##############################################################################
# #
# This CIF contains the data in a paper accepted for publication in #
# Acta Crystallographica Section E. It conforms to the requirements of #
# Notes for Authors for Acta Crystallographica Section E, and has been #
# peer reviewed under the auspices of the IUCr Commission on Journals. #
# #
# Full details of the Crystallographic Information File format #
# are given in the paper "The Crystallographic Information File (CIF): #
# a New Standard Archive File for Crystallography" by S. R. Hall, F. H. #
# Allen and I. D. Brown [Acta Cryst. (1991), A47, 655-685]. #
# #
# The current version of the core CIF dictionary is obtainable from #
# ftp://ftp.iucr.org/pub/cif_core.dic. #
# #
# Software is freely available for graphical display of the structure(s) #
# in this CIF. For information consult the CIF software page #
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# #
# This file may be used for bona fide research purposes within the #
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data_I
_audit_creation_method 'SHELXL-2014/7'
_journal_date_recd_electronic 2017-08-24
_journal_date_accepted 2017-09-06
_journal_name_full 'Acta Crystallographica, Section E'
_journal_year 2017
_journal_volume 73
_journal_issue 10
_journal_page_first 1475
_journal_page_last 1478
_journal_paper_category GO
_journal_paper_doi 10.1107/S2056989017012816
_journal_coeditor_code LH4023
_publ_contact_author_name 'Gumersindo Mir\'on-Lopez'
_publ_contact_author_address
;
Facultad de Qu\'imica, Universidad Aut\'onoma de Yucat\'an,
Calle 43 No. 613,
Col.
Inal\'ambrical, CP97069, M\'erida, Yucat\'an, M\'exico
;
_publ_contact_author_email gmiron@correo.uady.mx
_publ_contact_author_fax ?
_publ_contact_author_phone ?
_publ_section_title
;
Crystal structure of ochraceolide A isolated from Elaeodendron
trichotomum (Turcz.) Lundell
;
_publ_section_title_footnote .
loop_
_publ_author_name
_publ_author_footnote
_publ_author_address
'Herrera-Espa\~na, Angel D.' .
;
Facultad de Qu\'imica, Universidad Aut\'onoma de Yucat\'an, Calle 43 No. 613,
Col. Inal\'ambrica, 97069, M\'erida, Yucat\'an,
Mexico
;
'Mena-Rej\'on, Gonzalo J.' .
;
Facultad de Qu\'imica, Universidad Aut\'onoma de Yucat\'an, Calle 43 No. 613,
Col. Inal\'ambrica, 97069, M\'erida, Yucat\'an,
Mexico
;
'Hern\'andez-Ortega, Sim\'on' .
;
Instituto de Qu\'imica, Universidad Nacional Aut\'onoma de M\'exico, Circuito,
Exterior, Ciudad Universitaria, 04510, Mexico City,
Mexico
;
'Quijano, Leovigildo' .
;
Instituto de Qu\'imica, Universidad Nacional Aut\'onoma de M\'exico, Circuito,
Exterior, Ciudad Universitaria, 04510, Mexico City,
Mexico
;
'Mir\'on-L\'opez, Gumersindo' .
;
Facultad de Qu\'imica, Universidad Aut\'onoma de Yucat\'an, Calle 43 No. 613,
Col. Inal\'ambrica, 97069, M\'erida, Yucat\'an,
Mexico
;
_publ_section_synopsis
;
The crystal structure of the triterpene lactone ochraceolide A
(3-oxolup-20(29)-en-30,21\a-olide) isolated from Elaeodendron
trichotomum (Turcz.) Lundell is reported.
;
_chemical_name_systematic
;\
6aR,6
bR,8aS,9aR,12aR,14bR)-4,4,6a,6
b,8a,14b-Hexamethyl-12-methyleneicosahydro-3H-phenanthro[1',2':\
6,7]indeno[2,1-b]furan-3,11(2H)-dione
;
_chemical_name_common ?
_chemical_formula_moiety 'C30 H44 O3'
_chemical_formula_sum 'C30 H44 O3'
_chemical_formula_iupac 'C30 H44 O3'
_chemical_formula_weight 452.65
_chemical_melting_point ?
_shelx_space_group_comment
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_space_group_crystal_system orthorhombic
_space_group_name_H-M_alt 'P 21 21 21'
_space_group_name_Hall 'P 2ac 2ab'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, -y, z+1/2'
'-x, y+1/2, -z+1/2'
'x+1/2, -y+1/2, -z'
_cell_length_a 7.6131(5)
_cell_length_b 11.7216(7)
_cell_length_c 27.7076(17)
_cell_angle_alpha 90
_cell_angle_beta 90
_cell_angle_gamma 90
_cell_volume 2472.6(3)
_cell_formula_units_Z 4
_cell_measurement_reflns_used 9889
_cell_measurement_theta_min 3.19
_cell_measurement_theta_max 68.28
_cell_measurement_temperature 150(2)
_exptl_crystal_description Prism
_exptl_crystal_colour colourless
_exptl_crystal_size_max 0.359
_exptl_crystal_size_mid 0.274
_exptl_crystal_size_min 0.254
_exptl_crystal_density_diffrn 1.216
_exptl_crystal_density_meas ?
_exptl_crystal_density_method ?
_exptl_crystal_F_000 992
_exptl_absorpt_coefficient_mu 0.589
_exptl_absorpt_correction_type multi-scan
_exptl_absorpt_process_details
;
(SADABS; Krause et al., 2015)
;
_shelx_estimated_absorpt_T_min 0.817
_shelx_estimated_absorpt_T_max 0.865
_exptl_absorpt_correction_T_min 0.7834
_exptl_absorpt_correction_T_max 0.8643
_diffrn_ambient_temperature 150(2)
_diffrn_radiation_type CuK\a
_diffrn_radiation_wavelength 1.54178
_diffrn_measurement_device_type 'Bruker D8 Venture'
_diffrn_measurement_method \w-scans
_diffrn_detector_area_resol_mean 52.0833
_diffrn_reflns_number 14632
_diffrn_reflns_av_R_equivalents 0.0609
_diffrn_reflns_theta_min 3.190
_diffrn_reflns_theta_max 68.278
_diffrn_reflns_theta_full 67.679
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measured_fraction_theta_full 0.998
_diffrn_reflns_limit_h_min -9
_diffrn_reflns_limit_h_max 8
_diffrn_reflns_limit_k_min -13
_diffrn_reflns_limit_k_max 14
_diffrn_reflns_limit_l_min -33
_diffrn_reflns_limit_l_max 33
_refine_special_details ?
_reflns_number_total 4513
_reflns_number_gt 4057
_reflns_threshold_expression 'I > 2\s(I)'
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type full
_refine_ls_R_factor_all 0.0668
_refine_ls_R_factor_gt 0.0608
_refine_ls_wR_factor_gt 0.1565
_refine_ls_wR_factor_ref 0.1639
_refine_ls_goodness_of_fit_ref 1.088
_refine_ls_restrained_S_all 1.088
_refine_ls_number_reflns 4513
_refine_ls_number_parameters 304
_refine_ls_number_restraints 0
_refine_ls_hydrogen_treatment constr
_refine_ls_weighting_scheme calc
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0789P)^2^+0.8039P] where P=(Fo^2^+2Fc^2^)/3'
_atom_sites_solution_hydrogens geom
_atom_sites_solution_primary ?
_atom_sites_solution_secondary ?
_refine_ls_shift/su_max 0.000
_refine_ls_shift/su_mean 0.000
_refine_diff_density_max 0.284
_refine_diff_density_min -0.190
_refine_ls_extinction_method none
_refine_ls_extinction_coef .
_refine_ls_abs_structure_details
;
Flack x determined using 1515 quotients
[(I^+^)-(I^-^)]/[(I^+^)+(I^-^)]
(Parsons et al., 2013).
;
_refine_ls_abs_structure_Flack 0.2(3)
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
'C' 'C' 0.0181 0.0091
'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
'H' 'H' 0.0000 0.0000
'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
'O' 'O' 0.0492 0.0322
'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
_computing_data_collection
;
APEX3 (Bruker, 2014)
;
_computing_cell_refinement
;
APEX3 (Bruker, 2014)
;
_computing_data_reduction
;
SAINT (Bruker, 2014)
;
_computing_structure_solution
;
SHELXS2014 (Bruker, 2014)
;
_computing_structure_refinement
;
SHELXL2014/7 (Sheldrick, 2015)
;
_computing_molecular_graphics
;
Mercury (Macrae et al., 2006)
;
_computing_publication_material
;
PLATON (Spek, 2009) and publCIF (Westrip, 2010)
;
loop_
_atom_site_type_symbol
_atom_site_label
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_calc_flag
_atom_site_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
O O1 0.7000(9) 0.2747(4) 1.1228(2) 0.127(2) Uani d 1 . .
