Dioxasampsones A and B, two polycyclic polyprenylated acylphloroglucinols with unusual epoxy-ring-fused skeleton from Hypericum sampsonii.
Tian, Wen-Jing; Qiu, Yu-Qin; Yao, Xiao-Jun; Chen, Hai-Feng; Dai, Yi; Zhang, Xiao-Kun; Yao, Xin-Sheng; Organic letters 16 (2014) 6346–6349; doi:10.1021/ol503122m

data_1518385
_publ_section_title
;
 Dioxasampsones A and B, two polycyclic polyprenylated acylphloroglucinols
 with unusual epoxy-ring-fused skeleton from Hypericum sampsonii.
;
_journal_issue                   24
_journal_name_full               'Organic letters'
_journal_page_first              6346
_journal_page_last               6349
_journal_paper_doi               10.1021/ol503122m
_journal_volume                  16
_journal_year                    2014
_chemical_formula_sum            'C33 H42 O6'
_chemical_formula_weight         534.66
_space_group_IT_number           4
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  'P 2yb'
_symmetry_space_group_name_H-M   'P 1 21 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 103.862(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   7.6950(2)
_cell_length_b                   20.3926(4)
_cell_length_c                   9.0759(2)
_cell_measurement_reflns_used    5516
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      62.3730
_cell_measurement_theta_min      5.0080
_cell_volume                     1382.72(6)
_computing_data_reduction        'Bruker SAINT'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 0.989
_diffrn_measured_fraction_theta_max 0.990
_diffrn_measurement_device_type  'Xcalibur, Sapphire3, Gemini ultra'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0239
_diffrn_reflns_av_sigmaI/netI    0.0339
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       10
_diffrn_reflns_limit_l_min       -9
_diffrn_reflns_number            8144
_diffrn_reflns_theta_full        62.45
_diffrn_reflns_theta_max         62.45
_diffrn_reflns_theta_min         5.02
_diffrn_standards_number         8211
_exptl_absorpt_coefficient_mu    0.697
_exptl_absorpt_correction_T_max  0.9336
_exptl_absorpt_correction_T_min  0.8182
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.284
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             576
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.145
_refine_diff_density_min         -0.183
_refine_diff_density_rms         0.037
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.04(13)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.797
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     353
_refine_ls_number_reflns         4311
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      0.796
_refine_ls_R_factor_all          0.0319
_refine_ls_R_factor_gt           0.0306
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1000P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0898
_refine_ls_wR_factor_ref         0.0928
_reflns_number_gt                4175
_reflns_number_total             4311
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ol503122m_si_002.cif
_cod_data_source_block           1
_cod_depositor_comments
;
          Adding full bibliography for 1518385.cif.

2019-03-17
Wrong Z value fixed.                 miguel
;
_cod_original_cell_volume        1382.72(5)
_cod_original_sg_symbol_H-M      P21
_cod_original_formula_units_Z    6
_cod_database_code               1518385