CIF: _cell_formula_units_Z 8
From the CIF: _chemical_formula_sum C73 H62 Al2 Cl10 P6
TEST: Compare cell contents of formula and atom_site data
atom Z*formula cif sites diff
C 584.00 292.00 292.00
H 496.00 248.00 248.00
Al 16.00 8.00 8.00
Cl 80.00 40.00 40.00
P 48.00 24.00 24.00
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 27.50
From the CIF: _reflns_number_total 16737
Count of symmetry unique reflns 8669
Completeness (_total/calc) 193.07%
TEST3: Check Friedels for noncentro structure
Estimate of Friedel pairs measured 8068
Fraction of Friedel pairs measured 0.931
Are heavy atom types Z>Si present yes
2 ALERT level A = In general: serious problem
0 ALERT level B = Potentially serious problem
17 ALERT level C = Check and explain
5 ALERT level G = General alerts; check
9 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
4 ALERT type 4 Improvement, methodology, query or suggestion
0 ALERT type 5 Informative message, check
Data collection: SMART (Bruker, 1997); cell refinement: SAINT-Plus (Bruker, 1997); data reduction: SAINT-Plus; program(s) used to solve structure: SHELXS97 (Sheldrick, 1997); program(s) used to refine structure: SHELXL97 (Sheldrick, 1997); molecular graphics: SHELXTL (Bruker, 1997); software used to prepare material for publication: SHELXTL, PLATON (Spek, 2003) and WinGX (Farrugia, 1999).
1,1,1,3,3,3-hexaphenyltriphosphenium tetrachloroaluminate dichloromethane
hemisolvate
top
Crystal data top
(C36H30P3)[AlCl4]·0.5CH2Cl2 | Dx = 1.381 Mg m−3 |
Mr = 766.76 | Melting point: 78 K |
Orthorhombic, Pna21 | Mo Kα radiation, λ = 0.71073 Å |
Hall symbol: P 2c -2n | Cell parameters from 7634 reflections |
a = 33.283 (5) Å | θ = 1.2–27.5° |
b = 9.2443 (13) Å | µ = 0.57 mm−1 |
c = 23.979 (4) Å | T = 173 K |
V = 7378 (2) Å3 | Prism, colourless |
Z = 8 | 0.50 × 0.40 × 0.40 mm |
F(000) = 3144 | |
Data collection top
Bruker SMART CCD area-detector diffractometer | 16737 independent reflections |
Radiation source: fine-focus sealed tube | 14199 reflections with I > 2σ(I) |
Graphite monochromator | Rint = 0.043 |
φ and ω scans | θmax = 27.5°, θmin = 1.2° |
Absorption correction: multi-scan (SADABS; Bruker, 2000) | h = −42→43 |
Tmin = 0.652, Tmax = 0.795 | k = −11→12 |
79631 measured reflections | l = −31→30 |
Refinement top
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)] = 0.049 | H-atom parameters constrained |
wR(F2) = 0.131 | w = 1/[σ2(Fo2) + (0.0795P)2 + 1.5731P] where P = (Fo2 + 2Fc2)/3 |
S = 1.07 | (Δ/σ)max = 0.001 |
16737 reflections | Δρmax = 1.56 e Å−3 |
821 parameters | Δρmin = −0.62 e Å−3 |
2 restraints | Absolute structure: Flack (1983), 8081 Friedel pairs |
Primary atom site location: structure-invariant direct methods | Absolute structure parameter: −0.01 (4) |
Special details top
Geometry. All e.s.d.'s (except the e.s.d. in the dihedral angle between two l.s. planes)
are estimated using the full covariance matrix. The cell e.s.d.'s are taken
into account individually in the estimation of e.s.d.'s in distances, angles
and torsion angles; correlations between e.s.d.'s in cell parameters are only
used when they are defined by crystal symmetry. An approximate (isotropic)
treatment of cell e.s.d.'s is used for estimating e.s.d.'s involving l.s.
planes. |
Refinement. Refinement of F2 against ALL reflections. The weighted R-factor
wR and goodness of fit S are based on F2, conventional
R-factors R are based on F, with F set to zero for
negative F2. The threshold expression of F2 >
σ(F2) is used only for calculating R-factors(gt) etc.
and is not relevant to the choice of reflections for refinement.
R-factors based on F2 are statistically about twice as large
as those based on F, and R- factors based on ALL data will be
even larger. |
Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top | x | y | z | Uiso*/Ueq | |
P1 | 0.11889 (2) | 0.16432 (9) | 0.38841 (4) | 0.02138 (17) | |
P2 | 0.17365 (2) | 0.27356 (9) | 0.36996 (4) | 0.02369 (17) | |
P3 | 0.18304 (2) | 0.21808 (9) | 0.28495 (3) | 0.02099 (17) | |
C11 | 0.10915 (10) | 0.2199 (4) | 0.45975 (14) | 0.0291 (7) | |
C12 | 0.07287 (13) | 0.1854 (7) | 0.48336 (19) | 0.0646 (17) | |
H12 | 0.0540 | 0.1295 | 0.4629 | 0.078* | |
C13 | 0.06347 (15) | 0.2312 (9) | 0.5368 (2) | 0.079 (2) | |
H13 | 0.0383 | 0.2060 | 0.5529 | 0.095* | |
C14 | 0.08979 (14) | 0.3111 (6) | 0.56577 (18) | 0.0615 (15) | |
H14 | 0.0829 | 0.3450 | 0.6019 | 0.074* | |
C15 | 0.12609 (15) | 0.3436 (7) | 0.5438 (2) | 0.0668 (16) | |
H15 | 0.1450 | 0.3970 | 0.5651 | 0.080* | |
