Icacinlactone H and Icacintrichantholide from the Tuber of Icacina trichantha.
Zhao, Ming; Onakpa, Monday M.; Santarsiero, Bernard D.; Huang, Xiao-Jun; Zhang, Xiao-Qi; Chen, Jia; Cheng, Jian-Jun; Longnecker, Richard; Che, Chun-Tao; Organic letters 17 (2015) 3834–3837; doi:10.1021/acs.orglett.5b01806

data_1529874
_publ_section_title
;
 Icacinlactone H and Icacintrichantholide from the Tuber of Icacina
 trichantha.
;
_journal_issue                   15
_journal_name_full               'Organic letters'
_journal_page_first              3834
_journal_page_last               3837
_journal_paper_doi               10.1021/acs.orglett.5b01806
_journal_volume                  17
_journal_year                    2015
_chemical_formula_moiety         'C20 H18 O7'
_chemical_formula_sum            'C20 H18 O7'
_chemical_formula_weight         370.34
_chemical_name_common            Icacina9
_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'
_symmetry_space_group_name_Hall  'P 2ac 2ab'
_symmetry_space_group_name_H-M   'P 21 21 21'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2013
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   5.9680(9)
_cell_length_b                   10.5100(10)
_cell_length_c                   25.663(2)
_cell_measurement_reflns_used    27459
_cell_measurement_temperature    100.0(2)
_cell_measurement_theta_max      28.7
_cell_measurement_theta_min      1.6
_cell_volume                     1609.7(3)
_computing_data_reduction        'XDS (Kabsch)'
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_diffrn_ambient_temperature      100.0(2)
_diffrn_measured_fraction_theta_full 0.990
_diffrn_measured_fraction_theta_max 0.993
_diffrn_measurement_device_type  'MAR 300mm CCD'
_diffrn_measurement_method       'omega scans'
_diffrn_radiation_type           Synchrotron
_diffrn_radiation_wavelength     0.72925
_diffrn_reflns_av_R_equivalents  0.1355
_diffrn_reflns_av_unetI/netI     0.0749
_diffrn_reflns_Laue_measured_fraction_full 0.990
_diffrn_reflns_Laue_measured_fraction_max 0.993
_diffrn_reflns_limit_h_max       7
_diffrn_reflns_limit_h_min       -7
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       33
_diffrn_reflns_limit_l_min       -33
_diffrn_reflns_number            27458
_diffrn_reflns_point_group_measured_fraction_full 0.991
_diffrn_reflns_point_group_measured_fraction_max 0.993
_diffrn_reflns_theta_full        25.948
_diffrn_reflns_theta_max         28.684
_diffrn_reflns_theta_min         1.628
_diffrn_source                   'APS 21-ID-D'
_exptl_absorpt_coefficient_mu    0.122
_exptl_absorpt_correction_type   empirical
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.528
_exptl_crystal_description       needle
_exptl_crystal_F_000             776
_exptl_crystal_size_max          0.050
_exptl_crystal_size_mid          0.010
_exptl_crystal_size_min          0.010
_exptl_transmission_factor_max   0.999
_exptl_transmission_factor_min   0.998
_refine_diff_density_max         0.499
_refine_diff_density_min         -.399
_refine_diff_density_rms         0.087
_refine_ls_abs_structure_details
;
 Flack x determined using 1570 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons and Flack (2004), Acta Cryst. A60, s61).
;
_refine_ls_abs_structure_Flack   -.3(4)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.065
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     247
_refine_ls_number_reflns         3816
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.065
_refine_ls_R_factor_all          0.0494
_refine_ls_R_factor_gt           0.0491
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0732P)^2^+0.4523P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1243
_refine_ls_wR_factor_ref         0.1247
_reflns_Friedel_coverage         0.720
_reflns_Friedel_fraction_full    0.992
_reflns_Friedel_fraction_max     0.994
_reflns_number_gt                3764
_reflns_number_total             3816
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ol5b01806_si_003.cif
_cod_data_source_block           UIC2014Icacina9
_cod_database_code               1529874
_shelxl_version_number           2013-3
_shelx_res_checksum              56165
_shelx_hkl_checksum              37535