Supporting information
Crystallographic Information File (CIF) https://doi.org/10.1107/S1600536801000708/ob6020sup1.cif | |
Structure factor file (CIF format) https://doi.org/10.1107/S1600536801000708/ob6020Isup2.hkl |
CCDC reference: 159738
Key indicators
- Single-crystal X-ray study
- T = 298 K
- Mean (C-C) = 0.007 Å
- Disorder in main residue
- R factor = 0.055
- wR factor = 0.154
- Data-to-parameter ratio = 11.8
checkCIF results
No syntax errors found ADDSYM reports no extra symmetry
Alert Level C:
RINTA_01 Alert C The value of Rint is greater than 0.10 Rint given 0.118 PLAT_301 Alert C Main residue disorder ........................ 8.00 Perc.
0 Alert Level A = Potentially serious problem
0 Alert Level B = Potential problem
2 Alert Level C = Please check
The title compound, (I), was prepared by Spa Contract Synthesis. Crystals of (I) were grown from a methanol solution.
X-ray intensity data were measured with the maximum possible exposure time per frame (120 s) without overloading the detector due to background scatter. In addition, due to the very small size of the crystal, the rotating anode generator was operated at full power and equipped with a capillary lined collimator in order to increase incident X-ray intensity at the crystal position. However, even with this configuration the number of observed data was low and the resultant data(observed)/parameter ratio is 4.75. The large Rint value (> 0.10) may be due to a slight misalignment of the crystal in the X-ray beam. There is a positional disorder of the ethyl C atoms. A split-site model was applicable and it was assumed that there are two possible sets of positions C39A/C40A and C39B/C40B with 50% probability each. The geometry of O38—C39A—C40A and O38—C39B—C40B was restrained to be similar by the SAME instruction, and the displacement parameters of C39 and C40 (both A and B) were restrained to be nearly isotropic by the ISOR instraction of SHELXL97 (Sheldrick, 1997). All H atoms were included in the refinement at calculated positions as riding models with C—H set to 0.93 (Ar—H), 0.96 (CH3), 0.97 Å (CH2) and 0.98 Å (CH).
Data collection: DENZO (Otwinowski & Minor, 1997) and COLLECT (Hooft, 1998); cell refinement: DENZO and COLLECT; data reduction: DENZO and COLLECT; program(s) used to solve structure: SHELXS97 (Sheldrick, 1997); program(s) used to refine structure: SHELXL97 (Sheldrick, 1997); software used to prepare material for publication: SHELXL97.
Fig. 1. The molecular configuration and atom numbering scheme for (I), showing 50% probability ellipsoids. There is positional disorder of the ethyl group, C39 and C40. |