C16 | 0.13567 (13) | 0.2988 (5) | 0.49000 (18) | 0.0497 (11) | |
H16 | 0.1610 | 0.3237 | 0.4744 | 0.060* | |
C21 | 0.07490 (10) | 0.2191 (4) | 0.34941 (14) | 0.0255 (7) | |
C22 | 0.04369 (10) | 0.1276 (4) | 0.33589 (15) | 0.0281 (7) | |
H22 | 0.0452 | 0.0280 | 0.3454 | 0.034* | |
C23 | 0.01015 (11) | 0.1800 (5) | 0.30851 (16) | 0.0350 (8) | |
H23 | −0.0112 | 0.1162 | 0.2993 | 0.042* | |
C24 | 0.00757 (11) | 0.3241 (5) | 0.29444 (17) | 0.0388 (9) | |
H24 | −0.0153 | 0.3596 | 0.2751 | 0.047* | |
C25 | 0.03860 (12) | 0.4172 (4) | 0.30868 (18) | 0.0393 (9) | |
H25 | 0.0366 | 0.5171 | 0.2998 | 0.047* | |
C26 | 0.07213 (11) | 0.3660 (4) | 0.33551 (16) | 0.0316 (8) | |
H26 | 0.0935 | 0.4300 | 0.3447 | 0.038* | |
C31 | 0.12372 (10) | −0.0305 (3) | 0.38793 (16) | 0.0268 (7) | |
C32 | 0.14233 (11) | −0.0946 (4) | 0.43384 (18) | 0.0363 (9) | |
H32 | 0.1484 | −0.0388 | 0.4660 | 0.044* | |
C33 | 0.15184 (12) | −0.2404 (4) | 0.4321 (2) | 0.0466 (11) | |
H33 | 0.1645 | −0.2846 | 0.4633 | 0.056* | |
C34 | 0.14311 (12) | −0.3212 (4) | 0.3859 (2) | 0.0509 (12) | |
H34 | 0.1500 | −0.4210 | 0.3852 | 0.061* | |
C35 | 0.12462 (12) | −0.2604 (4) | 0.3404 (2) | 0.0426 (11) | |
H35 | 0.1183 | −0.3177 | 0.3087 | 0.051* | |
C36 | 0.11504 (11) | −0.1117 (4) | 0.34136 (17) | 0.0312 (8) | |
H36 | 0.1026 | −0.0678 | 0.3100 | 0.037* | |
C41 | 0.22829 (10) | 0.3184 (3) | 0.26770 (15) | 0.0246 (7) | |
C42 | 0.25175 (11) | 0.3851 (4) | 0.30814 (16) | 0.0309 (8) | |
H42 | 0.2440 | 0.3814 | 0.3462 | 0.037* | |
C43 | 0.28662 (11) | 0.4573 (4) | 0.29272 (18) | 0.0377 (9) | |
H43 | 0.3029 | 0.5013 | 0.3205 | 0.045* | |
C44 | 0.29774 (12) | 0.4655 (5) | 0.23778 (19) | 0.0423 (10) | |
H44 | 0.3214 | 0.5165 | 0.2276 | 0.051* | |
C45 | 0.27468 (13) | 0.3999 (5) | 0.19727 (18) | 0.0460 (10) | |
H45 | 0.2825 | 0.4050 | 0.1592 | 0.055* | |
C46 | 0.23980 (12) | 0.3257 (4) | 0.21255 (16) | 0.0380 (9) | |
H46 | 0.2239 | 0.2801 | 0.1847 | 0.046* | |
C51 | 0.14425 (10) | 0.2805 (4) | 0.23838 (14) | 0.0274 (7) | |
C52 | 0.11341 (10) | 0.1903 (4) | 0.22058 (15) | 0.0320 (8) | |
H52 | 0.1141 | 0.0898 | 0.2288 | 0.038* | |
C53 | 0.08139 (11) | 0.2489 (6) | 0.19055 (16) | 0.0437 (11) | |
H53 | 0.0600 | 0.1880 | 0.1789 | 0.052* | |
C54 | 0.08052 (14) | 0.3910 (6) | 0.17785 (18) | 0.0529 (13) | |
H54 | 0.0587 | 0.4292 | 0.1570 | 0.063* | |
C55 | 0.11121 (14) | 0.4815 (5) | 0.19499 (18) | 0.0489 (12) | |
H55 | 0.1104 | 0.5814 | 0.1858 | 0.059* | |
C56 | 0.14320 (12) | 0.4271 (4) | 0.22558 (16) | 0.0350 (8) | |
H56 | 0.1642 | 0.4894 | 0.2377 | 0.042* | |
C61 | 0.19467 (10) | 0.0308 (3) | 0.27021 (14) | 0.0231 (7) | |
C62 | 0.21264 (10) | −0.0504 (4) | 0.31220 (16) | 0.0283 (7) | |
H62 | 0.2164 | −0.0098 | 0.3482 | 0.034* | |
C63 | 0.22501 (11) | −0.1907 (4) | 0.30128 (18) | 0.0365 (9) | |
H63 | 0.2375 | −0.2459 | 0.3299 | 0.044* | |
C64 | 0.21939 (13) | −0.2499 (4) | 0.2499 (2) | 0.0428 (10) | |
H64 | 0.2277 | −0.3466 | 0.2430 | 0.051* | |
C65 | 0.20173 (13) | −0.1706 (4) | 0.20783 (17) | 0.0383 (9) | |
H65 | 0.1979 | −0.2127 | 0.1721 | 0.046* | |
C66 | 0.18952 (11) | −0.0287 (4) | 0.21771 (16) | 0.0301 (7) | |
H66 | 0.1778 | 0.0268 | 0.1886 | 0.036* | |
P4 | 0.36908 (2) | 0.06748 (8) | 0.36631 (4) | 0.02066 (16) | |
P5 | 0.42529 (3) | −0.03321 (9) | 0.38430 (4) | 0.02447 (18) | |
P6 | 0.43559 (2) | 0.03042 (9) | 0.46852 (3) | 0.02224 (17) | |
C71 | 0.35748 (10) | 0.0006 (3) | 0.29704 (14) | 0.0250 (7) | |
C72 | 0.32091 (11) | 0.0407 (4) | 0.27369 (16) | 0.0342 (8) | |
H72 | 0.3041 | 0.1085 | 0.2922 | 0.041* | |
C73 | 0.30925 (12) | −0.0182 (5) | 0.22370 (18) | 0.0421 (10) | |
H73 | 0.2844 | 0.0098 | 0.2075 | 0.051* | |
C74 | 0.33322 (14) | −0.1175 (5) | 0.19673 (17) | 0.0449 (10) | |
H74 | 0.3244 | −0.1600 | 0.1628 | 0.054* | |
C75 | 0.37005 (14) | −0.1554 (5) | 0.21885 (18) | 0.0471 (10) | |
H75 | 0.3869 | −0.2219 | 0.1997 | 0.056* | |
C76 | 0.38237 (12) | −0.0961 (4) | 0.26898 (16) | 0.0373 (9) | |
H76 | 0.4078 | −0.1214 | 0.2842 | 0.045* | |
C81 | 0.37166 (9) | 0.2623 (3) | 0.36353 (16) | 0.0250 (7) | |
C82 | 0.36258 (11) | 0.3483 (4) | 0.40940 (15) | 0.0295 (7) | |
H82 | 0.3511 | 0.3064 | 0.4419 | 0.035* | |
C83 | 0.37031 (12) | 0.4953 (4) | 0.40746 (17) | 0.0353 (9) | |
H83 | 0.3637 | 0.5548 | 0.4384 | 0.042* | |
C84 | 0.38754 (12) | 0.5550 (4) | 0.3609 (2) | 0.0396 (9) | |
H84 | 0.3934 | 0.6555 | 0.3601 | 0.048* | |
C85 | 0.39656 (11) | 0.4698 (4) | 0.31472 (18) | 0.0371 (9) | |
H85 | 0.4081 | 0.5123 | 0.2824 | 0.044* | |
C86 | 0.38880 (10) | 0.3257 (4) | 0.31616 (15) | 0.0280 (7) | |
