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_4130127
_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 H30 N2 O7'
_chemical_formula_sum            'C26 H30 N2 O7'
_chemical_formula_weight         482.52
_space_group_crystal_system      triclinic
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_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2014/6
_cell_angle_alpha                94.3941(8)
_cell_angle_beta                 97.2458(8)
_cell_angle_gamma                92.0699(8)
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_cell_length_b                   11.1546(2)
_cell_length_c                   11.7517(2)
_cell_measurement_reflns_used    9933
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      68.19
_cell_measurement_theta_min      3.80
_cell_volume                     1189.11(4)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
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_computing_publication_material  'Bruker SHELXTL'
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_computing_structure_solution    'SHELXS-97 (Sheldrick 2008)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 8.3333
_diffrn_measured_fraction_theta_full 0.953
_diffrn_measured_fraction_theta_max 0.951
_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  0.0291
_diffrn_reflns_av_unetI/netI     0.0217
_diffrn_reflns_Laue_measured_fraction_full 0.953
_diffrn_reflns_Laue_measured_fraction_max 0.951
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -11
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_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            21270
_diffrn_reflns_point_group_measured_fraction_full 0.953
_diffrn_reflns_point_group_measured_fraction_max 0.951
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         68.214
_diffrn_reflns_theta_min         3.804
_diffrn_source                   'I\mS micro--focus source'
_exptl_absorpt_coefficient_mu    0.813
_exptl_absorpt_correction_T_max  0.75
_exptl_absorpt_correction_T_min  0.67
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS V2014/2 (Bruker AXS Inc.)'
_exptl_crystal_colour            colorless
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_exptl_crystal_description       block
_exptl_crystal_F_000             512
_exptl_crystal_size_max          0.400
_exptl_crystal_size_mid          0.360
_exptl_crystal_size_min          0.240
_refine_diff_density_max         0.246
_refine_diff_density_min         -0.225
_refine_diff_density_rms         0.040
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.040
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     320
_refine_ls_number_reflns         4131
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.040
_refine_ls_R_factor_all          0.0392
_refine_ls_R_factor_gt           0.0349
_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^)+(0.0403P)^2^+0.5000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0845
_refine_ls_wR_factor_ref         0.0874
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_reflns_number_gt                3711
_reflns_number_total             4131
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja6b00567_si_002.cif
_cod_data_source_block           kw1408s
_cod_database_code               4130127
_shelx_estimated_absorpt_t_min   0.737
_shelx_estimated_absorpt_t_max   0.829
_shelxl_version_number           2014/6
_shelx_res_checksum              68459
_shelx_hkl_checksum              4508