C18H18ClNO4 | F(000) = 728 |
Mr = 347.78 | Dx = 1.389 Mg m−3 |
Monoclinic, P21/c | Mo Kα radiation, λ = 0.71073 Å |
a = 12.780 (3) Å | Cell parameters from 1591 reflections |
b = 16.931 (3) Å | θ = 1.0–27.5° |
c = 7.8532 (16) Å | µ = 0.25 mm−1 |
β = 101.85 (3)° | T = 298 K |
V = 1663.1 (6) Å3 | Needle, orange |
Z = 4 | 0.45 × 0.02 × 0.01 mm |
Enraf Nonius KappaCCD area-detector diffractometer | 2802 independent reflections |
Radiation source: Enraf Nonius FR591 rotating anode | 1040 reflections with I > 2σ(I) |
Graphite monochromator | Rint = 0.118 |
Detector resolution: 9.091 pixels mm-1 | θmax = 25.0°, θmin = 2.0° |
ϕ and ω scans | h = −14→15 |
Absorption correction: multi-scan (SORTAV; Blessing, 1995) | k = −20→19 |
Tmin = 0.895, Tmax = 0.998 | l = −9→9 |
9954 measured reflections |
Refinement on F2 | Secondary atom site location: difference Fourier map |
Least-squares matrix: full | Hydrogen site location: inferred from neighbouring sites |
R[F2 > 2σ(F2)] = 0.055 | H-atom parameters constrained |
wR(F2) = 0.154 | w = 1/[σ2(Fo2) + (0.0586P)2] where P = (Fo2 + 2Fc2)/3 |
S = 0.92 | (Δ/σ)max < 0.001 |
2802 reflections | Δρmax = 0.19 e Å−3 |
238 parameters | Δρmin = −0.22 e Å−3 |
27 restraints | Extinction correction: SHELXL97, Fc*=kFc[1+0.001xFc2λ3/sin(2θ)]-1/4 |
Primary atom site location: structure-invariant direct methods | Extinction coefficient: 0.0073 (15) |
C18H18ClNO4 | V = 1663.1 (6) Å3 |
Mr = 347.78 | Z = 4 |
Monoclinic, P21/c | Mo Kα radiation |
a = 12.780 (3) Å | µ = 0.25 mm−1 |
b = 16.931 (3) Å | T = 298 K |
c = 7.8532 (16) Å | 0.45 × 0.02 × 0.01 mm |
β = 101.85 (3)° |
Enraf Nonius KappaCCD area-detector diffractometer | 2802 independent reflections |
Absorption correction: multi-scan (SORTAV; Blessing, 1995) | 1040 reflections with I > 2σ(I) |
Tmin = 0.895, Tmax = 0.998 | Rint = 0.118 |
9954 measured reflections |
R[F2 > 2σ(F2)] = 0.055 | 27 restraints |
wR(F2) = 0.154 | H-atom parameters constrained |
S = 0.92 | Δρmax = 0.19 e Å−3 |
2802 reflections | Δρmin = −0.22 e Å−3 |
238 parameters |
Experimental. PLEASE NOTE cell_measurement_ fields are not relevant to area detector data, the entire data set is used to refine the cell, which is indexed from all observed reflections in a 10 degree phi range. |
x | y | z | Uiso*/Ueq | Occ. (<1) | |
C1 | 0.8680 (3) | 0.0461 (3) | 0.2380 (6) | 0.0584 (13) | |
O1 | 0.8973 (2) | 0.0793 (2) | 0.1157 (4) | 0.0865 (11) | |
C2 | 0.8018 (3) | 0.0873 (3) | 0.3404 (6) | 0.0537 (12) | |
Cl2 | 0.77616 (10) | 0.18514 (8) | 0.27846 (17) | 0.0864 (5) | |
C3 | 0.7683 (3) | 0.0558 (3) | 0.4778 (6) | 0.0533 (12) | |
