Phomopsterones A and B, Two Functionalized Ergostane-Type Steroids from the Endophytic Fungus Phomopsis sp. TJ507A.
Hu, Zhengxi; Wu, Ye; Xie, Shuangshuang; Sun, Weiguang; Guo, Yi; Li, Xiao-Nian; Liu, Junjun; Li, Hua; Wang, Jianping; Luo, Zengwei; Xue, Yongbo; Zhang, Yonghui; Organic letters 19 (2017) 258–261; doi:10.1021/acs.orglett.6b03557

data_1545220
_publ_section_title
;
 Phomopsterones A and B, Two Functionalized Ergostane-Type Steroids from
 the Endophytic Fungus Phomopsis sp. TJ507A.
;
_journal_issue                   1
_journal_name_full               'Organic letters'
_journal_page_first              258
_journal_page_last               261
_journal_paper_doi               10.1021/acs.orglett.6b03557
_journal_volume                  19
_journal_year                    2017
_chemical_absolute_configuration ad
_chemical_formula_moiety         'C29 H42 O6'
_chemical_formula_sum            'C29 H42 O6'
_chemical_formula_weight         486.62
_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
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2014/7
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   6.3717(2)
_cell_length_b                   18.6450(4)
_cell_length_c                   22.0515(5)
_cell_measurement_reflns_used    8127
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      68.66
_cell_measurement_theta_min      3.10
_cell_volume                     2619.73(12)
_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-2014 (Sheldrick 2014)'
_computing_structure_solution    'SHELXS-97 (Sheldrick 2008)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.938
_diffrn_measured_fraction_theta_max 0.923
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0448
_diffrn_reflns_av_unetI/netI     0.0480
_diffrn_reflns_Laue_measured_fraction_full 0.938
_diffrn_reflns_Laue_measured_fraction_max 0.923
_diffrn_reflns_limit_h_max       6
_diffrn_reflns_limit_h_min       -7
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            13153
_diffrn_reflns_point_group_measured_fraction_full 0.901
_diffrn_reflns_point_group_measured_fraction_max 0.884
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         69.319
_diffrn_reflns_theta_min         3.104
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    0.681
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   sadabs
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.234
_exptl_crystal_description       plate
_exptl_crystal_F_000             1056
_exptl_crystal_size_max          0.500
_exptl_crystal_size_mid          0.200
_exptl_crystal_size_min          0.040
_exptl_transmission_factor_max   0.7532
_exptl_transmission_factor_min   0.4033
_refine_diff_density_max         0.234
_refine_diff_density_min         -0.332
_refine_diff_density_rms         0.055
_refine_ls_abs_structure_details
;
 Flack x determined using 1617 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.04(8)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.051
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     324
_refine_ls_number_reflns         4332
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.051
_refine_ls_R_factor_all          0.0410
_refine_ls_R_factor_gt           0.0397
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0883P)^2^+0.2716P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1193
_refine_ls_wR_factor_ref         0.1208
_reflns_Friedel_coverage         0.662
_reflns_Friedel_fraction_full    0.852
_reflns_Friedel_fraction_max     0.830
_reflns_number_gt                4177
_reflns_number_total             4332
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ol6b03557_si_002.cif
_cod_data_source_block           cu_zyh_wy3352_0m
_cod_database_code               1545220
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.727
_shelx_estimated_absorpt_t_max   0.973
_shelx_res_checksum              10234
_shelx_hkl_checksum              99844