Pleurocins A and B: Unusual 11(9 →7)-abeo-Ergostanes and Eringiacetal B: A 13,14-seco-13,14-Epoxyergostane from Fruiting Bodies of Pleurotus eryngii and Their Inhibitory Effects on Nitric Oxide Production.
Kikuchi, Takashi; Horii, Yui; Maekawa, Yukina; Masumoto, Yuki; In, Yasuko; Tomoo, Koji; Sato, Hiroyasu; Yamano, Akihito; Yamada, Takeshi; Tanaka, Reiko; The Journal of organic chemistry 82 (2017) 10611–10616; doi:10.1021/acs.joc.7b01259

data_4032869
_publ_section_title
;
 Pleurocins A and B: Unusual 11(9 \\rightarrow 7)-abeo-Ergostanes and
 Eringiacetal B: A 13,14-seco-13,14-Epoxyergostane from Fruiting Bodies of
 Pleurotus eryngii and Their Inhibitory Effects on Nitric Oxide
 Production.
;
_journal_issue                   19
_journal_name_full               'The Journal of organic chemistry'
_journal_page_first              10611
_journal_page_last               10616
_journal_paper_doi               10.1021/acs.joc.7b01259
_journal_volume                  82
_journal_year                    2017
_chemical_absolute_configuration 'CHOOSE rm ad rmad syn or unk'
_chemical_formula_moiety         'C35 H47 Br O5'
_chemical_formula_sum            'C35 H47 Br O5'
_chemical_formula_weight         627.66
_space_group_crystal_system      monoclinic
_space_group_IT_number           4
_space_group_name_Hall           'P 2yb'
_space_group_name_H-M_alt        'P 1 21 1'
_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
_cell_angle_alpha                90.0000
_cell_angle_beta                 106.1654(4)
_cell_angle_gamma                90.0000
_cell_formula_units_Z            4
_cell_length_a                   6.01068(12)
_cell_length_b                   50.8074(9)
_cell_length_c                   10.79460(19)
_cell_measurement_reflns_used    23375
_cell_measurement_temperature    223
_cell_measurement_theta_max      77.64
_cell_measurement_theta_min      3.56
_cell_volume                     3166.19(10)
_computing_cell_refinement       'CrysAlisPro 1.171.39.7e (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.39.7e (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.39.7e (Rigaku OD, 2015)'
_computing_molecular_graphics    'CrystalStructure 4.2.1'
_computing_publication_material  'CrystalStructure 4.2.1 (Rigaku, 2015)'
_computing_structure_refinement  'SHELXL Version 2014/7 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXT Version 2014/4 (Sheldrick, 2014)'
_diffrn_ambient_temperature      223
_diffrn_detector_area_resol_mean 5.811
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.990
_diffrn_measurement_device_type  'Rigaku XtaLAB P200'
_diffrn_measurement_method       \w
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54187
_diffrn_reflns_av_R_equivalents  0.0720
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.990
_diffrn_reflns_limit_h_max       7
_diffrn_reflns_limit_h_min       -4
_diffrn_reflns_limit_k_max       63
_diffrn_reflns_limit_k_min       -63
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            30597
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.978
_diffrn_reflns_theta_full        67.687
_diffrn_reflns_theta_max         77.789
_diffrn_reflns_theta_min         3.480
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    2.086
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.317
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             1328.00
_exptl_crystal_size_max          0.389
_exptl_crystal_size_mid          0.085
_exptl_crystal_size_min          0.050
_refine_diff_density_max         2.81
_refine_diff_density_min         -0.95
_refine_ls_abs_structure_details
;
 Flack x determined using 4786 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.007(15)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.049
_refine_ls_hydrogen_treatment    constr
_refine_ls_number_parameters     741
_refine_ls_number_reflns         11753
_refine_ls_number_restraints     154
_refine_ls_R_factor_all          0.0895
_refine_ls_R_factor_gt           0.0879
_refine_ls_shift/su_max          0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w = 1/[\s^2^(Fo^2^)+(0.1397P)^2^+19.9466P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2491
_refine_ls_wR_factor_ref         0.2524
_reflns_Friedel_coverage         0.954
_reflns_Friedel_fraction_full    0.999
_reflns_Friedel_fraction_max     0.966
_reflns_number_gt                11532
_reflns_number_total             11753
_reflns_threshold_expression     F^2^>2.0\s(F^2^)
_cod_data_source_file            jo7b01259_si_002.cif
_cod_data_source_block           PE-14b
_cod_depositor_comments          'Adding full bibliography for 4032869.cif.'
_cod_database_code               4032869