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In the crystal structure of the title compound, C28H44B2N2O2, the square-planar B2N2 ring is slightly puckered. One of the thexyl groups exhibits disorder over two positions. The site occupancies for the disordered thexyl groups refined to 0.611 (4) and 0.389 (4).
Supporting information
CCDC reference: 640513
Key indicators
- Single-crystal X-ray study
- T = 105 K
- R factor = 0.059
- wR factor = 0.155
- Data-to-parameter ratio = 17.4
checkCIF/PLATON results
No syntax errors found
Alert level A
PLAT029_ALERT_3_A _diffrn_measured_fraction_theta_full Low ....... 0.93
| Author Response: Several samples were screened. The selected sample exhibited the
strongest diffraction behavior.
|
PLAT035_ALERT_1_A No _chemical_absolute_configuration info given . ?
PLAT305_ALERT_2_A Isolated Hydrogen Atom (Outside Bond Range ??) <H24D
| Author Response: Due to disorder of one thexyl group
|
PLAT305_ALERT_2_A Isolated Hydrogen Atom (Outside Bond Range ??) <H24E
| Author Response: Due to disorder of one thexyl group
|
PLAT305_ALERT_2_A Isolated Hydrogen Atom (Outside Bond Range ??) <H24F
| Author Response: Due to disorder of one thexyl group
|
PLAT305_ALERT_2_A Isolated Hydrogen Atom (Outside Bond Range ??) <H25D
| Author Response: Due to disorder of one thexyl group
|
PLAT305_ALERT_2_A Isolated Hydrogen Atom (Outside Bond Range ??) <H25E
| Author Response: Due to disorder of one thexyl group
|
PLAT305_ALERT_2_A Isolated Hydrogen Atom (Outside Bond Range ??) <H25F
| Author Response: Due to disorder of one thexyl group
|
PLAT305_ALERT_2_A Isolated Hydrogen Atom (Outside Bond Range ??) <H26B
| Author Response: Due to disorder of one thexyl group
|
PLAT305_ALERT_2_A Isolated Hydrogen Atom (Outside Bond Range ??) <H27D
| Author Response: Due to disorder of one thexyl group
|
PLAT305_ALERT_2_A Isolated Hydrogen Atom (Outside Bond Range ??) <H27E
| Author Response: Due to disorder of one thexyl group
|
PLAT305_ALERT_2_A Isolated Hydrogen Atom (Outside Bond Range ??) <H27F
| Author Response: Due to disorder of one thexyl group
|
PLAT305_ALERT_2_A Isolated Hydrogen Atom (Outside Bond Range ??) <H28D
| Author Response: Due to disorder of one thexyl group
|
PLAT305_ALERT_2_A Isolated Hydrogen Atom (Outside Bond Range ??) <H28E
| Author Response: Due to disorder of one thexyl group
|
PLAT305_ALERT_2_A Isolated Hydrogen Atom (Outside Bond Range ??) <H28F
| Author Response: Due to disorder of one thexyl group
|
Alert level C
DIFMX01_ALERT_2_C The maximum difference density is > 0.1*ZMAX*0.75
_refine_diff_density_max given = 0.658
Test value = 0.600
DIFMX02_ALERT_1_C The maximum difference density is > 0.1*ZMAX*0.75
The relevant atom site should be identified.
REFLT03_ALERT_1_C Reflection count < 95% complete
From the CIF: _diffrn_reflns_theta_max 34.64
From the CIF: _diffrn_reflns_theta_full 0.00
From the CIF: _reflns_number_total 5750
TEST2: Reflns within _diffrn_reflns_theta_max
Count of symmetry unique reflns 6169
Completeness (_total/calc) 93.21%
STRVA01_ALERT_4_C Flack test results are meaningless.
From the CIF: _refine_ls_abs_structure_Flack 0.300
From the CIF: _refine_ls_abs_structure_Flack_su 1.600
PLAT026_ALERT_3_C Ratio Observed / Unique Reflections too Low .... 45 Perc.
PLAT032_ALERT_4_C Std. Uncertainty in Flack Parameter too High ... 1.60
PLAT041_ALERT_1_C Calc. and Rep. SumFormula Strings Differ .... ?
PLAT042_ALERT_1_C Calc. and Rep. MoietyFormula Strings Differ .... ?
PLAT097_ALERT_2_C Maximum (Positive) Residual Density ............ 0.66 e/A 3
PLAT301_ALERT_3_C Main Residue Disorder ......................... 15.00 Perc.
