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The structure of the title methanol complex (P\bar 1, Z = 2) has been determined and compared with that of the title ethanol complex (C2/c, Z = 8) using published data. Both complexes have layer structures, the (essentially planar) layers being constructed from rings of six TMA molecules, hydrogen bonded through four `carboxyl dimers' and two `interrupted dimers', where methanol (ethanol) is included in the R^4_4(12) (graph set) ring. The packing of the layers differs in the two complexes, leading to different three-dimensional structures. In the methanol complex, one pyrene molecule is located within the layer and the other, at a centre of symmetry, between the layers in one type of interlayer space, while the methyls of methanol protrude into the other type of interlayer space. In the ethanol complex, the superpositioning of the layers is such that two types of stack are formed; one of these is mixed, containing pyrene and one of the independent TMA molecules in alternating sequence, while the other stack contains only the second type of TMA. Spectroscopic study is needed to establish whether the partial mixed stack arrangement in the crystalline ethanol complex implies donor-acceptor interaction.

Supporting information

cif

Crystallographic Information File (CIF) https://doi.org/10.1107/S0108768101010527/bk0091sup1.cif
Contains datablock tmapyr

hkl

Structure factor file (CIF format) https://doi.org/10.1107/S0108768101010527/bk0091tmapyrsup2.hkl
Contains datablock tmapyr

CCDC reference: 174976

Computing details top

Data collection: Nonius (1997), KappaCCD Collect Program; cell refinement: DENZO-SMN (Otwinowski & Minor 1997); data reduction: HKL DENZO and SCALEPACK (Otwinowski & Minor 1997); program(s) used to solve structure: SHELXS97 (Sheldrick, 1990); program(s) used to refine structure: SHELXL97 (Sheldrick, 1997); molecular graphics: Molecular Structure Corporation (1999). ORTEP. TEXRAY Structure Analysis Package. MSC, 3200 Research Forest Drive, The Woodlands,TX 77381, USA.; software used to prepare material for publication: SHELXL97 (Sheldrick, 1997), CrystalMaker (Palmer, 1999).