O O2 0.2109(5) 0.5554(3) 0.68677(10) 0.0712(10) Uani d 1 . .
O O3 0.0663(6) 0.3910(4) 0.68208(13) 0.0865(12) Uani d 1 . .
C C1 0.4287(7) 0.3773(4) 1.02722(13) 0.0568(11) Uani d 1 . .
H H1A 0.3012 0.3872 1.0216 0.068 Uiso calc 1 . .
H H1B 0.4687 0.3118 1.0075 0.068 Uiso calc 1 . .
C C2 0.4602(8) 0.3508(4) 1.08081(14) 0.0692(14) Uani d 1 . .
H H2A 0.3999 0.4094 1.1005 0.083 Uiso calc 1 . .
H H2B 0.4059 0.2762 1.0884 0.083 Uiso calc 1 . .
C C3 0.6490(8) 0.3471(4) 1.09523(16) 0.0674(14) Uani d 1 . .
C C4 0.7745(6) 0.4361(3) 1.07509(13) 0.0498(10) Uani d 1 . .
C C5 0.7231(6) 0.4658(3) 1.02182(11) 0.0415(8) Uani d 1 . .
H H5 0.7540 0.3957 1.0031 0.050 Uiso calc 1 . .
C C6 0.8379(6) 0.5589(3) 0.99999(13) 0.0482(9) Uani d 1 . .
H H6A 0.9620 0.5455 1.0091 0.058 Uiso calc 1 . .
H H6B 0.8022 0.6339 1.0131 0.058 Uiso calc 1 . .
C C7 0.8213(5) 0.5604(3) 0.94485(12) 0.0443(8) Uani d 1 . .
H H7A 0.8673 0.4876 0.9319 0.053 Uiso calc 1 . .
H H7B 0.8953 0.6228 0.9319 0.053 Uiso calc 1 . .
C C8 0.6322(5) 0.5770(3) 0.92684(11) 0.0347(7) Uani d 1 . .
C C9 0.5071(5) 0.4933(3) 0.95387(10) 0.0372(8) Uani d 1 . .
H H9 0.5416 0.4159 0.9420 0.045 Uiso calc 1 . .
C C10 0.5260(5) 0.4859(3) 1.01054(11) 0.0420(8) Uani d 1 . .
C C11 0.3177(5) 0.5085(4) 0.93680(12) 0.0460(9) Uani d 1 . .
H H11A 0.2746 0.5839 0.9478 0.055 Uiso calc 1 . .
H H11B 0.2436 0.4494 0.9522 0.055 Uiso calc 1 . .
C C12 0.2954(5) 0.5006(3) 0.88168(12) 0.0424(8) Uani d 1 . .
H H12A 0.3119 0.4204 0.8715 0.051 Uiso calc 1 . .
H H12B 0.1743 0.5235 0.8730 0.051 Uiso calc 1 . .
C C13 0.4255(5) 0.5761(3) 0.85450(11) 0.0326(7) Uani d 1 . .
H H13 0.3992 0.6569 0.8634 0.039 Uiso calc 1 . .
C C14 0.6178(4) 0.5509(3) 0.87041(11) 0.0321(7) Uani d 1 . .
C C15 0.7510(5) 0.6247(3) 0.84160(12) 0.0410(8) Uani d 1 . .
H H15A 0.7459 0.7039 0.8539 0.049 Uiso calc 1 . .
H H15B 0.8708 0.5953 0.8478 0.049 Uiso calc 1 . .
C C16 0.7197(5) 0.6269(4) 0.78673(12) 0.0457(9) Uani d 1 . .
H H16A 0.7982 0.6842 0.7718 0.055 Uiso calc 1 . .
H H16B 0.7496 0.5514 0.7730 0.055 Uiso calc 1 . .
C C17 0.5299(5) 0.6555(3) 0.77439(12) 0.0405(8) Uani d 1 . .
C C18 0.4109(4) 0.5670(3) 0.79938(11) 0.0336(7) Uani d 1 . .
H H18 0.4567 0.4900 0.7903 0.040 Uiso calc 1 . .
C C19 0.2307(5) 0.5807(3) 0.77408(12) 0.0415(8) Uani d 1 . .
H H19 0.1522 0.6334 0.7925 0.050 Uiso calc 1 . .
C C20 0.1359(5) 0.4732(3) 0.76020(13) 0.0460(9) Uani d 1 . .
C C21 0.2797(6) 0.6321(4) 0.72350(13) 0.0522(10) Uani d 1 . .
H H21 0.2275 0.7099 0.7198 0.063 Uiso calc 1 . .
C C22 0.4785(6) 0.6384(4) 0.72141(12) 0.0504(10) Uani d 1 . .
H H22A 0.5178 0.7034 0.7013 0.060 Uiso calc 1 . .
H H22B 0.5291 0.5670 0.7083 0.060 Uiso calc 1 . .
C C30 0.1290(6) 0.4657(5) 0.70646(16) 0.0625(13) Uani d 1 . .
C C29 0.0717(5) 0.3894(4) 0.78608(15) 0.0525(10) Uani d 1 . .
H H29A 0.0215 0.3248 0.7706 0.063 Uiso calc 1 . .
H H29B 0.0754 0.3932 0.8203 0.063 Uiso calc 1 . .
C C26 0.5821(6) 0.7027(3) 0.93685(12) 0.0470(9) Uani d 1 . .
H H26A 0.6189 0.7235 0.9696 0.071 Uiso calc 1 . .
H H26B 0.4546 0.7118 0.9339 0.071 Uiso calc 1 . .
H H26C 0.6411 0.7523 0.9134 0.071 Uiso calc 1 . .
C C28 0.4863(6) 0.7796(3) 0.78893(14) 0.0491(9) Uani d 1 . .
H H28A 0.5315 0.7947 0.8214 0.074 Uiso calc 1 . .
H H28B 0.3587 0.7905 0.7886 0.074 Uiso calc 1 . .
H H28C 0.5410 0.8324 0.7660 0.074 Uiso calc 1 . .
C C27 0.6651(5) 0.4251(3) 0.85928(11) 0.0382(8) Uani d 1 . .
H H27A 0.6767 0.4150 0.8243 0.057 Uiso calc 1 . .
H H27B 0.5721 0.3750 0.8715 0.057 Uiso calc 1 . .
H H27C 0.7765 0.4057 0.8750 0.057 Uiso calc 1 . .
C C25 0.4458(7) 0.5894(4) 1.03594(13) 0.0546(11) Uani d 1 . .
H H25A 0.3345 0.6096 1.0203 0.082 Uiso calc 1 . .
H H25B 0.5271 0.6540 1.0338 0.082 Uiso calc 1 . .
H H25C 0.4243 0.5709 1.0699 0.082 Uiso calc 1 . .
C C24 0.7708(7) 0.5395(4) 1.10971(13) 0.0584(12) Uani d 1 . .
H H24A 0.6501 0.5677 1.1127 0.088 Uiso calc 1 . .
H H24B 0.8460 0.6002 1.0969 0.088 Uiso calc 1 . .
H H24C 0.8140 0.5161 1.1415 0.088 Uiso calc 1 . .
C C23 0.9581(8) 0.3866(5) 1.07703(17) 0.0815(18) Uani d 1 . .
H H23A 0.9834 0.3605 1.1099 0.122 Uiso calc 1 . .
H H23B 1.0434 0.4453 1.0677 0.122 Uiso calc 1 . .