H86 | 0.3951 | 0.2673 | 0.2847 | 0.034* | |
C91 | 0.32601 (10) | 0.0126 (4) | 0.40740 (14) | 0.0235 (7) | |
C92 | 0.32485 (11) | −0.1302 (4) | 0.42480 (16) | 0.0331 (8) | |
H92 | 0.3472 | −0.1917 | 0.4178 | 0.040* | |
C93 | 0.29169 (12) | −0.1835 (4) | 0.45209 (18) | 0.0415 (10) | |
H93 | 0.2908 | −0.2821 | 0.4633 | 0.050* | |
C94 | 0.25958 (12) | −0.0931 (5) | 0.46319 (17) | 0.0424 (10) | |
H94 | 0.2368 | −0.1297 | 0.4824 | 0.051* | |
C95 | 0.26037 (11) | 0.0499 (5) | 0.44657 (17) | 0.0376 (9) | |
H95 | 0.2384 | 0.1118 | 0.4550 | 0.045* | |
C96 | 0.29332 (10) | 0.1031 (4) | 0.41746 (15) | 0.0288 (7) | |
H96 | 0.2936 | 0.2003 | 0.4046 | 0.035* | |
C101 | 0.48169 (10) | −0.0643 (4) | 0.48554 (15) | 0.0283 (7) | |
C102 | 0.50605 (11) | −0.1210 (5) | 0.44452 (17) | 0.0398 (9) | |
H102 | 0.4986 | −0.1119 | 0.4064 | 0.048* | |
C103 | 0.54140 (13) | −0.1913 (5) | 0.4588 (2) | 0.0523 (12) | |
H103 | 0.5583 | −0.2295 | 0.4305 | 0.063* | |
C104 | 0.55179 (14) | −0.2054 (6) | 0.5135 (2) | 0.0582 (13) | |
H104 | 0.5760 | −0.2538 | 0.5233 | 0.070* | |
C105 | 0.52740 (15) | −0.1499 (6) | 0.5544 (2) | 0.0671 (16) | |
H105 | 0.5347 | −0.1600 | 0.5925 | 0.081* | |
C106 | 0.49298 (14) | −0.0808 (5) | 0.54078 (18) | 0.0489 (11) | |
H106 | 0.4763 | −0.0431 | 0.5695 | 0.059* | |
C111 | 0.44602 (10) | 0.2202 (3) | 0.48190 (15) | 0.0254 (7) | |
C112 | 0.44415 (12) | 0.2780 (4) | 0.53574 (16) | 0.0356 (8) | |
H112 | 0.4347 | 0.2205 | 0.5659 | 0.043* | |
C113 | 0.45598 (13) | 0.4183 (4) | 0.54479 (19) | 0.0429 (10) | |
H113 | 0.4554 | 0.4571 | 0.5815 | 0.051* | |
C114 | 0.46850 (13) | 0.5019 (4) | 0.5016 (2) | 0.0435 (10) | |
H114 | 0.4759 | 0.5997 | 0.5081 | 0.052* | |
C115 | 0.47060 (11) | 0.4464 (4) | 0.44829 (18) | 0.0364 (8) | |
H115 | 0.4798 | 0.5053 | 0.4184 | 0.044* | |
C116 | 0.45934 (10) | 0.3042 (4) | 0.43838 (15) | 0.0292 (7) | |
H116 | 0.4608 | 0.2652 | 0.4018 | 0.035* | |
C121 | 0.39784 (10) | −0.0314 (4) | 0.51676 (15) | 0.0283 (7) | |
C122 | 0.39658 (13) | −0.1779 (4) | 0.52993 (17) | 0.0403 (9) | |
H122 | 0.4172 | −0.2407 | 0.5171 | 0.048* | |
C123 | 0.36568 (16) | −0.2318 (6) | 0.5615 (2) | 0.0560 (14) | |
H123 | 0.3653 | −0.3313 | 0.5714 | 0.067* | |
C124 | 0.33555 (15) | −0.1427 (7) | 0.57853 (19) | 0.0620 (15) | |
H124 | 0.3138 | −0.1816 | 0.5994 | 0.074* | |
C125 | 0.33593 (12) | 0.0044 (6) | 0.56606 (18) | 0.0495 (11) | |
H125 | 0.3151 | 0.0660 | 0.5789 | 0.059* | |
C126 | 0.36732 (11) | 0.0591 (5) | 0.53457 (16) | 0.0372 (9) | |
H126 | 0.3679 | 0.1590 | 0.5252 | 0.045* | |
Cl1 | 0.26207 (4) | 1.11194 (13) | 0.08992 (5) | 0.0552 (3) | |
Cl2 | 0.26741 (3) | 0.73508 (12) | 0.07842 (5) | 0.0477 (3) | |
Cl3 | 0.25535 (4) | 0.95393 (13) | −0.03950 (5) | 0.0578 (3) | |
Cl4 | 0.17718 (3) | 0.91235 (13) | 0.05536 (6) | 0.0534 (3) | |
Al1 | 0.24093 (4) | 0.92705 (13) | 0.04639 (5) | 0.0363 (3) | |
Cl5 | −0.00950 (3) | 0.79118 (11) | 0.30126 (4) | 0.0442 (2) | |
Cl6 | −0.01484 (3) | 0.60484 (13) | 0.17636 (5) | 0.0522 (3) | |
Cl7 | 0.06505 (3) | 0.83930 (12) | 0.20048 (5) | 0.0494 (3) | |
Cl8 | −0.03059 (5) | 0.97781 (15) | 0.17917 (5) | 0.0678 (4) | |
Al2 | 0.00243 (4) | 0.80408 (12) | 0.21404 (5) | 0.0344 (3) | |
Cl9 | 0.39934 (8) | 0.2046 (3) | 0.16412 (10) | 0.1340 (10) | |
Cl10 | 0.35829 (11) | 0.4197 (4) | 0.09593 (14) | 0.1843 (16) | |
C1 | 0.3648 (2) | 0.2413 (8) | 0.1288 (4) | 0.107 (3) | |
H1A | 0.3405 | 0.2240 | 0.1516 | 0.128* | |
H1B | 0.3643 | 0.1692 | 0.0983 | 0.128* | |
Atomic displacement parameters (Å2) top | U11 | U22 | U33 | U12 | U13 | U23 |
P1 | 0.0231 (4) | 0.0194 (4) | 0.0216 (4) | 0.0017 (3) | 0.0005 (3) | −0.0015 (3) |
P2 | 0.0255 (4) | 0.0227 (4) | 0.0229 (4) | −0.0008 (3) | 0.0010 (3) | −0.0065 (3) |
P3 | 0.0221 (4) | 0.0192 (4) | 0.0217 (4) | 0.0013 (3) | 0.0004 (3) | −0.0025 (3) |
C11 | 0.0282 (17) | 0.0375 (19) | 0.0216 (17) | 0.0094 (14) | 0.0011 (14) | −0.0021 (15) |
C12 | 0.031 (2) | 0.131 (5) | 0.031 (2) | −0.025 (3) | 0.0106 (18) | −0.014 (3) |
C13 | 0.036 (2) | 0.168 (7) | 0.034 (3) | −0.008 (3) | 0.014 (2) | −0.011 (3) |
C14 | 0.049 (3) | 0.109 (4) | 0.026 (2) | 0.021 (3) | 0.0065 (19) | −0.019 (2) |
C15 | 0.051 (3) | 0.107 (4) | 0.042 (3) | −0.013 (3) | 0.007 (2) | −0.032 (3) |
C16 | 0.040 (2) | 0.077 (3) | 0.032 (2) | −0.010 (2) | 0.0081 (18) | −0.018 (2) |
C21 | 0.0251 (16) | 0.0303 (17) | 0.0210 (16) | 0.0059 (14) | 0.0016 (13) | −0.0004 (13) |
C22 | 0.0272 (17) | 0.0287 (18) | 0.0285 (18) | 0.0027 (14) | 0.0030 (14) | −0.0030 (14) |
C23 | 0.0278 (18) | 0.048 (2) | 0.0292 (19) | 0.0028 (16) | −0.0024 (15) | −0.0024 (16) |
