Gram-scale synthesis of alstoscholarinoid B <i>via</i> a bio-inspired strategy.
He, Long; Zhang, Wenting; Zhang, Xiaocheng; Wu, Xiaohui; Han, Yimeng; Yan, Jiahang; Xie, Weiqing; Organic & biomolecular chemistry 21 (2023) 9346–9355; doi:10.1039/d3ob01625k

data_7159609
_publ_section_title
;
 Gram-scale synthesis of alstoscholarinoid B <i>via</i> a bio-inspired
 strategy.
;
_journal_issue                   47
_journal_name_full               'Organic &amp; biomolecular chemistry'
_journal_page_first              9346
_journal_page_last               9355
_journal_paper_doi               10.1039/d3ob01625k
_journal_volume                  21
_journal_year                    2023
_chemical_formula_sum            'C30 H46 O4'
_chemical_formula_weight         470.67
_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   geom
_audit_update_record
;
2023-08-20 deposited with the CCDC.	2023-10-25 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 99.819(17)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   7.415(4)
_cell_length_b                   10.967(5)
_cell_length_c                   15.805(7)
_cell_measurement_temperature    296.(2)
_cell_volume                     1266.4(11)
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_temperature      296.(2)
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0609
_diffrn_reflns_av_unetI/netI     0.0747
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            16211
_diffrn_reflns_theta_full        25.03
_diffrn_reflns_theta_max         25.03
_diffrn_reflns_theta_min         2.62
_exptl_absorpt_coefficient_mu    0.080
_exptl_absorpt_correction_T_max  1.00
_exptl_absorpt_correction_T_min  0.98
_exptl_absorpt_process_details
;
;
_exptl_crystal_density_diffrn    1.234
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             516
_exptl_crystal_size_max          0.240
_exptl_crystal_size_mid          0.200
_exptl_crystal_size_min          0.022
_refine_diff_density_max         0.179
_refine_diff_density_min         -0.203
_refine_ls_abs_structure_details
;

Flack x determined using 1102 quotients [(I+)-(I-)]/[(I+)+(I-)]
(Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -1.4(7)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.997
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     315
_refine_ls_number_reflns         4442
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      0.997
_refine_ls_R_factor_all          0.0958
_refine_ls_R_factor_gt           0.0514
_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^)+(0.0604P)^2^+0.0528P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1024
_refine_ls_wR_factor_ref         0.1174
_reflns_number_gt                3071
_reflns_number_total             4442
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3ob01625k2.cif
_cod_data_source_block           xwq01
_cod_depositor_comments
'Adding full bibliography for 7159609--7159611.cif.'
_cod_original_cell_volume        1266.4(10)
_cod_database_code               7159609
_shelx_res_checksum              91706