H H23C 0.9665 0.3220 1.0547 0.122 Uiso calc 1 . .
loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_12
_atom_site_aniso_U_13
_atom_site_aniso_U_23
O1 0.166(5) 0.085(3) 0.131(4) 0.003(3) -0.022(4) 0.066(3)
O2 0.079(2) 0.100(3) 0.0340(13) 0.015(2) -0.0172(15) 0.0057(15)
O3 0.090(3) 0.108(3) 0.062(2) 0.011(2) -0.0361(19) -0.023(2)
C1 0.084(3) 0.058(2) 0.0289(17) -0.010(2) 0.0078(19) 0.0033(16)
C2 0.116(4) 0.061(3) 0.0311(19) -0.014(3) 0.013(2) 0.0049(18)
C3 0.115(4) 0.041(2) 0.046(2) 0.011(2) -0.007(3) 0.0053(18)
C4 0.076(3) 0.0434(19) 0.0296(16) 0.0128(19) -0.0052(17) 0.0002(14)
C5 0.064(2) 0.0337(16) 0.0270(15) 0.0099(16) -0.0007(15) -0.0032(13)
C6 0.057(2) 0.050(2) 0.0371(18) -0.0026(18) -0.0093(17) 0.0000(15)
C7 0.050(2) 0.049(2) 0.0336(16) -0.0053(17) -0.0016(16) 0.0048(15)
C8 0.0472(19) 0.0259(14) 0.0312(15) -0.0022(13) 0.0003(14) -0.0001(12)
C9 0.050(2) 0.0376(17) 0.0242(14) -0.0016(15) 0.0050(14) -0.0011(12)
C10 0.060(2) 0.0402(18) 0.0253(14) 0.0005(17) 0.0048(15) -0.0029(13)
C11 0.045(2) 0.061(2) 0.0320(16) -0.0069(17) 0.0054(15) 0.0050(16)
C12 0.0439(19) 0.050(2) 0.0329(16) -0.0072(16) 0.0017(15) 0.0037(15)
C13 0.0406(17) 0.0297(15) 0.0274(14) 0.0047(13) 0.0028(13) 0.0006(12)
C14 0.0400(17) 0.0275(15) 0.0288(14) 0.0006(13) 0.0038(13) 0.0023(11)
C15 0.0418(19) 0.0447(18) 0.0364(17) -0.0028(15) 0.0029(14) 0.0093(14)
C16 0.047(2) 0.054(2) 0.0360(18) 0.0031(17) 0.0089(15) 0.0156(16)
C17 0.049(2) 0.0415(18) 0.0305(16) 0.0104(15) 0.0075(15) 0.0103(14)
C18 0.0394(18) 0.0333(16) 0.0280(15) 0.0087(14) -0.0002(13) 0.0013(12)
C19 0.0452(19) 0.0445(18) 0.0348(16) 0.0176(15) -0.0005(15) 0.0002(14)
C20 0.0397(19) 0.055(2) 0.0432(19) 0.0165(17) -0.0098(16) -0.0102(17)
C21 0.063(2) 0.058(2) 0.0356(18) 0.024(2) -0.0016(17) 0.0059(16)
C22 0.062(2) 0.061(2) 0.0288(17) 0.0212(19) 0.0064(16) 0.0122(16)
C30 0.057(3) 0.087(3) 0.044(2) 0.022(3) -0.021(2) -0.014(2)
C29 0.043(2) 0.060(2) 0.055(2) 0.0029(18) -0.0046(18) -0.0162(19)
C26 0.075(3) 0.0307(17) 0.0350(17) -0.0006(17) -0.0062(18) -0.0047(13)
C28 0.063(3) 0.0358(18) 0.049(2) 0.0035(17) 0.0063(19) 0.0128(16)
C27 0.052(2) 0.0354(17) 0.0271(14) 0.0116(15) -0.0014(14) 0.0004(13)
C25 0.070(3) 0.062(2) 0.0316(17) 0.020(2) 0.0030(18) -0.0088(17)
C24 0.093(3) 0.052(2) 0.0298(16) 0.011(2) -0.0087(19) -0.0049(16)
C23 0.106(4) 0.095(4) 0.044(2) 0.049(4) -0.019(3) -0.010(2)
_geom_special_details
;
All esds (except the esd in the dihedral angle between two l.s. planes)
are estimated using the full covariance matrix. The cell esds are taken
into account individually in the estimation of esds in distances, angles
and torsion angles; correlations between esds in cell parameters are only
used when they are defined by crystal symmetry. An approximate (isotropic)
treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_site_symmetry_2
_geom_bond_distance
_geom_bond_publ_flag
O1 C3 . 1.206(6) ?
O2 C30 . 1.338(7) ?
O2 C21 . 1.455(6) ?
O3 C30 . 1.205(6) ?
C1 C2 . 1.536(5) ?
C1 C10 . 1.544(6) ?
C1 H1A . 0.9900 ?
C1 H1B . 0.9900 ?
C2 C3 . 1.492(8) ?
C2 H2A . 0.9900 ?
C2 H2B . 0.9900 ?
C3 C4 . 1.521(7) ?
C4 C23 . 1.515(7) ?
C4 C24 . 1.546(5) ?
C4 C5 . 1.566(4) ?
C5 C6 . 1.523(6) ?
C5 C10 . 1.550(6) ?
C5 H5 . 1.0000 ?
C6 C7 . 1.533(5) ?
C6 H6A . 0.9900 ?
C6 H6B . 0.9900 ?
C7 C8 . 1.536(5) ?
C7 H7A . 0.9900 ?
C7 H7B . 0.9900 ?
C8 C26 . 1.546(5) ?
C8 C9 . 1.559(5) ?
C8 C14 . 1.597(4) ?
C9 C11 . 1.528(5) ?
C9 C10 . 1.579(4) ?
C9 H9 . 1.0000 ?
C10 C25 . 1.530(5) ?
C11 C12 . 1.539(4) ?
C11 H11A . 0.9900 ?
C11 H11B . 0.9900 ?
C12 C13 . 1.527(5) ?
C12 H12A . 0.9900 ?
C12 H12B . 0.9900 ?
C13 C18 . 1.535(4) ?
C13 C14 . 1.557(5) ?
C13 H13 . 1.0000 ?
C14 C27 . 1.549(4) ?
C14 C15 . 1.553(5) ?
C15 C16 . 1.539(5) ?
C15 H15A . 0.9900 ?
C15 H15B . 0.9900 ?
C16 C17 . 1.522(5) ?
C16 H16A . 0.9900 ?
C16 H16B . 0.9900 ?
C17 C22 . 1.532(5) ?
C17 C18 . 1.542(5) ?
C17 C28 . 1.545(5) ?
C18 C19 . 1.549(5) ?
C18 H18 . 1.0000 ?
C19 C20 . 1.502(6) ?
C19 C21 . 1.570(5) ?
C19 H19 . 1.0000 ?
C20 C29 . 1.311(6) ?
C20 C30 . 1.492(5) ?
C21 C22 . 1.517(6) ?
C21 H21 . 1.0000 ?
C22 H22A . 0.9900 ?
C22 H22B . 0.9900 ?
C29 H29A . 0.9500 ?
C29 H29B . 0.9500 ?
C26 H26A . 0.9800 ?
C26 H26B . 0.9800 ?
C26 H26C . 0.9800 ?
C28 H28A . 0.9800 ?
C28 H28B . 0.9800 ?
C28 H28C . 0.9800 ?
C27 H27A . 0.9800 ?
C27 H27B . 0.9800 ?
C27 H27C . 0.9800 ?
C25 H25A . 0.9800 ?
C25 H25B . 0.9800 ?
C25 H25C . 0.9800 ?
C24 H24A . 0.9800 ?
C24 H24B . 0.9800 ?
C24 H24C . 0.9800 ?
C23 H23A . 0.9800 ?
C23 H23B . 0.9800 ?
C23 H23C . 0.9800 ?
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle
_geom_angle_publ_flag
C30 O2 C21 . . 111.6(3) ?
C2 C1 C10 . . 112.4(4) ?
C2 C1 H1A . . 109.1 ?
C10 C1 H1A . . 109.1 ?
C2 C1 H1B . . 109.1 ?
C10 C1 H1B . . 109.1 ?
H1A C1 H1B . . 107.8 ?
C3 C2 C1 . . 114.5(4) ?
C3 C2 H2A . . 108.6 ?
C1 C2 H2A . . 108.6 ?
C3 C2 H2B . . 108.6 ?
C1 C2 H2B . . 108.6 ?
H2A C2 H2B . . 107.6 ?
O1 C3 C2 . . 120.0(6) ?
O1 C3 C4 . . 120.9(6) ?
C2 C3 C4 . . 119.1(4) ?
C23 C4 C3 . . 107.7(4) ?
C23 C4 C24 . . 107.2(4) ?
C3 C4 C24 . . 107.4(4) ?
C23 C4 C5 . . 110.4(3) ?
C3 C4 C5 . . 110.0(4) ?
C24 C4 C5 . . 113.9(3) ?
C6 C5 C10 . . 111.5(3) ?
C6 C5 C4 . . 113.0(3) ?
