Catalytic Asymmetric Total Synthesis of (-)-Actinophyllic Acid.
Cai, Lingchao; Zhang, Kui; Kwon, Ohyun; Journal of the American Chemical Society 138 (2016) 3298–3301; doi:10.1021/jacs.6b00567

data_4130126
_publ_section_title
;
 Catalytic Asymmetric Total Synthesis of (-)-Actinophyllic Acid.
;
_journal_issue                   10
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              3298
_journal_page_last               3301
_journal_paper_doi               10.1021/jacs.6b00567
_journal_volume                  138
_journal_year                    2016
_chemical_formula_moiety         'C26 H33 N2 O7, 2(C6 H6), I'
_chemical_formula_sum            'C38 H45 I N2 O7'
_chemical_formula_weight         768.66
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_atom_sites_solution_hydrogens   mixed
_audit_creation_method           SHELXL-2014/6
_cell_angle_alpha                90
_cell_angle_beta                 113.534(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   18.3255(6)
_cell_length_b                   9.8329(3)
_cell_length_c                   21.8331(7)
_cell_measurement_reflns_used    7561
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      68.90
_cell_measurement_theta_min      4.05
_cell_volume                     3606.9(2)
_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-2014/6 (Sheldrick, 2014)'
_computing_structure_solution    'SHELXS-97 (Sheldrick 2008)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 8.3333
_diffrn_measured_fraction_theta_full 0.992
_diffrn_measured_fraction_theta_max 0.981
_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  0.0840
_diffrn_reflns_av_unetI/netI     0.0815
_diffrn_reflns_Laue_measured_fraction_full 0.992
_diffrn_reflns_Laue_measured_fraction_max 0.981
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            33867
_diffrn_reflns_point_group_measured_fraction_full 0.992
_diffrn_reflns_point_group_measured_fraction_max 0.981
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         69.163
_diffrn_reflns_theta_min         2.674
_diffrn_source                   'I\mS micro--focus source'
_exptl_absorpt_coefficient_mu    7.388
_exptl_absorpt_correction_T_max  0.75
_exptl_absorpt_correction_T_min  0.37
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS V2014/2 (Bruker AXS Inc.)'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.415
_exptl_crystal_description       platelet
_exptl_crystal_F_000             1584
_exptl_crystal_size_max          0.400
_exptl_crystal_size_mid          0.200
_exptl_crystal_size_min          0.010
_refine_diff_density_max         1.248
_refine_diff_density_min         -1.848
_refine_diff_density_rms         0.116
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.096
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     442
_refine_ls_number_reflns         6597
_refine_ls_number_restraints     48
_refine_ls_restrained_S_all      1.111
_refine_ls_R_factor_all          0.0555
_refine_ls_R_factor_gt           0.0475
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0661P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1262
_refine_ls_wR_factor_ref         0.1301
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5492
_reflns_number_total             6597
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja6b00567_si_003.cif
_cod_data_source_block           kw1501bs
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               4130126
_shelx_estimated_absorpt_t_min   0.156
_shelx_estimated_absorpt_t_max   0.930
_shelxl_version_number           2014/6
_shelx_res_checksum              52859
_shelx_hkl_checksum              52757