PLAT322_ALERT_2_C Check Hybridisation of B2 in Main Residue . ?
Alert level G
REFLT03_ALERT_4_G Please check that the estimate of the number of Friedel pairs is
correct. If it is not, please give the correct count in the
_publ_section_exptl_refinement section of the submitted CIF.
From the CIF: _diffrn_reflns_theta_max 34.64
From the CIF: _reflns_number_total 5750
Count of symmetry unique reflns 6169
Completeness (_total/calc) 93.21%
TEST3: Check Friedels for noncentro structure
Estimate of Friedel pairs measured 0
Fraction of Friedel pairs measured 0.000
Are heavy atom types Z>Si present no
15 ALERT level A = In general: serious problem
0 ALERT level B = Potentially serious problem
11 ALERT level C = Check and explain
1 ALERT level G = General alerts; check
5 ALERT type 1 CIF construction/syntax error, inconsistent or missing data
16 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
3 ALERT type 4 Improvement, methodology, query or suggestion
0 ALERT type 5 Informative message, check
Data collection: CrysAlis CCD (Oxford Diffraction, 2006); cell refinement: CrysAlis RED (Oxford Diffraction, 2006); data reduction: CrysAlis RED; program(s) used to solve structure: SHELXS97 (Sheldrick, 1997); program(s) used to refine structure: SHELXL97 (Sheldrick, 1997); molecular graphics: ORTEP-3 (Farrugia, 1997) and PLATON (Spek, 2003); software used to prepare material for publication: SHELXTL (Bruker, 1997).
syn-2,4-Bis(4-methoxybenzylidene)-
trans-1,3-dithexyldi-
2,4-azadi-1,3-boracyclobutane
top
Crystal data top
C28H44B2N2O2 | F(000) = 504 |
Mr = 462.27 | Dx = 1.109 Mg m−3 |
Monoclinic, P21 | Melting point: 378 K |
Hall symbol: P 2yb | Mo Kα radiation, λ = 0.71073 Å |
a = 8.801 (5) Å | Cell parameters from 6619 reflections |
b = 11.141 (4) Å | θ = 3.7–34.6° |
c = 14.568 (7) Å | µ = 0.07 mm−1 |
β = 104.25 (5)° | T = 105 K |
V = 1384.3 (11) Å3 | Block, yellow |
Z = 2 | 0.30 × 0.29 × 0.12 mm |
Data collection top
Oxford Diffraction Sapphire CCD area-detector diffractometer | 5750 independent reflections |
Radiation source: fine-focus sealed tube | 2604 reflections with I > 2σ(I) |
Graphite monochromator | Rint = 0.046 |
ω scans | θmax = 34.6°, θmin = 3.7° |
Absorption correction: multi-scan (CrysAlis RED; Oxford Diffraction, 2006) | h = −13→14 |
Tmin = 0.942, Tmax = 1.000 | k = −17→17 |
26112 measured reflections | l = −22→21 |
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)] = 0.059 | H atoms treated by a mixture of independent and constrained refinement |
wR(F2) = 0.155 | w = 1/[σ2(Fo2) + (0.0737P)2P] where P = (Fo2 + 2Fc2)/3 |