C4 | 0.8034 (3) | −0.0272 (3) | 0.5313 (6) | 0.0565 (12) | |
O4 | 0.7686 (3) | −0.0615 (2) | 0.6433 (4) | 0.0873 (11) | |
C5 | 0.9145 (3) | −0.1432 (3) | 0.4887 (6) | 0.0690 (14) | |
H5 | 0.8970 | −0.1658 | 0.5872 | 0.083* | |
C6 | 0.9781 (3) | −0.1847 (3) | 0.3958 (7) | 0.0746 (15) | |
H6 | 1.0022 | −0.2353 | 0.4299 | 0.089* | |
C7 | 1.0047 (4) | −0.1496 (4) | 0.2524 (7) | 0.0795 (16) | |
H7 | 1.0476 | −0.1768 | 0.1898 | 0.095* | |
C8 | 0.9694 (3) | −0.0755 (3) | 0.2000 (6) | 0.0683 (14) | |
H8 | 0.9883 | −0.0527 | 0.1028 | 0.082* | |
C9 | 0.9047 (3) | −0.0341 (3) | 0.2935 (6) | 0.0522 (12) | |
C10 | 0.8766 (3) | −0.0682 (3) | 0.4364 (6) | 0.0514 (12) | |
N31 | 0.6976 (3) | 0.0888 (2) | 0.5680 (5) | 0.0612 (10) | |
C32 | 0.7219 (3) | 0.0921 (3) | 0.7569 (6) | 0.0666 (13) | |
H321 | 0.7486 | 0.1443 | 0.7942 | 0.080* | |
H322 | 0.7776 | 0.0541 | 0.8015 | 0.080* | |
C33 | 0.6247 (3) | 0.0745 (3) | 0.8309 (6) | 0.0715 (15) | |
H331 | 0.6426 | 0.0801 | 0.9564 | 0.086* | |
H332 | 0.6025 | 0.0203 | 0.8042 | 0.086* | |
C34 | 0.5335 (3) | 0.1298 (3) | 0.7565 (6) | 0.0620 (13) | |
H341 | 0.5556 | 0.1840 | 0.7895 | 0.074* | |
C35 | 0.5119 (3) | 0.1232 (3) | 0.5603 (6) | 0.0748 (15) | |
H351 | 0.4557 | 0.1600 | 0.5108 | 0.090* | |
H352 | 0.4865 | 0.0703 | 0.5267 | 0.090* | |
C36 | 0.6100 (3) | 0.1402 (3) | 0.4858 (6) | 0.0744 (14) | |
H361 | 0.5939 | 0.1311 | 0.3612 | 0.089* | |
H362 | 0.6308 | 0.1950 | 0.5062 | 0.089* | |
C37 | 0.4365 (4) | 0.1107 (4) | 0.8269 (7) | 0.0769 (16) | |
O37 | 0.3804 (3) | 0.0549 (3) | 0.7853 (5) | 0.1216 (16) | |
O38 | 0.4212 (3) | 0.1606 (2) | 0.9450 (6) | 0.1123 (14) | |
C39A | 0.3515 (8) | 0.1423 (7) | 1.0760 (16) | 0.087 (4) | 0.50 |
H39A | 0.3222 | 0.0893 | 1.0613 | 0.104* | 0.50 |
H39B | 0.3900 | 0.1493 | 1.1950 | 0.104* | 0.50 |
C40A | 0.2664 (8) | 0.2043 (8) | 1.0238 (17) | 0.097 (4) | 0.50 |
H40A | 0.2962 | 0.2556 | 1.0556 | 0.145* | 0.50 |
H40B | 0.2086 | 0.1946 | 1.0822 | 0.145* | 0.50 |
H40C | 0.2401 | 0.2023 | 0.9002 | 0.145* | 0.50 |
C39B | 0.3094 (8) | 0.1473 (7) | 0.9773 (15) | 0.072 (3) | 0.50 |
H39C | 0.2553 | 0.1562 | 0.8729 | 0.086* | 0.50 |
H39D | 0.3014 | 0.0944 | 1.0205 | 0.086* | 0.50 |
C40B | 0.3047 (9) | 0.2091 (7) | 1.1144 (14) | 0.076 (4) | 0.50 |
H40D | 0.3655 | 0.2034 | 1.2083 | 0.114* | 0.50 |
H40E | 0.2403 | 0.2023 | 1.1578 | 0.114* | 0.50 |
H40F | 0.3052 | 0.2607 | 1.0642 | 0.114* | 0.50 |
U11 | U22 | U33 | U12 | U13 | U23 | |
C1 | 0.061 (3) | 0.070 (4) | 0.047 (3) | −0.002 (3) | 0.016 (2) | 0.000 (3) |
O1 | 0.097 (2) | 0.099 (3) | 0.072 (2) | 0.010 (2) | 0.0381 (19) | 0.021 (2) |
C2 | 0.065 (3) | 0.044 (3) | 0.052 (3) | −0.005 (2) | 0.012 (2) | 0.002 (2) |
