Tsavoenones A-C: unprecedented polyketides with a 1,7-dioxadispiro[4.0.4.4]tetradecane core from the lichen Parmotrema tsavoense.
Duong, Thuc-Huy; Beniddir, Mehdi A.; Genta-Jouve, Grégory; Aree, Thammarat; Chollet-Krugler, Marylène; Boustie, Joël; Ferron, Solenn; Sauvager, Aurélie; Nguyen, Huu-Hung; Nguyen, Kim-Phi-Phung; Chavasiri, Warinthorn; Le Pogam, Pierre; Organic & biomolecular chemistry 16 (2018) 5913–5919; doi:10.1039/c8ob01280f

data_7156352
_publ_section_title
;
 Tsavoenones A-C: unprecedented polyketides with a
 1,7-dioxadispiro[4.0.4.4]tetradecane core from the lichen Parmotrema
 tsavoense.
;
_journal_issue                   32
_journal_name_full               'Organic &amp; biomolecular chemistry'
_journal_page_first              5913
_journal_page_last               5919
_journal_paper_doi               10.1039/c8ob01280f
_journal_volume                  16
_journal_year                    2018
_chemical_formula_moiety         'C28 H26 O11, H2 O'
_chemical_formula_sum            'C28 H28 O12'
_chemical_formula_weight         556.50
_chemical_name_common            'Tsavoenones A'
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   mixed
_audit_creation_method           SHELXL-2014/7
_audit_update_record
;
2017-07-20 deposited with the CCDC.
2018-07-31 downloaded from the CCDC.
;
_cell_angle_alpha                69.302(1)
_cell_angle_beta                 81.446(2)
_cell_angle_gamma                65.245(2)
_cell_formula_units_Z            2
_cell_length_a                   9.4743(5)
_cell_length_b                   10.9625(5)
_cell_length_c                   15.3255(7)
_cell_measurement_reflns_used    4871
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      25.16
_cell_measurement_theta_min      2.50
_cell_volume                     1352.17(12)
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_diffrn_ambient_temperature      296(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.993
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0339
_diffrn_reflns_av_unetI/netI     0.0495
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.993
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            23716
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.993
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         30.639
_diffrn_reflns_theta_min         1.420
_diffrn_source                   'sealed tube'
_exptl_absorpt_coefficient_mu    0.108
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Bruker-AXS)'
_exptl_crystal_colour            'light yellow'
_exptl_crystal_density_diffrn    1.367
_exptl_crystal_description       rod
_exptl_crystal_F_000             584
_exptl_crystal_size_max          0.300
_exptl_crystal_size_mid          0.260
_exptl_crystal_size_min          0.100
_exptl_transmission_factor_max   0.746
_exptl_transmission_factor_min   0.709
_refine_diff_density_max         0.254
_refine_diff_density_min         -0.269
_refine_diff_density_rms         0.049
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.039
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     369
_refine_ls_number_reflns         8289
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.039
_refine_ls_R_factor_all          0.1032
_refine_ls_R_factor_gt           0.0555
_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^)+(0.0760P)^2^+0.1155P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1394
_refine_ls_wR_factor_ref         0.1642
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4858
_reflns_number_total             8289
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8ob01280f2.cif
_cod_data_source_block           Tsavoenones-A
_cod_depositor_comments          'Adding full bibliography for 7156352.cif.'
_cod_original_cell_volume        1352.17(11)
_cod_database_code               7156352
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.968
_shelx_estimated_absorpt_t_max   0.989
_shelx_res_checksum              3623