C24 | 0.0287 (19) | 0.055 (2) | 0.033 (2) | 0.0131 (17) | 0.0011 (16) | 0.0034 (18) |
C25 | 0.044 (2) | 0.036 (2) | 0.037 (2) | 0.0171 (17) | 0.0037 (17) | 0.0024 (17) |
C26 | 0.0295 (18) | 0.0283 (18) | 0.037 (2) | 0.0057 (14) | 0.0029 (15) | −0.0021 (15) |
C31 | 0.0268 (17) | 0.0177 (15) | 0.0358 (19) | 0.0003 (12) | 0.0044 (15) | 0.0008 (14) |
C32 | 0.0304 (19) | 0.0301 (19) | 0.048 (2) | −0.0028 (15) | −0.0099 (16) | 0.0050 (17) |
C33 | 0.036 (2) | 0.028 (2) | 0.076 (3) | 0.0019 (16) | −0.009 (2) | 0.017 (2) |
C34 | 0.038 (2) | 0.0171 (17) | 0.097 (4) | 0.0032 (15) | 0.009 (2) | 0.003 (2) |
C35 | 0.039 (2) | 0.0231 (18) | 0.066 (3) | −0.0092 (16) | 0.012 (2) | −0.0127 (19) |
C36 | 0.0297 (18) | 0.0244 (17) | 0.040 (2) | −0.0024 (14) | 0.0056 (15) | −0.0013 (15) |
C41 | 0.0243 (16) | 0.0179 (15) | 0.0316 (18) | 0.0006 (12) | 0.0028 (14) | −0.0035 (13) |
C42 | 0.0309 (18) | 0.0294 (18) | 0.0323 (19) | 0.0018 (15) | 0.0030 (15) | 0.0007 (15) |
C43 | 0.0297 (19) | 0.038 (2) | 0.046 (2) | −0.0043 (16) | −0.0034 (17) | −0.0025 (17) |
C44 | 0.031 (2) | 0.038 (2) | 0.057 (3) | −0.0082 (17) | 0.0123 (19) | 0.0027 (19) |
C45 | 0.043 (2) | 0.059 (3) | 0.036 (2) | −0.012 (2) | 0.0164 (18) | −0.007 (2) |
C46 | 0.037 (2) | 0.047 (2) | 0.030 (2) | −0.0094 (17) | 0.0038 (16) | −0.0097 (17) |
C51 | 0.0242 (16) | 0.0361 (19) | 0.0218 (17) | 0.0063 (14) | 0.0040 (13) | 0.0011 (14) |
C52 | 0.0269 (17) | 0.045 (2) | 0.0244 (18) | 0.0018 (15) | 0.0004 (14) | 0.0018 (15) |
C53 | 0.0252 (18) | 0.083 (3) | 0.023 (2) | 0.005 (2) | −0.0022 (15) | −0.003 (2) |
C54 | 0.046 (2) | 0.083 (4) | 0.030 (2) | 0.035 (2) | 0.0016 (19) | 0.011 (2) |
C55 | 0.060 (3) | 0.050 (3) | 0.036 (2) | 0.028 (2) | 0.011 (2) | 0.0110 (19) |
C56 | 0.040 (2) | 0.0328 (19) | 0.032 (2) | 0.0119 (16) | 0.0106 (16) | 0.0038 (15) |
C61 | 0.0270 (16) | 0.0142 (13) | 0.0282 (17) | 0.0022 (12) | 0.0046 (14) | −0.0048 (12) |
C62 | 0.0296 (18) | 0.0236 (17) | 0.0316 (18) | 0.0045 (13) | 0.0004 (14) | −0.0034 (14) |
C63 | 0.034 (2) | 0.0273 (18) | 0.048 (2) | 0.0102 (15) | 0.0016 (17) | 0.0022 (16) |
C64 | 0.041 (2) | 0.0248 (18) | 0.062 (3) | 0.0039 (16) | 0.005 (2) | −0.0117 (18) |
C65 | 0.048 (2) | 0.0290 (18) | 0.038 (2) | 0.0015 (17) | 0.0043 (18) | −0.0115 (16) |
C66 | 0.0368 (19) | 0.0231 (16) | 0.0304 (18) | 0.0001 (14) | −0.0016 (15) | −0.0045 (14) |
P4 | 0.0225 (4) | 0.0179 (4) | 0.0215 (4) | 0.0001 (3) | −0.0002 (3) | −0.0014 (3) |
P5 | 0.0244 (4) | 0.0238 (4) | 0.0252 (4) | 0.0028 (3) | −0.0025 (3) | −0.0058 (3) |
P6 | 0.0226 (4) | 0.0208 (4) | 0.0234 (4) | 0.0005 (3) | −0.0010 (3) | −0.0021 (3) |
C71 | 0.0302 (17) | 0.0218 (16) | 0.0230 (17) | −0.0063 (13) | 0.0026 (13) | −0.0008 (13) |
C72 | 0.0287 (18) | 0.040 (2) | 0.034 (2) | 0.0010 (16) | −0.0019 (15) | −0.0035 (16) |
C73 | 0.031 (2) | 0.062 (3) | 0.034 (2) | −0.0042 (18) | −0.0065 (17) | 0.0017 (19) |
C74 | 0.056 (3) | 0.052 (2) | 0.027 (2) | −0.013 (2) | −0.0111 (18) | −0.0066 (18) |
C75 | 0.063 (3) | 0.048 (2) | 0.030 (2) | 0.011 (2) | −0.0015 (19) | −0.0081 (18) |
C76 | 0.043 (2) | 0.039 (2) | 0.030 (2) | 0.0069 (17) | −0.0050 (16) | −0.0062 (16) |
C81 | 0.0237 (15) | 0.0201 (15) | 0.0314 (18) | −0.0012 (12) | −0.0002 (14) | 0.0010 (14) |
C82 | 0.0332 (18) | 0.0273 (18) | 0.0279 (18) | 0.0012 (15) | −0.0023 (14) | −0.0005 (14) |
C83 | 0.043 (2) | 0.0237 (18) | 0.039 (2) | 0.0022 (15) | −0.0015 (17) | −0.0083 (16) |
C84 | 0.041 (2) | 0.0187 (16) | 0.059 (3) | −0.0050 (15) | −0.001 (2) | −0.0001 (17) |
C85 | 0.0339 (19) | 0.034 (2) | 0.044 (2) | −0.0029 (16) | 0.0030 (17) | 0.0079 (17) |
C86 | 0.0265 (17) | 0.0260 (17) | 0.0315 (19) | −0.0011 (13) | 0.0014 (14) | 0.0008 (14) |
C91 | 0.0239 (16) | 0.0267 (17) | 0.0198 (16) | −0.0037 (13) | −0.0026 (13) | −0.0015 (13) |
C92 | 0.0325 (19) | 0.0297 (19) | 0.037 (2) | −0.0036 (15) | −0.0020 (15) | 0.0010 (15) |
C93 | 0.039 (2) | 0.040 (2) | 0.045 (2) | −0.0137 (17) | −0.0042 (18) | 0.0110 (18) |
C94 | 0.032 (2) | 0.062 (3) | 0.034 (2) | −0.0176 (18) | 0.0011 (17) | 0.010 (2) |
C95 | 0.0254 (18) | 0.055 (2) | 0.032 (2) | 0.0004 (16) | −0.0013 (15) | 0.0003 (18) |
C96 | 0.0282 (17) | 0.0333 (19) | 0.0250 (18) | 0.0026 (14) | −0.0020 (14) | 0.0016 (14) |
C101 | 0.0260 (17) | 0.0269 (17) | 0.0319 (19) | 0.0015 (14) | −0.0052 (14) | −0.0040 (14) |
C102 | 0.0334 (19) | 0.054 (2) | 0.032 (2) | 0.0101 (17) | 0.0007 (16) | 0.0000 (18) |
C103 | 0.037 (2) | 0.072 (3) | 0.048 (3) | 0.017 (2) | 0.0011 (19) | −0.011 (2) |
C104 | 0.041 (2) | 0.076 (3) | 0.058 (3) | 0.027 (2) | −0.021 (2) | −0.012 (3) |