S = 0.83 | (Δ/σ)max < 0.001 |
5750 reflections | Δρmax = 0.66 e Å−3 |
331 parameters | Δρmin = −0.39 e Å−3 |
12 restraints | Absolute structure: Flack (1983) |
Primary atom site location: structure-invariant direct methods | Absolute structure parameter: 0.3 (16) |
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 | Occ. (<1) |
N1 | 0.7246 (2) | 0.58089 (19) | 0.31185 (15) | 0.0257 (4) | |
O1 | 0.5710 (2) | 0.68092 (18) | 0.71995 (13) | 0.0396 (5) | |
B1 | 0.7124 (4) | 0.5591 (3) | 0.2023 (2) | 0.0308 (7) | |
C1 | 0.5352 (4) | 0.5973 (3) | 0.7864 (2) | 0.0456 (8) | |
H1A | 0.5192 | 0.6408 | 0.8417 | 0.068* | |
H1B | 0.6223 | 0.5407 | 0.8064 | 0.068* | |
H1C | 0.4395 | 0.5531 | 0.7564 | 0.068* | |
O2 | 1.1012 (2) | 1.19588 (16) | 0.12099 (13) | 0.0335 (4) | |
N2 | 0.8114 (2) | 0.67932 (18) | 0.20450 (15) | 0.0267 (4) | |
C2 | 0.5979 (3) | 0.6359 (3) | 0.63783 (18) | 0.0297 (5) | |
B2 | 0.8430 (3) | 0.6898 (3) | 0.3164 (2) | 0.0263 (6) | |
C3 | 0.5956 (3) | 0.5146 (3) | 0.61506 (19) | 0.0323 (6) | |
H3A | 0.5801 | 0.4555 | 0.6588 | 0.039* | |
C4 | 0.6164 (3) | 0.4818 (2) | 0.52745 (19) | 0.0300 (6) | |
H4A | 0.6117 | 0.3991 | 0.5109 | 0.036* | |
C5 | 0.6442 (3) | 0.5659 (2) | 0.46236 (18) | 0.0268 (5) | |
C6 | 0.6481 (3) | 0.6879 (2) | 0.48783 (19) | 0.0296 (5) | |
H6A | 0.6665 | 0.7473 | 0.4450 | 0.036* | |
C7 | 0.6255 (3) | 0.7220 (2) | 0.57467 (19) | 0.0310 (6) | |
H7A | 0.6289 | 0.8046 | 0.5913 | 0.037* | |
C8 | 0.6579 (3) | 0.5260 (2) | 0.36878 (18) | 0.0279 (5) | |
H8A | 0.6119 | 0.4505 | 0.3478 | 0.033* | |
C9 | 0.8454 (3) | 0.7370 (2) | 0.13665 (18) | 0.0262 (5) | |
H9A | 0.8233 | 0.6972 | 0.0771 | 0.031* | |
C10 | 0.9147 (3) | 0.8573 (2) | 0.13914 (17) | 0.0260 (5) | |
C11 | 0.9014 (3) | 0.9439 (2) | 0.20568 (19) | 0.0334 (6) | |
H11A | 0.8506 | 0.9246 | 0.2542 | 0.040* | |
C12 | 0.9621 (3) | 1.0585 (2) | 0.20147 (18) | 0.0324 (6) | |
H12A | 0.9514 | 1.1175 | 0.2466 | 0.039* | |
C13 | 1.0381 (3) | 1.0867 (2) | 0.13168 (18) | 0.0262 (5) | |
C14 | 1.0531 (3) | 0.9997 (2) | 0.06448 (18) | 0.0304 (6) | |
H14A | 1.1060 | 1.0184 | 0.0168 | 0.037* | |
C15 | 0.9902 (3) | 0.8873 (2) | 0.06860 (18) | 0.0289 (6) | |
H15A | 0.9984 | 0.8289 | 0.0225 | 0.035* | |
C16 | 1.0777 (3) | 1.2903 (2) | 0.1831 (2) | 0.0367 (6) | |
H16A | 1.1288 | 1.3638 | 0.1689 | 0.055* | |
H16B | 1.1231 | 1.2667 | 0.2490 | 0.055* | |
H16C | 0.9651 | 1.3050 | 0.1739 | 0.055* | |
C17 | 1.0244 (3) | 0.6512 (2) | 0.36967 (17) | 0.0272 (5) | |
C18 | 1.0717 (3) | 0.5323 (2) | 0.3296 (2) | 0.0374 (6) | |
H18A | 1.1798 | 0.5120 | 0.3624 | 0.056* | |