C10 C5 C4 . . 117.7(3) ?
C6 C5 H5 . . 104.3 ?
C10 C5 H5 . . 104.3 ?
C4 C5 H5 . . 104.3 ?
C5 C6 C7 . . 110.9(3) ?
C5 C6 H6A . . 109.5 ?
C7 C6 H6A . . 109.5 ?
C5 C6 H6B . . 109.5 ?
C7 C6 H6B . . 109.5 ?
H6A C6 H6B . . 108.0 ?
C6 C7 C8 . . 113.7(3) ?
C6 C7 H7A . . 108.8 ?
C8 C7 H7A . . 108.8 ?
C6 C7 H7B . . 108.8 ?
C8 C7 H7B . . 108.8 ?
H7A C7 H7B . . 107.7 ?
C7 C8 C26 . . 107.0(3) ?
C7 C8 C9 . . 109.7(3) ?
C26 C8 C9 . . 111.3(3) ?
C7 C8 C14 . . 111.0(3) ?
C26 C8 C14 . . 110.0(3) ?
C9 C8 C14 . . 107.9(2) ?
C11 C9 C8 . . 110.7(3) ?
C11 C9 C10 . . 113.6(3) ?
C8 C9 C10 . . 117.1(3) ?
C11 C9 H9 . . 104.6 ?
C8 C9 H9 . . 104.6 ?
C10 C9 H9 . . 104.6 ?
C25 C10 C1 . . 108.9(3) ?
C25 C10 C5 . . 114.5(3) ?
C1 C10 C5 . . 106.2(3) ?
C25 C10 C9 . . 112.2(3) ?
C1 C10 C9 . . 107.4(3) ?
C5 C10 C9 . . 107.3(3) ?
C9 C11 C12 . . 113.8(3) ?
C9 C11 H11A . . 108.8 ?
C12 C11 H11A . . 108.8 ?
C9 C11 H11B . . 108.8 ?
C12 C11 H11B . . 108.8 ?
H11A C11 H11B . . 107.7 ?
C13 C12 C11 . . 112.5(3) ?
C13 C12 H12A . . 109.1 ?
C11 C12 H12A . . 109.1 ?
C13 C12 H12B . . 109.1 ?
C11 C12 H12B . . 109.1 ?
H12A C12 H12B . . 107.8 ?
C12 C13 C18 . . 113.8(3) ?
C12 C13 C14 . . 111.1(3) ?
C18 C13 C14 . . 109.7(3) ?
C12 C13 H13 . . 107.3 ?
C18 C13 H13 . . 107.3 ?
C14 C13 H13 . . 107.3 ?
C27 C14 C15 . . 106.0(3) ?
C27 C14 C13 . . 110.0(3) ?
C15 C14 C13 . . 111.3(3) ?
C27 C14 C8 . . 111.2(2) ?
C15 C14 C8 . . 110.6(3) ?
C13 C14 C8 . . 107.8(2) ?
C16 C15 C14 . . 114.6(3) ?
C16 C15 H15A . . 108.6 ?
C14 C15 H15A . . 108.6 ?
C16 C15 H15B . . 108.6 ?
C14 C15 H15B . . 108.6 ?
H15A C15 H15B . . 107.6 ?
C17 C16 C15 . . 111.9(3) ?
C17 C16 H16A . . 109.2 ?
C15 C16 H16A . . 109.2 ?
C17 C16 H16B . . 109.2 ?
C15 C16 H16B . . 109.2 ?
H16A C16 H16B . . 107.9 ?
C16 C17 C22 . . 115.4(3) ?
C16 C17 C18 . . 108.0(3) ?
C22 C17 C18 . . 101.1(3) ?
C16 C17 C28 . . 110.7(4) ?
C22 C17 C28 . . 108.5(3) ?
C18 C17 C28 . . 112.9(3) ?
C13 C18 C17 . . 111.0(3) ?
C13 C18 C19 . . 120.5(3) ?
C17 C18 C19 . . 104.3(3) ?
C13 C18 H18 . . 106.8 ?
C17 C18 H18 . . 106.8 ?
C19 C18 H18 . . 106.8 ?
C20 C19 C18 . . 117.0(3) ?
C20 C19 C21 . . 101.9(3) ?
C18 C19 C21 . . 103.5(3) ?
C20 C19 H19 . . 111.2 ?
C18 C19 H19 . . 111.2 ?
C21 C19 H19 . . 111.2 ?
C29 C20 C30 . . 119.2(4) ?
C29 C20 C19 . . 131.9(3) ?
C30 C20 C19 . . 108.8(4) ?
O2 C21 C22 . . 111.3(3) ?
O2 C21 C19 . . 107.6(4) ?
C22 C21 C19 . . 106.9(3) ?
O2 C21 H21 . . 110.3 ?
C22 C21 H21 . . 110.3 ?
C19 C21 H21 . . 110.3 ?
C21 C22 C17 . . 103.0(3) ?
C21 C22 H22A . . 111.2 ?
C17 C22 H22A . . 111.2 ?
C21 C22 H22B . . 111.2 ?
C17 C22 H22B . . 111.2 ?
H22A C22 H22B . . 109.1 ?
O3 C30 O2 . . 121.8(4) ?
O3 C30 C20 . . 128.1(5) ?
O2 C30 C20 . . 110.1(4) ?
C20 C29 H29A . . 120.0 ?
C20 C29 H29B . . 120.0 ?
H29A C29 H29B . . 120.0 ?
C8 C26 H26A . . 109.5 ?
C8 C26 H26B . . 109.5 ?
H26A C26 H26B . . 109.5 ?
C8 C26 H26C . . 109.5 ?
H26A C26 H26C . . 109.5 ?
H26B C26 H26C . . 109.5 ?
C17 C28 H28A . . 109.5 ?
C17 C28 H28B . . 109.5 ?
H28A C28 H28B . . 109.5 ?
C17 C28 H28C . . 109.5 ?
H28A C28 H28C . . 109.5 ?
H28B C28 H28C . . 109.5 ?
C14 C27 H27A . . 109.5 ?
C14 C27 H27B . . 109.5 ?
H27A C27 H27B . . 109.5 ?
C14 C27 H27C . . 109.5 ?
H27A C27 H27C . . 109.5 ?
H27B C27 H27C . . 109.5 ?
C10 C25 H25A . . 109.5 ?
C10 C25 H25B . . 109.5 ?
H25A C25 H25B . . 109.5 ?
C10 C25 H25C . . 109.5 ?
H25A C25 H25C . . 109.5 ?
H25B C25 H25C . . 109.5 ?
C4 C24 H24A . . 109.5 ?
C4 C24 H24B . . 109.5 ?
H24A C24 H24B . . 109.5 ?
C4 C24 H24C . . 109.5 ?
H24A C24 H24C . . 109.5 ?
H24B C24 H24C . . 109.5 ?
C4 C23 H23A . . 109.5 ?
C4 C23 H23B . . 109.5 ?
H23A C23 H23B . . 109.5 ?
C4 C23 H23C . . 109.5 ?
H23A C23 H23C . . 109.5 ?
H23B C23 H23C . . 109.5 ?
loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion
_geom_torsion_publ_flag
C10 C1 C2 C3 . . . . -52.1(6) ?
C1 C2 C3 O1 . . . . -139.3(5) ?
C1 C2 C3 C4 . . . . 41.2(6) ?
O1 C3 C4 C23 . . . . 24.3(6) ?
C2 C3 C4 C23 . . . . -156.2(4) ?
O1 C3 C4 C24 . . . . -90.8(6) ?
C2 C3 C4 C24 . . . . 88.7(5) ?
O1 C3 C4 C5 . . . . 144.7(5) ?
C2 C3 C4 C5 . . . . -35.8(5) ?
C23 C4 C5 C6 . . . . -64.0(5) ?
C3 C4 C5 C6 . . . . 177.2(3) ?
C24 C4 C5 C6 . . . . 56.6(5) ?
C23 C4 C5 C10 . . . . 163.7(4) ?
C3 C4 C5 C10 . . . . 44.9(4) ?
C24 C4 C5 C10 . . . . -75.7(5) ?
C10 C5 C6 C7 . . . . -61.6(4) ?
C4 C5 C6 C7 . . . . 163.1(3) ?
C5 C6 C7 C8 . . . . 57.3(4) ?
C6 C7 C8 C26 . . . . 72.4(4) ?
C6 C7 C8 C9 . . . . -48.5(4) ?