C105 | 0.061 (3) | 0.099 (4) | 0.041 (3) | 0.036 (3) | −0.024 (2) | −0.018 (3) |
C106 | 0.049 (2) | 0.063 (3) | 0.034 (2) | 0.020 (2) | −0.0138 (19) | −0.015 (2) |
C111 | 0.0227 (16) | 0.0203 (15) | 0.0331 (19) | 0.0002 (13) | 0.0016 (13) | −0.0059 (14) |
C112 | 0.040 (2) | 0.035 (2) | 0.032 (2) | 0.0008 (16) | −0.0008 (16) | −0.0030 (16) |
C113 | 0.054 (2) | 0.033 (2) | 0.042 (2) | −0.0019 (18) | −0.001 (2) | −0.0183 (18) |
C114 | 0.044 (2) | 0.0258 (19) | 0.060 (3) | −0.0037 (17) | −0.006 (2) | −0.0099 (18) |
C115 | 0.0343 (19) | 0.0290 (19) | 0.046 (2) | −0.0031 (15) | 0.0042 (17) | 0.0033 (17) |
C116 | 0.0253 (17) | 0.0322 (19) | 0.0299 (19) | −0.0024 (14) | −0.0009 (14) | −0.0036 (15) |
C121 | 0.0288 (18) | 0.0335 (18) | 0.0227 (17) | −0.0013 (15) | −0.0016 (14) | 0.0032 (14) |
C122 | 0.050 (2) | 0.039 (2) | 0.032 (2) | −0.0104 (18) | −0.0102 (18) | 0.0052 (16) |
C123 | 0.068 (3) | 0.059 (3) | 0.041 (3) | −0.034 (3) | −0.019 (2) | 0.020 (2) |
C124 | 0.050 (3) | 0.105 (4) | 0.031 (2) | −0.040 (3) | 0.001 (2) | 0.007 (3) |
C125 | 0.031 (2) | 0.089 (4) | 0.029 (2) | −0.010 (2) | 0.0017 (17) | −0.002 (2) |
C126 | 0.0315 (19) | 0.053 (2) | 0.0271 (19) | 0.0008 (17) | 0.0013 (15) | 0.0031 (17) |
Cl1 | 0.0647 (7) | 0.0507 (6) | 0.0503 (7) | 0.0010 (5) | −0.0154 (5) | −0.0207 (5) |
Cl2 | 0.0495 (6) | 0.0487 (6) | 0.0448 (6) | 0.0140 (5) | −0.0121 (5) | −0.0012 (5) |
Cl3 | 0.0875 (9) | 0.0546 (7) | 0.0312 (5) | 0.0297 (6) | 0.0049 (5) | −0.0065 (5) |
Cl4 | 0.0385 (5) | 0.0547 (6) | 0.0670 (8) | 0.0120 (5) | −0.0114 (5) | −0.0155 (6) |
Al1 | 0.0393 (6) | 0.0414 (6) | 0.0282 (6) | 0.0115 (5) | −0.0074 (5) | −0.0100 (5) |
Cl5 | 0.0637 (7) | 0.0370 (5) | 0.0319 (5) | 0.0053 (5) | 0.0044 (5) | 0.0020 (4) |
Cl6 | 0.0461 (6) | 0.0523 (6) | 0.0582 (7) | 0.0076 (5) | −0.0175 (5) | −0.0231 (5) |
Cl7 | 0.0438 (6) | 0.0476 (6) | 0.0570 (7) | −0.0003 (5) | 0.0022 (5) | −0.0078 (5) |
Cl8 | 0.0906 (9) | 0.0664 (8) | 0.0466 (7) | 0.0446 (7) | −0.0115 (6) | 0.0065 (6) |
Al2 | 0.0386 (6) | 0.0357 (6) | 0.0289 (6) | 0.0097 (5) | −0.0053 (5) | −0.0025 (5) |
Cl9 | 0.1251 (19) | 0.195 (3) | 0.0823 (13) | −0.0538 (18) | 0.0411 (13) | −0.0144 (15) |
Cl10 | 0.214 (3) | 0.185 (3) | 0.154 (3) | −0.026 (2) | 0.126 (3) | 0.020 (2) |
C1 | 0.104 (6) | 0.074 (4) | 0.142 (8) | −0.006 (4) | 0.046 (6) | 0.022 (5) |
Geometric parameters (Å, º) top
P1—C31 | 1.808 (3) | P6—C101 | 1.813 (3) |
P1—C21 | 1.809 (3) | P6—C111 | 1.817 (3) |
P1—C11 | 1.816 (3) | C71—C72 | 1.390 (5) |
P1—P2 | 2.1301 (12) | C71—C76 | 1.392 (5) |
P2—P3 | 2.1249 (12) | C72—C73 | 1.373 (6) |
P3—C51 | 1.802 (3) | C72—H72 | 0.9500 |
P3—C61 | 1.809 (3) | C73—C74 | 1.378 (6) |
P3—C41 | 1.816 (3) | C73—H73 | 0.9500 |
C11—C16 | 1.355 (6) | C74—C75 | 1.381 (6) |
C11—C12 | 1.371 (5) | C74—H74 | 0.9500 |
C12—C13 | 1.386 (7) | C75—C76 | 1.383 (6) |
C12—H12 | 0.9500 | C75—H75 | 0.9500 |
C13—C14 | 1.339 (8) | C76—H76 | 0.9500 |
C13—H13 | 0.9500 | C81—C82 | 1.390 (5) |
C14—C15 | 1.352 (7) | C81—C86 | 1.400 (5) |
C14—H14 | 0.9500 | C82—C83 | 1.383 (5) |
C15—C16 | 1.391 (6) | C82—H82 | 0.9500 |
C15—H15 | 0.9500 | C83—C84 | 1.372 (6) |
C16—H16 | 0.9500 | C83—H83 | 0.9500 |
C21—C22 | 1.378 (5) | C84—C85 | 1.391 (6) |
C21—C26 | 1.401 (5) | C84—H84 | 0.9500 |
C22—C23 | 1.383 (5) | C85—C86 | 1.358 (5) |
C22—H22 | 0.9500 | C85—H85 | 0.9500 |
C23—C24 | 1.377 (6) | C86—H86 | 0.9500 |
C23—H23 | 0.9500 | C91—C92 | 1.385 (5) |
C24—C25 | 1.387 (6) | C91—C96 | 1.393 (5) |
C24—H24 | 0.9500 | C92—C93 | 1.375 (5) |
C25—C26 | 1.373 (5) | C92—H92 | 0.9500 |
C25—H25 | 0.9500 | C93—C94 | 1.382 (6) |
C26—H26 | 0.9500 | C93—H93 | 0.9500 |
C31—C36 | 1.376 (5) | C94—C95 | 1.381 (6) |
C31—C32 | 1.395 (5) | C94—H94 | 0.9500 |
C32—C33 | 1.385 (6) | C95—C96 | 1.390 (5) |
C32—H32 | 0.9500 | C95—H95 | 0.9500 |
C33—C34 | 1.369 (7) | C96—H96 | 0.9500 |
C33—H33 | 0.9500 | C101—C102 | 1.378 (5) |
C34—C35 | 1.372 (7) | C101—C106 | 1.385 (5) |
C34—H34 | 0.9500 | C102—C103 | 1.387 (6) |
C35—C36 | 1.412 (5) | C102—H102 | 0.9500 |
C35—H35 | 0.9500 | C103—C104 | 1.363 (7) |
C36—H36 | 0.9500 | C103—H103 | 0.9500 |
C41—C46 | 1.379 (5) | C104—C105 | 1.373 (7) |
C41—C42 | 1.389 (5) | C104—H104 | 0.9500 |
C42—C43 | 1.389 (5) | C105—C106 | 1.351 (6) |
C42—H42 | 0.9500 | C105—H105 | 0.9500 |
C43—C44 | 1.370 (6) | C106—H106 | 0.9500 |
C43—H43 | 0.9500 | C111—C116 | 1.374 (5) |
C44—C45 | 1.379 (6) | C111—C112 | 1.398 (5) |
C44—H44 | 0.9500 | C112—C113 | 1.373 (5) |
C45—C46 | 1.397 (6) | C112—H112 | 0.9500 |