Cl2 | 0.1009 (9) | 0.0642 (10) | 0.0989 (11) | 0.0039 (8) | 0.0319 (7) | 0.0184 (9) |
C3 | 0.055 (3) | 0.056 (3) | 0.049 (3) | −0.003 (2) | 0.010 (2) | −0.004 (3) |
C4 | 0.059 (3) | 0.055 (4) | 0.058 (3) | −0.005 (2) | 0.019 (2) | 0.002 (3) |
O4 | 0.110 (2) | 0.074 (3) | 0.095 (3) | 0.0127 (19) | 0.060 (2) | 0.023 (2) |
C5 | 0.066 (3) | 0.069 (4) | 0.073 (4) | −0.004 (3) | 0.017 (3) | −0.004 (3) |
C6 | 0.067 (3) | 0.058 (4) | 0.097 (4) | 0.013 (3) | 0.012 (3) | 0.005 (4) |
C7 | 0.068 (3) | 0.088 (5) | 0.085 (4) | −0.001 (3) | 0.022 (3) | −0.015 (4) |
C8 | 0.058 (3) | 0.085 (5) | 0.065 (4) | −0.006 (3) | 0.018 (2) | −0.003 (3) |
C9 | 0.051 (2) | 0.055 (4) | 0.053 (3) | 0.002 (2) | 0.015 (2) | −0.003 (3) |
C10 | 0.046 (2) | 0.050 (3) | 0.059 (3) | 0.000 (2) | 0.011 (2) | −0.002 (3) |
N31 | 0.065 (2) | 0.073 (3) | 0.048 (3) | 0.017 (2) | 0.0171 (19) | −0.001 (2) |
C32 | 0.068 (3) | 0.076 (4) | 0.059 (4) | 0.004 (3) | 0.019 (2) | −0.006 (3) |
C33 | 0.064 (3) | 0.093 (4) | 0.060 (3) | 0.000 (3) | 0.019 (2) | −0.009 (3) |
C34 | 0.062 (3) | 0.055 (3) | 0.075 (4) | −0.004 (2) | 0.028 (2) | −0.008 (3) |
C35 | 0.063 (3) | 0.084 (4) | 0.079 (4) | 0.013 (3) | 0.018 (3) | −0.001 (3) |
C36 | 0.081 (3) | 0.076 (4) | 0.068 (3) | 0.024 (3) | 0.020 (3) | 0.008 (3) |
C37 | 0.068 (3) | 0.076 (5) | 0.090 (4) | −0.003 (3) | 0.027 (3) | −0.009 (4) |
O37 | 0.107 (3) | 0.133 (4) | 0.136 (4) | −0.056 (3) | 0.053 (2) | −0.044 (3) |
O38 | 0.113 (3) | 0.095 (3) | 0.157 (4) | −0.018 (2) | 0.093 (3) | −0.034 (3) |
C39A | 0.084 (5) | 0.093 (6) | 0.086 (6) | 0.004 (4) | 0.023 (4) | 0.007 (4) |
C40A | 0.091 (6) | 0.097 (6) | 0.102 (6) | 0.002 (4) | 0.020 (4) | −0.002 (5) |
C39B | 0.069 (5) | 0.077 (5) | 0.075 (5) | −0.006 (4) | 0.025 (4) | −0.004 (4) |
C40B | 0.077 (5) | 0.083 (5) | 0.075 (5) | 0.008 (4) | 0.031 (4) | 0.001 (4) |
C1—O1 | 1.235 (5) | C33—H332 | 0.97 |
C1—C2 | 1.459 (6) | C34—C37 | 1.493 (6) |
C1—C9 | 1.471 (6) | C34—C35 | 1.513 (5) |
C2—C3 | 1.350 (5) | C34—H341 | 0.98 |
C2—Cl2 | 1.739 (4) | C35—C36 | 1.517 (5) |
C3—N31 | 1.376 (5) | C35—H351 | 0.97 |
C3—C4 | 1.509 (6) | C35—H352 | 0.97 |
C4—O4 | 1.212 (5) | C36—H361 | 0.97 |
C4—C10 | 1.483 (5) | C36—H362 | 0.97 |
C5—C6 | 1.389 (6) | C37—O37 | 1.190 (6) |
C5—C10 | 1.391 (6) | C37—O38 | 1.299 (6) |
C5—H5 | 0.93 | O38—C39A | 1.525 (9) |
C6—C7 | 1.377 (6) | O38—C39B | 1.518 (9) |
C6—H6 | 0.93 | C39A—C40A | 1.506 (11) |
C7—C8 | 1.367 (6) | C39A—H39A | 0.97 |
C7—H7 | 0.93 | C39A—H39B | 0.97 |
C8—C9 | 1.402 (6) | C40A—H40A | 0.96 |
C8—H8 | 0.93 | C40A—H40B | 0.96 |
C9—C10 | 1.374 (5) | C40A—H40C | 0.96 |
N31—C32 | 1.453 (5) | C39B—C40B | 1.512 (11) |
