Pterolobirins A and B, Oxygen-Bridged Cassane Diterpenoid Dimers from the Fruits of Pterolobium macropterum
Raksat, Achara; Aree, Thammarat; Pudhom, Khanitha; Journal of Natural Products  (2020) –; doi:10.1021/acs.jnatprod.0c00354

data_1558447
_publ_section_title
;
 Pterolobirins A and B, Oxygen-Bridged Cassane Diterpenoid Dimers from the
 Fruits of Pterolobium macropterum
;
_journal_name_full               'Journal of Natural Products'
_journal_paper_doi               10.1021/acs.jnatprod.0c00354
_journal_year                    2020
_chemical_absolute_configuration ad
_chemical_formula_moiety         'C40 H56 O5'
_chemical_formula_sum            'C40 H56 O5'
_chemical_formula_weight         616.84
_chemical_name_common            'Macropterin A'
_space_group_crystal_system      orthorhombic
_space_group_IT_number           19
_space_group_name_Hall           'P 2ac 2ab'
_space_group_name_H-M_alt        'P 21 21 21'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2018/3
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   6.9234(2)
_cell_length_b                   12.1772(3)
_cell_length_c                   41.1985(9)
_cell_measurement_reflns_used    9976
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      67.88
_cell_measurement_theta_min      3.79
_cell_volume                     3473.35(15)
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_diffrn_ambient_temperature      296(2)
_diffrn_measured_fraction_theta_full 0.992
_diffrn_measured_fraction_theta_max 0.986
_diffrn_measurement_device_type  PROSPECTOR
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0386
_diffrn_reflns_av_unetI/netI     0.0375
_diffrn_reflns_Laue_measured_fraction_full 0.992
_diffrn_reflns_Laue_measured_fraction_max 0.986
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -6
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       49
_diffrn_reflns_limit_l_min       -48
_diffrn_reflns_number            21426
_diffrn_reflns_point_group_measured_fraction_full 0.982
_diffrn_reflns_point_group_measured_fraction_max 0.974
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         68.351
_diffrn_reflns_theta_min         2.145
_diffrn_source                   'microfocus I\mS'
_exptl_absorpt_coefficient_mu    0.593
_exptl_absorpt_correction_T_max  0.753
_exptl_absorpt_correction_T_min  0.594
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Bruker-AXS)'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.180
_exptl_crystal_description       rod
_exptl_crystal_F_000             1344
_exptl_crystal_size_max          0.480
_exptl_crystal_size_mid          0.400
_exptl_crystal_size_min          0.180
_refine_diff_density_max         0.143
_refine_diff_density_min         -0.206
_refine_diff_density_rms         0.047
_refine_ls_abs_structure_details
;
 Flack x determined using 2314 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.02(7)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.045
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     413
_refine_ls_number_reflns         6216
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.045
_refine_ls_R_factor_all          0.0435
_refine_ls_R_factor_gt           0.0418
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0487P)^2^+0.6900P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1054
_refine_ls_wR_factor_ref         0.1066
_reflns_Friedel_coverage         0.717
_reflns_Friedel_fraction_full    0.968
_reflns_Friedel_fraction_max     0.957
_reflns_number_gt                5920
_reflns_number_total             6216
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            np0c00354_si_002.cif
_cod_data_source_block           pf2b
_cod_database_code               1558447
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_min   0.764
_shelx_estimated_absorpt_t_max   0.901
_shelx_res_checksum              24030
_shelx_hkl_checksum              93962