C6 C7 C8 C14 . . . . -167.6(3) ?
C7 C8 C9 C11 . . . . 179.7(3) ?
C26 C8 C9 C11 . . . . 61.4(4) ?
C14 C8 C9 C11 . . . . -59.3(3) ?
C7 C8 C9 C10 . . . . 47.2(4) ?
C26 C8 C9 C10 . . . . -71.1(4) ?
C14 C8 C9 C10 . . . . 168.2(3) ?
C2 C1 C10 C25 . . . . -66.7(5) ?
C2 C1 C10 C5 . . . . 57.0(5) ?
C2 C1 C10 C9 . . . . 171.6(4) ?
C6 C5 C10 C25 . . . . -68.7(4) ?
C4 C5 C10 C25 . . . . 64.3(4) ?
C6 C5 C10 C1 . . . . 171.1(3) ?
C4 C5 C10 C1 . . . . -56.0(4) ?
C6 C5 C10 C9 . . . . 56.5(4) ?
C4 C5 C10 C9 . . . . -170.6(3) ?
C11 C9 C10 C25 . . . . -55.7(4) ?
C8 C9 C10 C25 . . . . 75.5(4) ?
C11 C9 C10 C1 . . . . 64.0(4) ?
C8 C9 C10 C1 . . . . -164.8(3) ?
C11 C9 C10 C5 . . . . 177.8(3) ?
C8 C9 C10 C5 . . . . -51.0(4) ?
C8 C9 C11 C12 . . . . 53.1(4) ?
C10 C9 C11 C12 . . . . -172.7(3) ?
C9 C11 C12 C13 . . . . -49.7(4) ?
C11 C12 C13 C18 . . . . 178.0(3) ?
C11 C12 C13 C14 . . . . 53.6(4) ?
C12 C13 C14 C27 . . . . 60.9(3) ?
C18 C13 C14 C27 . . . . -65.8(3) ?
C12 C13 C14 C15 . . . . 178.1(3) ?
C18 C13 C14 C15 . . . . 51.4(3) ?
C12 C13 C14 C8 . . . . -60.5(3) ?
C18 C13 C14 C8 . . . . 172.8(2) ?
C7 C8 C14 C27 . . . . 62.4(4) ?
C26 C8 C14 C27 . . . . -179.3(3) ?
C9 C8 C14 C27 . . . . -57.8(4) ?
C7 C8 C14 C15 . . . . -55.1(3) ?
C26 C8 C14 C15 . . . . 63.2(4) ?
C9 C8 C14 C15 . . . . -175.3(3) ?
C7 C8 C14 C13 . . . . -176.9(3) ?
C26 C8 C14 C13 . . . . -58.7(4) ?
C9 C8 C14 C13 . . . . 62.9(3) ?
C27 C14 C15 C16 . . . . 72.7(4) ?
C13 C14 C15 C16 . . . . -46.9(4) ?
C8 C14 C15 C16 . . . . -166.6(3) ?
C14 C15 C16 C17 . . . . 50.6(4) ?
C15 C16 C17 C22 . . . . -169.3(3) ?
C15 C16 C17 C18 . . . . -57.2(4) ?
C15 C16 C17 C28 . . . . 66.9(4) ?
C12 C13 C18 C17 . . . . 173.2(3) ?
C14 C13 C18 C17 . . . . -61.6(3) ?
C12 C13 C18 C19 . . . . 51.0(4) ?
C14 C13 C18 C19 . . . . 176.2(3) ?
C16 C17 C18 C13 . . . . 64.1(4) ?
C22 C17 C18 C13 . . . . -174.3(3) ?
C28 C17 C18 C13 . . . . -58.6(4) ?
C16 C17 C18 C19 . . . . -164.7(3) ?
C22 C17 C18 C19 . . . . -43.1(3) ?
C28 C17 C18 C19 . . . . 72.6(4) ?
C13 C18 C19 C20 . . . . -98.8(4) ?
C17 C18 C19 C20 . . . . 135.8(3) ?
C13 C18 C19 C21 . . . . 150.0(3) ?
C17 C18 C19 C21 . . . . 24.7(3) ?
C18 C19 C20 C29 . . . . 63.3(5) ?
C21 C19 C20 C29 . . . . 175.3(4) ?
C18 C19 C20 C30 . . . . -113.1(3) ?
C21 C19 C20 C30 . . . . -1.0(4) ?
C30 O2 C21 C22 . . . . 116.4(4) ?
C30 O2 C21 C19 . . . . -0.3(4) ?
C20 C19 C21 O2 . . . . 0.8(4) ?
C18 C19 C21 O2 . . . . 122.7(3) ?
C20 C19 C21 C22 . . . . -118.8(4) ?
C18 C19 C21 C22 . . . . 3.1(4) ?
O2 C21 C22 C17 . . . . -146.9(3) ?
C19 C21 C22 C17 . . . . -29.8(4) ?
C16 C17 C22 C21 . . . . 160.8(3) ?
C18 C17 C22 C21 . . . . 44.7(4) ?
C28 C17 C22 C21 . . . . -74.3(4) ?
C21 O2 C30 O3 . . . . -178.3(4) ?
C21 O2 C30 C20 . . . . -0.4(5) ?
C29 C20 C30 O3 . . . . 1.8(7) ?
C19 C20 C30 O3 . . . . 178.7(4) ?
C29 C20 C30 O2 . . . . -176.0(4) ?
C19 C20 C30 O2 . . . . 0.9(5) ?
loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_site_symmetry_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
C2 H2A O2 2_565 0.99 2.57 3.395(5) 141
C12 H12A O1 3_457 0.99 2.45 3.310(6) 146
C24 H24A O3 2_565 0.98 2.58 3.357(6) 137
_shelx_hkl_file
;
1 0 0 0.71465 0.23271 4
2 0 0 143.119 10.8442 4
-2 0 0 128.499 10.7930 6
3 0 0 1.91013 0.70344 4
-5 0 0 0.55362 0.73484 1
-6 0 0 20.2240 2.94540 3
-6 0 0 11.9473 3.18240 1
-7 0 0 -0.9989 1.08947 3
-8 0 0 0.76534 0.90393 3
-9 0 0 0.09866 0.59741 3
0 1 0 1.04797 0.16556 6
-1 -1 0 121.298 10.0748 4
1 1 0 130.703 10.0824 6
1 1 0 138.236 10.0841 4
-1 -1 0 116.000 10.0712 6
2 -1 0 522.030 39.3557 4
2 1 0 482.160 39.4047 4
-2 -1 0 490.344 39.4044 6
3 -1 0 1106.75 92.1963 4
3 1 0 1230.27 92.2892 4
4 -1 0 22.6217 2.53482 4
-4 -1 0 27.0190 2.80595 1
-5 -1 0 109.363 8.94508 1
5 1 0 98.6489 9.06171 4
-6 1 0 1.50632 1.27401 3
-6 -1 0 -1.5435 1.21946 3
-6 -1 0 -0.2209 0.89194 1
-7 -1 0 1.31845 1.18286 3
-7 1 0 2.82519 1.20158 3
-8 1 0 1.02340 0.96849 3
-8 -1 0 0.55413 0.94423 3
-9 -1 0 54.1984 4.46290 3
-9 1 0 50.3672 4.47484 3
1 -2 0 3816.59 294.771 4
1 2 0 3512.42 294.972 4
-1 2 0 3840.58 294.787 6
1 -2 0 3571.27 294.663 6
-1 -2 0 3833.70 295.208 6
1 2 0 3850.61 295.314 6
2 2 0 2752.42 206.421 4
2 2 0 2474.51 206.426 6
3 -2 0 1280.70 96.9649 4
3 2 0 1176.94 97.0815 4
-4 -2 0 25.7075 2.73314 1
4 -2 0 21.2444 2.50139 4
-5 -2 0 236.658 17.9802 1
5 2 0 204.257 18.1501 4
-6 -2 0 9.91276 2.68068 3