C45—H45 | 0.9500 | C113—C114 | 1.358 (7) |
C46—H46 | 0.9500 | C113—H113 | 0.9500 |
C51—C52 | 1.389 (5) | C114—C115 | 1.379 (6) |
C51—C56 | 1.390 (5) | C114—H114 | 0.9500 |
C52—C53 | 1.396 (5) | C115—C116 | 1.387 (5) |
C52—H52 | 0.9500 | C115—H115 | 0.9500 |
C53—C54 | 1.349 (7) | C116—H116 | 0.9500 |
C53—H53 | 0.9500 | C121—C126 | 1.384 (5) |
C54—C55 | 1.383 (7) | C121—C122 | 1.391 (5) |
C54—H54 | 0.9500 | C122—C123 | 1.370 (6) |
C55—C56 | 1.387 (6) | C122—H122 | 0.9500 |
C55—H55 | 0.9500 | C123—C124 | 1.361 (8) |
C56—H56 | 0.9500 | C123—H123 | 0.9500 |
C61—C66 | 1.385 (5) | C124—C125 | 1.392 (8) |
C61—C62 | 1.391 (5) | C124—H124 | 0.9500 |
C62—C63 | 1.386 (5) | C125—C126 | 1.385 (6) |
C62—H62 | 0.9500 | C125—H125 | 0.9500 |
C63—C64 | 1.361 (6) | C126—H126 | 0.9500 |
C63—H63 | 0.9500 | Cl1—Al1 | 2.1228 (16) |
C64—C65 | 1.379 (6) | Cl2—Al1 | 2.1250 (16) |
C64—H64 | 0.9500 | Cl3—Al1 | 2.1294 (17) |
C65—C66 | 1.394 (5) | Cl4—Al1 | 2.1367 (16) |
C65—H65 | 0.9500 | Cl5—Al2 | 2.1322 (15) |
C66—H66 | 0.9500 | Cl6—Al2 | 2.1304 (16) |
P4—C81 | 1.804 (3) | Cl7—Al2 | 2.1344 (17) |
P4—C91 | 1.812 (3) | Cl8—Al2 | 2.1181 (16) |
P4—C71 | 1.814 (3) | Cl9—C1 | 1.466 (8) |
P4—P5 | 2.1337 (12) | Cl10—C1 | 1.841 (7) |
P5—P6 | 2.1312 (12) | C1—H1A | 0.9900 |
P6—C121 | 1.801 (4) | C1—H1B | 0.9900 |
| | | |
C31—P1—C21 | 110.32 (16) | C101—P6—C111 | 105.37 (15) |
C31—P1—C11 | 107.69 (17) | C121—P6—P5 | 114.13 (12) |
C21—P1—C11 | 105.26 (15) | C101—P6—P5 | 102.47 (12) |
C31—P1—P2 | 113.25 (11) | C111—P6—P5 | 117.68 (12) |
C21—P1—P2 | 116.90 (12) | C72—C71—C76 | 119.8 (3) |
C11—P1—P2 | 102.37 (13) | C72—C71—P4 | 117.7 (3) |
P3—P2—P1 | 102.16 (5) | C76—C71—P4 | 122.3 (3) |
C51—P3—C61 | 109.80 (16) | C73—C72—C71 | 119.6 (4) |
C51—P3—C41 | 106.83 (16) | C73—C72—H72 | 120.2 |
C61—P3—C41 | 105.46 (15) | C71—C72—H72 | 120.2 |
C51—P3—P2 | 114.33 (11) | C72—C73—C74 | 120.7 (4) |
C61—P3—P2 | 116.74 (12) | C72—C73—H73 | 119.6 |
C41—P3—P2 | 102.54 (12) | C74—C73—H73 | 119.6 |
C16—C11—C12 | 118.5 (4) | C73—C74—C75 | 120.2 (4) |
C16—C11—P1 | 122.7 (3) | C73—C74—H74 | 119.9 |
C12—C11—P1 | 118.7 (3) | C75—C74—H74 | 119.9 |
C11—C12—C13 | 120.6 (5) | C74—C75—C76 | 119.8 (4) |
C11—C12—H12 | 119.7 | C74—C75—H75 | 120.1 |
C13—C12—H12 | 119.7 | C76—C75—H75 | 120.1 |
C14—C13—C12 | 120.0 (5) | C75—C76—C71 | 119.9 (4) |
C14—C13—H13 | 120.0 | C75—C76—H76 | 120.1 |
C12—C13—H13 | 120.0 | C71—C76—H76 | 120.1 |
C13—C14—C15 | 120.3 (4) | C82—C81—C86 | 119.4 (3) |
C13—C14—H14 | 119.8 | C82—C81—P4 | 122.1 (3) |
C15—C14—H14 | 119.8 | C86—C81—P4 | 117.9 (3) |
C14—C15—C16 | 120.0 (5) | C83—C82—C81 | 119.6 (3) |
C14—C15—H15 | 120.0 | C83—C82—H82 | 120.2 |
C16—C15—H15 | 120.0 | C81—C82—H82 | 120.2 |
C11—C16—C15 | 120.4 (4) | C84—C83—C82 | 120.0 (4) |
C11—C16—H16 | 119.8 | C84—C83—H83 | 120.0 |
C15—C16—H16 | 119.8 | C82—C83—H83 | 120.0 |
C22—C21—C26 | 119.3 (3) | C83—C84—C85 | 120.7 (3) |
C22—C21—P1 | 124.1 (3) | C83—C84—H84 | 119.6 |
C26—C21—P1 | 116.6 (3) | C85—C84—H84 | 119.6 |
C21—C22—C23 | 120.4 (3) | C86—C85—C84 | 119.6 (4) |
C21—C22—H22 | 119.8 | C86—C85—H85 | 120.2 |
C23—C22—H22 | 119.8 | C84—C85—H85 | 120.2 |
C24—C23—C22 | 120.4 (4) | C85—C86—C81 | 120.6 (3) |
C24—C23—H23 | 119.8 | C85—C86—H86 | 119.7 |
C22—C23—H23 | 119.8 | C81—C86—H86 | 119.7 |
C23—C24—C25 | 119.6 (4) | C92—C91—C96 | 119.9 (3) |
C23—C24—H24 | 120.2 | C92—C91—P4 | 116.9 (3) |
C25—C24—H24 | 120.2 | C96—C91—P4 | 122.9 (3) |
C26—C25—C24 | 120.4 (4) | C93—C92—C91 | 120.5 (4) |
C26—C25—H25 | 119.8 | C93—C92—H92 | 119.7 |
C24—C25—H25 | 119.8 | C91—C92—H92 | 119.7 |
C25—C26—C21 | 120.0 (4) | C92—C93—C94 | 119.7 (4) |
C25—C26—H26 | 120.0 | C92—C93—H93 | 120.2 |
C21—C26—H26 | 120.0 | C94—C93—H93 | 120.2 |
C36—C31—C32 | 120.1 (3) | C95—C94—C93 | 120.6 (4) |
C36—C31—P1 | 122.0 (3) | C95—C94—H94 | 119.7 |
C32—C31—P1 | 117.2 (3) | C93—C94—H94 | 119.7 |
C33—C32—C31 | 119.5 (4) | C94—C95—C96 | 119.9 (4) |
C33—C32—H32 | 120.3 | C94—C95—H95 | 120.0 |
C31—C32—H32 | 120.3 | C96—C95—H95 | 120.0 |
C34—C33—C32 | 120.4 (4) | C95—C96—C91 | 119.4 (3) |
C34—C33—H33 | 119.8 | C95—C96—H96 | 120.3 |
C32—C33—H33 | 119.8 | C91—C96—H96 | 120.3 |
C33—C34—C35 | 121.0 (4) | C102—C101—C106 | 118.8 (3) |
C33—C34—H34 | 119.5 | C102—C101—P6 | 121.4 (3) |
C35—C34—H34 | 119.5 | C106—C101—P6 | 119.9 (3) |
C34—C35—C36 | 119.2 (4) | C101—C102—C103 | 120.0 (4) |
C34—C35—H35 | 120.4 | C101—C102—H102 | 120.0 |
C36—C35—H35 | 120.4 | C103—C102—H102 | 120.0 |
C31—C36—C35 | 119.8 (4) | C104—C103—C102 | 119.9 (4) |
C31—C36—H36 | 120.1 | C104—C103—H103 | 120.1 |
