Dongtingnoids A-G: Fusicoccane Diterpenoids from a Penicillium Species.
Bie, Qiong; Chen, Chunmei; Yu, Muyuan; Guo, Jieru; Wang, Jianping; Liu, Junjun; Zhou, Yuan; Zhu, Hucheng; Zhang, Yonghui; Journal of natural products 82 (2019) 80–86; doi:10.1021/acs.jnatprod.8b00694

data_1552600
_publ_section_title
;
 Dongtingnoids A-G: Fusicoccane Diterpenoids from a Penicillium Species.
;
_journal_issue                   1
_journal_name_full               'Journal of natural products'
_journal_page_first              80
_journal_page_last               86
_journal_paper_doi               10.1021/acs.jnatprod.8b00694
_journal_volume                  82
_journal_year                    2019
_chemical_absolute_configuration ad
_chemical_formula_moiety         'C29 H48 O9, 3.5(O)'
_chemical_formula_sum            'C29 H48 O12.5'
_chemical_formula_weight         596.67
_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   mixed
_audit_creation_method           SHELXL-2014/7
_cell_angle_alpha                90
_cell_angle_beta                 98.595(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   17.3169(8)
_cell_length_b                   10.1910(5)
_cell_length_c                   19.8401(8)
_cell_measurement_reflns_used    6997
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      54.11
_cell_measurement_theta_min      2.58
_cell_volume                     3462.0(3)
_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      296(2)
_diffrn_measured_fraction_theta_full 0.972
_diffrn_measured_fraction_theta_max 0.972
_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  0.0772
_diffrn_reflns_av_unetI/netI     0.0839
_diffrn_reflns_Laue_measured_fraction_full 0.972
_diffrn_reflns_Laue_measured_fraction_max 0.972
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            37471
_diffrn_reflns_point_group_measured_fraction_full 0.937
_diffrn_reflns_point_group_measured_fraction_max 0.937
_diffrn_reflns_theta_full        57.916
_diffrn_reflns_theta_max         57.916
_diffrn_reflns_theta_min         2.252
_exptl_absorpt_coefficient_mu    0.744
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.145
_exptl_crystal_description       block
_exptl_crystal_F_000             1288
_exptl_crystal_size_max          0.100
_exptl_crystal_size_mid          0.040
_exptl_crystal_size_min          0.020
_refine_diff_density_max         0.999
_refine_diff_density_min         -0.328
_refine_diff_density_rms         0.101
_refine_ls_abs_structure_details
; 
 Flack x determined using 3030 quotients [(I+)-(I-)]/[(I+)+(I-)] 
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259). 
;
_refine_ls_abs_structure_Flack   0.10(12)
_refine_ls_extinction_coef       0.0085(11)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2014/7 (Sheldrick 2014'
_refine_ls_goodness_of_fit_ref   1.069
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     838
_refine_ls_number_reflns         8999
_refine_ls_number_restraints     119
_refine_ls_restrained_S_all      1.088
_refine_ls_R_factor_all          0.0839
_refine_ls_R_factor_gt           0.0753
_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^)+(0.1586P)^2^+0.1774P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2029
_refine_ls_wR_factor_ref         0.2166
_reflns_Friedel_coverage         0.808
_reflns_Friedel_fraction_full    0.898
_reflns_Friedel_fraction_max     0.898
_reflns_number_gt                7835
_reflns_number_total             8999
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            np8b00694_si_002.cif
_cod_data_source_block           cu_180426a_0m
_cod_depositor_comments
;

2022-11-30
Z value and formula fixed to values more according to usual
chemical conventions.                 miguel
;
_cod_original_formula_sum            'C58 H96 O25'
_cod_original_formula_weight         1193.34
_cod_original_formula_moiety         '2(C29 H48 O9), 7(O)'
_cod_original_formula_units_Z            2
_cod_original_sg_symbol_H-M      'P 21'
_cod_database_code               1552600
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.929
_shelx_estimated_absorpt_t_max   0.985
_shelx_res_checksum              45555
_shelx_hkl_checksum              19092