Figures top
[Figure 1]
[Figure 2]
[Figure 3]
[Figure 4]
[Figure 5]
(tmapyr) top
Crystal data top
C44H35O14Z = 2
Mr = 787.72F(000) = 822
Triclinic, P1Dx = 1.393 Mg m3
a = 9.5330 (5) ÅMo Kα radiation, λ = 0.71070 Å
b = 13.5400 (7) ÅCell parameters from 7840 reflections
c = 14.6440 (9) Åθ = 2.0–25.0°
α = 93.880 (2)°µ = 0.11 mm1
β = 95.020 (2)°T = 293 K
γ = 90.140 (3)°Prism, brown
V = 1878.57 (18) Å30.35 × 0.30 × 0.25 mm
Data collection top
KappaCCD
diffractometer
3827 reflections with I > 2σ(I)
Radiation source: fine-focus sealed tubeRint = 0.000
Graphite monochromatorθmax = 25.0°, θmin = 1.4°
CCD scansh = 011
6639 measured reflectionsk = 1616
6639 independent reflectionsl = 1717
Refinement top
Refinement on F2Secondary atom site location: difference Fourier map
Least-squares matrix: fullHydrogen site location: inferred from neighbouring sites
R[F2 > 2σ(F2)] = 0.058H atoms treated by a mixture of independent and constrained refinement
wR(F2) = 0.141 w = 1/[σ2(Fo2) + (0.058P)2 + 0.2978P]
where P = (Fo2 + 2Fc2)/3
S = 1.02(Δ/σ)max = 0.005
6639 reflectionsΔρmax = 0.24 e Å3
655 parametersΔρmin = 0.17 e Å3
0 restraintsExtinction correction: SHELXL, Fc*=kFc[1+0.001xFc2λ3/sin(2θ)]-1/4
Primary atom site location: structure-invariant direct methodsExtinction coefficient: 0.018 (3)
Crystal data top
C44H35O14γ = 90.140 (3)°
Mr = 787.72V = 1878.57 (18) Å3
Triclinic, P1Z = 2
a = 9.5330 (5) ÅMo Kα radiation
b = 13.5400 (7) ŵ = 0.11 mm1
c = 14.6440 (9) ÅT = 293 K
α = 93.880 (2)°0.35 × 0.30 × 0.25 mm
β = 95.020 (2)°
Data collection top
KappaCCD
diffractometer
3827 reflections with I > 2σ(I)
6639 measured reflectionsRint = 0.000
6639 independent reflections
Refinement top
R[F2 > 2σ(F2)] = 0.0580 restraints
wR(F2) = 0.141H atoms treated by a mixture of independent and constrained refinement
S = 1.02Δρmax = 0.24 e Å3
6639 reflectionsΔρmin = 0.17 e Å3
655 parameters
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
xyzUiso*/Ueq
C10.4224 (2)0.91240 (17)0.24107 (16)0.0450 (6)
C20.3746 (3)0.94852 (18)0.32396 (18)0.0478 (6)
C30.4265 (2)1.03779 (17)0.36599 (16)0.0443 (6)
C40.5248 (2)1.09116 (18)0.32459 (18)0.0468 (6)
C50.5716 (2)1.05629 (17)0.24158 (17)0.0458 (6)
C60.5208 (3)0.96617 (18)0.19998 (19)0.0483 (6)
C70.3674 (3)0.81756 (18)0.19504 (19)0.0524 (7)
C80.3794 (3)1.07867 (18)0.45520 (18)0.0500 (6)
C90.6729 (2)1.11616 (17)0.19628 (18)0.0484 (6)
O100.4170 (2)0.78509 (13)0.12282 (14)0.0722 (6)
O110.2711 (2)0.77369 (14)0.23194 (14)0.0729 (6)
O120.2810 (2)1.02586 (14)0.48618 (14)0.0685 (6)
O130.4304 (2)1.15272 (14)0.49533 (13)0.0705 (6)
O140.71991 (19)1.19484 (13)0.23637 (13)0.0642 (5)
O150.70589 (19)1.08326 (14)0.11754 (14)0.0684 (6)
C160.1915 (2)0.46915 (16)0.03896 (16)0.0437 (6)
C170.0898 (2)0.41711 (17)0.07887 (18)0.0439 (6)
C180.0374 (2)0.32817 (16)0.03695 (16)0.0437 (6)
C190.0879 (3)0.29080 (19)0.04426 (18)0.0482 (6)
C200.1905 (2)0.34239 (17)0.08451 (17)0.0470 (6)
C210.2418 (3)0.43170 (18)0.04320 (17)0.0481 (6)
C220.2436 (3)0.56566 (17)0.08294 (18)0.0477 (6)
C230.0711 (2)0.27235 (17)0.07904 (18)0.0482 (6)
C240.2423 (3)0.29838 (19)0.17123 (19)0.0543 (7)
O250.3396 (2)0.61008 (14)0.04615 (14)0.0746 (6)
O260.19201 (19)0.60031 (13)0.15391 (13)0.0623 (5)
