Corymbulosins I-W, Cytotoxic Clerodane Diterpenes from the Bark of Laetia corymbulosa.
Aimaiti, Simayijiang; Suzuki, Airi; Saito, Yohei; Fukuyoshi, Shuichi; Goto, Masuo; Miyake, Katsunori; Newman, David J.; O'Keefe, Barry R; Lee, Kuo-Hsiung; Nakagawa-Goto, Kyoko; The Journal of organic chemistry 83 (2018) 951–963; doi:10.1021/acs.joc.7b02951

data_4033342
_publ_section_title
;
 Corymbulosins I-W, Cytotoxic Clerodane Diterpenes from the Bark of Laetia
 corymbulosa.
;
_journal_issue                   2
_journal_name_full               'The Journal of organic chemistry'
_journal_page_first              951
_journal_page_last               963
_journal_paper_doi               10.1021/acs.joc.7b02951
_journal_volume                  83
_journal_year                    2018
_chemical_compound_source        'Extracted from the bark of Laetia corymbulosa'
_chemical_formula_moiety         'C29 H42 O8'
_chemical_formula_sum            'C29 H42 O8'
_chemical_formula_weight         518.65
_chemical_name_systematic
18,19-di-O-acetyl-18,19-epoxy-6-hydroxy-2-(2?-methylbutanoyloxy)cleroda-3,13(16),14-triene
_space_group_crystal_system      tetragonal
_space_group_IT_number           96
_space_group_name_Hall           'P 4nw 2abw'
_space_group_name_H-M_alt        'P 43 21 2'
_symmetry_space_group_name_Hall  'P 4nw 2abw'
_symmetry_space_group_name_H-M   'P 43 21 2'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_cell_angle_alpha                90.0000
_cell_angle_beta                 90.0000
_cell_angle_gamma                90.0000
_cell_formula_units_Z            8
_cell_length_a                   10.5837(13)
_cell_length_b                   10.5837(13)
_cell_length_c                   52.904(3)
_cell_measurement_reflns_used    54742
_cell_measurement_temperature    103
_cell_measurement_theta_max      27.43
_cell_measurement_theta_min      3.00
_cell_volume                     5926.0(11)
_computing_cell_refinement       'RAPID AUTO'
_computing_data_collection       'RAPID AUTO (Rigaku, ????)'
_computing_data_reduction        'RAPID AUTO'
_computing_molecular_graphics    'CrystalStructure 4.2.2'
_computing_publication_material  'CrystalStructure 4.2.2 (Rigaku, 2016)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_solution    'SIR2011 (Burla, et al., 2012)'
_diffrn_ambient_temperature      103
_diffrn_detector_area_resol_mean 10.000
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'Rigaku R-AXIS RAPID'
_diffrn_measurement_method       \w
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71075
_diffrn_reflns_av_R_equivalents  0.0745
_diffrn_reflns_Laue_measured_fraction_full 0.000
_diffrn_reflns_Laue_measured_fraction_max 0.000
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       68
_diffrn_reflns_limit_l_min       -68
_diffrn_reflns_number            88491
_diffrn_reflns_point_group_measured_fraction_full 0.000
_diffrn_reflns_point_group_measured_fraction_max 0.000
_diffrn_reflns_theta_full        27.440
_diffrn_reflns_theta_max         27.440
_diffrn_reflns_theta_min         3.007
_diffrn_source                   'sealed X-ray tube'
_diffrn_source_type              'R-AXIS RAPID'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.084
_exptl_absorpt_correction_T_max  0.992
_exptl_absorpt_correction_T_min  0.535
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'ABSCOR (Rigaku, 1995)'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.163
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             2240.00
_exptl_crystal_size_max          0.300
_exptl_crystal_size_mid          0.200
_exptl_crystal_size_min          0.100
_refine_diff_density_max         0.52
_refine_diff_density_min         -0.32
_refine_ls_abs_structure_details
'Flack, H. D. (1983), Acta Cryst. A39, 876-881.  2747 Friedel Pairs'
_refine_ls_abs_structure_Flack   -0.1(13)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.044
_refine_ls_hydrogen_treatment    mixed
_refine_ls_number_parameters     337
_refine_ls_number_reflns         6763
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0771
_refine_ls_R_factor_gt           0.0617
_refine_ls_shift/su_max          0.050
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w = 1/[\s^2^(Fo^2^)+(0.0999P)^2^+1.8516P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1689
_refine_ls_wR_factor_ref         0.1827
_reflns_number_gt                5407
_reflns_number_total             6763
_reflns_threshold_expression     F^2^>2.0\s(F^2^)
_cod_data_source_file            jo7b02951_si_002.cif
_cod_data_source_block           bunshishouyaku1-2
_cod_depositor_comments          'Adding full bibliography for 4033342.cif.'
_cod_database_code               4033342