Amiaspochalasins A-H, Undescribed Aspochalasins with a C-21 Ester Carbonyl from Aspergillus micronesiensis.
Wu, Zhaodi; Zhang, Xiaotian; Al Anbari, Weaam Hasan; Zhang, Mi; Chen, Xia; Luo, Zengwei; Li, Xiao-Nian; Chen, Chunmei; Liu, Junjun; Wang, Jianping; Zhu, Hucheng; Zhang, Yonghui; The Journal of organic chemistry 84 (2019) 5483–5491; doi:10.1021/acs.joc.9b00440

data_4034298
_publ_section_title
;
 Amiaspochalasins A-H, Undescribed Aspochalasins with a C-21 Ester
 Carbonyl from Aspergillus micronesiensis.
;
_journal_issue                   9
_journal_name_full               'The Journal of organic chemistry'
_journal_page_first              5483
_journal_page_last               5491
_journal_paper_doi               10.1021/acs.joc.9b00440
_journal_volume                  84
_journal_year                    2019
_chemical_absolute_configuration ad
_chemical_formula_moiety         '4(C24 H35 N O4), C H4 O'
_chemical_formula_sum            'C24.25 H36 N O4.25'
_chemical_formula_weight         409.54
_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'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2014/7
_cell_angle_alpha                90
_cell_angle_beta                 108.1070(10)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   13.09160(10)
_cell_length_b                   27.1113(2)
_cell_length_c                   13.53230(10)
_cell_measurement_reflns_used    55522
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      73.55
_cell_measurement_theta_min      3.26
_cell_volume                     4565.17(6)
_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    'SHELXS-97 (Sheldrick 2008)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.987
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0418
_diffrn_reflns_av_unetI/netI     0.0256
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.987
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       33
_diffrn_reflns_limit_k_min       -33
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            85847
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.975
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         74.086
_diffrn_reflns_theta_min         3.260
_exptl_absorpt_coefficient_mu    0.643
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.745
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS, Sheldrick,2014'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.192
_exptl_crystal_description       block
_exptl_crystal_F_000             1780
_exptl_crystal_size_max          0.170
_exptl_crystal_size_mid          0.140
_exptl_crystal_size_min          0.110
_refine_diff_density_max         1.027
_refine_diff_density_min         -0.435
_refine_diff_density_rms         0.047
_refine_ls_abs_structure_details
;
 Flack x determined using 7592 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.04(4)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.032
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1282
_refine_ls_number_reflns         18096
_refine_ls_number_restraints     109
_refine_ls_restrained_S_all      1.036
_refine_ls_R_factor_all          0.0559
_refine_ls_R_factor_gt           0.0532
_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^)+(0.0809P)^2^+1.7091P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1408
_refine_ls_wR_factor_ref         0.1431
_reflns_Friedel_coverage         0.934
_reflns_Friedel_fraction_full    0.995
_reflns_Friedel_fraction_max     0.963
_reflns_number_gt                17109
_reflns_number_total             18096
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            jo9b00440_si_002.cif
_cod_data_source_block           D3-74-3
_cod_original_sg_symbol_H-M      'P 21'
_cod_database_code               4034298
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.899
_shelx_estimated_absorpt_t_max   0.933
_shelx_res_checksum              82001
_shelx_hkl_checksum              18050