H18B | 1.0642 | 0.5416 | 0.2617 | 0.056* | |
H18C | 1.0013 | 0.4680 | 0.3393 | 0.056* | |
C19 | 1.1384 (3) | 0.7473 (3) | 0.3492 (2) | 0.0347 (6) | |
H19A | 1.2463 | 0.7246 | 0.3804 | 0.052* | |
H19B | 1.1141 | 0.8251 | 0.3735 | 0.052* | |
H19C | 1.1271 | 0.7530 | 0.2807 | 0.052* | |
C20 | 1.0413 (3) | 0.6380 (2) | 0.47786 (19) | 0.0326 (6) | |
H20A | 0.9521 | 0.5870 | 0.4861 | 0.039* | |
C21 | 1.0302 (3) | 0.7575 (3) | 0.52779 (19) | 0.0376 (6) | |
H21A | 1.0420 | 0.7432 | 0.5956 | 0.056* | |
H21B | 0.9280 | 0.7945 | 0.5007 | 0.056* | |
H21C | 1.1136 | 0.8114 | 0.5191 | 0.056* | |
C22 | 1.1942 (3) | 0.5755 (3) | 0.5317 (2) | 0.0421 (7) | |
H22A | 1.1961 | 0.5700 | 0.5991 | 0.063* | |
H22B | 1.2847 | 0.6222 | 0.5240 | 0.063* | |
H22C | 1.1989 | 0.4946 | 0.5060 | 0.063* | |
C23 | 0.5388 (3) | 0.5510 (3) | 0.1317 (2) | 0.0423 (8) | 0.611 (4) |
C24 | 0.4875 (6) | 0.4160 (5) | 0.1374 (4) | 0.0471 (12) | 0.611 (4) |
H24A | 0.3826 | 0.4042 | 0.0959 | 0.071* | 0.611 (4) |
H24B | 0.4860 | 0.3966 | 0.2028 | 0.071* | 0.611 (4) |
H24C | 0.5622 | 0.3633 | 0.1170 | 0.071* | 0.611 (4) |
C25 | 0.5323 (7) | 0.5788 (6) | 0.0283 (4) | 0.0523 (13) | 0.611 (4) |
H25A | 0.4239 | 0.5722 | −0.0094 | 0.078* | 0.611 (4) |
H25B | 0.5983 | 0.5216 | 0.0047 | 0.078* | 0.611 (4) |
H25C | 0.5706 | 0.6606 | 0.0232 | 0.078* | 0.611 (4) |
C26 | 0.4142 (6) | 0.6260 (4) | 0.1648 (3) | 0.0434 (10) | 0.611 (4) |
H26A | 0.4074 | 0.5932 | 0.2276 | 0.052* | 0.611 (4) |
C27 | 0.2485 (6) | 0.6195 (5) | 0.0987 (4) | 0.0529 (12) | 0.611 (4) |
H27A | 0.1772 | 0.6702 | 0.1239 | 0.079* | 0.611 (4) |
H27B | 0.2113 | 0.5363 | 0.0945 | 0.079* | 0.611 (4) |
H27C | 0.2514 | 0.6479 | 0.0355 | 0.079* | 0.611 (4) |
C28 | 0.4642 (17) | 0.7592 (11) | 0.1803 (10) | 0.037 (2) | 0.611 (4) |
H28A | 0.3826 | 0.8044 | 0.2007 | 0.056* | 0.611 (4) |
H28B | 0.4786 | 0.7930 | 0.1210 | 0.056* | 0.611 (4) |
H28C | 0.5629 | 0.7646 | 0.2292 | 0.056* | 0.611 (4) |
C23B | 0.5388 (3) | 0.5510 (3) | 0.1317 (2) | 0.0423 (8) | 0.39 |
C24B | 0.4275 (10) | 0.4715 (8) | 0.1635 (6) | 0.0471 (12) | 0.39 |
H24D | 0.4095 | 0.5021 | 0.2230 | 0.071* | 0.389 (4) |
H24E | 0.4713 | 0.3903 | 0.1735 | 0.071* | 0.389 (4) |
H24F | 0.3280 | 0.4694 | 0.1152 | 0.071* | 0.389 (4) |
C25B | 0.5640 (12) | 0.5080 (9) | 0.0332 (6) | 0.0523 (13) | 0.39 |
H25D | 0.4622 | 0.5018 | −0.0128 | 0.078* | 0.389 (4) |
H25E | 0.6154 | 0.4293 | 0.0408 | 0.078* | 0.389 (4) |
H25F | 0.6300 | 0.5661 | 0.0105 | 0.078* | 0.389 (4) |
C26B | 0.4664 (9) | 0.6789 (7) | 0.1040 (5) | 0.0434 (10) | 0.39 |