N31—C36 | 1.458 (5) | C39B—H39C | 0.97 |
C32—C33 | 1.505 (5) | C39B—H39D | 0.97 |
C32—H321 | 0.97 | C40B—H40D | 0.96 |
C32—H322 | 0.97 | C40B—H40E | 0.96 |
C33—C34 | 1.515 (5) | C40B—H40F | 0.96 |
C33—H331 | 0.97 | ||
O1—C1—C2 | 120.8 (5) | C34—C33—H332 | 109.4 |
O1—C1—C9 | 121.4 (4) | H331—C33—H332 | 108.0 |
C2—C1—C9 | 117.6 (4) | C37—C34—C35 | 111.6 (4) |
C3—C2—C1 | 124.5 (4) | C37—C34—C33 | 110.8 (4) |
C3—C2—Cl2 | 121.8 (4) | C35—C34—C33 | 108.2 (4) |
C1—C2—Cl2 | 113.5 (3) | C37—C34—H341 | 108.7 |
C2—C3—N31 | 126.9 (4) | C35—C34—H341 | 108.7 |
C2—C3—C4 | 117.7 (4) | C33—C34—H341 | 108.7 |
N31—C3—C4 | 115.1 (4) | C34—C35—C36 | 112.7 (4) |
O4—C4—C10 | 120.3 (4) | C34—C35—H351 | 109.1 |
O4—C4—C3 | 121.0 (4) | C36—C35—H351 | 109.1 |
C10—C4—C3 | 118.6 (4) | C34—C35—H352 | 109.1 |
C6—C5—C10 | 120.8 (5) | C36—C35—H352 | 109.1 |
C6—C5—H5 | 119.6 | H351—C35—H352 | 107.8 |
C10—C5—H5 | 119.6 | N31—C36—C35 | 109.7 (4) |
C7—C6—C5 | 118.7 (5) | N31—C36—H361 | 109.7 |
C7—C6—H6 | 120.6 | C35—C36—H361 | 109.7 |
C5—C6—H6 | 120.6 | N31—C36—H362 | 109.7 |
C8—C7—C6 | 121.4 (5) | C35—C36—H362 | 109.7 |
C8—C7—H7 | 119.3 | H361—C36—H362 | 108.2 |
C6—C7—H7 | 119.3 | O37—C37—O38 | 122.8 (5) |
C7—C8—C9 | 119.7 (5) | O37—C37—C34 | 124.7 (5) |
C7—C8—H8 | 120.2 | O38—C37—C34 | 112.5 (5) |
C9—C8—H8 | 120.2 | C37—O38—C39A | 122.9 (6) |
C10—C9—C8 | 119.9 (4) | C40A—C39A—O38 | 99.4 (8) |
C10—C9—C1 | 120.6 (4) | O38—C39A—H39A | 111.9 |
C8—C9—C1 | 119.5 (5) | O38—C39A—H39B | 111.9 |
C9—C10—C5 | 119.5 (4) | C40A—C39A—H39A | 111.9 |
C9—C10—C4 | 120.8 (4) | C40A—C39A—H39B | 111.9 |
C5—C10—C4 | 119.7 (4) | H39A—C39A—H39B | 109.6 |
C3—N31—C32 | 121.0 (3) | C40B—C39B—O38 | 101.1 (8) |
C3—N31—C36 | 122.6 (4) | O38—C39B—H39C | 111.5 |
C32—N31—C36 | 114.4 (3) | O38—C39B—H39D | 111.5 |
N31—C32—C33 | 111.5 (3) | C40B—C39B—H39C | 111.5 |
N31—C32—H321 | 109.3 | C40B—C39B—H39D | 111.5 |
C33—C32—H321 | 109.3 | H39C—C39B—H39D | 109.4 |
N31—C32—H322 | 109.3 | C39B—C40B—H40D | 109.5 |
C33—C32—H322 | 109.3 | C39B—C40B—H40E | 109.5 |
H321—C32—H322 | 108.0 | H40D—C40B—H40E | 109.5 |
C32—C33—C34 | 111.0 (4) | C39B—C40B—H40F | 109.5 |
C32—C33—H331 | 109.4 | H40D—C40B—H40F | 109.5 |
C34—C33—H331 | 109.4 | H40E—C40B—H40F | 109.5 |
C32—C33—H332 | 109.4 | ||
O1—C1—C2—C3 | −178.6 (4) | C6—C5—C10—C4 | 176.2 (4) |
C9—C1—C2—C3 | −2.8 (6) | O4—C4—C10—C9 | 170.8 (4) |
O1—C1—C2—Cl2 | −2.8 (5) | C3—C4—C10—C9 | −5.5 (6) |
C9—C1—C2—Cl2 | 173.0 (3) | O4—C4—C10—C5 | −6.9 (6) |
C1—C2—C3—N31 | −173.2 (4) | C3—C4—C10—C5 | 176.8 (4) |
Cl2—C2—C3—N31 | 11.4 (6) | C2—C3—N31—C32 | −131.7 (5) |
C1—C2—C3—C4 | 1.1 (6) | C4—C3—N31—C32 | 53.9 (5) |
