Isolation, Structures, and Biological Activities of Triterpenoids from a Penares sp. Marine Sponge.
Kolesnikova, Sophia A.; Lyakhova, Ekaterina G.; Kalinovsky, Anatoly I.; Pushilin, Michail A.; Afiyatullov, Shamil Sh; Yurchenko, Ekaterina A.; Dyshlovoy, Sergey A.; Minh, Chau V.; Stonik, Valentin A.; Journal of natural products 76 (2013) 1746–1752; doi:10.1021/np400388x

data_1512276
_publ_section_title
;
 Isolation, Structures, and Biological Activities of Triterpenoids from a
 Penares sp. Marine Sponge.
;
_journal_issue                   9
_journal_name_full               'Journal of natural products'
_journal_page_first              1746
_journal_page_last               1752
_journal_paper_doi               10.1021/np400388x
_journal_volume                  76
_journal_year                    2013
_chemical_absolute_configuration unk
_chemical_formula_moiety         'C29 H42 O4'
_chemical_formula_sum            'C29 H42 O4'
_chemical_formula_weight         454.63
_chemical_name_systematic
;
(1R,3aS,3bS,4aS,5aS,6S,9aS,9bS,11aR)-6,9a,11a-trimethyl-1-
((R)-6-methylhept-5-en-2-yl)dodecahydro-9b,3a-
(epoxymethano)cyclopenta[7,8]phenanthro[8a,9-b]oxirene-7,13(8H)-dione
;
_space_group_IT_number           4
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      4
_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                 93.6950(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            6
_cell_length_a                   20.9983(6)
_cell_length_b                   7.8332(2)
_cell_length_c                   23.1219(9)
_cell_measurement_reflns_used    4373
_cell_measurement_temperature    140(1)
_cell_measurement_theta_max      24.30
_cell_measurement_theta_min      2.54
_cell_volume                     3795.3(2)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      140(1)
_diffrn_detector_area_resol_mean 83.33
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0276
_diffrn_reflns_av_sigmaI/netI    0.0381
_diffrn_reflns_limit_h_max       25
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_k_max       8
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            16663
_diffrn_reflns_theta_full        25.11
_diffrn_reflns_theta_max         25.11
_diffrn_reflns_theta_min         1.27
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    0.077
_exptl_absorpt_correction_T_max  0.7452
_exptl_absorpt_correction_T_min  0.6848
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS-2008/1
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.193
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             1488
_exptl_crystal_size_max          0.26
_exptl_crystal_size_mid          0.22
_exptl_crystal_size_min          0.03
_refine_diff_density_max         0.223
_refine_diff_density_min         -0.172
_refine_diff_density_rms         0.036
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0(10)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.022
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     910
_refine_ls_number_reflns         7292
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.022
_refine_ls_R_factor_all          0.0524
_refine_ls_R_factor_gt           0.0385
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0544P)^2^+0.0579P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0850
_refine_ls_wR_factor_ref         0.0908
_reflns_number_gt                6119
_reflns_number_total             7292
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            np400388x_si_001.cif
_cod_data_source_block           tb2013_01b_0m
_cod_original_sg_symbol_H-M      'P 21'
_cod_database_code               1512276