H26B | 0.5464 | 0.7254 | 0.0805 | 0.052* | 0.389 (4) |
C27B | 0.3109 (8) | 0.6813 (8) | 0.0217 (6) | 0.0529 (12) | 0.39 |
H27D | 0.2750 | 0.7644 | 0.0094 | 0.079* | 0.389 (4) |
H27E | 0.2296 | 0.6341 | 0.0405 | 0.079* | 0.389 (4) |
H27F | 0.3318 | 0.6469 | −0.0359 | 0.079* | 0.389 (4) |
C28B | 0.439 (3) | 0.7487 (19) | 0.1902 (17) | 0.037 (2) | 0.39 |
H28D | 0.3938 | 0.8275 | 0.1695 | 0.056* | 0.389 (4) |
H28E | 0.5387 | 0.7591 | 0.2372 | 0.056* | 0.389 (4) |
H28F | 0.3661 | 0.7036 | 0.2185 | 0.056* | 0.389 (4) |
H2B | 0.784 (3) | 0.483 (3) | 0.189 (2) | 0.038 (8)* | |
H2A | 0.805 (3) | 0.781 (3) | 0.3441 (17) | 0.030 (7)* | |
Atomic displacement parameters (Å2) top | U11 | U22 | U33 | U12 | U13 | U23 |
N1 | 0.0253 (10) | 0.0222 (10) | 0.0296 (12) | −0.0018 (8) | 0.0069 (9) | 0.0041 (8) |
O1 | 0.0507 (11) | 0.0384 (11) | 0.0316 (11) | −0.0032 (10) | 0.0141 (9) | 0.0023 (9) |
B1 | 0.0373 (15) | 0.0273 (15) | 0.0273 (15) | −0.0125 (13) | 0.0070 (13) | 0.0009 (12) |
C1 | 0.0571 (18) | 0.0476 (19) | 0.0356 (18) | −0.0049 (15) | 0.0179 (14) | 0.0086 (14) |
O2 | 0.0436 (10) | 0.0213 (9) | 0.0374 (11) | −0.0074 (8) | 0.0134 (8) | −0.0003 (8) |
N2 | 0.0278 (10) | 0.0211 (10) | 0.0316 (11) | −0.0049 (8) | 0.0080 (8) | −0.0011 (9) |
C2 | 0.0262 (12) | 0.0371 (14) | 0.0259 (13) | −0.0019 (11) | 0.0066 (10) | 0.0028 (12) |
B2 | 0.0283 (13) | 0.0191 (12) | 0.0324 (15) | −0.0058 (11) | 0.0092 (11) | −0.0004 (12) |
C3 | 0.0301 (13) | 0.0327 (14) | 0.0335 (15) | −0.0024 (11) | 0.0064 (11) | 0.0078 (12) |
C4 | 0.0243 (12) | 0.0247 (13) | 0.0392 (15) | −0.0011 (10) | 0.0041 (11) | 0.0051 (11) |
C5 | 0.0221 (11) | 0.0275 (13) | 0.0303 (14) | −0.0008 (10) | 0.0055 (10) | 0.0042 (11) |
C6 | 0.0305 (12) | 0.0242 (12) | 0.0350 (14) | −0.0001 (11) | 0.0100 (11) | 0.0072 (12) |
C7 | 0.0320 (13) | 0.0257 (13) | 0.0364 (15) | −0.0004 (11) | 0.0105 (11) | 0.0022 (11) |
C8 | 0.0299 (12) | 0.0180 (11) | 0.0354 (14) | −0.0013 (9) | 0.0075 (10) | 0.0044 (10) |
C9 | 0.0275 (11) | 0.0226 (12) | 0.0301 (13) | −0.0029 (10) | 0.0099 (10) | −0.0014 (10) |
C10 | 0.0302 (13) | 0.0210 (12) | 0.0269 (13) | −0.0016 (10) | 0.0070 (10) | 0.0014 (10) |
C11 | 0.0480 (16) | 0.0227 (12) | 0.0353 (15) | −0.0017 (11) | 0.0211 (13) | 0.0008 (11) |
C12 | 0.0467 (15) | 0.0220 (12) | 0.0313 (14) | −0.0016 (11) | 0.0150 (12) | −0.0035 (11) |
C13 | 0.0289 (12) | 0.0173 (11) | 0.0304 (14) | −0.0024 (10) | 0.0036 (10) | 0.0035 (10) |
C14 | 0.0380 (14) | 0.0256 (13) | 0.0313 (14) | −0.0037 (11) | 0.0154 (11) | 0.0008 (11) |
C15 | 0.0351 (14) | 0.0242 (13) | 0.0283 (14) | −0.0011 (10) | 0.0094 (11) | −0.0011 (11) |