-6 -2 0 7.57666 2.72000 1
-6 2 0 8.46154 2.78988 3
-7 2 0 26.0205 3.37923 3
-7 -2 0 32.1123 3.90278 1
-7 -2 0 29.7577 3.49055 3
-8 -2 0 -1.2175 0.87660 3
-8 2 0 1.45730 1.01884 3
-9 -2 0 4.09759 1.15508 3
-9 2 0 5.74489 1.73361 3
-1 -3 0 526.904 40.6529 6
1 3 0 502.757 40.6309 6
1 3 0 462.812 40.5867 4
-1 3 0 558.157 40.5397 6
2 3 0 1625.45 129.679 4
2 3 0 1566.01 129.712 6
-2 3 0 1737.64 129.500 6
3 -3 0 60.4443 4.55571 4
3 3 0 47.9404 4.80024 4
4 3 0 344.211 26.5136 4
-4 -3 0 313.659 26.3765 1
5 3 0 87.1961 7.90118 4
-5 -3 0 79.2499 7.26298 1
-6 -3 0 0.46398 0.85358 1
-6 3 0 1.73968 1.39084 3
-6 -3 0 1.39023 1.13882 3
-7 -3 0 1.79880 1.05007 3
-7 -3 0 0.34342 0.95506 1
-7 3 0 1.77959 1.21041 3
-8 -3 0 2.05922 1.09963 3
-8 3 0 2.13682 0.87623 3
0 -4 0 1380.61 108.993 6
-1 4 0 550.593 44.5878 4
1 4 0 604.811 44.7755 6
1 -4 0 499.315 44.5857 6
-1 4 0 600.594 44.6546 6
2 -4 0 408.695 30.3566 6
2 4 0 407.688 30.6991 6
2 4 0 334.473 30.5708 4
-3 -4 0 42.8119 3.84372 1
3 4 0 33.7967 3.72772 4
-4 -4 0 35.7460 3.59795 1
4 4 0 28.2643 3.80597 4
-5 -4 0 516.460 37.7618 1
5 4 0 425.316 37.9964 4
-6 -4 0 203.796 16.5403 1
6 4 0 198.788 16.3273 7
-6 -4 0 199.069 16.2758 3
-6 4 0 199.781 16.4385 3
-6 -4 0 193.421 16.1632 5
-7 -4 0 2.51524 0.98533 3
7 4 0 2.19974 1.36697 7
-7 -4 0 2.17065 0.93280 1
-7 4 0 7.19257 2.45124 3
-8 -4 0 3.56757 1.28277 3
-8 4 0 2.79801 0.93905 3
0 5 0 -0.1895 0.41320 4
0 5 0 -0.2518 0.67194 6
1 5 0 0.46535 0.72233 6
1 -5 0 1.40189 0.66010 6
-1 5 0 1.67591 0.86165 4
1 5 0 0.61455 0.59146 4
2 5 0 381.280 33.9027 4
2 5 0 405.399 34.0567 6
-2 -5 0 489.031 33.9321 1
3 5 0 563.575 42.5021 4
-3 -5 0 493.048 42.0370 1
-4 -5 0 31.6882 3.51158 1
4 5 0 40.6975 4.35787 4
-4 5 0 22.6725 4.16638 2
-5 -5 0 572.891 45.1872 3
5 5 0 570.743 45.2388 7
-5 -5 0 550.936 45.1557 5
-5 -5 0 554.371 45.3491 1
-5 5 0 590.147 45.3624 3
6 5 0 16.8063 4.09639 7
-6 5 0 17.2867 3.76819 3
-6 -5 0 22.8987 3.00842 1
-7 -5 0 7.27803 2.63698 1
7 5 0 8.26996 2.50783 7
-7 5 0 3.05457 1.36295 3
-7 -5 0 3.13864 1.05257 3
-8 -5 0 9.24794 1.44326 3
8 5 0 9.72355 1.85452 7
0 6 0 424.983 36.1818 4
0 6 0 484.170 36.3748 6
-1 6 0 98.4528 8.43085 6
2 6 0 248.338 19.9012 4
-2 -6 0 256.760 19.7974 1
2 6 0 228.837 20.0500 6
-3 -6 0 35.5861 3.59731 1
3 6 0 32.3504 3.81974 4
-3 6 0 31.2004 4.01143 2
-4 -6 0 112.989 9.70010 1
-4 6 0 113.461 9.99846 2
-5 -6 0 640.125 48.0317 3
-5 -6 0 583.827 48.2157 1
5 6 0 637.514 48.0881 7
-5 -6 0 551.026 47.9648 5
-5 6 0 605.954 48.1704 3
6 6 0 114.784 9.95975 7
-6 -6 0 119.106 9.92502 3
-6 -6 0 118.444 10.1686 1
-6 6 0 118.267 10.1735 3
-6 -6 0 119.842 9.87075 5
7 6 0 13.6499 2.49235 7
-7 -6 0 18.2393 3.18576 1
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3 4 30 8.16940 1.42313 7
0 -5 30 15.7883 1.97718 7
0 -5 -30 16.7478 2.18076 5
0 5 30 17.4640 2.21438 5
1 -5 30 2.80474 1.26611 7
-1 -5 -30 3.50391 1.39516 5
-1 -5 30 4.21060 1.34957 7
2 -5 30 10.2841 1.55783 7
-2 -5 -30 9.70821 1.48444 5
-2 5 30 8.13494 1.51761 5
-2 -5 30 8.93099 1.61335 7
2 5 30 11.0938 1.61453 7
-2 -5 30 7.82699 1.98073 5
0 6 30 14.8049 1.91763 5
0 -6 30 13.2667 1.77371 7
0 -6 -30 15.9026 2.12185 5
-1 -6 -30 38.5497 3.53677 5
-1 6 30 38.6175 3.48022 5
1 6 30 34.1081 3.29615 5
0 0 -31 3.95398 1.58744 5
0 0 31 1.70522 0.78608 7
0 0 31 1.00786 1.19130 5
-1 0 31 13.9767 2.08970 7
-1 0 31 12.5149 2.31355 5
1 0 31 17.2039 1.98263 7
1 0 -31 15.4916 2.04980 5
-1 0 -31 10.5566 1.93360 5
2 0 31 8.40593 1.50965 7
-2 0 31 10.0050 1.68627 5
-2 0 -31 8.02476 1.43968 5
3 0 31 24.6269 2.42364 7
-3 0 31 22.3543 2.45271 5
0 1 31 7.45542 1.69847 7
0 -1 -31 4.59349 1.69980 5
0 1 -31 8.01942 1.51123 5
0 -1 31 5.27268 1.62657 7
-1 1 31 3.41208 0.91779 5
-1 1 31 4.22806 1.89749 7
1 -1 31 2.65689 0.78270 7
-1 -1 -31 1.42916 0.70809 5
-1 -1 31 5.69317 1.97820 5
-1 -1 31 4.84304 1.71026 7
-1 1 -31 1.97907 0.63725 5
1 -1 -31 6.85080 1.75793 5
1 1 31 2.63862 0.76829 7
-2 1 31 28.2113 2.76177 5
2 -1 31 26.6692 2.67738 7
-2 -1 -31 25.1427 2.64257 5
-2 -1 31 24.1981 2.77762 5
2 1 31 26.4935 2.68176 7
2 -1 -31 27.5664 2.93756 5
3 -1 31 2.32330 0.71947 7
3 1 31 3.04864 1.29683 7
-3 -1 31 4.51734 1.31997 5
0 -2 31 36.1439 3.67135 7
0 2 31 41.2168 3.78491 7
0 -2 -31 45.7754 3.88527 5
-1 2 31 19.9899 2.47114 7
1 -2 31 16.2205 2.09224 7
-1 2 31 13.5215 2.31787 5
-1 -2 -31 17.0636 2.03569 5