C35—C36—H36 | 120.1 | C102—C103—H103 | 120.1 |
C46—C41—C42 | 119.4 (3) | C103—C104—C105 | 120.1 (4) |
C46—C41—P3 | 118.3 (3) | C103—C104—H104 | 119.9 |
C42—C41—P3 | 122.3 (3) | C105—C104—H104 | 119.9 |
C43—C42—C41 | 119.8 (4) | C106—C105—C104 | 120.3 (4) |
C43—C42—H42 | 120.1 | C106—C105—H105 | 119.8 |
C41—C42—H42 | 120.1 | C104—C105—H105 | 119.8 |
C44—C43—C42 | 120.5 (4) | C105—C106—C101 | 120.9 (4) |
C44—C43—H43 | 119.7 | C105—C106—H106 | 119.6 |
C42—C43—H43 | 119.7 | C101—C106—H106 | 119.6 |
C43—C44—C45 | 120.2 (4) | C116—C111—C112 | 120.0 (3) |
C43—C44—H44 | 119.9 | C116—C111—P6 | 118.2 (3) |
C45—C44—H44 | 119.9 | C112—C111—P6 | 121.6 (3) |
C44—C45—C46 | 119.6 (4) | C113—C112—C111 | 119.6 (4) |
C44—C45—H45 | 120.2 | C113—C112—H112 | 120.2 |
C46—C45—H45 | 120.2 | C111—C112—H112 | 120.2 |
C41—C46—C45 | 120.4 (4) | C114—C113—C112 | 120.3 (4) |
C41—C46—H46 | 119.8 | C114—C113—H113 | 119.8 |
C45—C46—H46 | 119.8 | C112—C113—H113 | 119.8 |
C52—C51—C56 | 119.9 (3) | C113—C114—C115 | 120.7 (4) |
C52—C51—P3 | 121.9 (3) | C113—C114—H114 | 119.7 |
C56—C51—P3 | 117.8 (3) | C115—C114—H114 | 119.7 |
C51—C52—C53 | 119.3 (4) | C114—C115—C116 | 119.9 (4) |
C51—C52—H52 | 120.3 | C114—C115—H115 | 120.1 |
C53—C52—H52 | 120.3 | C116—C115—H115 | 120.1 |
C54—C53—C52 | 120.7 (4) | C111—C116—C115 | 119.5 (3) |
C54—C53—H53 | 119.6 | C111—C116—H116 | 120.3 |
C52—C53—H53 | 119.6 | C115—C116—H116 | 120.3 |
C53—C54—C55 | 120.4 (4) | C126—C121—C122 | 119.8 (4) |
C53—C54—H54 | 119.8 | C126—C121—P6 | 121.2 (3) |
C55—C54—H54 | 119.8 | C122—C121—P6 | 118.4 (3) |
C54—C55—C56 | 120.3 (4) | C123—C122—C121 | 120.1 (4) |
C54—C55—H55 | 119.8 | C123—C122—H122 | 119.9 |
C56—C55—H55 | 119.8 | C121—C122—H122 | 119.9 |
C55—C56—C51 | 119.3 (4) | C124—C123—C122 | 119.9 (5) |
C55—C56—H56 | 120.3 | C124—C123—H123 | 120.0 |
C51—C56—H56 | 120.3 | C122—C123—H123 | 120.0 |
C66—C61—C62 | 119.8 (3) | C123—C124—C125 | 121.3 (4) |
C66—C61—P3 | 122.1 (3) | C123—C124—H124 | 119.3 |
C62—C61—P3 | 117.8 (3) | C125—C124—H124 | 119.3 |
C63—C62—C61 | 119.7 (3) | C126—C125—C124 | 118.8 (5) |
C63—C62—H62 | 120.1 | C126—C125—H125 | 120.6 |
C61—C62—H62 | 120.1 | C124—C125—H125 | 120.6 |
C64—C63—C62 | 120.5 (4) | C121—C126—C125 | 120.1 (4) |
C64—C63—H63 | 119.8 | C121—C126—H126 | 120.0 |
C62—C63—H63 | 119.8 | C125—C126—H126 | 120.0 |
C63—C64—C65 | 120.5 (3) | Cl1—Al1—Cl2 | 110.93 (7) |
C63—C64—H64 | 119.8 | Cl1—Al1—Cl3 | 107.87 (8) |
C65—C64—H64 | 119.8 | Cl2—Al1—Cl3 | 110.70 (7) |
C64—C65—C66 | 120.0 (4) | Cl1—Al1—Cl4 | 109.32 (7) |
C64—C65—H65 | 120.0 | Cl2—Al1—Cl4 | 108.80 (7) |
C66—C65—H65 | 120.0 | Cl3—Al1—Cl4 | 109.19 (7) |
C61—C66—C65 | 119.5 (3) | Cl8—Al2—Cl6 | 110.38 (7) |
C61—C66—H66 | 120.2 | Cl8—Al2—Cl5 | 109.45 (7) |
C65—C66—H66 | 120.2 | Cl6—Al2—Cl5 | 108.51 (7) |
C81—P4—C91 | 109.70 (16) | Cl8—Al2—Cl7 | 109.32 (8) |
C81—P4—C71 | 108.45 (16) | Cl6—Al2—Cl7 | 109.31 (7) |
C91—P4—C71 | 103.55 (15) | Cl5—Al2—Cl7 | 109.86 (7) |
C81—P4—P5 | 113.65 (11) | Cl9—C1—Cl10 | 123.2 (6) |
C91—P4—P5 | 117.50 (12) | Cl9—C1—H1A | 106.5 |
C71—P4—P5 | 102.89 (12) | Cl10—C1—H1A | 106.5 |
P6—P5—P4 | 102.25 (5) | Cl9—C1—H1B | 106.5 |
C121—P6—C101 | 107.01 (17) | Cl10—C1—H1B | 106.5 |
C121—P6—C111 | 109.04 (16) | H1A—C1—H1B | 106.5 |
| | | |
C31—P1—P2—P3 | 67.57 (14) | C81—P4—P5—P6 | 68.14 (14) |
C21—P1—P2—P3 | −62.35 (13) | C91—P4—P5—P6 | −61.86 (13) |
C11—P1—P2—P3 | −176.77 (12) | C71—P4—P5—P6 | −174.82 (11) |
P1—P2—P3—C51 | 61.92 (14) | P4—P5—P6—C121 | 61.15 (14) |
P1—P2—P3—C61 | −68.17 (13) | P4—P5—P6—C101 | 176.46 (12) |
P1—P2—P3—C41 | 177.13 (11) | P4—P5—P6—C111 | −68.54 (13) |
C31—P1—C11—C16 | 113.3 (4) | C81—P4—C71—C72 | −62.6 (3) |
C21—P1—C11—C16 | −129.0 (4) | C91—P4—C71—C72 | 53.9 (3) |
P2—P1—C11—C16 | −6.3 (4) | P5—P4—C71—C72 | 176.7 (3) |
C31—P1—C11—C12 | −69.2 (4) | C81—P4—C71—C76 | 122.1 (3) |
C21—P1—C11—C12 | 48.5 (4) | C91—P4—C71—C76 | −121.4 (3) |
P2—P1—C11—C12 | 171.2 (4) | P5—P4—C71—C76 | 1.4 (3) |
C16—C11—C12—C13 | 0.5 (9) | C76—C71—C72—C73 | 1.5 (6) |
P1—C11—C12—C13 | −177.1 (5) | P4—C71—C72—C73 | −173.9 (3) |
C11—C12—C13—C14 | 0.5 (10) | C71—C72—C73—C74 | 0.6 (6) |
C12—C13—C14—C15 | −2.0 (11) | C72—C73—C74—C75 | −2.2 (7) |
C13—C14—C15—C16 | 2.5 (10) | C73—C74—C75—C76 | 1.7 (7) |
C12—C11—C16—C15 | −0.1 (8) | C74—C75—C76—C71 | 0.4 (7) |
P1—C11—C16—C15 | 177.4 (4) | C72—C71—C76—C75 | −2.0 (6) |
C14—C15—C16—C11 | −1.4 (9) | P4—C71—C76—C75 | 173.2 (3) |
C31—P1—C21—C22 | 17.7 (3) | C91—P4—C81—C82 | 38.9 (3) |
C11—P1—C21—C22 | −98.2 (3) | C71—P4—C81—C82 | 151.3 (3) |
P2—P1—C21—C22 | 149.0 (3) | P5—P4—C81—C82 | −95.0 (3) |