O270.1129 (2)0.30864 (13)0.15392 (14)0.0641 (5)
O280.1180 (2)0.19280 (13)0.03883 (13)0.0681 (6)
O290.2051 (2)0.21756 (15)0.20487 (14)0.0822 (7)
O300.3321 (2)0.35434 (14)0.20649 (14)0.0709 (6)
C310.3055 (4)0.1082 (3)0.0585 (2)0.0851 (10)
C320.3880 (4)0.1884 (3)0.0657 (2)0.0834 (11)
C330.3848 (3)0.2630 (2)0.1395 (2)0.0659 (8)
C340.4688 (4)0.3483 (3)0.1483 (3)0.0891 (11)
C350.4582 (4)0.4168 (3)0.2189 (4)0.0974 (13)
C360.3650 (4)0.4057 (3)0.2838 (3)0.0853 (11)
C370.2783 (3)0.3210 (2)0.2804 (2)0.0611 (7)
C380.1803 (4)0.3051 (3)0.3458 (2)0.0744 (9)
C390.1004 (3)0.2242 (3)0.3398 (2)0.0718 (9)
C400.1074 (3)0.1491 (2)0.2663 (2)0.0592 (7)
C410.0245 (3)0.0639 (3)0.2594 (3)0.0832 (11)
C420.0320 (4)0.0041 (3)0.1868 (4)0.0980 (13)
C430.1213 (4)0.0080 (2)0.1208 (3)0.0881 (11)
C440.2095 (3)0.0917 (2)0.1249 (2)0.0659 (8)
C450.2025 (3)0.16312 (18)0.19952 (17)0.0482 (6)
C460.2882 (3)0.24936 (19)0.20683 (18)0.0506 (6)
C470.7631 (4)0.3628 (3)0.4108 (4)0.0855 (11)
C480.8687 (3)0.4360 (2)0.4134 (2)0.0632 (8)
C490.9461 (2)0.46348 (18)0.49768 (19)0.0513 (6)
C500.9164 (3)0.4182 (2)0.5787 (2)0.0655 (8)
C510.8089 (4)0.3467 (3)0.5717 (4)0.0936 (12)
C520.7353 (4)0.3198 (3)0.4893 (4)0.1012 (14)
C530.9017 (4)0.4835 (3)0.3339 (3)0.0789 (10)
C540.9974 (4)0.4486 (3)0.6624 (3)0.0792 (10)
O550.8316 (2)0.89668 (16)0.37023 (16)0.0750 (6)
C560.9601 (6)0.8527 (5)0.4014 (4)0.1114 (15)
O570.5858 (3)0.7016 (2)0.36560 (17)0.0946 (8)
C580.6061 (6)0.6252 (3)0.4244 (3)0.1074 (13)
H58A0.70050.62850.45330.30 (4)*
H58B0.59120.56270.38990.21 (2)*
H58C0.54060.63170.47060.22 (3)*
H20.302 (3)0.9097 (19)0.3514 (18)0.065 (8)*
H40.559 (3)1.155 (2)0.3513 (18)0.070 (8)*
H60.554 (2)0.9401 (17)0.1421 (18)0.056 (7)*
H110.236 (4)0.704 (3)0.193 (3)0.159 (16)*
H120.248 (3)1.056 (2)0.540 (2)0.093 (11)*
H150.787 (4)1.133 (3)0.085 (3)0.159 (16)*
H170.056 (2)0.4431 (16)0.1357 (16)0.043 (6)*
H190.058 (3)0.2310 (19)0.0719 (18)0.061 (8)*
H210.313 (2)0.4710 (16)0.0716 (16)0.049 (6)*
H250.380 (4)0.685 (3)0.084 (3)0.152 (15)*
H270.184 (5)0.255 (4)0.192 (3)0.189 (19)*
H300.369 (4)0.325 (3)0.259 (3)0.116 (13)*
H310.313 (4)0.053 (3)0.002 (3)0.140 (14)*
H320.450 (3)0.195 (2)0.022 (2)0.078 (9)*
H340.534 (4)0.360 (3)0.099 (3)0.113 (12)*
H350.517 (4)0.480 (3)0.224 (3)0.126 (13)*
H360.351 (3)0.450 (3)0.334 (2)0.096 (12)*
H380.172 (3)0.360 (2)0.397 (2)0.106 (11)*
H390.034 (3)0.211 (2)0.385 (2)0.107 (11)*
H410.040 (4)0.051 (2)0.307 (3)0.110 (12)*
H420.028 (4)0.068 (3)0.184 (3)0.123 (13)*
H430.133 (3)0.036 (3)0.070 (2)0.096 (11)*
H470.713 (4)0.348 (3)0.352 (3)0.117 (14)*
H510.789 (4)0.314 (3)0.628 (3)0.128 (14)*
H520.652 (4)0.265 (3)0.488 (3)0.151 (15)*
H530.847 (3)0.460 (2)0.276 (2)0.092 (11)*
H540.977 (3)0.416 (2)0.717 (2)0.099 (11)*
H550.787 (5)0.863 (4)0.312 (4)0.18 (2)*
H56A1.012 (5)0.840 (4)0.356 (4)0.17 (2)*
H56B0.938 (6)0.788 (5)0.425 (4)0.22 (3)*
H56C1.008 (7)0.891 (5)0.452 (5)0.24 (3)*
H570.594 (5)0.758 (4)0.403 (3)0.153 (18)*
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
C10.0526 (14)0.0406 (13)0.0418 (15)0.0113 (11)0.0102 (12)0.0043 (11)
C20.0535 (15)0.0436 (14)0.0471 (16)0.0100 (12)0.0139 (12)0.0022 (12)
C30.0492 (14)0.0410 (13)0.0427 (15)0.0038 (11)0.0086 (11)0.0035 (11)