C16 | 0.0502 (17) | 0.0207 (13) | 0.0396 (16) | −0.0048 (12) | 0.0120 (13) | −0.0027 (11) |
C17 | 0.0287 (12) | 0.0221 (12) | 0.0311 (13) | −0.0016 (10) | 0.0080 (10) | −0.0031 (10) |
C18 | 0.0333 (14) | 0.0303 (15) | 0.0464 (17) | 0.0028 (11) | 0.0058 (12) | −0.0088 (13) |
C19 | 0.0283 (12) | 0.0327 (14) | 0.0410 (16) | −0.0045 (11) | 0.0045 (11) | −0.0053 (12) |
C20 | 0.0252 (12) | 0.0283 (13) | 0.0428 (16) | −0.0007 (11) | 0.0055 (11) | −0.0002 (12) |
C21 | 0.0394 (15) | 0.0422 (16) | 0.0304 (15) | −0.0003 (13) | 0.0073 (12) | −0.0053 (13) |
C22 | 0.0345 (14) | 0.0371 (15) | 0.0487 (19) | 0.0002 (13) | −0.0009 (13) | 0.0071 (14) |
C23 | 0.0397 (16) | 0.0382 (17) | 0.0471 (18) | −0.0039 (13) | 0.0073 (13) | −0.0008 (14) |
C24 | 0.045 (3) | 0.044 (3) | 0.051 (3) | −0.016 (2) | 0.008 (2) | 0.002 (2) |
C25 | 0.073 (3) | 0.048 (3) | 0.034 (2) | −0.013 (3) | 0.011 (2) | 0.016 (3) |
C26 | 0.059 (3) | 0.031 (2) | 0.036 (2) | 0.0007 (19) | 0.0048 (19) | −0.0033 (18) |
C27 | 0.037 (2) | 0.040 (3) | 0.075 (3) | 0.0013 (19) | 0.001 (2) | 0.001 (2) |
C28 | 0.032 (5) | 0.031 (3) | 0.050 (3) | 0.002 (3) | 0.013 (3) | −0.010 (3) |
C23B | 0.0397 (16) | 0.0382 (17) | 0.0471 (18) | −0.0039 (13) | 0.0073 (13) | −0.0008 (14) |
C24B | 0.045 (3) | 0.044 (3) | 0.051 (3) | −0.016 (2) | 0.008 (2) | 0.002 (2) |
C25B | 0.073 (3) | 0.048 (3) | 0.034 (2) | −0.013 (3) | 0.011 (2) | 0.016 (3) |
C26B | 0.059 (3) | 0.031 (2) | 0.036 (2) | 0.0007 (19) | 0.0048 (19) | −0.0033 (18) |
C27B | 0.037 (2) | 0.040 (3) | 0.075 (3) | 0.0013 (19) | 0.001 (2) | 0.001 (2) |
C28B | 0.032 (5) | 0.031 (3) | 0.050 (3) | 0.002 (3) | 0.013 (3) | −0.010 (3) |
Geometric parameters (Å, º) top
N1—C8 | 1.283 (3) | C18—H18B | 0.9800 |
N1—B2 | 1.590 (3) | C18—H18C | 0.9800 |
N1—B1 | 1.591 (4) | C19—H19A | 0.9800 |
O1—C2 | 1.371 (3) | C19—H19B | 0.9800 |
O1—C1 | 1.433 (3) | C19—H19C | 0.9800 |
B1—N2 | 1.594 (3) | C20—C21 | 1.532 (4) |
B1—C23 | 1.621 (4) | C20—C22 | 1.547 (4) |
B1—H2B | 1.10 (3) | C20—H20A | 1.0000 |
C1—H1A | 0.9800 | C21—H21A | 0.9800 |
C1—H1B | 0.9800 | C21—H21B | 0.9800 |
C1—H1C | 0.9800 | C21—H21C | 0.9800 |
O2—C13 | 1.362 (3) | C22—H22A | 0.9800 |
O2—C16 | 1.436 (3) | C22—H22B | 0.9800 |
N2—C9 | 1.275 (3) | C22—H22C | 0.9800 |
N2—B2 | 1.589 (4) | C23—C25 | 1.525 (6) |
C2—C3 | 1.390 (4) | C23—C26 | 1.547 (6) |
C2—C7 | 1.392 (4) | C23—C24 | 1.579 (6) |
B2—C17 | 1.651 (4) | C24—H24A | 0.9800 |
B2—H2A | 1.17 (3) | C24—H24B | 0.9800 |
C3—C4 | 1.382 (4) | C24—H24C | 0.9800 |
C3—H3A | 0.9500 | C25—H25A | 0.9800 |
