Phomopchalasins A and B, Two Cytochalasans with Polycyclic-Fused Skeletons from the Endophytic Fungus Phomopsis sp. shj2.
Yan, Bing-Chao; Wang, Wei-Guang; Hu, Dong-Bao; Sun, Xiang; Kong, Ling-Mei; Li, Xiao-Nian; Du, Xue; Luo, Shi-Hong; Liu, Yan; Li, Yan; Sun, Han-Dong; Pu, Jian-Xin; Organic letters 18 (2016) 1108–; doi:10.1021/acs.orglett.6b00214

data_1542446
_publ_section_title
;
 Phomopchalasins A and B, Two Cytochalasans with Polycyclic-Fused
 Skeletons from the Endophytic Fungus Phomopsis sp. shj2.
;
_journal_issue                   5
_journal_name_full               'Organic letters'
_journal_page_first              1108
_journal_paper_doi               10.1021/acs.orglett.6b00214
_journal_volume                  18
_journal_year                    2016
_chemical_absolute_configuration ad
_chemical_formula_moiety         'C30 H39 N O6, C H4 O'
_chemical_formula_sum            'C31 H43 N O7'
_chemical_formula_weight         541.66
_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
_audit_creation_method           SHELXL-2014/7
_cell_angle_alpha                90
_cell_angle_beta                 102.0990(10)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   9.7486(2)
_cell_length_b                   14.4556(3)
_cell_length_c                   10.3782(2)
_cell_measurement_reflns_used    7322
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      68.79
_cell_measurement_theta_min      4.36
_cell_volume                     1430.03(5)
_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-2014/7 (Sheldrick, 2014)'
_computing_structure_solution    'SHELXL-2014/7 (Sheldrick, 2014)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.911
_diffrn_measured_fraction_theta_max 0.895
_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  0.0638
_diffrn_reflns_av_unetI/netI     0.0767
_diffrn_reflns_Laue_measured_fraction_full 0.911
_diffrn_reflns_Laue_measured_fraction_max 0.895
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            11710
_diffrn_reflns_point_group_measured_fraction_full 0.853
_diffrn_reflns_point_group_measured_fraction_max 0.833
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         69.435
_diffrn_reflns_theta_min         4.639
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    0.716
_exptl_absorpt_correction_T_max  0.9789
_exptl_absorpt_correction_T_min  0.4683
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   sadabs
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.258
_exptl_crystal_description       sheet
_exptl_crystal_F_000             584
_exptl_crystal_size_max          1.250
_exptl_crystal_size_mid          0.150
_exptl_crystal_size_min          0.030
_refine_diff_density_max         0.402
_refine_diff_density_min         -0.406
_refine_diff_density_rms         0.094
_refine_ls_abs_structure_details
;
 Flack x determined using 1395 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.15(9)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.176
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     361
_refine_ls_number_reflns         4470
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.175
_refine_ls_R_factor_all          0.0888
_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^)+(0.0961P)^2^+0.5343P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1459
_refine_ls_wR_factor_ref         0.1718
_reflns_Friedel_coverage         0.785
_reflns_Friedel_fraction_full    0.790
_reflns_Friedel_fraction_max     0.765
_reflns_number_gt                3664
_reflns_number_total             4470
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ol6b00214_si_004.cif
_cod_data_source_block           cu_shj12_0m
_cod_depositor_comments
'Adding full bibliography for 1542445--1542446.cif.'
_cod_database_code               1542446
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.468
_shelx_estimated_absorpt_t_max   0.979
_shelx_res_checksum              28499
_shelx_hkl_checksum              19552