C40.0493 (14)0.0393 (14)0.0517 (17)0.0083 (12)0.0083 (12)0.0027 (12)
C50.0481 (14)0.0407 (13)0.0491 (16)0.0077 (11)0.0110 (12)0.0020 (12)
C60.0548 (15)0.0443 (14)0.0465 (16)0.0122 (12)0.0155 (13)0.0056 (12)
C70.0628 (16)0.0454 (14)0.0502 (17)0.0192 (13)0.0173 (14)0.0020 (13)
C80.0572 (15)0.0431 (14)0.0501 (17)0.0035 (13)0.0125 (13)0.0032 (13)
C90.0494 (14)0.0416 (14)0.0546 (18)0.0114 (12)0.0142 (13)0.0063 (13)
O100.0922 (14)0.0616 (12)0.0640 (13)0.0361 (10)0.0377 (11)0.0240 (10)
O110.0982 (15)0.0569 (11)0.0662 (14)0.0397 (11)0.0367 (12)0.0141 (10)
O120.0833 (13)0.0672 (12)0.0570 (13)0.0223 (10)0.0322 (11)0.0139 (10)
O130.0851 (13)0.0612 (12)0.0651 (13)0.0198 (10)0.0260 (11)0.0218 (10)
O140.0691 (12)0.0487 (10)0.0753 (14)0.0252 (9)0.0253 (10)0.0159 (9)
O150.0749 (12)0.0677 (12)0.0641 (14)0.0311 (10)0.0319 (10)0.0164 (10)
C160.0525 (14)0.0368 (13)0.0417 (15)0.0095 (11)0.0040 (12)0.0026 (11)
C170.0498 (14)0.0391 (13)0.0430 (16)0.0066 (11)0.0068 (12)0.0005 (12)
C180.0487 (14)0.0388 (13)0.0428 (15)0.0083 (11)0.0027 (11)0.0006 (11)
C190.0578 (16)0.0376 (14)0.0481 (17)0.0105 (12)0.0030 (13)0.0020 (12)
C200.0544 (15)0.0427 (14)0.0434 (16)0.0112 (12)0.0061 (12)0.0019 (12)
C210.0574 (15)0.0441 (14)0.0432 (16)0.0111 (12)0.0090 (13)0.0011 (12)
C220.0548 (15)0.0411 (13)0.0472 (16)0.0130 (12)0.0087 (13)0.0018 (12)
C230.0524 (14)0.0421 (14)0.0498 (17)0.0149 (12)0.0078 (13)0.0026 (13)
C240.0601 (16)0.0525 (16)0.0499 (17)0.0125 (13)0.0097 (13)0.0064 (13)
O250.0998 (15)0.0601 (12)0.0660 (14)0.0446 (11)0.0378 (11)0.0184 (10)
O260.0785 (12)0.0514 (11)0.0582 (12)0.0219 (9)0.0268 (10)0.0149 (9)
O270.0789 (12)0.0519 (11)0.0632 (13)0.0224 (9)0.0274 (10)0.0093 (9)
O280.0823 (13)0.0553 (11)0.0673 (13)0.0333 (10)0.0248 (10)0.0148 (10)
O290.1092 (16)0.0673 (13)0.0703 (15)0.0345 (12)0.0352 (12)0.0286 (11)
O300.0929 (14)0.0602 (12)0.0623 (14)0.0254 (11)0.0354 (12)0.0122 (10)
C310.108 (3)0.091 (3)0.059 (2)0.024 (2)0.018 (2)0.003 (2)
C320.087 (2)0.107 (3)0.063 (2)0.026 (2)0.035 (2)0.023 (2)
C330.0597 (17)0.074 (2)0.068 (2)0.0035 (15)0.0112 (15)0.0273 (17)
C340.069 (2)0.096 (3)0.107 (3)0.009 (2)0.006 (2)0.044 (3)
C350.079 (3)0.082 (3)0.130 (4)0.027 (2)0.016 (3)0.033 (3)
C360.092 (3)0.066 (2)0.091 (3)0.004 (2)0.023 (2)0.004 (2)
C370.0608 (17)0.0546 (17)0.065 (2)0.0019 (14)0.0112 (15)0.0014 (15)
C380.082 (2)0.085 (2)0.053 (2)0.020 (2)0.0050 (17)0.0094 (18)
C390.071 (2)0.091 (3)0.058 (2)0.0123 (19)0.0197 (17)0.0154 (19)
C400.0570 (16)0.0605 (17)0.063 (2)0.0010 (14)0.0085 (14)0.0177 (15)
C410.067 (2)0.079 (3)0.107 (3)0.0076 (18)0.011 (2)0.033 (2)
C420.085 (3)0.072 (3)0.136 (4)0.018 (2)0.003 (3)0.017 (3)
C430.109 (3)0.053 (2)0.096 (3)0.001 (2)0.011 (2)0.015 (2)
C440.079 (2)0.0565 (17)0.061 (2)0.0092 (15)0.0005 (16)0.0024 (15)
C450.0539 (15)0.0465 (14)0.0451 (16)0.0031 (12)0.0049 (12)0.0079 (12)
C460.0530 (15)0.0509 (15)0.0488 (17)0.0040 (12)0.0032 (12)0.0113 (13)
C470.069 (2)0.080 (2)0.102 (3)0.0017 (19)0.006 (2)0.035 (2)
C480.0599 (17)0.0583 (17)0.070 (2)0.0032 (14)0.0102 (16)0.0122 (16)
C490.0542 (15)0.0478 (14)0.0524 (17)0.0013 (11)0.0172 (13)0.0086 (13)
C500.0724 (19)0.0557 (17)0.072 (2)0.0017 (15)0.0310 (17)0.0005 (15)
C510.104 (3)0.069 (2)0.116 (4)0.012 (2)0.058 (3)0.008 (2)