C4—C5 | 1.397 (3) | C25—H25B | 0.9800 |
C4—H4A | 0.9500 | C25—H25C | 0.9800 |
C5—C6 | 1.407 (4) | C26—C27 | 1.539 (7) |
C5—C8 | 1.467 (4) | C26—C28 | 1.549 (12) |
C6—C7 | 1.381 (4) | C26—H26A | 1.0000 |
C6—H6A | 0.9500 | C27—H27A | 0.9800 |
C7—H7A | 0.9500 | C27—H27B | 0.9800 |
C8—H8A | 0.9500 | C27—H27C | 0.9800 |
C9—C10 | 1.469 (3) | C28—H28A | 0.9800 |
C9—H9A | 0.9500 | C28—H28B | 0.9800 |
C10—C11 | 1.393 (4) | C28—H28C | 0.9800 |
C10—C15 | 1.395 (4) | C24B—H24D | 0.9800 |
C11—C12 | 1.391 (4) | C24B—H24E | 0.9800 |
C11—H11A | 0.9500 | C24B—H24F | 0.9800 |
C12—C13 | 1.383 (3) | C25B—H25D | 0.9800 |
C12—H12A | 0.9500 | C25B—H25E | 0.9800 |
C13—C14 | 1.406 (3) | C25B—H25F | 0.9800 |
C14—C15 | 1.377 (3) | C26B—C28B | 1.545 (15) |
C14—H14A | 0.9500 | C26B—C27B | 1.582 (10) |
C15—H15A | 0.9500 | C26B—H26B | 1.0000 |
C16—H16A | 0.9800 | C27B—H27D | 0.9800 |
C16—H16B | 0.9800 | C27B—H27E | 0.9800 |
C16—H16C | 0.9800 | C27B—H27F | 0.9800 |
C17—C19 | 1.545 (3) | C28B—H28D | 0.9800 |
C17—C18 | 1.546 (3) | C28B—H28E | 0.9800 |
C17—C20 | 1.553 (4) | C28B—H28F | 0.9800 |
C18—H18A | 0.9800 | | |
| | | |
C8—N1—B2 | 137.4 (2) | H18A—C18—H18C | 109.5 |
C8—N1—B1 | 130.3 (2) | H18B—C18—H18C | 109.5 |
B2—N1—B1 | 92.28 (18) | C17—C19—H19A | 109.5 |
C2—O1—C1 | 117.7 (2) | C17—C19—H19B | 109.5 |
N1—B1—N2 | 87.15 (18) | H19A—C19—H19B | 109.5 |
N1—B1—C23 | 117.7 (2) | C17—C19—H19C | 109.5 |
N2—B1—C23 | 119.0 (2) | H19A—C19—H19C | 109.5 |
N1—B1—H2B | 113.2 (15) | H19B—C19—H19C | 109.5 |
N2—B1—H2B | 108.4 (14) | C21—C20—C22 | 107.5 (2) |
C23—B1—H2B | 109.6 (15) | C21—C20—C17 | 113.5 (2) |
O1—C1—H1A | 109.5 | C22—C20—C17 | 114.3 (2) |
O1—C1—H1B | 109.5 | C21—C20—H20A | 107.1 |
H1A—C1—H1B | 109.5 | C22—C20—H20A | 107.1 |
O1—C1—H1C | 109.5 | C17—C20—H20A | 107.1 |
H1A—C1—H1C | 109.5 | C20—C21—H21A | 109.5 |
H1B—C1—H1C | 109.5 | C20—C21—H21B | 109.5 |
C13—O2—C16 | 117.13 (18) | H21A—C21—H21B | 109.5 |
C9—N2—B2 | 138.0 (2) | C20—C21—H21C | 109.5 |
C9—N2—B1 | 129.8 (2) | H21A—C21—H21C | 109.5 |
B2—N2—B1 | 92.22 (18) | H21B—C21—H21C | 109.5 |
O1—C2—C3 | 124.7 (2) | C20—C22—H22A | 109.5 |
O1—C2—C7 | 114.9 (3) | C20—C22—H22B | 109.5 |
C3—C2—C7 | 120.5 (2) | H22A—C22—H22B | 109.5 |
N2—B2—N1 | 87.37 (18) | C20—C22—H22C | 109.5 |
N2—B2—C17 | 111.61 (19) | H22A—C22—H22C | 109.5 |
N1—B2—C17 | 111.6 (2) | H22B—C22—H22C | 109.5 |
N2—B2—H2A | 115.2 (12) | C25—C23—C26 | 110.0 (4) |
N1—B2—H2A | 115.7 (12) | C25—C23—C24 | 107.7 (4) |
C17—B2—H2A | 112.9 (13) | C26—C23—C24 | 105.3 (3) |
C4—C3—C2 | 118.7 (2) | C25—C23—B1 | 114.6 (3) |
C4—C3—H3A | 120.6 | C26—C23—B1 | 113.7 (3) |