Cl2—C2—C3—C4 | −174.3 (3) | C2—C3—N31—C36 | 31.7 (6) |
C2—C3—C4—O4 | −173.3 (4) | C4—C3—N31—C36 | −142.7 (4) |
N31—C3—C4—O4 | 1.6 (6) | C3—N31—C32—C33 | −139.9 (4) |
C2—C3—C4—C10 | 2.9 (6) | C36—N31—C32—C33 | 55.4 (5) |
N31—C3—C4—C10 | 177.9 (3) | N31—C32—C33—C34 | −55.8 (5) |
C10—C5—C6—C7 | 1.2 (7) | C32—C33—C34—C37 | 178.6 (4) |
C5—C6—C7—C8 | −0.4 (7) | C32—C33—C34—C35 | 55.8 (5) |
C6—C7—C8—C9 | 0.0 (7) | C37—C34—C35—C36 | −178.5 (4) |
C7—C8—C9—C10 | −0.3 (6) | C33—C34—C35—C36 | −56.3 (5) |
C7—C8—C9—C1 | 179.2 (4) | C3—N31—C36—C35 | 141.7 (4) |
O1—C1—C9—C10 | 176.0 (4) | C32—N31—C36—C35 | −53.9 (5) |
C2—C1—C9—C10 | 0.2 (6) | C34—C35—C36—N31 | 54.8 (5) |
O1—C1—C9—C8 | −3.6 (6) | C35—C34—C37—O37 | 46.9 (7) |
C2—C1—C9—C8 | −179.3 (4) | C33—C34—C37—O37 | −73.8 (7) |
C8—C9—C10—C5 | 1.1 (6) | C35—C34—C37—O38 | −135.4 (5) |
C1—C9—C10—C5 | −178.4 (4) | C33—C34—C37—O38 | 103.9 (5) |
C8—C9—C10—C4 | −176.6 (4) | O37—C37—O38—C39A | 17.3 (10) |
C1—C9—C10—C4 | 3.9 (6) | C34—C37—O38—C39A | −160.5 (6) |
C6—C5—C10—C9 | −1.6 (6) | C37—O38—C39A—C40A | −117.0 (9) |
D—H···A | D—H | H···A | D···A | D—H···A |
C8—H8···O1i | 0.93 | 2.51 | 3.285 (6) | 141 |
C32—H322···O4 | 0.97 | 2.31 | 2.852 (6) | 115 |
C36—H361···Cl2 | 0.97 | 2.70 | 3.026 (5) | 100 |
Symmetry code: (i) −x+2, −y, −z. |
Experimental details
Crystal data | |
Chemical formula | C18H18ClNO4 |
Mr | 347.78 |
Crystal system, space group | Monoclinic, P21/c |
Temperature (K) | 298 |
a, b, c (Å) | 12.780 (3), 16.931 (3), 7.8532 (16) |
β (°) | 101.85 (3) |
V (Å3) | 1663.1 (6) |
Z | 4 |
Radiation type | Mo Kα |
µ (mm−1) | 0.25 |
Crystal size (mm) | 0.45 × 0.02 × 0.01 |
Data collection | |
Diffractometer | Enraf Nonius KappaCCD area-detector diffractometer |
Absorption correction | Multi-scan (SORTAV; Blessing, 1995) |
Tmin, Tmax | 0.895, 0.998 |
No. of measured, independent and observed [I > 2σ(I)] reflections | 9954, 2802, 1040 |
Rint | 0.118 |
(sin θ/λ)max (Å−1) | 0.595 |
Refinement | |
R[F2 > 2σ(F2)], wR(F2), S | 0.055, 0.154, 0.92 |
No. of reflections | 2802 |
No. of parameters | 238 |
No. of restraints | 27 |
H-atom treatment | H-atom parameters constrained |
Δρmax, Δρmin (e Å−3) | 0.19, −0.22 |
Computer programs: DENZO (Otwinowski & Minor, 1997) and COLLECT (Hooft, 1998), DENZO and COLLECT, SHELXS97 (Sheldrick, 1997), SHELXL97 (Sheldrick, 1997), SHELXL97.
D—H···A | D—H | H···A | D···A | D—H···A |
C8—H8···O1i | 0.93 | 2.51 | 3.285 (6) | 140.5 |
C32—H322···O4 | 0.97 | 2.31 | 2.852 (6) | 114.6 |
C36—H361···Cl2 | 0.97 | 2.70 | 3.026 (5) | 100.0 |
Symmetry code: (i) −x+2, −y, −z. |
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