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_1542445
_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_formula_moiety         'C28 H37 N O4, 0.34(H2 O)'
_chemical_formula_sum            'C28 H37.68 N O4.34'
_chemical_formula_weight         469.60
_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                   8.8230(16)
_cell_length_b                   9.7832(15)
_cell_length_c                   28.016(5)
_cell_measurement_reflns_used    5236
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      68.82
_cell_measurement_theta_min      5.26
_cell_volume                     2418.3(7)
_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 0.959
_diffrn_measured_fraction_theta_max 0.946
_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  0.1421
_diffrn_reflns_av_unetI/netI     0.1945
_diffrn_reflns_laue_measured_fraction_full 0.959
_diffrn_reflns_laue_measured_fraction_max 0.946
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       33
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            9803
_diffrn_reflns_point_group_measured_fraction_full 0.868
_diffrn_reflns_point_group_measured_fraction_max 0.852
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         68.951
_diffrn_reflns_theta_min         4.788
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    0.701
_exptl_absorpt_correction_T_max  0.9658
_exptl_absorpt_correction_T_min  0.8173
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   sadabs
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.290
_exptl_crystal_description       sheet
_exptl_crystal_F_000             1016
_exptl_crystal_size_max          0.300
_exptl_crystal_size_mid          0.300
_exptl_crystal_size_min          0.050
_refine_diff_density_max         0.750
_refine_diff_density_min         -0.486
_refine_diff_density_rms         0.124
_refine_ls_abs_structure_details
;
 Flack x determined using 692 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.17(19)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.084
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     304
_refine_ls_number_reflns         3832
_refine_ls_number_restraints     30
_refine_ls_restrained_S_all      1.088
_refine_ls_R_factor_all          0.2088
_refine_ls_R_factor_gt           0.1134
_refine_ls_shift/su_max          0.007
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1758P)^2^+6.3102P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.3009
_refine_ls_wR_factor_ref         0.3545
_reflns_Friedel_coverage         0.569
_reflns_friedel_fraction_full    0.744
_reflns_friedel_fraction_max     0.725
_reflns_number_gt                2582
_reflns_number_total             3832
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ol6b00214_si_003.cif
_cod_data_source_block           cu_shj24_0m
_cod_depositor_comments
'Adding full bibliography for 1542445--1542446.cif.'
_cod_original_cell_volume        2418.2(7)
_cod_database_code               1542445
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.817
_shelx_estimated_absorpt_t_max   0.966
_shelx_res_checksum              26547
_shelx_hkl_checksum              3903