-1 -2 31 18.0598 2.28141 7
-1 -2 31 21.5704 2.77686 5
1 2 31 18.3272 2.25745 7
-2 2 31 34.6354 3.27934 5
2 -2 31 34.2852 3.16621 7
-2 -2 -31 31.7941 3.06416 5
2 2 31 30.1599 3.00179 7
2 -2 -31 32.2980 3.41490 5
-2 -2 31 32.1142 3.17482 5
-2 -2 31 32.7370 3.49547 7
-3 2 31 15.8110 1.86762 5
3 -2 31 19.5490 1.97197 7
-3 -2 -31 16.9353 1.84815 5
-3 -2 31 21.0245 2.22143 5
3 2 31 18.2469 2.04926 7
0 -3 31 24.5885 2.57553 7
0 3 31 28.4253 2.66091 7
0 3 31 20.8663 2.86294 5
0 -3 -31 21.6827 2.56273 5
-1 -3 -31 18.3332 2.09278 5
-1 3 31 15.6102 2.25814 5
1 -3 31 20.3486 2.11718 7
1 3 31 19.8936 2.37022 7
1 3 31 13.6519 3.72261 5
-1 -3 31 21.4924 3.27763 5
1 -3 -31 24.6663 2.56087 5
-1 -3 31 22.4057 2.38864 7
2 -3 31 11.1721 1.74081 7
-2 3 31 11.9291 1.74479 5
-2 -3 -31 14.7837 1.63505 5
2 -3 -31 16.8519 2.52860 5
2 3 31 17.3526 1.96937 7
-2 -3 31 14.7259 2.19180 7
-2 -3 31 18.1651 2.27210 5
0 -4 31 0.83887 0.66031 7
0 4 31 2.10318 0.97456 7
0 4 31 -0.3263 0.80867 5
0 -4 -31 0.70941 0.64848 5
1 -4 31 26.7824 2.67940 7
-1 -4 -31 24.6984 2.69813 5
-1 4 31 30.5514 2.77942 5
-1 -4 31 26.6939 2.61730 7
1 4 31 26.9925 2.66559 7
1 -4 -31 22.2003 2.75840 5
1 4 31 26.6691 3.07134 5
-2 -4 -31 30.8739 2.99899 5
-2 4 31 33.5604 3.02451 5
2 -4 31 34.6754 3.13150 7
-2 -4 31 32.7307 3.31596 7
-2 -4 31 36.9063 3.52018 5
2 -4 -31 42.6750 3.76584 5
2 4 31 33.9677 3.30023 7
0 -5 -31 18.2464 2.23647 5
0 5 31 14.4414 3.18193 5
0 -5 31 18.8745 1.99930 7
-1 -5 -31 0.60282 0.57028 5
-1 5 31 0.11634 0.63480 5
1 -5 31 0.63439 0.62517 7
1 5 31 -1.4590 0.88396 5
1 -5 -31 0.27102 0.79061 5
1 5 31 -0.2851 0.83993 7
0 0 32 10.4271 3.90950 5
1 0 -32 3.69340 1.49632 5
-1 0 32 2.68960 0.94554 7
1 0 32 3.05370 1.36312 7
-1 0 32 2.32258 0.86211 5
2 0 32 16.5542 1.89912 7
-2 0 32 14.7214 1.99302 5
0 1 32 1.19459 1.13835 5
0 -1 -32 0.63224 0.63239 5
0 1 32 4.17767 1.57856 7
0 -1 32 -0.9572 0.65591 7
1 -1 32 23.4441 2.43725 7
-1 -1 -32 21.8457 2.44350 5
-1 1 32 25.7790 3.22866 7
-1 1 32 24.9053 2.71927 5
-1 -1 32 25.2814 2.76012 5
1 1 32 21.4886 2.38738 7
-1 -1 32 23.2621 2.57549 7
1 -1 -32 22.0752 2.59426 5
2 -1 32 3.09729 1.24770 7
-2 1 32 1.41472 0.64513 5
-2 -1 -32 -0.1147 0.52635 5
-2 -1 32 5.40455 1.67158 5
0 -2 32 42.9380 4.05077 7
0 2 32 46.5103 4.11252 7
0 2 32 53.1448 4.32932 5
0 -2 -32 41.1651 4.13498 5
-1 -2 -32 3.11936 0.73887 5
1 -2 32 4.14473 1.30018 7
-1 2 32 4.34386 1.67689 5
-1 -2 32 4.44299 1.64310 7
-1 -2 32 8.71800 2.18848 5
1 -2 -32 5.40752 1.73604 5
1 2 32 5.45854 1.46771 7
-2 2 32 46.1059 3.76303 5
-2 -2 -32 38.7049 3.60375 5
2 -2 32 40.4759 3.67015 7
2 2 32 44.4026 4.01025 7
-2 -2 32 47.6609 4.17196 5
0 3 32 10.7251 1.82987 7
0 -3 -32 7.10810 1.59072 5
0 -3 32 6.85213 1.50717 7
0 3 32 2.75394 1.60774 5
1 -3 32 25.2247 2.47004 7
-1 -3 -32 23.8527 2.47124 5
-1 3 32 25.5839 2.60081 5
-1 -3 32 29.0845 2.80210 7
1 -3 -32 28.6646 2.97270 5
-1 -3 32 31.6119 3.31481 5
1 3 32 26.4701 2.75632 7
0 4 32 31.8189 3.32784 5
0 -4 -32 36.0524 3.64076 5
0 -4 32 36.9758 3.17817 7
0 0 33 -0.5928 0.65051 7
1 0 33 -0.1191 0.63705 7
-1 0 33 -0.3961 0.78591 5
0 -1 33 9.84950 1.77831 7
0 -1 -33 13.1422 1.69748 5
0 1 33 16.3702 2.16574 7
0 1 33 16.7062 2.48117 5
1 -1 33 15.8717 1.85207 7
-1 1 33 17.4653 2.15240 5
-1 -1 -33 18.5887 1.84053 5
1 1 33 14.3428 1.94320 7
-1 -1 33 21.8383 2.45500 5
-1 -1 33 17.1012 2.16075 7
0 2 33 15.8972 2.47143 5
0 -2 -33 13.6304 1.86783 5
0 -2 33 15.1416 1.95781 7
0 2 33 15.4932 2.03713 7
0 0 0 0.00 0.00 0
_exptl_absorpt_process_details
)
SADABS 2016/2: Krause, L., Herbst-Irmer, R., Sheldrick G.M. & Stalke D.,
J. Appl. Cryst. 48 (2015) 3-10
)
_exptl_absorpt_correction_type multi-scan
_exptl_absorpt_correction_T_max 0.8643
_exptl_absorpt_correction_T_min 0.7834
_exptl_special_details
)
The following wavelength and cell were deduced by SADABS from the
direction cosines etc. They are given here for emergency use only:
CELL 1.54184 7.611 11.733 27.701 90.018 89.994 89.981
)
;
_shelx_hkl_checksum 91552
_shelx_res_file
;
462QUL16.res created by SHELXL-2014/7
TITL 462QUL16 in P2(1)2(1)2(1)
CELL 1.54178 7.61310 11.72160 27.70760 90.0000 90.0000 90.0000
ZERR 4.00 0.00050 0.00070 0.00170 0.0000 0.0000 0.0000
LATT -1
SYMM 0.5-X, -Y, 0.5+Z
SYMM -X, 0.5+Y, 0.5-Z
SYMM 0.5+X, 0.5-Y, -Z
SFAC C H O
UNIT 120 176 12
LIST 6 ! automatically inserted. Change 6 to 4 for CHECKCIF!!