C520.088 (3)0.080 (3)0.137 (4)0.024 (2)0.042 (3)0.026 (3)
C530.087 (2)0.089 (3)0.058 (2)0.017 (2)0.001 (2)0.015 (2)
C540.106 (3)0.080 (2)0.057 (2)0.015 (2)0.029 (2)0.010 (2)
O550.0800 (15)0.0840 (15)0.0612 (14)0.0085 (12)0.0255 (12)0.0170 (12)
C560.115 (4)0.135 (4)0.086 (3)0.027 (3)0.017 (3)0.006 (3)
O570.143 (2)0.0753 (16)0.0687 (17)0.0128 (15)0.0480 (15)0.0187 (14)
C580.152 (4)0.084 (3)0.088 (3)0.024 (2)0.028 (3)0.004 (2)
Geometric parameters (Å, º) top
C1—C61.388 (3)C31—C441.420 (4)
C1—C21.392 (3)C32—C331.430 (5)
C1—C71.482 (3)C33—C341.396 (5)
C2—C31.388 (3)C33—C461.427 (4)
C3—C41.387 (3)C34—C351.353 (6)
C3—C81.490 (3)C35—C361.372 (6)
C4—C51.385 (3)C36—C371.407 (4)
C5—C61.393 (3)C37—C461.410 (4)
C5—C91.487 (3)C37—C381.421 (4)
C7—O101.249 (3)C38—C391.326 (4)
C7—O111.271 (3)C39—C401.436 (4)
C8—O131.206 (3)C40—C411.390 (4)
C8—O121.308 (3)C40—C451.412 (3)
C9—O141.244 (3)C41—C421.365 (5)
C9—O151.274 (3)C42—C431.360 (5)
C16—C171.389 (3)C43—C441.405 (5)
C16—C211.398 (3)C44—C451.415 (4)
C16—C221.482 (3)C45—C461.416 (3)
C17—C181.386 (3)C47—C521.368 (6)
C18—C191.387 (3)C47—C481.407 (4)
C18—C231.480 (3)C48—C491.408 (4)
C19—C201.395 (3)C48—C531.425 (5)
C20—C211.383 (3)C49—C49i1.419 (5)
C20—C241.490 (3)C49—C501.422 (4)
C22—O261.252 (3)C50—C511.400 (5)
C22—O251.272 (3)C50—C541.426 (5)
C23—O281.254 (3)C51—C521.369 (6)
C23—O271.268 (3)C53—C54i1.324 (5)
C24—O291.209 (3)C54—C53i1.324 (5)
C24—O301.304 (3)O55—C561.416 (5)
C31—C321.333 (5)O57—C581.394 (4)
C6—C1—C2120.0 (2)C32—C31—C44121.3 (3)
C6—C1—C7119.4 (2)C31—C32—C33122.5 (3)
C2—C1—C7120.7 (2)C34—C33—C46118.6 (3)
C3—C2—C1120.0 (2)C34—C33—C32123.8 (3)
C4—C3—C2119.7 (2)C46—C33—C32117.6 (3)
C4—C3—C8118.5 (2)C35—C34—C33120.6 (4)
C2—C3—C8121.8 (2)C34—C35—C36121.7 (4)
C5—C4—C3120.6 (2)C35—C36—C37121.0 (4)
C4—C5—C6119.6 (2)C36—C37—C46117.7 (3)
C4—C5—C9120.0 (2)C36—C37—C38123.6 (3)
C6—C5—C9120.4 (2)C46—C37—C38118.7 (3)
C1—C6—C5120.0 (2)C39—C38—C37121.5 (3)
O10—C7—O11123.6 (2)C38—C39—C40121.7 (3)
O10—C7—C1119.0 (2)C41—C40—C45119.6 (3)
O11—C7—C1117.4 (2)C41—C40—C39122.2 (3)
O13—C8—O12123.7 (2)C45—C40—C39118.2 (3)
O13—C8—C3122.4 (2)C42—C41—C40120.0 (4)
O12—C8—C3113.9 (2)C43—C42—C41121.7 (4)
O14—C9—O15123.8 (2)C42—C43—C44120.9 (4)
O14—C9—C5119.0 (2)C43—C44—C45118.1 (3)
O15—C9—C5117.3 (2)C43—C44—C31123.5 (3)
C17—C16—C21120.1 (2)C45—C44—C31118.4 (3)
C17—C16—C22119.5 (2)C40—C45—C44119.7 (3)
C21—C16—C22120.4 (2)C40—C45—C46119.7 (2)
C18—C17—C16120.0 (2)C44—C45—C46120.6 (2)
C17—C18—C19119.8 (2)C37—C46—C45120.1 (2)
C17—C18—C23120.3 (2)C37—C46—C33120.4 (3)
C19—C18—C23119.9 (2)C45—C46—C33119.6 (3)
C18—C19—C20120.5 (2)C52—C47—C48120.4 (4)
C21—C20—C19119.7 (2)C47—C48—C49119.0 (3)
C21—C20—C24122.0 (2)C47—C48—C53122.8 (4)
C19—C20—C24118.3 (2)C49—C48—C53118.2 (3)
C20—C21—C16119.9 (2)C48—C49—C49i120.3 (3)
O26—C22—O25122.7 (2)C48—C49—C50120.1 (3)
O26—C22—C16119.4 (2)C49i—C49—C50119.6 (3)
O25—C22—C16117.9 (2)C51—C50—C49118.1 (3)
O28—C23—O27123.4 (2)C51—C50—C54123.9 (4)
O28—C23—C18118.8 (2)C49—C50—C54118.0 (3)
O27—C23—C18117.8 (2)C52—C51—C50121.3 (4)
O29—C24—O30123.4 (2)C47—C52—C51121.1 (4)
O29—C24—C20122.6 (2)C54i—C53—C48121.9 (4)
O30—C24—C20114.0 (2)C53i—C54—C50122.0 (3)
Symmetry code: (i) x+2, y+1, z+1.