C31—P1—C21—C26 | −166.1 (3) | C91—P4—C81—C86 | −150.4 (3) |
C11—P1—C21—C26 | 78.0 (3) | C71—P4—C81—C86 | −37.9 (3) |
P2—P1—C21—C26 | −34.8 (3) | P5—P4—C81—C86 | 75.8 (3) |
C26—C21—C22—C23 | 0.5 (5) | C86—C81—C82—C83 | 0.5 (5) |
P1—C21—C22—C23 | 176.5 (3) | P4—C81—C82—C83 | 171.1 (3) |
C21—C22—C23—C24 | 0.0 (6) | C81—C82—C83—C84 | −1.2 (6) |
C22—C23—C24—C25 | −1.0 (6) | C82—C83—C84—C85 | 1.5 (6) |
C23—C24—C25—C26 | 1.5 (6) | C83—C84—C85—C86 | −1.1 (6) |
C24—C25—C26—C21 | −0.9 (6) | C84—C85—C86—C81 | 0.3 (6) |
C22—C21—C26—C25 | −0.1 (5) | C82—C81—C86—C85 | 0.0 (5) |
P1—C21—C26—C25 | −176.4 (3) | P4—C81—C86—C85 | −171.1 (3) |
C21—P1—C31—C36 | 38.7 (3) | C81—P4—C91—C92 | −165.1 (3) |
C11—P1—C31—C36 | 153.1 (3) | C71—P4—C91—C92 | 79.3 (3) |
P2—P1—C31—C36 | −94.5 (3) | P5—P4—C91—C92 | −33.3 (3) |
C21—P1—C31—C32 | −150.7 (3) | C81—P4—C91—C96 | 20.7 (3) |
C11—P1—C31—C32 | −36.3 (3) | C71—P4—C91—C96 | −94.9 (3) |
P2—P1—C31—C32 | 76.2 (3) | P5—P4—C91—C96 | 152.5 (3) |
C36—C31—C32—C33 | −0.2 (6) | C96—C91—C92—C93 | −0.1 (5) |
P1—C31—C32—C33 | −171.0 (3) | P4—C91—C92—C93 | −174.5 (3) |
C31—C32—C33—C34 | 0.0 (6) | C91—C92—C93—C94 | −1.3 (6) |
C32—C33—C34—C35 | −0.4 (7) | C92—C93—C94—C95 | 0.7 (6) |
C33—C34—C35—C36 | 0.9 (6) | C93—C94—C95—C96 | 1.3 (6) |
C32—C31—C36—C35 | 0.7 (5) | C94—C95—C96—C91 | −2.6 (6) |
P1—C31—C36—C35 | 171.1 (3) | C92—C91—C96—C95 | 2.1 (5) |
C34—C35—C36—C31 | −1.0 (5) | P4—C91—C96—C95 | 176.1 (3) |
C51—P3—C41—C46 | −49.4 (3) | C121—P6—C101—C102 | 136.9 (3) |
C61—P3—C41—C46 | 67.4 (3) | C111—P6—C101—C102 | −107.1 (3) |
P2—P3—C41—C46 | −169.9 (3) | P5—P6—C101—C102 | 16.5 (3) |
C51—P3—C41—C42 | 131.7 (3) | C121—P6—C101—C106 | −43.1 (4) |
C61—P3—C41—C42 | −111.5 (3) | C111—P6—C101—C106 | 72.9 (4) |
P2—P3—C41—C42 | 11.2 (3) | P5—P6—C101—C106 | −163.5 (3) |
C46—C41—C42—C43 | −0.5 (5) | C106—C101—C102—C103 | −0.8 (7) |
P3—C41—C42—C43 | 178.3 (3) | P6—C101—C102—C103 | 179.2 (4) |
C41—C42—C43—C44 | 1.2 (6) | C101—C102—C103—C104 | 0.6 (8) |
C42—C43—C44—C45 | −1.1 (7) | C102—C103—C104—C105 | −0.2 (9) |
C43—C44—C45—C46 | 0.4 (7) | C103—C104—C105—C106 | 0.0 (9) |
C42—C41—C46—C45 | −0.2 (6) | C104—C105—C106—C101 | −0.2 (9) |
P3—C41—C46—C45 | −179.1 (3) | C102—C101—C106—C105 | 0.6 (7) |
C44—C45—C46—C41 | 0.2 (7) | P6—C101—C106—C105 | −179.4 (4) |
C61—P3—C51—C52 | 35.0 (3) | C121—P6—C111—C116 | −152.4 (3) |
C41—P3—C51—C52 | 148.9 (3) | C101—P6—C111—C116 | 93.1 (3) |
P2—P3—C51—C52 | −98.4 (3) | P5—P6—C111—C116 | −20.3 (3) |
C61—P3—C51—C56 | −152.4 (3) | C121—P6—C111—C112 | 33.3 (3) |
C41—P3—C51—C56 | −38.5 (3) | C101—P6—C111—C112 | −81.3 (3) |
P2—P3—C51—C56 | 74.2 (3) | P5—P6—C111—C112 | 165.3 (3) |
C56—C51—C52—C53 | −0.8 (5) | C116—C111—C112—C113 | −0.5 (6) |
P3—C51—C52—C53 | 171.7 (3) | P6—C111—C112—C113 | 173.7 (3) |
C51—C52—C53—C54 | 1.2 (6) | C111—C112—C113—C114 | 1.6 (6) |
C52—C53—C54—C55 | −0.7 (6) | C112—C113—C114—C115 | −1.8 (7) |
C53—C54—C55—C56 | −0.2 (6) | C113—C114—C115—C116 | 0.9 (6) |
C54—C55—C56—C51 | 0.6 (6) | C112—C111—C116—C115 | −0.4 (5) |
C52—C51—C56—C55 | −0.1 (5) | P6—C111—C116—C115 | −174.9 (3) |
P3—C51—C56—C55 | −172.8 (3) | C114—C115—C116—C111 | 0.3 (5) |
C51—P3—C61—C66 | 27.8 (3) | C101—P6—C121—C126 | 147.8 (3) |
C41—P3—C61—C66 | −87.0 (3) | C111—P6—C121—C126 | 34.3 (3) |
P2—P3—C61—C66 | 160.0 (3) | P5—P6—C121—C126 | −99.6 (3) |
C51—P3—C61—C62 | −158.0 (3) | C101—P6—C121—C122 | −41.0 (3) |
C41—P3—C61—C62 | 87.3 (3) | C111—P6—C121—C122 | −154.5 (3) |
P2—P3—C61—C62 | −25.8 (3) | P5—P6—C121—C122 | 71.6 (3) |
C66—C61—C62—C63 | −0.4 (5) | C126—C121—C122—C123 | −1.4 (6) |
P3—C61—C62—C63 | −174.8 (3) | P6—C121—C122—C123 | −172.7 (3) |
C61—C62—C63—C64 | −0.6 (6) | C121—C122—C123—C124 | 1.9 (6) |
C62—C63—C64—C65 | 0.8 (6) | C122—C123—C124—C125 | −2.0 (7) |
C63—C64—C65—C66 | 0.1 (6) | C123—C124—C125—C126 | 1.4 (7) |
C62—C61—C66—C65 | 1.2 (5) | C122—C121—C126—C125 | 0.9 (6) |
P3—C61—C66—C65 | 175.4 (3) | P6—C121—C126—C125 | 172.0 (3) |
C64—C65—C66—C61 | −1.0 (6) | C124—C125—C126—C121 | −0.9 (6) |
Hydrogen-bond geometry (Å, º) top
D—H···A | D—H | H···A | D···A | D—H···A |
C16—H16···P2 | 0.95 | 2.58 | 3.152 (4) | 119 |
C42—H42···Cl3i | 0.95 | 2.82 | 3.716 (4) | 157 |
C42—H42···P2 | 0.95 | 2.61 | 3.165 (4) | 118 |
C76—H76···P5 | 0.95 | 2.60 | 3.166 (4) | 118 |
C102—H102···P5 | 0.95 | 2.60 | 3.157 (4) | 118 |
C105—H105···Cl9ii | 0.95 | 2.82 | 3.623 (6) | 143 |
C123—H123···Cl4iii | 0.95 | 2.79 | 3.589 (6) | 143 |
Symmetry codes: (i) −x+1/2, y−1/2, z+1/2; (ii) −x+1, −y, z+1/2; (iii) −x+1/2, y−3/2, z+1/2. |