Asymmetric total synthesis of (+)-xestoquinone and (+)-adociaquinones A and B
Lu, Xiao-Long; Qiu, Yuanyou; Yang, Baochao; He, Haibing; Gao, Shuanhu; Chemical Science 12 (2021) 4747–4752; doi:10.1039/D0SC07089K

data_1560502
_publ_section_title
;
 Asymmetric total synthesis of (+)-xestoquinone and (+)-adociaquinones A
 and B
;
_journal_issue                   13
_journal_name_full               'Chemical Science'
_journal_page_first              4747
_journal_page_last               4752
_journal_paper_doi               10.1039/D0SC07089K
_journal_volume                  12
_journal_year                    2021
_chemical_formula_sum            'C22 H20 O4'
_chemical_formula_weight         348.38
_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'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2017/1
_audit_update_record
;
2020-12-27 deposited with the CCDC.	2021-02-19 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   8.97980(10)
_cell_length_b                   11.03890(10)
_cell_length_c                   17.28090(10)
_cell_measurement_temperature    293(2)
_cell_volume                     1713.01(3)
_computing_structure_refinement  'SHELXL-2017/1 (Sheldrick, 2017)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.993
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0369
_diffrn_reflns_av_unetI/netI     0.0129
_diffrn_reflns_Laue_measured_fraction_full 0.993
_diffrn_reflns_Laue_measured_fraction_max 0.993
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            37913
_diffrn_reflns_point_group_measured_fraction_full 0.995
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_theta_full        67.033
_diffrn_reflns_theta_max         67.033
_diffrn_reflns_theta_min         4.754
_exptl_absorpt_coefficient_mu    0.749
_exptl_crystal_density_diffrn    1.351
_exptl_crystal_F_000             736
_exptl_crystal_size_max          0.420
_exptl_crystal_size_mid          0.260
_exptl_crystal_size_min          0.220
_refine_diff_density_max         0.131
_refine_diff_density_min         -0.190
_refine_diff_density_rms         0.030
_refine_ls_abs_structure_details
;
 Flack x determined using 1259 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.02(4)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.092
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     238
_refine_ls_number_reflns         3043
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.092
_refine_ls_R_factor_all          0.0248
_refine_ls_R_factor_gt           0.0246
_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^)+(0.0345P)^2^+0.3111P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0640
_refine_ls_wR_factor_ref         0.0641
_reflns_Friedel_coverage         0.734
_reflns_Friedel_fraction_full    0.998
_reflns_Friedel_fraction_max     0.998
_reflns_number_gt                3023
_reflns_number_total             3043
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0sc07089k2.cif
_cod_data_source_block           exp_1183
_cod_depositor_comments
'Adding full bibliography for 1560502--1560504.cif.'
_cod_database_code               1560502
_shelx_shelxl_version_number     2017/1
_shelx_estimated_absorpt_t_min   0.744
_shelx_estimated_absorpt_t_max   0.853
_shelx_res_checksum              91957
_shelx_hkl_checksum              13092