C2—C3—H3A | 120.6 | C24—C23—B1 | 104.9 (3) |
C3—C4—C5 | 122.3 (3) | C23—C24—H24A | 109.5 |
C3—C4—H4A | 118.9 | C23—C24—H24B | 109.5 |
C5—C4—H4A | 118.9 | H24A—C24—H24B | 109.5 |
C4—C5—C6 | 117.8 (2) | C23—C24—H24C | 109.5 |
C4—C5—C8 | 119.7 (2) | H24A—C24—H24C | 109.5 |
C6—C5—C8 | 122.4 (2) | H24B—C24—H24C | 109.5 |
C7—C6—C5 | 120.5 (2) | C23—C25—H25A | 109.5 |
C7—C6—H6A | 119.8 | C23—C25—H25B | 109.5 |
C5—C6—H6A | 119.8 | H25A—C25—H25B | 109.5 |
C6—C7—C2 | 120.2 (2) | C23—C25—H25C | 109.5 |
C6—C7—H7A | 119.9 | H25A—C25—H25C | 109.5 |
C2—C7—H7A | 119.9 | H25B—C25—H25C | 109.5 |
N1—C8—C5 | 127.7 (2) | C27—C26—C23 | 114.5 (4) |
N1—C8—H8A | 116.1 | C27—C26—C28 | 109.1 (7) |
C5—C8—H8A | 116.1 | C23—C26—C28 | 111.4 (6) |
N2—C9—C10 | 128.0 (2) | C27—C26—H26A | 107.2 |
N2—C9—H9A | 116.0 | C23—C26—H26A | 107.2 |
C10—C9—H9A | 116.0 | C28—C26—H26A | 107.2 |
C11—C10—C15 | 118.9 (2) | C26—C27—H27A | 109.5 |
C11—C10—C9 | 123.0 (2) | C26—C27—H27B | 109.5 |
C15—C10—C9 | 118.1 (2) | H27A—C27—H27B | 109.5 |
C12—C11—C10 | 120.4 (2) | C26—C27—H27C | 109.5 |
C12—C11—H11A | 119.8 | H27A—C27—H27C | 109.5 |
C10—C11—H11A | 119.8 | H27B—C27—H27C | 109.5 |
C13—C12—C11 | 120.1 (2) | C26—C28—H28A | 109.5 |
C13—C12—H12A | 120.0 | C26—C28—H28B | 109.5 |
C11—C12—H12A | 120.0 | H28A—C28—H28B | 109.5 |
O2—C13—C12 | 124.9 (2) | C26—C28—H28C | 109.5 |
O2—C13—C14 | 115.1 (2) | H28A—C28—H28C | 109.5 |
C12—C13—C14 | 120.0 (2) | H28B—C28—H28C | 109.5 |
C15—C14—C13 | 119.3 (2) | H24D—C24B—H24E | 109.5 |
C15—C14—H14A | 120.4 | H24D—C24B—H24F | 109.5 |
C13—C14—H14A | 120.4 | H24E—C24B—H24F | 109.5 |
C14—C15—C10 | 121.3 (2) | H25D—C25B—H25E | 109.5 |
C14—C15—H15A | 119.4 | H25D—C25B—H25F | 109.5 |
C10—C15—H15A | 119.4 | H25E—C25B—H25F | 109.5 |
O2—C16—H16A | 109.5 | C28B—C26B—C27B | 109.1 (11) |
O2—C16—H16B | 109.5 | C28B—C26B—H26B | 106.4 |
H16A—C16—H16B | 109.5 | C27B—C26B—H26B | 106.4 |
O2—C16—H16C | 109.5 | C26B—C27B—H27D | 109.5 |
H16A—C16—H16C | 109.5 | C26B—C27B—H27E | 109.5 |
H16B—C16—H16C | 109.5 | H27D—C27B—H27E | 109.5 |
C19—C17—C18 | 105.79 (19) | C26B—C27B—H27F | 109.5 |
C19—C17—C20 | 110.9 (2) | H27D—C27B—H27F | 109.5 |
C18—C17—C20 | 109.6 (2) | H27E—C27B—H27F | 109.5 |
C19—C17—B2 | 109.1 (2) | C26B—C28B—H28D | 109.5 |
C18—C17—B2 | 111.4 (2) | C26B—C28B—H28E | 109.5 |
C20—C17—B2 | 110.00 (19) | H28D—C28B—H28E | 109.5 |
C17—C18—H18A | 109.5 | C26B—C28B—H28F | 109.5 |
C17—C18—H18B | 109.5 | H28D—C28B—H28F | 109.5 |
H18A—C18—H18B | 109.5 | H28E—C28B—H28F | 109.5 |
C17—C18—H18C | 109.5 | | |
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