OMIT 0 2 8
OMIT 3 3 2
ACTA
L.S. 10
BOND $H
CONF
FMAP 2
PLAN 10
SIZE 0.254 0.274 0.359
TEMP -123.150
WGHT 0.078900 0.803900
FVAR 0.61107
O1 3 0.699973 0.274659 1.122806 11.00000 0.16599 0.08474 =
0.13108 0.06589 -0.02247 0.00341
O2 3 0.210871 0.555385 0.686766 11.00000 0.07938 0.10024 =
0.03402 0.00574 -0.01719 0.01495
O3 3 0.066280 0.390999 0.682081 11.00000 0.08968 0.10823 =
0.06156 -0.02308 -0.03609 0.01063
C1 1 0.428741 0.377311 1.027216 11.00000 0.08385 0.05758 =
0.02894 0.00334 0.00777 -0.01004
AFIX 23
H1A 2 0.301198 0.387208 1.021646 11.00000 -1.20000
H1B 2 0.468712 0.311778 1.007533 11.00000 -1.20000
AFIX 0
C2 1 0.460218 0.350765 1.080812 11.00000 0.11566 0.06070 =
0.03111 0.00494 0.01298 -0.01431
AFIX 23
H2A 2 0.399890 0.409369 1.100490 11.00000 -1.20000
H2B 2 0.405918 0.276154 1.088414 11.00000 -1.20000
AFIX 0
C3 1 0.649007 0.347063 1.095234 11.00000 0.11514 0.04079 =
0.04616 0.00534 -0.00675 0.01076
C4 1 0.774488 0.436058 1.075094 11.00000 0.07641 0.04342 =
0.02957 0.00025 -0.00516 0.01281
C5 1 0.723094 0.465813 1.021822 11.00000 0.06383 0.03372 =
0.02696 -0.00324 -0.00072 0.00988
AFIX 13
H5 2 0.753960 0.395708 1.003085 11.00000 -1.20000
AFIX 0
C6 1 0.837873 0.558868 0.999993 11.00000 0.05719 0.05021 =
0.03710 0.00003 -0.00930 -0.00262
AFIX 23
H6A 2 0.961954 0.545453 1.009053 11.00000 -1.20000
H6B 2 0.802192 0.633919 1.013125 11.00000 -1.20000
AFIX 0
C7 1 0.821318 0.560438 0.944850 11.00000 0.05005 0.04938 =
0.03361 0.00480 -0.00161 -0.00531
AFIX 23
H7A 2 0.867305 0.487635 0.931872 11.00000 -1.20000
H7B 2 0.895337 0.622798 0.931926 11.00000 -1.20000
AFIX 0
C8 1 0.632189 0.577024 0.926839 11.00000 0.04719 0.02587 =
0.03117 -0.00007 0.00032 -0.00219
C9 1 0.507068 0.493278 0.953870 11.00000 0.04994 0.03760 =
0.02418 -0.00111 0.00502 -0.00165
AFIX 13
H9 2 0.541608 0.415880 0.942020 11.00000 -1.20000
AFIX 0
C10 1 0.526046 0.485903 1.010541 11.00000 0.06046 0.04015 =
0.02527 -0.00285 0.00476 0.00055
C11 1 0.317691 0.508549 0.936796 11.00000 0.04485 0.06121 =
0.03197 0.00504 0.00544 -0.00693
AFIX 23
H11A 2 0.274606 0.583901 0.947767 11.00000 -1.20000
H11B 2 0.243620 0.449428 0.952188 11.00000 -1.20000
AFIX 0
C12 1 0.295379 0.500593 0.881676 11.00000 0.04388 0.05042 =
0.03287 0.00371 0.00172 -0.00716
AFIX 23
H12A 2 0.311857 0.420370 0.871461 11.00000 -1.20000
H12B 2 0.174269 0.523515 0.873001 11.00000 -1.20000
AFIX 0
C13 1 0.425489 0.576075 0.854496 11.00000 0.04063 0.02971 =
0.02743 0.00065 0.00280 0.00471
AFIX 13
H13 2 0.399232 0.656950 0.863437 11.00000 -1.20000
AFIX 0
C14 1 0.617813 0.550894 0.870409 11.00000 0.03998 0.02752 =
0.02879 0.00231 0.00382 0.00058
C15 1 0.750957 0.624660 0.841601 11.00000 0.04180 0.04473 =
0.03641 0.00931 0.00294 -0.00277
AFIX 23
H15A 2 0.745892 0.703861 0.853934 11.00000 -1.20000
H15B 2 0.870807 0.595322 0.847781 11.00000 -1.20000
AFIX 0
C16 1 0.719682 0.626859 0.786727 11.00000 0.04730 0.05393 =
0.03599 0.01559 0.00889 0.00307
AFIX 23
H16A 2 0.798221 0.684242 0.771839 11.00000 -1.20000
H16B 2 0.749638 0.551372 0.772976 11.00000 -1.20000
AFIX 0
C17 1 0.529943 0.655535 0.774387 11.00000 0.04936 0.04154 =
0.03052 0.01029 0.00749 0.01037
C18 1 0.410860 0.567029 0.799376 11.00000 0.03941 0.03326 =
0.02801 0.00127 -0.00015 0.00869
AFIX 13
H18 2 0.456713 0.490045 0.790256 11.00000 -1.20000
AFIX 0
C19 1 0.230680 0.580728 0.774085 11.00000 0.04515 0.04451 =
0.03484 0.00016 -0.00055 0.01758
AFIX 13
H19 2 0.152169 0.633391 0.792547 11.00000 -1.20000
AFIX 0
C20 1 0.135939 0.473202 0.760197 11.00000 0.03972 0.05520 =
0.04324 -0.01021 -0.00980 0.01654
C21 1 0.279661 0.632076 0.723496 11.00000 0.06291 0.05818 =
0.03564 0.00587 -0.00161 0.02425
AFIX 13
H21 2 0.227472 0.709864 0.719753 11.00000 -1.20000
AFIX 0
C22 1 0.478497 0.638447 0.721406 11.00000 0.06176 0.06062 =
0.02882 0.01224 0.00643 0.02117
AFIX 23
H22A 2 0.517803 0.703441 0.701305 11.00000 -1.20000
H22B 2 0.529144 0.567043 0.708347 11.00000 -1.20000
AFIX 0
C30 1 0.129003 0.465693 0.706462 11.00000 0.05672 0.08729 =
0.04361 -0.01395 -0.02052 0.02247
C29 1 0.071716 0.389397 0.786077 11.00000 0.04290 0.05972 =
0.05475 -0.01615 -0.00456 0.00288
AFIX 93
H29A 2 0.021504 0.324849 0.770600 11.00000 -1.20000
H29B 2 0.075383 0.393209 0.820311 11.00000 -1.20000
AFIX 0
C26 1 0.582140 0.702653 0.936854 11.00000 0.07539 0.03072 =
0.03503 -0.00469 -0.00625 -0.00060
AFIX 137
H26A 2 0.618928 0.723520 0.969578 11.00000 -1.50000
H26B 2 0.454646 0.711810 0.933887 11.00000 -1.50000
H26C 2 0.641124 0.752255 0.913445 11.00000 -1.50000
AFIX 0
C28 1 0.486289 0.779627 0.788926 11.00000 0.06254 0.03578 =
0.04891 0.01280 0.00630 0.00354
AFIX 137
H28A 2 0.531500 0.794672 0.821425 11.00000 -1.50000
H28B 2 0.358665 0.790514 0.788597 11.00000 -1.50000
H28C 2 0.541020 0.832384 0.765976 11.00000 -1.50000
AFIX 0
C27 1 0.665115 0.425105 0.859276 11.00000 0.05217 0.03539 =
0.02708 0.00040 -0.00140 0.01161
AFIX 137
H27A 2 0.676720 0.414961 0.824313 11.00000 -1.50000
H27B 2 0.572064 0.375039 0.871471 11.00000 -1.50000
H27C 2 0.776491 0.405722 0.875001 11.00000 -1.50000
AFIX 0
C25 1 0.445791 0.589411 1.035942 11.00000 0.07030 0.06188 =
0.03164 -0.00879 0.00297 0.01991
AFIX 137
H25A 2 0.334544 0.609579 1.020326 11.00000 -1.50000
H25B 2 0.527115 0.654029 1.033843 11.00000 -1.50000
H25C 2 0.424307 0.570926 1.069927 11.00000 -1.50000
AFIX 0
C24 1 0.770824 0.539482 1.109713 11.00000 0.09330 0.05204 =
0.02981 -0.00487 -0.00874 0.01110
AFIX 137
H24A 2 0.650121 0.567680 1.112676 11.00000 -1.50000
H24B 2 0.846017 0.600172 1.096870 11.00000 -1.50000
H24C 2 0.814010 0.516150 1.141537 11.00000 -1.50000
AFIX 0
C23 1 0.958131 0.386587 1.077026 11.00000 0.10565 0.09464 =
0.04424 -0.00971 -0.01935 0.04911
AFIX 137
H23A 2 0.983361 0.360482 1.109904 11.00000 -1.50000
H23B 2 1.043378 0.445263 1.067742 11.00000 -1.50000
H23C 2 0.966484 0.322004 1.054682 11.00000 -1.50000
AFIX 0
HKLF 4
REM 462QUL16 in P2(1)2(1)2(1)
REM R1 = 0.0608 for 4057 Fo > 4sig(Fo) and 0.0668 for all 4513 data
REM 304 parameters refined using 0 restraints
END
WGHT 0.0801 0.7689
REM Highest difference peak 0.284, deepest hole -0.190, 1-sigma level 0.046
Q1 1 0.6257 0.3384 1.1486 11.00000 0.05 0.28
Q2 1 0.6054 0.2362 1.1044 11.00000 0.05 0.25
Q3 1 0.4041 0.5645 0.8284 11.00000 0.05 0.22
Q4 1 0.7290 0.4573 1.0499 11.00000 0.05 0.21
Q5 1 0.6199 0.5665 0.8995 11.00000 0.05 0.20
Q6 1 0.7263 0.6209 0.8136 11.00000 0.05 0.20
Q7 1 0.7482 0.4847 1.0905 11.00000 0.05 0.20
Q8 1 0.5104 0.5478 1.0195 11.00000 0.05 0.19
Q9 1 0.8332 0.5620 0.9717 11.00000 0.05 0.19
Q10 1 -0.0045 0.3576 0.7093 11.00000 0.05 0.18
;
_shelx_res_checksum 41874