Experimental details

Crystal data
Chemical formulaC44H35O14
Mr787.72
Crystal system, space groupTriclinic, P1
Temperature (K)293
a, b, c (Å)9.5330 (5), 13.5400 (7), 14.6440 (9)
α, β, γ (°)93.880 (2), 95.020 (2), 90.140 (3)
V3)1878.57 (18)
Z2
Radiation typeMo Kα
µ (mm1)0.11
Crystal size (mm)0.35 × 0.30 × 0.25
Data collection
DiffractometerKappaCCD
diffractometer
Absorption correction
No. of measured, independent and
observed [I > 2σ(I)] reflections
6639, 6639, 3827
Rint0.000
(sin θ/λ)max1)0.596
Refinement
R[F2 > 2σ(F2)], wR(F2), S 0.058, 0.141, 1.02
No. of reflections6639
No. of parameters655
H-atom treatmentH atoms treated by a mixture of independent and constrained refinement
Δρmax, Δρmin (e Å3)0.24, 0.17

Computer programs: Nonius (1997), KappaCCD Collect Program, DENZO-SMN (Otwinowski & Minor 1997), HKL DENZO and SCALEPACK (Otwinowski & Minor 1997), SHELXS97 (Sheldrick, 1990), Molecular Structure Corporation (1999). ORTEP. TEXRAY Structure Analysis Package. MSC, 3200 Research Forest Drive, The Woodlands,TX 77381, USA., SHELXL97 (Sheldrick, 1997), CrystalMaker (Palmer, 1999).

 

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